# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound-1_JL9-10D _database_code_depnum_ccdc_archive 'CCDC 903260' #TrackingRef 'compound 1-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Sn9 Se20,4(C8 H15 N2)' _chemical_formula_sum 'C32 H60 N8 Se20 Sn9' _chemical_formula_weight 3204.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 18.652(6) _cell_length_b 20.353(6) _cell_length_c 20.196(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.244(6) _cell_angle_gamma 90.00 _cell_volume 7397(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5960 _cell_measurement_theta_min 2.2574 _cell_measurement_theta_max 27.4719 _exptl_crystal_description lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5752 _exptl_absorpt_coefficient_mu 12.856 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3122 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 17403 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57208 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16902 _reflns_number_gt 12076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0600P)^2^+15.0000P] 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 16902 _refine_ls_number_parameters 690 _refine_ls_number_restraints 1076 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.58682(3) 0.28806(3) 0.30626(3) 0.03129(15) Uani 1 1 d . . . Sn2 Sn 0.74429(3) 0.19935(3) 0.42624(3) 0.03170(15) Uani 1 1 d . . . Sn3 Sn 0.43231(4) 0.19821(4) 0.18864(3) 0.03665(16) Uani 1 1 d . . . Sn4 Sn 0.37953(4) 0.28356(4) 0.34792(3) 0.03774(16) Uani 1 1 d U . . Sn5 Sn 0.33853(4) 0.30194(4) 0.51525(3) 0.03692(16) Uani 1 1 d . . . Sn6 Sn 0.18411(3) 0.31885(4) 0.35356(3) 0.03638(16) Uani 1 1 d . . . Sn7 Sn 0.98995(3) 0.18314(3) 0.76215(3) 0.03329(15) Uani 1 1 d . . . Sn8 Sn 0.79287(3) 0.21907(3) 0.76455(3) 0.03499(16) Uani 1 1 d U . . Sn9 Sn 0.83921(3) 0.19935(4) 0.59908(3) 0.03486(15) Uani 1 1 d U . . Se1 Se 0.60924(6) 0.22416(6) 0.41712(6) 0.0443(3) Uani 1 1 d . . . Se2 Se 0.70176(6) 0.35490(5) 0.31791(6) 0.0439(3) Uani 1 1 d . . . Se3 Se 0.47021(5) 0.35403(5) 0.28796(6) 0.0422(2) Uani 1 1 d . . . Se4 Se 0.57030(6) 0.21255(6) 0.20369(6) 0.0492(3) Uani 1 1 d . . . Se5 Se 0.40257(6) 0.17151(5) 0.30062(5) 0.0436(3) Uani 1 1 d . . . Se6 Se 0.44811(6) 0.32613(6) 0.46545(5) 0.0455(3) Uani 1 1 d . . . Se7 Se 0.28692(5) 0.21580(5) 0.41199(5) 0.0367(2) Uani 1 1 d U . . Se8 Se 0.26978(6) 0.34867(6) 0.27811(6) 0.0518(3) Uani 1 1 d . . . Se9 Se 0.21843(6) 0.36630(6) 0.47456(6) 0.0491(3) Uani 1 1 d . . . Se10 Se 0.39052(6) 0.39810(5) 0.61274(6) 0.0488(3) Uani 1 1 d . . . Se11 Se 0.35658(6) 0.21500(5) 0.61084(5) 0.0449(3) Uani 1 1 d . . . Se12 Se 0.08795(5) 0.22860(5) 0.30924(6) 0.0428(2) Uani 1 1 d . . . Se13 Se 0.08459(5) 0.41008(5) 0.30952(6) 0.0448(3) Uani 1 1 d . . . Se14 Se 0.95822(6) 0.13350(6) 0.64083(5) 0.0456(3) Uani 1 1 d . . . Se15 Se 0.90074(5) 0.15177(6) 0.83434(5) 0.0432(3) Uani 1 1 d . . . Se16 Se 0.89056(5) 0.28502(5) 0.70341(5) 0.0339(2) Uani 1 1 d U . . Se17 Se 0.72729(6) 0.17882(7) 0.64548(6) 0.0529(3) Uani 1 1 d . . . Se18 Se 0.77203(6) 0.33016(5) 0.81438(5) 0.0382(2) Uani 1 1 d . . . Se19 Se 0.78055(6) 0.10238(5) 0.50278(5) 0.0428(2) Uani 1 1 d U . . Se20 Se 0.82845(6) 0.28280(5) 0.50159(5) 0.0396(2) Uani 1 1 d . . . N1 N 1.1089(8) 0.1348(7) 0.4823(7) 0.094(3) Uani 1 1 d U . . N2 N 1.0310(7) 0.0772(6) 0.4061(7) 0.085(3) Uani 1 1 d U . . C1 C 1.1458(11) 0.0792(9) 0.4667(10) 0.107(4) Uani 1 1 d U . . H1A H 1.1950 0.0685 0.4874 0.128 Uiso 1 1 calc R . . C2 C 1.1003(10) 0.0443(9) 0.4183(10) 0.101(4) Uani 1 1 d U . . H2A H 1.1113 0.0065 0.3970 0.122 Uiso 1 1 calc R . . C3 C 1.0385(9) 0.1296(8) 0.4433(9) 0.082(3) Uani 1 1 d U . . C4 C 1.1418(11) 0.1855(9) 0.5349(11) 0.124(6) Uani 1 1 d U . . H4A H 1.1028 0.2074 0.5493 0.186 Uiso 1 1 calc R . . H4B H 1.1687 0.2171 0.5155 0.186 Uiso 1 1 calc R . . H4C H 1.1750 0.1648 0.5737 0.186 Uiso 1 1 calc R . . C5 C 0.9810(9) 0.1800(8) 0.4448(9) 0.095(5) Uani 1 1 d U . . H5A H 0.9413 0.1769 0.4036 0.143 Uiso 1 1 calc R . . H5B H 1.0028 0.2230 0.4480 0.143 Uiso 1 1 calc R . . H5C H 0.9619 0.1724 0.4839 0.143 Uiso 1 1 calc R . . C6 C 0.9612(9) 0.0508(9) 0.3572(9) 0.098(4) Uani 1 1 d U . . H6A H 0.9734 0.0237 0.3222 0.118 Uiso 1 1 calc R . . H6B H 0.9295 0.0866 0.3350 0.118 Uiso 1 1 calc R . . C7 C 0.9216(10) 0.0093(9) 0.4018(10) 0.111(4) Uani 1 1 d U . . H7A H 0.9550 -0.0240 0.4270 0.134 Uiso 1 1 calc R . . H7B H 0.9061 0.0373 0.4344 0.134 Uiso 1 1 calc R . . C8 C 0.8568(11) -0.0215(11) 0.3547(10) 0.133(6) Uani 1 1 d U . . H8A H 0.8393 -0.0569 0.3778 0.200 Uiso 1 1 calc R . . H8B H 0.8706 -0.0383 0.3154 0.200 Uiso 1 1 calc R . . H8C H 0.8180 0.0105 0.3402 0.200 Uiso 1 1 calc R . . N3 N 0.8354(12) 0.5611(11) 0.2776(11) 0.160(5) Uani 1 1 d U . . N4 N 0.9293(12) 0.6136(11) 0.3434(11) 0.148(4) Uani 1 1 d DU . . C9 C 0.8995(12) 0.5237(11) 0.2779(12) 0.164(5) Uani 1 1 d DU . . H9A H 0.9021 0.4843 0.2553 0.196 Uiso 1 1 calc R . . C10 C 0.9610(15) 0.5615(13) 0.3220(13) 0.155(5) Uani 1 1 d U . . H10A H 1.0114 0.5514 0.3327 0.187 Uiso 1 1 calc R . . C11 C 0.8562(15) 0.6115(11) 0.3227(13) 0.146(4) Uani 1 1 d DU . . C12 C 0.7794(12) 0.5361(14) 0.2176(14) 0.198(9) Uani 1 1 d DU . . H12A H 0.8036 0.5203 0.1841 0.296 Uiso 1 1 calc R . . H12B H 0.7456 0.5707 0.1979 0.296 Uiso 1 1 calc R . . H12C H 0.7525 0.5007 0.2314 0.296 Uiso 1 1 calc R . . C13 C 0.8013(12) 0.6644(11) 0.3228(12) 0.139(6) Uani 1 1 d U . . H13A H 0.8270 0.7037 0.3421 0.209 Uiso 1 1 calc R . . H13B H 0.7686 0.6509 0.3499 0.209 Uiso 1 1 calc R . . H13C H 0.7729 0.6729 0.2766 0.209 Uiso 1 1 calc R . . C14 C 0.9662(15) 0.6648(12) 0.3871(12) 0.165(5) Uani 1 1 d DU . . H14A H 0.9442 0.7070 0.3710 0.198 Uiso 1 1 calc R . . H14B H 1.0184 0.6660 0.3878 0.198 Uiso 1 1 calc R . . C15 C 0.9579(16) 0.6509(13) 0.4569(13) 0.176(6) Uani 1 1 d DU . . H15A H 0.9071 0.6610 0.4567 0.211 Uiso 1 1 calc R . . H15B H 0.9896 0.6815 0.4883 0.211 Uiso 1 1 calc R . . C16 C 0.9757(16) 0.5800(13) 0.4879(14) 0.204(9) Uani 1 1 d DU . . H16A H 0.9698 0.5792 0.5337 0.306 Uiso 1 1 calc R . . H16B H 1.0259 0.5686 0.4889 0.306 Uiso 1 1 calc R . . H16C H 0.9422 0.5490 0.4600 0.306 Uiso 1 1 calc R . . N5A N 0.5195(11) -0.0944(9) 0.4556(11) 0.070(2) Uani 0.640(11) 1 d PU A 1 N6A N 0.5560(10) -0.0066(9) 0.4193(9) 0.072(2) Uani 0.640(11) 1 d PDU A 1 C17A C 0.5833(13) -0.0721(11) 0.5038(12) 0.071(3) Uani 0.640(11) 1 d PU A 1 H17A H 0.6063 -0.0938 0.5444 0.085 Uiso 0.640(11) 1 calc PR A 1 C18A C 0.6062(13) -0.0159(12) 0.4836(10) 0.075(3) Uani 0.640(11) 1 d PDU A 1 H18A H 0.6456 0.0106 0.5062 0.090 Uiso 0.640(11) 1 calc PR A 1 C19A C 0.5051(12) -0.0553(13) 0.4083(11) 0.071(2) Uani 0.640(11) 1 d PDU A 1 C20A C 0.4729(14) -0.1542(12) 0.4545(13) 0.077(4) Uani 0.640(11) 1 d PU A 1 H20A H 0.4571 -0.1710 0.4086 0.116 Uiso 0.640(11) 1 calc PR A 1 H20B H 0.4301 -0.1430 0.4701 0.116 Uiso 0.640(11) 1 calc PR A 1 H20C H 0.5014 -0.1870 0.4842 0.116 Uiso 0.640(11) 1 calc PR A 1 C21A C 0.4404(12) -0.0583(12) 0.3436(11) 0.076(4) Uani 0.640(11) 1 d PDU A 1 H21A H 0.4489 -0.0275 0.3104 0.114 Uiso 0.640(11) 1 calc PR A 1 H21B H 0.3951 -0.0473 0.3550 0.114 Uiso 0.640(11) 1 calc PR A 1 H21C H 0.4367 -0.1018 0.3248 0.114 Uiso 0.640(11) 1 calc PR A 1 C22A C 0.5606(14) 0.0483(11) 0.3700(11) 0.076(2) Uani 0.640(11) 1 d PDU A 1 H22A H 0.5816 0.0865 0.3969 0.091 Uiso 0.640(11) 1 calc PR A 1 H22B H 0.5104 0.0597 0.3447 0.091 Uiso 0.640(11) 1 calc PR A 1 C23A C 0.6059(12) 0.0357(11) 0.3174(12) 0.080(3) Uani 0.640(11) 1 d PDU A 1 H23A H 0.5723 0.0222 0.2743 0.096 Uiso 0.640(11) 1 calc PR A 1 H23B H 0.6293 0.0764 0.3094 0.096 Uiso 0.640(11) 1 calc PR A 1 C24A C 0.6661(14) -0.0170(12) 0.3405(14) 0.084(5) Uani 0.640(11) 1 d PDU A 1 H24A H 0.6786 -0.0351 0.3011 0.126 Uiso 0.640(11) 1 calc PR A 1 H24B H 0.6479 -0.0512 0.3645 0.126 Uiso 0.640(11) 1 calc PR A 1 H24C H 0.7096 0.0025 0.3705 0.126 Uiso 0.640(11) 1 calc PR A 1 N5B N 0.487(2) -0.1001(16) 0.4212(17) 0.070(2) Uani 0.360(11) 1 d PDU A 2 N6B N 0.5316(15) -0.0107(15) 0.3872(14) 0.072(2) Uani 0.360(11) 1 d PDU A 2 C18B C 0.4654(17) -0.0198(19) 0.3351(15) 0.075(3) Uani 0.360(11) 1 d PDU A 2 H18B H 0.4443 0.0073 0.2980 0.090 Uiso 0.360(11) 1 calc PR A 2 C17B C 0.4355(18) -0.088(2) 0.3557(18) 0.071(3) Uani 0.360(11) 1 d PDU A 2 H17B H 0.3954 -0.1128 0.3318 0.085 Uiso 0.360(11) 1 calc PR A 2 C19B C 0.5372(17) -0.056(2) 0.4358(16) 0.071(2) Uani 0.360(11) 1 d PDU A 2 C20B C 0.497(3) -0.143(2) 0.4822(19) 0.077(4) Uani 0.360(11) 1 d PDU A 2 H20D H 0.5343 -0.1243 0.5198 0.116 Uiso 0.360(11) 1 calc PR A 2 H20E H 0.5127 -0.1858 0.4718 0.116 Uiso 0.360(11) 1 calc PR A 2 H20F H 0.4510 -0.1463 0.4946 0.116 Uiso 0.360(11) 1 calc PR A 2 C21B C 0.6124(19) -0.0429(19) 0.4864(18) 0.076(4) Uani 0.360(11) 1 d PDU A 2 H21D H 0.6279 0.0012 0.4803 0.114 Uiso 0.360(11) 1 calc PR A 2 H21E H 0.6485 -0.0733 0.4781 0.114 Uiso 0.360(11) 1 calc PR A 2 H21F H 0.6082 -0.0482 0.5324 0.114 Uiso 0.360(11) 1 calc PR A 2 C22B C 0.577(3) 0.0503(19) 0.3840(18) 0.076(2) Uani 0.360(11) 1 d PDU A 2 H22C H 0.6266 0.0504 0.4155 0.091 Uiso 0.360(11) 1 calc PR A 2 H22D H 0.5516 0.0915 0.3850 0.091 Uiso 0.360(11) 1 calc PR A 2 C23B C 0.574(2) 0.024(2) 0.3115(19) 0.080(3) Uani 0.360(11) 1 d PDU A 2 H23C H 0.5393 -0.0119 0.2992 0.096 Uiso 0.360(11) 1 calc PR A 2 H23D H 0.5597 0.0588 0.2774 0.096 Uiso 0.360(11) 1 calc PR A 2 C24B C 0.654(2) 0.002(3) 0.318(3) 0.084(5) Uani 0.360(11) 1 d PDU A 2 H24D H 0.6647 0.0038 0.2744 0.126 Uiso 0.360(11) 1 calc PR A 2 H24E H 0.6600 -0.0428 0.3349 0.126 Uiso 0.360(11) 1 calc PR A 2 H24F H 0.6880 0.0296 0.3502 0.126 Uiso 0.360(11) 1 calc PR A 2 N7A N 0.2640(13) 0.5388(12) 0.5341(12) 0.106(3) Uani 0.552(7) 1 d PDU B 1 N8A N 0.3036(14) 0.5866(14) 0.4479(12) 0.108(3) Uani 0.552(7) 1 d PDU B 1 C25A C 0.3381(14) 0.5589(16) 0.5596(17) 0.105(3) Uani 0.552(7) 1 d PDU B 1 H25A H 0.3676 0.5510 0.6037 0.127 Uiso 0.552(7) 1 calc PR B 1 C26A C 0.3600(11) 0.5915(18) 0.5097(14) 0.106(3) Uani 0.552(7) 1 d PDU B 1 H26A H 0.4049 0.6136 0.5154 0.127 Uiso 0.552(7) 1 calc PR B 1 C27A C 0.2438(11) 0.5560(16) 0.4650(12) 0.107(3) Uani 0.552(7) 1 d PDU B 1 C28A C 0.2073(15) 0.5136(15) 0.5698(15) 0.103(5) Uani 0.552(7) 1 d PDU B 1 H28A H 0.1609 0.5060 0.5364 0.155 Uiso 0.552(7) 1 calc PR B 1 H28B H 0.2004 0.5457 0.6024 0.155 Uiso 0.552(7) 1 calc PR B 1 H28C H 0.2247 0.4733 0.5931 0.155 Uiso 0.552(7) 1 calc PR B 1 C29A C 0.1619(11) 0.5455(19) 0.4293(16) 0.104(4) Uani 0.552(7) 1 d PDU B 1 H29A H 0.1525 0.5578 0.3819 0.156 Uiso 0.552(7) 1 calc PR B 1 H29B H 0.1322 0.5722 0.4511 0.156 Uiso 0.552(7) 1 calc PR B 1 H29C H 0.1495 0.5001 0.4326 0.156 Uiso 0.552(7) 1 calc PR B 1 C30A C 0.3075(18) 0.6071(12) 0.3767(13) 0.110(3) Uani 0.552(7) 1 d PDU B 1 H30A H 0.3250 0.6520 0.3770 0.132 Uiso 0.552(7) 1 calc PR B 1 H30B H 0.2590 0.6039 0.3443 0.132 Uiso 0.552(7) 1 calc PR B 1 C31A C 0.3625(13) 0.5592(13) 0.3573(18) 0.111(3) Uani 0.552(7) 1 d PDU B 1 H31A H 0.3786 0.5747 0.3181 0.133 Uiso 0.552(7) 1 calc PR B 1 H31B H 0.4056 0.5512 0.3956 0.133 Uiso 0.552(7) 1 calc PR B 1 C32A C 0.3129(18) 0.4982(12) 0.3398(17) 0.119(5) Uani 0.552(7) 1 d PDU B 1 H32A H 0.3407 0.4629 0.3270 0.178 Uiso 0.552(7) 1 calc PR B 1 H32B H 0.2707 0.5080 0.3022 0.178 Uiso 0.552(7) 1 calc PR B 1 H32C H 0.2963 0.4854 0.3791 0.178 Uiso 0.552(7) 1 calc PR B 1 N7B N 0.4358(14) 0.5397(14) 0.5082(14) 0.106(3) Uani 0.448(7) 1 d PDU . 2 N8B N 0.3413(17) 0.5902(16) 0.4315(14) 0.108(3) Uani 0.448(7) 1 d PDU B 2 C25B C 0.391(2) 0.5737(19) 0.543(2) 0.105(3) Uani 0.448(7) 1 d PDU B 2 H25B H 0.4000 0.5755 0.5904 0.127 Uiso 0.448(7) 1 calc PR B 2 C26B C 0.3349(19) 0.603(2) 0.4980(17) 0.106(3) Uani 0.448(7) 1 d PDU B 2 H26B H 0.2978 0.6280 0.5090 0.127 Uiso 0.448(7) 1 calc PR B 2 C27B C 0.3997(18) 0.5456(18) 0.4383(12) 0.107(3) Uani 0.448(7) 1 d PDU . 2 C28B C 0.5099(16) 0.5048(19) 0.5323(18) 0.103(5) Uani 0.448(7) 1 d PDU . 2 H28D H 0.5238 0.4869 0.4935 0.155 Uiso 0.448(7) 1 d PR B 2 H28E H 0.5470 0.5354 0.5558 0.155 Uiso 0.448(7) 1 d PR B 2 H28F H 0.5056 0.4699 0.5631 0.155 Uiso 0.448(7) 1 d PR B 2 C29B C 0.414(2) 0.5106(18) 0.3764(15) 0.104(4) Uani 0.448(7) 1 d PDU . 2 H29D H 0.3818 0.5263 0.3345 0.156 Uiso 0.448(7) 1 d PR B 2 H29E H 0.4651 0.5173 0.3754 0.156 Uiso 0.448(7) 1 d PR B 2 H29F H 0.4059 0.4645 0.3814 0.156 Uiso 0.448(7) 1 d PR B 2 C30B C 0.2760(15) 0.6187(16) 0.3780(17) 0.110(3) Uani 0.448(7) 1 d PDU B 2 H30C H 0.2921 0.6403 0.3416 0.132 Uiso 0.448(7) 1 calc PR B 2 H30D H 0.2485 0.6498 0.3983 0.132 Uiso 0.448(7) 1 calc PR B 2 C31B C 0.229(2) 0.5571(17) 0.3514(17) 0.111(3) Uani 0.448(7) 1 d PDU B 2 H31C H 0.1967 0.5638 0.3059 0.133 Uiso 0.448(7) 1 calc PR B 2 H31D H 0.2602 0.5188 0.3513 0.133 Uiso 0.448(7) 1 calc PR B 2 C32B C 0.186(2) 0.552(2) 0.406(2) 0.119(5) Uani 0.448(7) 1 d PDU B 2 H32D H 0.1544 0.5135 0.3968 0.178 Uiso 0.448(7) 1 calc PR B 2 H32E H 0.1556 0.5902 0.4042 0.178 Uiso 0.448(7) 1 calc PR B 2 H32F H 0.2197 0.5479 0.4504 0.178 Uiso 0.448(7) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0181(3) 0.0429(3) 0.0325(3) -0.0005(3) 0.0059(2) 0.0001(3) Sn2 0.0249(3) 0.0436(3) 0.0250(3) -0.0001(3) 0.0037(2) 0.0011(3) Sn3 0.0262(3) 0.0537(4) 0.0275(3) -0.0017(3) 0.0024(3) -0.0012(3) Sn4 0.0225(3) 0.0565(4) 0.0335(3) 0.0001(3) 0.0059(3) 0.0066(3) Sn5 0.0255(3) 0.0552(4) 0.0279(3) 0.0060(3) 0.0032(3) 0.0032(3) Sn6 0.0178(3) 0.0565(4) 0.0328(3) -0.0012(3) 0.0030(2) -0.0023(3) Sn7 0.0177(3) 0.0475(4) 0.0326(3) -0.0014(3) 0.0029(2) -0.0014(3) Sn8 0.0227(3) 0.0496(4) 0.0323(3) -0.0029(3) 0.0066(3) 0.0054(3) Sn9 0.0249(3) 0.0512(4) 0.0269(3) 0.0026(3) 0.0041(2) 0.0029(3) Se1 0.0283(5) 0.0632(7) 0.0441(6) 0.0149(5) 0.0142(4) 0.0045(5) Se2 0.0283(5) 0.0485(6) 0.0590(7) -0.0133(5) 0.0186(5) -0.0102(4) Se3 0.0266(5) 0.0523(6) 0.0505(6) 0.0122(5) 0.0151(4) 0.0096(4) Se4 0.0273(5) 0.0724(8) 0.0485(6) -0.0206(6) 0.0109(5) -0.0018(5) Se5 0.0465(6) 0.0494(6) 0.0373(6) 0.0006(5) 0.0152(5) -0.0019(5) Se6 0.0279(5) 0.0676(7) 0.0406(6) -0.0034(5) 0.0079(4) -0.0130(5) Se7 0.0264(5) 0.0475(5) 0.0345(5) 0.0011(4) 0.0051(4) 0.0000(4) Se8 0.0270(5) 0.0785(8) 0.0518(7) 0.0290(6) 0.0135(5) 0.0113(5) Se9 0.0389(6) 0.0628(7) 0.0390(6) -0.0100(5) -0.0016(4) 0.0175(5) Se10 0.0519(7) 0.0476(6) 0.0400(6) 0.0039(5) -0.0002(5) 0.0033(5) Se11 0.0448(6) 0.0489(6) 0.0367(6) 0.0054(5) 0.0028(5) -0.0089(5) Se12 0.0264(5) 0.0444(5) 0.0534(6) 0.0012(5) 0.0032(4) 0.0026(4) Se13 0.0249(5) 0.0448(6) 0.0576(7) -0.0022(5) -0.0018(4) -0.0002(4) Se14 0.0352(5) 0.0586(6) 0.0382(6) -0.0102(5) 0.0010(4) 0.0140(5) Se15 0.0257(5) 0.0583(6) 0.0467(6) 0.0175(5) 0.0114(4) 0.0061(5) Se16 0.0263(5) 0.0423(5) 0.0319(5) -0.0003(4) 0.0053(4) -0.0009(4) Se17 0.0298(5) 0.0892(9) 0.0398(6) -0.0163(6) 0.0091(4) -0.0222(6) Se18 0.0415(6) 0.0426(5) 0.0331(5) 0.0028(4) 0.0141(4) -0.0004(4) Se19 0.0495(6) 0.0394(5) 0.0341(5) 0.0015(4) 0.0010(4) 0.0020(5) Se20 0.0393(6) 0.0425(5) 0.0333(5) 0.0004(4) 0.0030(4) -0.0062(4) N1 0.086(5) 0.088(5) 0.108(6) 0.002(5) 0.024(5) 0.003(5) N2 0.077(5) 0.085(5) 0.098(5) -0.004(4) 0.031(4) 0.012(4) C1 0.096(6) 0.100(6) 0.121(6) -0.002(6) 0.022(5) 0.012(5) C2 0.093(6) 0.096(6) 0.114(6) -0.003(5) 0.026(5) 0.012(5) C3 0.073(5) 0.082(5) 0.095(6) 0.004(5) 0.026(5) 0.003(5) C4 0.114(9) 0.112(9) 0.139(9) -0.019(7) 0.021(7) -0.002(7) C5 0.087(8) 0.100(8) 0.101(8) 0.003(7) 0.028(6) 0.012(7) C6 0.090(6) 0.100(6) 0.107(6) -0.008(5) 0.032(5) 0.013(5) C7 0.102(7) 0.116(7) 0.119(7) -0.012(6) 0.034(6) 0.010(6) C8 0.124(9) 0.132(9) 0.141(9) -0.011(8) 0.029(7) 0.003(8) N3 0.156(7) 0.157(7) 0.170(7) 0.007(6) 0.047(6) 0.013(6) N4 0.144(6) 0.148(6) 0.158(6) 0.005(5) 0.048(5) 0.007(5) C9 0.163(7) 0.159(7) 0.170(7) 0.004(6) 0.044(6) 0.015(6) C10 0.154(7) 0.153(7) 0.161(7) 0.004(6) 0.045(6) 0.013(6) C11 0.140(7) 0.145(7) 0.158(7) 0.003(6) 0.047(6) 0.014(5) C12 0.192(11) 0.188(11) 0.207(11) -0.004(8) 0.044(8) 0.000(8) C13 0.130(9) 0.143(9) 0.149(10) 0.006(8) 0.045(8) 0.010(6) C14 0.160(7) 0.168(7) 0.168(7) 0.004(6) 0.046(6) 0.001(6) C15 0.177(8) 0.182(8) 0.172(8) 0.006(7) 0.053(7) -0.003(7) C16 0.205(12) 0.196(12) 0.209(12) 0.008(8) 0.050(8) -0.001(9) N5A 0.069(4) 0.068(4) 0.073(4) 0.004(3) 0.021(3) -0.002(3) N6A 0.071(3) 0.069(3) 0.074(3) 0.002(3) 0.017(3) -0.001(3) C17A 0.069(4) 0.071(4) 0.072(4) 0.004(4) 0.018(3) 0.002(4) C18A 0.073(4) 0.074(4) 0.076(4) -0.001(4) 0.017(3) 0.002(4) C19A 0.070(3) 0.070(3) 0.073(3) 0.002(3) 0.019(3) 0.000(3) C20A 0.078(6) 0.075(6) 0.080(6) 0.005(5) 0.022(5) -0.005(5) C21A 0.071(5) 0.075(6) 0.079(6) -0.004(5) 0.015(5) -0.001(5) C22A 0.076(4) 0.072(4) 0.078(4) 0.004(3) 0.017(3) -0.001(3) C23A 0.078(4) 0.078(4) 0.082(4) 0.004(4) 0.018(4) -0.003(4) C24A 0.082(6) 0.086(7) 0.085(7) 0.003(5) 0.025(5) 0.000(5) N5B 0.069(4) 0.068(4) 0.073(4) 0.004(3) 0.021(3) -0.002(3) N6B 0.071(3) 0.069(3) 0.074(3) 0.002(3) 0.017(3) -0.001(3) C18B 0.073(4) 0.074(4) 0.076(4) -0.001(4) 0.017(3) 0.002(4) C17B 0.069(4) 0.071(4) 0.072(4) 0.004(4) 0.018(3) 0.002(4) C19B 0.070(3) 0.070(3) 0.073(3) 0.002(3) 0.019(3) 0.000(3) C20B 0.078(6) 0.075(6) 0.080(6) 0.005(5) 0.022(5) -0.005(5) C21B 0.071(5) 0.075(6) 0.079(6) -0.004(5) 0.015(5) -0.001(5) C22B 0.076(4) 0.072(4) 0.078(4) 0.004(3) 0.017(3) -0.001(3) C23B 0.078(4) 0.078(4) 0.082(4) 0.004(4) 0.018(4) -0.003(4) C24B 0.082(6) 0.086(7) 0.085(7) 0.003(5) 0.025(5) 0.000(5) N7A 0.106(5) 0.101(5) 0.109(5) -0.006(4) 0.026(4) 0.000(4) N8A 0.109(4) 0.106(4) 0.108(4) -0.002(3) 0.026(3) 0.002(3) C25A 0.105(4) 0.103(4) 0.107(4) -0.004(4) 0.026(4) 0.002(4) C26A 0.106(4) 0.105(4) 0.107(4) -0.004(3) 0.027(3) 0.002(4) C27A 0.108(4) 0.102(4) 0.110(4) -0.003(4) 0.026(4) 0.002(4) C28A 0.104(7) 0.101(7) 0.106(7) -0.007(5) 0.030(5) 0.002(5) C29A 0.104(6) 0.100(6) 0.107(6) -0.003(5) 0.027(5) 0.002(5) C30A 0.110(4) 0.108(4) 0.109(4) 0.002(3) 0.026(3) 0.001(3) C31A 0.113(5) 0.108(5) 0.111(5) 0.001(4) 0.028(4) -0.003(4) C32A 0.119(7) 0.116(7) 0.119(7) -0.002(5) 0.027(5) 0.000(5) N7B 0.106(5) 0.101(5) 0.109(5) -0.006(4) 0.026(4) 0.000(4) N8B 0.109(4) 0.106(4) 0.108(4) -0.002(3) 0.026(3) 0.002(3) C25B 0.105(4) 0.103(4) 0.107(4) -0.004(4) 0.026(4) 0.002(4) C26B 0.106(4) 0.105(4) 0.107(4) -0.004(3) 0.027(3) 0.002(4) C27B 0.108(4) 0.102(4) 0.110(4) -0.003(4) 0.026(4) 0.002(4) C28B 0.104(7) 0.101(7) 0.106(7) -0.007(5) 0.030(5) 0.002(5) C29B 0.104(6) 0.100(6) 0.107(6) -0.003(5) 0.027(5) 0.002(5) C30B 0.110(4) 0.108(4) 0.109(4) 0.002(3) 0.026(3) 0.001(3) C31B 0.113(5) 0.108(5) 0.111(5) 0.001(4) 0.028(4) -0.003(4) C32B 0.119(7) 0.116(7) 0.119(7) -0.002(5) 0.027(5) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Se2 2.4975(13) . ? Sn1 Se3 2.4994(13) . ? Sn1 Se1 2.5271(14) . ? Sn1 Se4 2.5323(14) . ? Sn2 Se19 2.4884(13) . ? Sn2 Se18 2.5195(13) 4_565 ? Sn2 Se1 2.5279(14) . ? Sn2 Se20 2.5314(12) . ? Sn3 Se10 2.4843(14) 4_565 ? Sn3 Se5 2.5253(14) . ? Sn3 Se4 2.5279(15) . ? Sn3 Se11 2.5333(13) 4_565 ? Sn4 Se8 2.5331(13) . ? Sn4 Se6 2.5348(14) . ? Sn4 Se5 2.5523(14) . ? Sn4 Se3 2.7315(13) . ? Sn4 Se7 2.7813(13) . ? Sn5 Se9 2.5378(13) . ? Sn5 Se6 2.5520(14) . ? Sn5 Se11 2.5750(13) . ? Sn5 Se7 2.7007(13) . ? Sn5 Se10 2.7648(14) . ? Sn6 Se9 2.5479(14) . ? Sn6 Se8 2.5542(13) . ? Sn6 Se12 2.5589(13) . ? Sn6 Se13 2.6108(13) . ? Sn6 Se7 2.8773(13) . ? Sn7 Se12 2.5609(13) 4_666 ? Sn7 Se15 2.5648(13) . ? Sn7 Se14 2.5713(14) . ? Sn7 Se13 2.5968(13) 4_666 ? Sn7 Se16 2.8261(13) . ? Sn8 Se17 2.5306(14) . ? Sn8 Se15 2.5337(13) . ? Sn8 Se18 2.5458(14) . ? Sn8 Se2 2.6980(13) 4_566 ? Sn8 Se16 2.7982(13) . ? Sn9 Se17 2.5376(14) . ? Sn9 Se14 2.5398(13) . ? Sn9 Se20 2.5678(13) . ? Sn9 Se16 2.7085(13) . ? Sn9 Se19 2.7848(13) . ? Se2 Sn8 2.6980(13) 4_565 ? Se10 Sn3 2.4843(14) 4_566 ? Se11 Sn3 2.5333(13) 4_566 ? Se12 Sn7 2.5609(13) 4_465 ? Se13 Sn7 2.5968(13) 4_465 ? Se18 Sn2 2.5195(13) 4_566 ? N1 C3 1.346(19) . ? N1 C1 1.40(2) . ? N1 C4 1.49(2) . ? N2 C3 1.292(19) . ? N2 C2 1.419(19) . ? N2 C6 1.51(2) . ? C1 C2 1.32(2) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C5 1.49(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.55(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.47(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N3 C11 1.36(3) . ? N3 C9 1.42(2) . ? N3 C12 1.47(3) . ? N4 C11 1.32(3) . ? N4 C10 1.34(3) . ? N4 C14 1.422(16) . ? C9 C10 1.47(3) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C13 1.49(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.48(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.57(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N5A C19A 1.22(3) . ? N5A C17A 1.40(3) . ? N5A C20A 1.49(3) . ? N6A C19A 1.35(3) . ? N6A C18A 1.399(11) . ? N6A C22A 1.516(14) . ? C17A C18A 1.32(3) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? C19A C21A 1.528(9) . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A C23A 1.542(9) . ? C22A H22A 0.9700 . ? C22A H22B 0.9700 . ? C23A C24A 1.533(10) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? N5B C19B 1.27(5) . ? N5B C17B 1.44(4) . ? N5B C20B 1.479(19) . ? N6B C19B 1.33(5) . ? N6B C18B 1.408(11) . ? N6B C22B 1.518(15) . ? C18B C17B 1.59(5) . ? C18B H18B 0.9300 . ? C17B H17B 0.9300 . ? C19B C21B 1.527(10) . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B C23B 1.541(10) . ? C22B H22C 0.9700 . ? C22B H22D 0.9700 . ? C23B C24B 1.537(10) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? N7A C27A 1.392(11) . ? N7A C25A 1.403(11) . ? N7A C28A 1.516(15) . ? N8A C27A 1.396(11) . ? N8A C26A 1.409(11) . ? N8A C30A 1.518(15) . ? C25A C26A 1.36(4) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C27A C29A 1.523(10) . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C30A C31A 1.538(10) . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C31A C32A 1.534(10) . ? C31A H31A 0.9700 . ? C31A H31B 0.9700 . ? C31A H29D 0.9362 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? N7B C27B 1.399(11) . ? N7B C25B 1.401(11) . ? N7B C28B 1.516(15) . ? N8B C27B 1.398(11) . ? N8B C26B 1.404(11) . ? N8B C30B 1.515(15) . ? C25B C26B 1.34(5) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C27B C29B 1.525(10) . ? C28B H28D 0.9599 . ? C28B H28E 0.9601 . ? C28B H28F 0.9600 . ? C29B H29D 0.9599 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C30B C31B 1.541(10) . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? C31B C32B 1.533(10) . ? C31B H31C 0.9700 . ? C31B H31D 0.9700 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se3 114.42(5) . . ? Se2 Sn1 Se1 105.00(4) . . ? Se3 Sn1 Se1 110.02(4) . . ? Se2 Sn1 Se4 108.93(4) . . ? Se3 Sn1 Se4 106.92(4) . . ? Se1 Sn1 Se4 111.63(5) . . ? Se19 Sn2 Se18 106.36(4) . 4_565 ? Se19 Sn2 Se1 107.86(4) . . ? Se18 Sn2 Se1 114.70(4) 4_565 . ? Se19 Sn2 Se20 97.72(4) . . ? Se18 Sn2 Se20 117.25(4) 4_565 . ? Se1 Sn2 Se20 111.00(5) . . ? Se10 Sn3 Se5 106.00(5) 4_565 . ? Se10 Sn3 Se4 108.04(5) 4_565 . ? Se5 Sn3 Se4 111.94(5) . . ? Se10 Sn3 Se11 97.71(5) 4_565 4_565 ? Se5 Sn3 Se11 119.18(5) . 4_565 ? Se4 Sn3 Se11 112.21(5) . 4_565 ? Se8 Sn4 Se6 118.51(5) . . ? Se8 Sn4 Se5 116.75(5) . . ? Se6 Sn4 Se5 124.25(5) . . ? Se8 Sn4 Se3 89.00(4) . . ? Se6 Sn4 Se3 90.96(4) . . ? Se5 Sn4 Se3 96.80(4) . . ? Se8 Sn4 Se7 90.48(4) . . ? Se6 Sn4 Se7 87.48(4) . . ? Se5 Sn4 Se7 85.26(4) . . ? Se3 Sn4 Se7 177.89(4) . . ? Se9 Sn5 Se6 120.21(5) . . ? Se9 Sn5 Se11 121.85(5) . . ? Se6 Sn5 Se11 117.88(5) . . ? Se9 Sn5 Se7 88.85(4) . . ? Se6 Sn5 Se7 88.90(4) . . ? Se11 Sn5 Se7 94.74(5) . . ? Se9 Sn5 Se10 88.84(4) . . ? Se6 Sn5 Se10 88.67(4) . . ? Se11 Sn5 Se10 90.02(5) . . ? Se7 Sn5 Se10 175.24(4) . . ? Se9 Sn6 Se8 116.31(5) . . ? Se9 Sn6 Se12 125.72(5) . . ? Se8 Sn6 Se12 116.92(5) . . ? Se9 Sn6 Se13 91.95(4) . . ? Se8 Sn6 Se13 97.36(5) . . ? Se12 Sn6 Se13 91.21(4) . . ? Se9 Sn6 Se7 84.87(4) . . ? Se8 Sn6 Se7 87.93(4) . . ? Se12 Sn6 Se7 87.16(4) . . ? Se13 Sn6 Se7 174.64(4) . . ? Se12 Sn7 Se15 118.03(5) 4_666 . ? Se12 Sn7 Se14 126.33(5) 4_666 . ? Se15 Sn7 Se14 115.00(5) . . ? Se12 Sn7 Se13 91.49(4) 4_666 4_666 ? Se15 Sn7 Se13 95.08(4) . 4_666 ? Se14 Sn7 Se13 91.60(4) . 4_666 ? Se12 Sn7 Se16 88.08(4) 4_666 . ? Se15 Sn7 Se16 88.24(4) . . ? Se14 Sn7 Se16 85.82(4) . . ? Se13 Sn7 Se16 176.44(4) 4_666 . ? Se17 Sn8 Se15 117.93(5) . . ? Se17 Sn8 Se18 125.26(5) . . ? Se15 Sn8 Se18 116.21(5) . . ? Se17 Sn8 Se2 90.06(5) . 4_566 ? Se15 Sn8 Se2 88.14(4) . 4_566 ? Se18 Sn8 Se2 99.21(4) . 4_566 ? Se17 Sn8 Se16 86.80(4) . . ? Se15 Sn8 Se16 89.48(4) . . ? Se18 Sn8 Se16 86.17(4) . . ? Se2 Sn8 Se16 174.62(4) 4_566 . ? Se17 Sn9 Se14 121.51(5) . . ? Se17 Sn9 Se20 119.08(5) . . ? Se14 Sn9 Se20 119.26(5) . . ? Se17 Sn9 Se16 88.61(4) . . ? Se14 Sn9 Se16 88.97(4) . . ? Se20 Sn9 Se16 96.37(5) . . ? Se17 Sn9 Se19 86.04(4) . . ? Se14 Sn9 Se19 90.37(4) . . ? Se20 Sn9 Se19 89.78(4) . . ? Se16 Sn9 Se19 173.29(4) . . ? Sn1 Se1 Sn2 95.57(4) . . ? Sn1 Se2 Sn8 105.88(5) . 4_565 ? Sn1 Se3 Sn4 105.58(5) . . ? Sn3 Se4 Sn1 93.98(4) . . ? Sn3 Se5 Sn4 103.95(5) . . ? Sn4 Se6 Sn5 92.51(4) . . ? Sn5 Se7 Sn4 84.17(4) . . ? Sn5 Se7 Sn6 84.68(4) . . ? Sn4 Se7 Sn6 82.89(4) . . ? Sn4 Se8 Sn6 94.85(5) . . ? Sn5 Se9 Sn6 95.32(4) . . ? Sn3 Se10 Sn5 82.83(5) 4_566 . ? Sn3 Se11 Sn5 85.84(4) 4_566 . ? Sn6 Se12 Sn7 89.58(5) . 4_465 ? Sn7 Se13 Sn6 87.67(5) 4_465 . ? Sn9 Se14 Sn7 94.08(4) . . ? Sn8 Se15 Sn7 95.06(4) . . ? Sn9 Se16 Sn8 84.05(4) . . ? Sn9 Se16 Sn7 85.01(4) . . ? Sn8 Se16 Sn7 83.93(4) . . ? Sn8 Se17 Sn9 93.35(4) . . ? Sn2 Se18 Sn8 103.38(4) 4_566 . ? Sn2 Se19 Sn9 82.21(4) . . ? Sn2 Se20 Sn9 85.88(4) . . ? C3 N1 C1 105.4(15) . . ? C3 N1 C4 128.8(15) . . ? C1 N1 C4 125.7(16) . . ? C3 N2 C2 109.5(15) . . ? C3 N2 C6 128.1(14) . . ? C2 N2 C6 122.4(14) . . ? C2 C1 N1 110.1(17) . . ? C2 C1 H1A 125.0 . . ? N1 C1 H1A 125.0 . . ? C1 C2 N2 104.7(16) . . ? C1 C2 H2A 127.7 . . ? N2 C2 H2A 127.7 . . ? N2 C3 N1 110.2(15) . . ? N2 C3 C5 127.7(16) . . ? N1 C3 C5 122.0(15) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 105.9(14) . . ? N2 C6 H6A 110.6 . . ? C7 C6 H6A 110.6 . . ? N2 C6 H6B 110.6 . . ? C7 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? C8 C7 C6 107.1(16) . . ? C8 C7 H7A 110.3 . . ? C6 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? C6 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 N3 C9 108.1(18) . . ? C11 N3 C12 146(2) . . ? C9 N3 C12 103.4(16) . . ? C11 N4 C10 112(2) . . ? C11 N4 C14 121(2) . . ? C10 N4 C14 127(3) . . ? N3 C9 C10 104.2(18) . . ? N3 C9 H9A 127.9 . . ? C10 C9 H9A 127.9 . . ? N4 C10 C9 106(2) . . ? N4 C10 H10A 127.2 . . ? C9 C10 H10A 127.2 . . ? N4 C11 N3 109(2) . . ? N4 C11 C13 129(2) . . ? N3 C11 C13 118(3) . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 107(2) . . ? N4 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? N4 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.5 . . ? C14 C15 C16 119(2) . . ? C14 C15 H15A 107.5 . . ? C16 C15 H15A 107.5 . . ? C14 C15 H15B 107.5 . . ? C16 C15 H15B 107.5 . . ? H15A C15 H15B 107.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19A N5A C17A 108(2) . . ? C19A N5A C20A 121(2) . . ? C17A N5A C20A 131(2) . . ? C19A N6A C18A 109.0(19) . . ? C19A N6A C22A 126.3(19) . . ? C18A N6A C22A 124.7(19) . . ? C18A C17A N5A 110(2) . . ? C18A C17A H17A 124.8 . . ? N5A C17A H17A 124.8 . . ? C17A C18A N6A 102(2) . . ? C17A C18A H18A 128.9 . . ? N6A C18A H18A 128.9 . . ? N5A C19A N6A 110.4(18) . . ? N5A C19A C21A 127(2) . . ? N6A C19A C21A 122(2) . . ? N5A C20A H20A 109.5 . . ? N5A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? N5A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5 . . ? C19A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? N6A C22A C23A 118(2) . . ? N6A C22A H22A 107.9 . . ? C23A C22A H22A 107.9 . . ? N6A C22A H22B 107.9 . . ? C23A C22A H22B 107.9 . . ? H22A C22A H22B 107.2 . . ? C24A C23A C22A 113(2) . . ? C24A C23A H23A 108.9 . . ? C22A C23A H23A 108.9 . . ? C24A C23A H23B 108.9 . . ? C22A C23A H23B 108.9 . . ? H23A C23A H23B 107.7 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C19B N5B C17B 111(3) . . ? C19B N5B C20B 107(3) . . ? C17B N5B C20B 141(4) . . ? C19B N6B C18B 110(3) . . ? C19B N6B C22B 131(3) . . ? C18B N6B C22B 118(3) . . ? N6B C18B C17B 103(2) . . ? N6B C18B H18B 128.7 . . ? C17B C18B H18B 128.7 . . ? N5B C17B C18B 101(2) . . ? N5B C17B H17B 129.3 . . ? C18B C17B H17B 129.3 . . ? N5B C19B N6B 114(2) . . ? N5B C19B C21B 140(3) . . ? N6B C19B C21B 105(2) . . ? N5B C20B H20D 109.5 . . ? N5B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? N5B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19B C21B H21D 109.5 . . ? C19B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? N6B C22B C23B 83(3) . . ? N6B C22B H22C 114.8 . . ? C23B C22B H22C 114.8 . . ? N6B C22B H22D 114.8 . . ? C23B C22B H22D 114.8 . . ? H22C C22B H22D 111.9 . . ? C24B C23B C22B 103(4) . . ? C24B C23B H23C 111.2 . . ? C22B C23B H23C 111.2 . . ? C24B C23B H23D 111.2 . . ? C22B C23B H23D 111.2 . . ? H23C C23B H23D 109.1 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C27A N7A C25A 105.9(18) . . ? C27A N7A C28A 122(2) . . ? C25A N7A C28A 132(3) . . ? C27A N8A C26A 105.8(12) . . ? C27A N8A C30A 127(2) . . ? C26A N8A C30A 128(2) . . ? C26A C25A N7A 109(2) . . ? C26A C25A H25A 125.3 . . ? N7A C25A H25A 125.3 . . ? C25A C26A N8A 108.8(13) . . ? C25A C26A H26A 125.6 . . ? N8A C26A H26A 125.6 . . ? N7A C27A N8A 109.7(9) . . ? N7A C27A C29A 114(2) . . ? N8A C27A C29A 135(2) . . ? N7A C28A H28A 109.5 . . ? N7A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? N7A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? N8A C30A C31A 106(2) . . ? N8A C30A H30A 110.6 . . ? C31A C30A H30A 110.6 . . ? N8A C30A H30B 110.6 . . ? C31A C30A H30B 110.6 . . ? H30A C30A H30B 108.8 . . ? C32A C31A C30A 99.7(8) . . ? C32A C31A H31A 111.8 . . ? C30A C31A H31A 111.8 . . ? C32A C31A H31B 111.8 . . ? C30A C31A H31B 111.8 . . ? H31A C31A H31B 109.5 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C27B N7B C25B 106(2) . . ? C27B N7B C28B 121(3) . . ? C25B N7B C28B 133(3) . . ? C27B N8B C26B 106.7(12) . . ? C27B N8B C30B 141(3) . . ? C26B N8B C30B 111(3) . . ? C26B C25B N7B 110(3) . . ? C26B C25B H25B 124.9 . . ? N7B C25B H25B 124.9 . . ? C25B C26B N8B 108.3(14) . . ? C25B C26B H26B 125.8 . . ? N8B C26B H26B 125.8 . . ? N8B C27B N7B 108.1(10) . . ? N8B C27B C29B 122(3) . . ? N7B C27B C29B 130(3) . . ? N7B C28B H28D 109.5 . . ? N7B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? N7B C28B H28F 109.4 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 110.9 . . ? C27B C29B H29E 110.0 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 107.4 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? N8B C30B C31B 102(3) . . ? N8B C30B H30C 111.3 . . ? C31B C30B H30C 111.3 . . ? N8B C30B H30D 111.3 . . ? C31B C30B H30D 111.3 . . ? H30C C30B H30D 109.2 . . ? C32B C31B C30B 99.6(8) . . ? C32B C31B H31C 111.8 . . ? C30B C31B H31C 111.8 . . ? C32B C31B H31D 111.8 . . ? C30B C31B H31D 111.8 . . ? H31C C31B H31D 109.6 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.169 _refine_diff_density_min -1.667 _refine_diff_density_rms 0.224 data_compound-2_JL9-10E _database_code_depnum_ccdc_archive 'CCDC 903261' #TrackingRef 'compound 1-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Sn3 Se7, 2(C8 H15 N2)' _chemical_formula_sum 'C16 H30 N4 Se7 Sn3' _chemical_formula_weight 1187.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.270(5) _cell_length_b 15.549(6) _cell_length_c 14.377(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.749(7) _cell_angle_gamma 90.00 _cell_volume 3186(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6492 _cell_measurement_theta_min 3.1148 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 10.342 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5403 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 7515 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24428 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7259 _reflns_number_gt 5697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+4.0000P] 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 7259 _refine_ls_number_parameters 277 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.73657(3) 0.00865(3) 0.72971(3) 0.03781(13) Uani 1 1 d . . . Sn2 Sn 0.61177(3) 0.00547(3) 0.94020(3) 0.03692(13) Uani 1 1 d U . . Sn3 Sn 0.88660(3) 0.01536(3) 0.94891(4) 0.03986(14) Uani 1 1 d . . . Se1 Se 0.73082(6) -0.10948(5) 0.84999(6) 0.0491(2) Uani 1 1 d . . . Se2 Se 0.60026(5) 0.09685(5) 0.79225(5) 0.04343(19) Uani 1 1 d . . . Se3 Se 0.88330(5) 0.08906(5) 0.79211(6) 0.0510(2) Uani 1 1 d . . . Se4 Se 0.75164(5) 0.04077(5) 1.05380(5) 0.04290(19) Uani 1 1 d . . . Se5 Se 0.73066(6) -0.01876(6) 0.56410(6) 0.0541(2) Uani 1 1 d . . . Se6 Se 0.50478(5) 0.11314(5) 1.03562(6) 0.04343(19) Uani 1 1 d U . . Se7 Se 1.01418(5) 0.11725(5) 1.02719(6) 0.0472(2) Uani 1 1 d . . . N1 N 0.2750(5) 0.1874(5) 0.8145(5) 0.0624(19) Uani 1 1 d . . . N2 N 0.2048(5) 0.1627(5) 0.6832(5) 0.0651(19) Uani 1 1 d U . . N3 N 0.5505(5) 0.1437(5) 1.4502(5) 0.0603(19) Uani 1 1 d . . . N4 N 0.6499(5) 0.1632(5) 1.3446(6) 0.066(2) Uani 1 1 d . . . C1 C 0.3333(7) 0.1377(7) 0.7641(9) 0.084(3) Uani 1 1 d . . . H1A H 0.3929 0.1188 0.7838 0.100 Uiso 1 1 calc R . . C2 C 0.2904(7) 0.1212(7) 0.6829(8) 0.074(3) Uani 1 1 d . . . H2A H 0.3131 0.0882 0.6349 0.089 Uiso 1 1 calc R . . C3 C 0.1967(6) 0.2019(6) 0.7640(6) 0.054(2) Uani 1 1 d . . . C4 C 0.2911(10) 0.2207(8) 0.9084(8) 0.115(5) Uani 1 1 d . . . H4A H 0.2498 0.2684 0.9178 0.172 Uiso 1 1 calc R . . H4B H 0.3551 0.2395 0.9169 0.172 Uiso 1 1 calc R . . H4C H 0.2792 0.1763 0.9527 0.172 Uiso 1 1 calc R . . C5 C 0.1170(7) 0.2530(7) 0.7948(7) 0.085(3) Uani 1 1 d . . . H5A H 0.0791 0.2713 0.7414 0.128 Uiso 1 1 calc R . . H5B H 0.1402 0.3026 0.8285 0.128 Uiso 1 1 calc R . . H5C H 0.0799 0.2186 0.8344 0.128 Uiso 1 1 calc R . . C6 C 0.1390(7) 0.1706(6) 0.5973(7) 0.078(3) Uani 1 1 d DU . . H6A H 0.1124 0.2279 0.5934 0.093 Uiso 1 1 calc R . . H6B H 0.1730 0.1601 0.5415 0.093 Uiso 1 1 calc R . . C7 C 0.0625(7) 0.1047(8) 0.6057(8) 0.091(3) Uani 1 1 d DU . . H7A H 0.0331 0.1110 0.6648 0.109 Uiso 1 1 calc R . . H7B H 0.0880 0.0471 0.6022 0.109 Uiso 1 1 calc R . . C8 C -0.0107(9) 0.1210(8) 0.5231(9) 0.111(4) Uani 1 1 d U . . H8A H -0.0668 0.0889 0.5330 0.167 Uiso 1 1 calc R . . H8B H 0.0152 0.1029 0.4658 0.167 Uiso 1 1 calc R . . H8C H -0.0254 0.1812 0.5196 0.167 Uiso 1 1 calc R . . C9 C 0.5128(8) 0.1090(8) 1.3704(8) 0.092(4) Uani 1 1 d . . . H9A H 0.4546 0.0824 1.3628 0.110 Uiso 1 1 calc R . . C10 C 0.5750(7) 0.1203(8) 1.3045(7) 0.088(4) Uani 1 1 d . . . H10A H 0.5683 0.1023 1.2428 0.106 Uiso 1 1 calc R . . C11 C 0.6363(6) 0.1755(5) 1.4339(7) 0.057(2) Uani 1 1 d . . . C12 C 0.5089(7) 0.1399(6) 1.5403(7) 0.075(3) Uani 1 1 d . . . H12A H 0.5037 0.1970 1.5648 0.112 Uiso 1 1 calc R . . H12B H 0.5479 0.1058 1.5822 0.112 Uiso 1 1 calc R . . H12C H 0.4477 0.1144 1.5334 0.112 Uiso 1 1 calc R . . C13 C 0.6994(7) 0.2192(6) 1.5016(7) 0.079(3) Uani 1 1 d . . . H13A H 0.7279 0.2675 1.4723 0.119 Uiso 1 1 calc R . . H13B H 0.7473 0.1800 1.5240 0.119 Uiso 1 1 calc R . . H13C H 0.6644 0.2389 1.5528 0.119 Uiso 1 1 calc R . . C14 C 0.7363(7) 0.1834(7) 1.2973(7) 0.080(3) Uani 1 1 d . . . H14A H 0.7621 0.2370 1.3217 0.096 Uiso 1 1 calc R . . H14B H 0.7212 0.1913 1.2313 0.096 Uiso 1 1 calc R . . C15 C 0.8088(7) 0.1140(7) 1.3098(8) 0.077(3) Uani 1 1 d . . . H15A H 0.8204 0.1029 1.3758 0.093 Uiso 1 1 calc R . . H15B H 0.7849 0.0614 1.2811 0.093 Uiso 1 1 calc R . . C16 C 0.8989(7) 0.1377(9) 1.2679(8) 0.099(4) Uani 1 1 d . . . H16A H 0.9421 0.0906 1.2746 0.149 Uiso 1 1 calc R . . H16B H 0.9250 0.1874 1.2992 0.149 Uiso 1 1 calc R . . H16C H 0.8874 0.1505 1.2031 0.149 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0316(2) 0.0487(3) 0.0335(3) -0.0004(2) 0.00550(19) 0.0021(2) Sn2 0.0214(2) 0.0508(3) 0.0388(3) 0.0043(2) 0.00491(19) -0.00103(19) Sn3 0.0237(2) 0.0521(3) 0.0439(3) 0.0047(2) 0.0040(2) 0.0056(2) Se1 0.0562(5) 0.0443(4) 0.0482(5) 0.0048(3) 0.0185(4) 0.0131(3) Se2 0.0354(4) 0.0532(4) 0.0420(4) 0.0075(3) 0.0057(3) 0.0122(3) Se3 0.0368(4) 0.0651(5) 0.0511(5) 0.0137(4) 0.0030(3) -0.0128(4) Se4 0.0263(3) 0.0614(5) 0.0410(4) -0.0089(3) 0.0022(3) 0.0005(3) Se5 0.0607(5) 0.0661(5) 0.0362(4) -0.0068(4) 0.0083(4) -0.0015(4) Se6 0.0316(3) 0.0445(4) 0.0551(5) -0.0062(3) 0.0119(3) -0.0031(3) Se7 0.0330(4) 0.0421(4) 0.0659(5) -0.0065(4) -0.0021(3) 0.0015(3) N1 0.065(5) 0.056(4) 0.064(5) -0.001(4) -0.009(4) 0.008(4) N2 0.051(4) 0.080(5) 0.065(4) -0.015(4) 0.005(3) -0.002(4) N3 0.058(4) 0.063(4) 0.059(5) 0.013(4) -0.005(4) -0.012(4) N4 0.054(4) 0.080(5) 0.064(5) 0.014(4) -0.001(4) -0.011(4) C1 0.054(6) 0.077(7) 0.119(10) 0.005(7) 0.000(6) 0.012(5) C2 0.061(6) 0.087(7) 0.076(7) 0.000(6) 0.025(5) 0.019(5) C3 0.047(4) 0.064(5) 0.052(5) 0.005(4) 0.008(4) 0.004(4) C4 0.164(13) 0.086(8) 0.089(9) -0.020(7) -0.061(9) 0.029(8) C5 0.065(6) 0.100(8) 0.094(8) -0.012(6) 0.040(6) 0.019(6) C6 0.096(8) 0.077(6) 0.059(6) 0.007(5) -0.004(4) -0.006(6) C7 0.064(6) 0.129(10) 0.079(7) 0.001(7) 0.012(5) -0.010(6) C8 0.094(9) 0.107(10) 0.129(11) -0.006(8) -0.032(7) -0.012(7) C9 0.062(6) 0.131(10) 0.081(8) -0.007(7) -0.015(6) -0.036(7) C10 0.069(7) 0.137(10) 0.059(7) -0.001(6) -0.008(5) -0.034(7) C11 0.047(5) 0.049(5) 0.074(6) 0.005(4) -0.011(4) 0.000(4) C12 0.078(7) 0.073(6) 0.075(7) 0.014(5) 0.014(5) -0.003(5) C13 0.074(7) 0.067(6) 0.096(8) -0.018(6) -0.018(6) 0.001(5) C14 0.071(7) 0.087(7) 0.083(7) 0.018(6) 0.009(6) -0.009(6) C15 0.070(7) 0.087(7) 0.076(7) 0.004(6) 0.013(5) -0.006(6) C16 0.064(7) 0.142(11) 0.093(8) -0.011(8) 0.029(6) -0.013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Se5 2.4163(13) . ? Sn1 Se1 2.5267(11) . ? Sn1 Se3 2.5636(12) . ? Sn1 Se2 2.5770(10) . ? Sn2 Se6 2.5188(11) 3_657 ? Sn2 Se2 2.5567(11) . ? Sn2 Se4 2.5767(11) . ? Sn2 Se6 2.6863(10) . ? Sn2 Se1 2.8239(11) . ? Sn3 Se7 2.5155(11) 3_757 ? Sn3 Se3 2.5272(12) . ? Sn3 Se4 2.5334(11) . ? Sn3 Se7 2.6257(11) . ? Se6 Sn2 2.5188(11) 3_657 ? Se7 Sn3 2.5155(11) 3_757 ? N1 C3 1.322(10) . ? N1 C1 1.369(12) . ? N1 C4 1.455(12) . ? N2 C3 1.322(10) . ? N2 C2 1.382(11) . ? N2 C6 1.520(12) . ? N3 C11 1.352(10) . ? N3 C9 1.356(12) . ? N3 C12 1.450(11) . ? N4 C11 1.321(11) . ? N4 C10 1.365(12) . ? N4 C14 1.471(11) . ? C1 C2 1.318(14) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C5 1.472(11) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.506(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.565(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.340(14) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C13 1.461(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.500(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.492(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 Se5 Sn1 Se1 123.05(4) . . ? Se5 Sn1 Se3 114.85(3) . . ? Se1 Sn1 Se3 99.66(4) . . ? Se5 Sn1 Se2 116.51(4) . . ? Se1 Sn1 Se2 95.64(3) . . ? Se3 Sn1 Se2 103.64(4) . . ? Se6 Sn2 Se2 120.35(4) 3_657 . ? Se6 Sn2 Se4 124.41(4) 3_657 . ? Se2 Sn2 Se4 115.20(3) . . ? Se6 Sn2 Se6 89.46(4) 3_657 . ? Se2 Sn2 Se6 93.62(4) . . ? Se4 Sn2 Se6 89.17(4) . . ? Se6 Sn2 Se1 90.90(4) 3_657 . ? Se2 Sn2 Se1 89.18(3) . . ? Se4 Sn2 Se1 87.78(4) . . ? Se6 Sn2 Se1 176.53(3) . . ? Se7 Sn3 Se3 118.67(4) 3_757 . ? Se7 Sn3 Se4 119.05(4) 3_757 . ? Se3 Sn3 Se4 118.56(4) . . ? Se7 Sn3 Se7 93.55(4) 3_757 . ? Se3 Sn3 Se7 95.26(4) . . ? Se4 Sn3 Se7 100.49(4) . . ? Sn1 Se1 Sn2 83.93(3) . . ? Sn2 Se2 Sn1 88.57(3) . . ? Sn3 Se3 Sn1 94.07(3) . . ? Sn3 Se4 Sn2 100.22(4) . . ? Sn2 Se6 Sn2 90.54(4) 3_657 . ? Sn3 Se7 Sn3 86.45(4) 3_757 . ? C3 N1 C1 109.0(8) . . ? C3 N1 C4 122.7(9) . . ? C1 N1 C4 128.3(10) . . ? C3 N2 C2 109.5(8) . . ? C3 N2 C6 127.0(8) . . ? C2 N2 C6 123.1(8) . . ? C11 N3 C9 108.9(8) . . ? C11 N3 C12 125.6(8) . . ? C9 N3 C12 125.3(8) . . ? C11 N4 C10 109.5(8) . . ? C11 N4 C14 125.7(8) . . ? C10 N4 C14 124.5(9) . . ? C2 C1 N1 108.1(9) . . ? C2 C1 H1A 126.0 . . ? N1 C1 H1A 126.0 . . ? C1 C2 N2 106.2(9) . . ? C1 C2 H2A 126.9 . . ? N2 C2 H2A 126.9 . . ? N2 C3 N1 107.3(7) . . ? N2 C3 C5 127.9(9) . . ? N1 C3 C5 124.9(9) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N2 107.5(8) . . ? C7 C6 H6A 110.2 . . ? N2 C6 H6A 110.2 . . ? C7 C6 H6B 110.2 . . ? N2 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 C7 C8 106.8(9) . . ? C6 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? C6 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N3 107.3(9) . . ? C10 C9 H9A 126.3 . . ? N3 C9 H9A 126.3 . . ? C9 C10 N4 107.2(9) . . ? C9 C10 H10A 126.4 . . ? N4 C10 H10A 126.4 . . ? N4 C11 N3 107.0(8) . . ? N4 C11 C13 126.8(9) . . ? N3 C11 C13 126.1(9) . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 112.3(8) . . ? N4 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.1(9) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.960 _refine_diff_density_min -1.341 _refine_diff_density_rms 0.181 data_compound-3_JL11-25E _database_code_depnum_ccdc_archive 'CCDC 903262' #TrackingRef 'compound 1-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Sn3 Se7, 2(C8 H15 N2)' _chemical_formula_sum 'C16 H30 N4 Se7 Sn3' _chemical_formula_weight 1187.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32 21' _symmetry_space_group_name_Hall 'P 32 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 13.9470(3) _cell_length_b 13.9470(3) _cell_length_c 27.8553(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4692.5(2) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2559 _cell_measurement_theta_min 2.7614 _cell_measurement_theta_max 27.7086 _exptl_crystal_description lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3252 _exptl_absorpt_coefficient_mu 10.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.61967 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10635 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5613 _reflns_number_gt 4159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0500P)^2^+4.0000P] 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 0.010(19) _refine_ls_number_reflns 5613 _refine_ls_number_parameters 353 _refine_ls_number_restraints 894 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.33595(8) 0.43174(7) 0.66673(3) 0.0266(2) Uani 1 1 d . . . Sn2 Sn 0.59769(7) 0.41391(8) 0.66337(3) 0.0281(2) Uani 1 1 d . . . Sn3 Sn 0.31789(8) 0.15357(7) 0.66499(3) 0.0281(2) Uani 1 1 d . . . Se1 Se 0.41628(10) 0.33161(11) 0.72658(4) 0.0259(3) Uani 1 1 d . . . Se2 Se 0.52971(12) 0.54036(11) 0.62935(4) 0.0347(4) Uani 1 1 d . . . Se3 Se 0.27056(13) 0.50512(13) 0.73456(4) 0.0347(4) Uani 1 1 d . . . Se4 Se 0.51088(13) 0.21682(12) 0.62959(5) 0.0386(4) Uani 1 1 d . . . Se5 Se 0.21193(12) 0.24202(12) 0.62840(5) 0.0399(4) Uani 1 1 d . . . Se6 Se 0.25971(13) 0.52458(12) 0.60238(4) 0.0356(4) Uani 1 1 d . . . Se7 Se 0.22512(14) -0.01508(12) 0.60085(4) 0.0417(4) Uani 1 1 d . . . N1 N 0.3169(11) 0.8719(11) 0.4460(4) 0.117(5) Uani 1 1 d DU . . N2 N 0.3823(10) 0.8851(11) 0.5185(4) 0.120(5) Uani 1 1 d DU . . C1 C 0.3852(14) 0.9815(10) 0.4557(5) 0.130(7) Uani 1 1 d DU . . H1A H 0.4010 1.0398 0.4349 0.156 Uiso 1 1 calc R . . C2 C 0.4253(14) 0.9909(10) 0.4998(6) 0.139(7) Uani 1 1 d DU . . H2A H 0.4737 1.0566 0.5153 0.167 Uiso 1 1 calc R . . C3 C 0.3157(14) 0.8145(9) 0.4850(5) 0.112(6) Uani 1 1 d DU . . C4 C 0.2594(15) 0.8250(16) 0.4014(5) 0.133(8) Uani 1 1 d DU . . H4A H 0.2169 0.7459 0.4043 0.199 Uiso 1 1 calc R . . H4B H 0.3122 0.8446 0.3759 0.199 Uiso 1 1 calc R . . H4C H 0.2108 0.8534 0.3945 0.199 Uiso 1 1 calc R . . C5 C 0.2496(14) 0.6942(10) 0.4894(5) 0.092(6) Uani 1 1 d DU . . H5A H 0.2619 0.6721 0.5204 0.139 Uiso 1 1 calc R . . H5B H 0.2707 0.6603 0.4648 0.139 Uiso 1 1 calc R . . H5C H 0.1725 0.6713 0.4860 0.139 Uiso 1 1 calc R . . C6 C 0.4008(14) 0.8597(15) 0.5666(5) 0.125(6) Uani 1 1 d DU . . H6A H 0.3478 0.7824 0.5727 0.150 Uiso 1 1 calc R . . H6B H 0.3838 0.9030 0.5886 0.150 Uiso 1 1 calc R . . C7 C 0.5129(17) 0.878(2) 0.5792(7) 0.172(8) Uani 1 1 d DU . . H7A H 0.5656 0.9572 0.5777 0.207 Uiso 1 1 calc R . . H7B H 0.5115 0.8545 0.6120 0.207 Uiso 1 1 calc R . . C8 C 0.552(2) 0.819(3) 0.5473(10) 0.226(13) Uani 1 1 d DU . . H8A H 0.6241 0.8350 0.5572 0.338 Uiso 1 1 calc R . . H8B H 0.5549 0.8436 0.5148 0.338 Uiso 1 1 calc R . . H8C H 0.5013 0.7410 0.5493 0.338 Uiso 1 1 calc R . . N3 N 0.4026(12) 0.4026(12) 0.5000 0.106(6) Uani 1 2 d SDU A 1 N4 N 0.2241(12) 0.3273(14) 0.4913(8) 0.137(8) Uani 0.50 1 d PDU A 1 C11 C 0.3786(14) 0.4855(13) 0.4904(7) 0.133(9) Uani 0.50 1 d PDU A 1 H11A H 0.4310 0.5634 0.4893 0.160 Uiso 0.50 1 d PR A 1 C12 C 0.2709(14) 0.4386(14) 0.4826(10) 0.121(8) Uani 0.50 1 d PDU A 1 H12A H 0.2323 0.4760 0.4725 0.146 Uiso 0.50 1 d PR A 1 C13 C 0.3069(12) 0.3069(12) 0.5000 0.112(7) Uani 1 2 d SDU A 1 C14 C 0.5138(13) 0.4213(19) 0.5050(10) 0.138(9) Uani 0.50 1 d PDU A 1 H14A H 0.5105 0.3522 0.5118 0.207 Uiso 0.50 1 d PR A 1 H14B H 0.5533 0.4512 0.4756 0.207 Uiso 0.50 1 d PR A 1 H14C H 0.5514 0.4724 0.5307 0.207 Uiso 0.50 1 d PR A 1 C15 C 0.293(2) 0.1969(14) 0.5074(16) 0.140(8) Uani 0.50 1 d PDU A 1 H15A H 0.3638 0.2033 0.5124 0.210 Uiso 0.50 1 d PR A 1 H15B H 0.2474 0.1645 0.5353 0.210 Uiso 0.50 1 d PR A 1 H15C H 0.2576 0.1508 0.4800 0.210 Uiso 0.50 1 d PR A 1 C16 C 0.1071(13) 0.2484(19) 0.4884(12) 0.148(9) Uani 0.50 1 d PDU A 1 H16A H 0.0898 0.2214 0.4560 0.178 Uiso 0.50 1 d PR A 1 H16D H 0.0689 0.2884 0.4946 0.178 Uiso 0.50 1 d PR A 1 C17 C 0.0592(19) 0.157(3) 0.5235(12) 0.147(9) Uani 0.50 1 d PDU A 1 H17A H 0.0908 0.1804 0.5549 0.177 Uiso 0.50 1 d PR A 1 H17B H 0.0805 0.1051 0.5119 0.177 Uiso 0.50 1 d PR A 1 C18 C -0.0645(19) 0.096(2) 0.5254(11) 0.094(11) Uani 0.50 1 d PDU A 1 H18A H -0.0893 0.0339 0.5468 0.142 Uiso 0.50 1 d PR A 1 H18B H -0.0865 0.1462 0.5377 0.142 Uiso 0.50 1 d PR A 1 H18C H -0.0970 0.0700 0.4943 0.142 Uiso 0.50 1 d PR A 1 N3A N 0.836(2) 0.933(2) 0.4946(8) 0.169(11) Uani 0.50 1 d PDU . 2 N4A N 0.893(2) 0.944(2) 0.5682(9) 0.161(10) Uani 0.50 1 d PDU . 2 C11A C 0.880(3) 1.041(2) 0.5095(12) 0.161(11) Uani 0.50 1 d PDU . 2 H11B H 0.8830 1.1001 0.4908 0.193 Uiso 0.50 1 d PR . 2 C12A C 0.917(3) 1.048(2) 0.5541(12) 0.169(11) Uani 0.50 1 d PDU . 2 H12B H 0.9545 1.1147 0.5729 0.203 Uiso 0.50 1 d PR . 2 C13A C 0.844(3) 0.875(2) 0.5312(8) 0.158(11) Uani 0.50 1 d PDU . 2 C14A C 0.791(3) 0.892(3) 0.4473(9) 0.168(11) Uani 0.50 1 d PDU . 2 H14D H 0.7658 0.8136 0.4459 0.252 Uiso 0.50 1 d PR . 2 H14E H 0.7310 0.9040 0.4409 0.252 Uiso 0.50 1 d PR . 2 H14F H 0.8484 0.9294 0.4237 0.252 Uiso 0.50 1 d PR . 2 C15A C 0.806(4) 0.757(2) 0.5301(11) 0.162(11) Uani 0.50 1 d PDU . 2 H15D H 0.8221 0.7350 0.5604 0.244 Uiso 0.50 1 d PR . 2 H15E H 0.7282 0.7162 0.5242 0.244 Uiso 0.50 1 d PR . 2 H15F H 0.8444 0.7421 0.5050 0.244 Uiso 0.50 1 d PR . 2 C16A C 0.915(3) 0.916(3) 0.6156(9) 0.159(11) Uani 0.50 1 d PDU . 2 H16B H 0.9818 0.9790 0.6275 0.191 Uiso 0.50 1 d PR . 2 H16C H 0.9289 0.8557 0.6128 0.191 Uiso 0.50 1 d PR . 2 C17A C 0.825(3) 0.888(3) 0.6520(10) 0.169(11) Uani 0.50 1 d PDU . 2 H17C H 0.8259 0.8374 0.6751 0.203 Uiso 0.50 1 d PR . 2 H17D H 0.7543 0.8510 0.6360 0.203 Uiso 0.50 1 d PR . 2 C18A C 0.839(4) 0.989(5) 0.6773(16) 0.177(13) Uani 0.50 1 d PDU . 2 H18D H 0.7795 0.9675 0.7000 0.265 Uiso 0.50 1 d PR . 2 H18F H 0.9083 1.0257 0.6938 0.265 Uiso 0.50 1 d PR . 2 H18G H 0.8360 1.0395 0.6543 0.265 Uiso 0.50 1 d PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0223(5) 0.0228(5) 0.0388(4) -0.0031(4) 0.0008(4) 0.0143(5) Sn2 0.0172(5) 0.0251(6) 0.0415(4) -0.0052(4) -0.0037(4) 0.0103(4) Sn3 0.0242(5) 0.0188(5) 0.0394(4) 0.0005(4) -0.0003(4) 0.0092(5) Se1 0.0233(7) 0.0233(8) 0.0316(5) -0.0017(6) -0.0034(5) 0.0120(6) Se2 0.0313(9) 0.0321(9) 0.0445(7) 0.0100(6) 0.0096(7) 0.0187(7) Se3 0.0386(9) 0.0465(10) 0.0327(6) -0.0030(7) -0.0019(6) 0.0317(8) Se4 0.0298(9) 0.0307(9) 0.0538(8) -0.0114(7) 0.0052(7) 0.0139(7) Se5 0.0369(9) 0.0298(9) 0.0539(8) -0.0097(7) -0.0208(7) 0.0174(8) Se6 0.0444(10) 0.0450(10) 0.0326(6) 0.0002(7) -0.0010(7) 0.0338(9) Se7 0.0584(11) 0.0223(8) 0.0336(7) -0.0007(6) -0.0036(7) 0.0120(8) N1 0.113(10) 0.110(9) 0.154(10) 0.003(9) 0.044(9) 0.076(8) N2 0.111(9) 0.106(9) 0.159(10) 0.010(8) 0.054(8) 0.067(8) C1 0.121(10) 0.117(10) 0.163(10) 0.015(10) 0.045(10) 0.068(9) C2 0.122(10) 0.131(10) 0.169(10) -0.002(9) 0.035(9) 0.067(9) C3 0.117(10) 0.117(10) 0.129(10) 0.021(9) 0.035(9) 0.079(8) C4 0.131(14) 0.152(14) 0.151(13) 0.036(12) 0.031(11) 0.097(11) C5 0.107(12) 0.097(12) 0.091(10) 0.012(9) 0.022(9) 0.064(10) C6 0.107(10) 0.125(10) 0.164(10) -0.017(9) 0.027(9) 0.073(8) C7 0.155(12) 0.156(12) 0.198(12) -0.015(11) 0.037(11) 0.071(10) C8 0.194(17) 0.238(18) 0.228(17) -0.008(15) 0.019(14) 0.095(13) N3 0.124(8) 0.124(8) 0.081(9) -0.010(5) 0.010(5) 0.071(9) N4 0.138(11) 0.153(11) 0.096(9) -0.037(9) 0.015(9) 0.054(9) C11 0.138(12) 0.142(11) 0.111(10) -0.019(10) 0.022(10) 0.063(9) C12 0.134(11) 0.136(11) 0.100(10) -0.014(9) 0.010(9) 0.073(9) C13 0.131(8) 0.131(8) 0.080(9) -0.007(6) 0.007(6) 0.070(9) C14 0.142(12) 0.151(12) 0.112(11) -0.029(10) 0.007(10) 0.067(10) C15 0.152(11) 0.143(11) 0.104(10) -0.014(9) 0.020(9) 0.059(9) C16 0.146(11) 0.149(12) 0.122(11) -0.019(10) 0.006(10) 0.053(9) C17 0.150(12) 0.151(13) 0.108(11) -0.012(11) -0.011(11) 0.051(10) C18 0.108(18) 0.113(18) 0.090(15) -0.021(14) 0.036(14) 0.077(14) N3A 0.159(13) 0.178(13) 0.163(13) 0.007(10) 0.002(10) 0.079(10) N4A 0.158(12) 0.173(13) 0.164(13) 0.017(10) 0.007(10) 0.092(10) C11A 0.161(13) 0.168(14) 0.159(13) 0.005(11) 0.010(10) 0.086(10) C12A 0.165(13) 0.174(13) 0.166(13) 0.011(10) 0.004(10) 0.083(10) C13A 0.155(13) 0.166(13) 0.167(13) 0.012(10) 0.007(10) 0.090(10) C14A 0.159(14) 0.175(14) 0.160(14) 0.006(11) 0.007(11) 0.076(11) C15A 0.157(13) 0.169(13) 0.170(13) 0.003(10) 0.008(10) 0.088(10) C16A 0.157(13) 0.170(13) 0.161(13) 0.015(10) 0.000(10) 0.090(10) C17A 0.170(14) 0.177(14) 0.165(14) 0.011(11) 0.000(11) 0.089(11) C18A 0.178(15) 0.178(16) 0.166(16) 0.020(12) -0.001(12) 0.082(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Se3 2.5263(14) . ? Sn1 Se5 2.5606(17) . ? Sn1 Se2 2.5667(17) . ? Sn1 Se6 2.7197(15) . ? Sn1 Se1 2.7475(14) . ? Sn2 Se6 2.5119(15) 5_666 ? Sn2 Se2 2.5649(17) . ? Sn2 Se4 2.5651(17) . ? Sn2 Se3 2.7102(15) 5_666 ? Sn2 Se1 2.8134(15) . ? Sn3 Se7 2.5192(15) 5_556 ? Sn3 Se5 2.5627(17) . ? Sn3 Se4 2.5732(17) . ? Sn3 Se7 2.7120(16) . ? Sn3 Se1 2.7541(15) . ? Se3 Sn2 2.7102(15) 5_566 ? Se6 Sn2 2.5119(15) 5_566 ? Se7 Sn3 2.5192(15) 5_556 ? N1 C3 1.345(7) . ? N1 C1 1.363(8) . ? N1 C4 1.445(7) . ? N2 C3 1.336(7) . ? N2 C2 1.387(8) . ? N2 C6 1.442(7) . ? C1 C2 1.330(8) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C5 1.461(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.492(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.487(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N3 C13 1.336(8) . ? N3 C11 1.381(8) . ? N3 C14 1.445(7) . ? N4 C13 1.342(8) . ? N4 C12 1.372(8) . ? N4 C16 1.444(7) . ? C11 C12 1.322(8) . ? C11 H11A 0.9600 . ? C12 H12A 0.9600 . ? C13 C15 1.460(7) . ? C14 H14A 0.9601 . ? C14 H14B 0.9600 . ? C14 H14C 0.9601 . ? C15 H15A 0.9599 . ? C15 H15B 0.9601 . ? C15 H15C 0.9598 . ? C16 C17 1.479(9) . ? C16 H16A 0.9601 . ? C16 H16D 0.9600 . ? C17 C18 1.496(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9601 . ? C18 H18A 0.9600 . ? C18 H18B 0.9601 . ? C18 H18C 0.9599 . ? N3A C13A 1.340(8) . ? N3A C11A 1.374(8) . ? N3A C14A 1.448(7) . ? N4A C13A 1.335(8) . ? N4A C12A 1.380(8) . ? N4A C16A 1.450(7) . ? C11A C12A 1.331(8) . ? C11A H11B 0.9599 . ? C12A H12B 0.9600 . ? C13A C15A 1.459(7) . ? C14A H14D 0.9599 . ? C14A H14E 0.9601 . ? C14A H14F 0.9600 . ? C15A H15D 0.9599 . ? C15A H15E 0.9600 . ? C15A H15F 0.9600 . ? C16A C17A 1.511(10) . ? C16A H16B 0.9601 . ? C16A H16C 0.9599 . ? C17A C18A 1.505(10) . ? C17A H17C 0.9600 . ? C17A H17D 0.9600 . ? C18A H18D 0.9599 . ? C18A H18F 0.9599 . ? C18A H18G 0.9601 . ? 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 Sn1 Se5 122.44(6) . . ? Se3 Sn1 Se2 123.44(6) . . ? Se5 Sn1 Se2 114.12(5) . . ? Se3 Sn1 Se6 89.65(5) . . ? Se5 Sn1 Se6 89.67(5) . . ? Se2 Sn1 Se6 89.91(5) . . ? Se3 Sn1 Se1 94.22(4) . . ? Se5 Sn1 Se1 87.95(5) . . ? Se2 Sn1 Se1 88.26(5) . . ? Se6 Sn1 Se1 176.11(5) . . ? Se6 Sn2 Se2 121.56(6) 5_666 . ? Se6 Sn2 Se4 120.77(6) 5_666 . ? Se2 Sn2 Se4 117.56(5) . . ? Se6 Sn2 Se3 90.16(5) 5_666 5_666 ? Se2 Sn2 Se3 90.41(5) . 5_666 ? Se4 Sn2 Se3 92.84(5) . 5_666 ? Se6 Sn2 Se1 92.72(4) 5_666 . ? Se2 Sn2 Se1 86.88(5) . . ? Se4 Sn2 Se1 86.91(5) . . ? Se3 Sn2 Se1 176.79(5) 5_666 . ? Se7 Sn3 Se5 122.37(6) 5_556 . ? Se7 Sn3 Se4 121.60(6) 5_556 . ? Se5 Sn3 Se4 116.02(6) . . ? Se7 Sn3 Se7 89.47(5) 5_556 . ? Se5 Sn3 Se7 90.90(5) . . ? Se4 Sn3 Se7 90.49(5) . . ? Se7 Sn3 Se1 93.20(5) 5_556 . ? Se5 Sn3 Se1 87.76(5) . . ? Se4 Sn3 Se1 88.02(5) . . ? Se7 Sn3 Se1 177.32(5) . . ? Sn1 Se1 Sn3 86.23(4) . . ? Sn1 Se1 Sn2 85.70(4) . . ? Sn3 Se1 Sn2 85.35(4) . . ? Sn2 Se2 Sn1 94.96(5) . . ? Sn1 Se3 Sn2 89.95(4) . 5_566 ? Sn2 Se4 Sn3 94.54(5) . . ? Sn1 Se5 Sn3 94.44(5) . . ? Sn2 Se6 Sn1 90.04(4) 5_566 . ? Sn3 Se7 Sn3 90.29(5) 5_556 . ? C3 N1 C1 107.5(5) . . ? C3 N1 C4 125.9(8) . . ? C1 N1 C4 126.6(8) . . ? C3 N2 C2 107.0(5) . . ? C3 N2 C6 127.7(8) . . ? C2 N2 C6 125.1(8) . . ? C2 C1 N1 108.5(6) . . ? C2 C1 H1A 125.8 . . ? N1 C1 H1A 125.8 . . ? C1 C2 N2 107.8(6) . . ? C1 C2 H2A 126.1 . . ? N2 C2 H2A 126.1 . . ? N2 C3 N1 109.2(5) . . ? N2 C3 C5 126.5(7) . . ? N1 C3 C5 124.3(7) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 118.5(9) . . ? N2 C6 H6A 107.7 . . ? C7 C6 H6A 107.7 . . ? N2 C6 H6B 107.7 . . ? C7 C6 H6B 107.7 . . ? H6A C6 H6B 107.1 . . ? C8 C7 C6 113.7(9) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 N3 C11 107.3(5) . . ? C13 N3 C14 128.8(8) . . ? C11 N3 C14 123.8(8) . . ? C13 N4 C12 107.4(5) . . ? C13 N4 C16 127.8(8) . . ? C12 N4 C16 124.7(8) . . ? C12 C11 N3 108.0(6) . . ? C12 C11 H11A 126.1 . . ? N3 C11 H11A 125.9 . . ? C11 C12 N4 108.1(6) . . ? C11 C12 H12A 125.9 . . ? N4 C12 H12A 126.0 . . ? N3 C13 N4 108.9(5) . . ? N3 C13 C15 126.4(8) . . ? N4 C13 C15 124.7(8) . . ? N3 C14 H14A 109.3 . . ? N3 C14 H14B 109.0 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 110.1 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.4 . . ? C13 C15 H15B 108.8 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 110.3 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 118.2(10) . . ? N4 C16 H16A 108.6 . . ? C17 C16 H16A 111.4 . . ? N4 C16 H16D 107.0 . . ? C17 C16 H16D 104.0 . . ? H16A C16 H16D 107.1 . . ? C16 C17 C18 114.1(11) . . ? C16 C17 H17A 111.8 . . ? C18 C17 H17A 111.3 . . ? C16 C17 H17B 104.6 . . ? C18 C17 H17B 106.7 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.0 . . ? C17 C18 H18B 107.3 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 112.0 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13A N3A C11A 107.5(5) . . ? C13A N3A C14A 127.1(8) . . ? C11A N3A C14A 125.4(8) . . ? C13A N4A C12A 107.7(5) . . ? C13A N4A C16A 127.9(8) . . ? C12A N4A C16A 124.4(8) . . ? C12A C11A N3A 108.1(6) . . ? C12A C11A H11B 126.1 . . ? N3A C11A H11B 125.7 . . ? C11A C12A N4A 107.6(6) . . ? C11A C12A H12B 126.0 . . ? N4A C12A H12B 126.4 . . ? N4A C13A N3A 109.0(5) . . ? N4A C13A C15A 126.3(8) . . ? N3A C13A C15A 124.8(8) . . ? N3A C14A H14D 109.3 . . ? N3A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? N3A C14A H14F 109.6 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C13A C15A H15D 109.3 . . ? C13A C15A H15E 109.7 . . ? H15D C15A H15E 109.5 . . ? C13A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? N4A C16A C17A 114.7(10) . . ? N4A C16A H16B 108.4 . . ? C17A C16A H16B 108.0 . . ? N4A C16A H16C 108.7 . . ? C17A C16A H16C 109.3 . . ? H16B C16A H16C 107.5 . . ? C18A C17A C16A 111.6(10) . . ? C18A C17A H17C 109.7 . . ? C16A C17A H17C 108.9 . . ? C18A C17A H17D 109.7 . . ? C16A C17A H17D 109.0 . . ? H17C C17A H17D 108.0 . . ? C17A C18A H18D 108.7 . . ? C17A C18A H18F 109.8 . . ? H18D C18A H18F 109.5 . . ? C17A C18A H18G 109.8 . . ? H18D C18A H18G 109.5 . . ? H18F C18A H18G 109.5 . . ? 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 Sn1 Se1 Sn3 136.17(5) . . . . ? Se5 Sn1 Se1 Sn3 13.80(5) . . . . ? Se2 Sn1 Se1 Sn3 -100.42(4) . . . . ? Se6 Sn1 Se1 Sn3 -38.5(9) . . . . ? Se3 Sn1 Se1 Sn2 -138.21(5) . . . . ? Se5 Sn1 Se1 Sn2 99.41(5) . . . . ? Se2 Sn1 Se1 Sn2 -14.80(4) . . . . ? Se6 Sn1 Se1 Sn2 47.1(9) . . . . ? Se7 Sn3 Se1 Sn1 -136.09(5) 5_556 . . . ? Se5 Sn3 Se1 Sn1 -13.79(5) . . . . ? Se4 Sn3 Se1 Sn1 102.36(5) . . . . ? Se7 Sn3 Se1 Sn1 46.3(13) . . . . ? Se7 Sn3 Se1 Sn2 137.92(5) 5_556 . . . ? Se5 Sn3 Se1 Sn2 -99.77(5) . . . . ? Se4 Sn3 Se1 Sn2 16.38(5) . . . . ? Se7 Sn3 Se1 Sn2 -39.7(13) . . . . ? Se6 Sn2 Se1 Sn1 136.30(5) 5_666 . . . ? Se2 Sn2 Se1 Sn1 14.83(5) . . . . ? Se4 Sn2 Se1 Sn1 -103.01(5) . . . . ? Se3 Sn2 Se1 Sn1 -17.4(10) 5_666 . . . ? Se6 Sn2 Se1 Sn3 -137.13(5) 5_666 . . . ? Se2 Sn2 Se1 Sn3 101.39(5) . . . . ? Se4 Sn2 Se1 Sn3 -16.44(5) . . . . ? Se3 Sn2 Se1 Sn3 69.1(10) 5_666 . . . ? Se6 Sn2 Se2 Sn1 -107.19(6) 5_666 . . . ? Se4 Sn2 Se2 Sn1 68.96(6) . . . . ? Se3 Sn2 Se2 Sn1 162.37(5) 5_666 . . . ? Se1 Sn2 Se2 Sn1 -15.92(5) . . . . ? Se3 Sn1 Se2 Sn2 110.20(6) . . . . ? Se5 Sn1 Se2 Sn2 -70.68(6) . . . . ? Se6 Sn1 Se2 Sn2 -160.28(5) . . . . ? Se1 Sn1 Se2 Sn2 16.29(5) . . . . ? Se5 Sn1 Se3 Sn2 -86.10(7) . . . 5_566 ? Se2 Sn1 Se3 Sn2 92.95(6) . . . 5_566 ? Se6 Sn1 Se3 Sn2 3.29(6) . . . 5_566 ? Se1 Sn1 Se3 Sn2 -176.35(5) . . . 5_566 ? Se6 Sn2 Se4 Sn3 108.96(6) 5_666 . . . ? Se2 Sn2 Se4 Sn3 -67.22(6) . . . . ? Se3 Sn2 Se4 Sn3 -159.16(5) 5_666 . . . ? Se1 Sn2 Se4 Sn3 17.64(5) . . . . ? Se7 Sn3 Se4 Sn2 -110.55(6) 5_556 . . . ? Se5 Sn3 Se4 Sn2 68.53(7) . . . . ? Se7 Sn3 Se4 Sn2 159.77(5) . . . . ? Se1 Sn3 Se4 Sn2 -18.01(5) . . . . ? Se3 Sn1 Se5 Sn3 -108.56(6) . . . . ? Se2 Sn1 Se5 Sn3 72.31(7) . . . . ? Se6 Sn1 Se5 Sn3 162.07(5) . . . . ? Se1 Sn1 Se5 Sn3 -14.86(5) . . . . ? Se7 Sn3 Se5 Sn1 107.20(7) 5_556 . . . ? Se4 Sn3 Se5 Sn1 -71.87(7) . . . . ? Se7 Sn3 Se5 Sn1 -162.85(5) . . . . ? Se1 Sn3 Se5 Sn1 14.83(5) . . . . ? Se3 Sn1 Se6 Sn2 -3.55(6) . . . 5_566 ? Se5 Sn1 Se6 Sn2 118.89(6) . . . 5_566 ? Se2 Sn1 Se6 Sn2 -126.99(5) . . . 5_566 ? Se1 Sn1 Se6 Sn2 171.1(8) . . . 5_566 ? Se7 Sn3 Se7 Sn3 -5.35(9) 5_556 . . 5_556 ? Se5 Sn3 Se7 Sn3 -127.72(6) . . . 5_556 ? Se4 Sn3 Se7 Sn3 116.25(5) . . . 5_556 ? Se1 Sn3 Se7 Sn3 172.3(12) . . . 5_556 ? C3 N1 C1 C2 0.3(15) . . . . ? C4 N1 C1 C2 -177.6(16) . . . . ? N1 C1 C2 N2 0.3(18) . . . . ? C3 N2 C2 C1 -1(2) . . . . ? C6 N2 C2 C1 -176.4(12) . . . . ? C2 N2 C3 N1 1(2) . . . . ? C6 N2 C3 N1 176.4(12) . . . . ? C2 N2 C3 C5 -177.9(19) . . . . ? C6 N2 C3 C5 -2(3) . . . . ? C1 N1 C3 N2 -0.8(17) . . . . ? C4 N1 C3 N2 177.1(13) . . . . ? C1 N1 C3 C5 178.2(17) . . . . ? C4 N1 C3 C5 -4(3) . . . . ? C3 N2 C6 C7 114.0(19) . . . . ? C2 N2 C6 C7 -71(2) . . . . ? N2 C6 C7 C8 -56(3) . . . . ? C13 N3 C11 C14 170(4) . . . 4_556 ? C11 N3 C11 C14 -10(4) 4_556 . . 4_556 ? C14 N3 C11 C14 -14(6) . . . 4_556 ? C13 N3 C11 C12 -2.8(17) . . . . ? C11 N3 C11 C12 177.2(17) 4_556 . . . ? C14 N3 C11 C12 172.9(18) . . . . ? C14 N3 C11 C12 -173(5) 4_556 . . . ? C14 C11 C12 N4 -148(16) 4_556 . . . ? N3 C11 C12 N4 5(2) . . . . ? C14 C11 C12 C15 -148(15) 4_556 . . 4_556 ? N3 C11 C12 C15 5(3) . . . 4_556 ? N3 C11 C12 C14 154(17) . . . 4_556 ? C15 N4 C12 C11 178(100) 4_556 . . . ? C13 N4 C12 C11 -6(2) . . . . ? C16 N4 C12 C11 177.6(16) . . . . ? C13 N4 C12 C15 177(24) . . . 4_556 ? C16 N4 C12 C15 0(22) . . . 4_556 ? C15 N4 C12 C14 175(22) 4_556 . . 4_556 ? C13 N4 C12 C14 -8(3) . . . 4_556 ? C16 N4 C12 C14 175.1(17) . . . 4_556 ? C11 N3 C13 N4 179.3(15) 4_556 . . . ? C11 N3 C13 N4 -0.7(15) . . . . ? C14 N3 C13 N4 -176.1(16) . . . . ? C14 N3 C13 N4 3.9(16) 4_556 . . . ? C11 N3 C13 N4 -0.7(15) 4_556 . . 4_556 ? C11 N3 C13 N4 179.3(15) . . . 4_556 ? C14 N3 C13 N4 3.9(16) . . . 4_556 ? C14 N3 C13 N4 -176.1(16) 4_556 . . 4_556 ? C11 N3 C13 C15 178.5(19) 4_556 . . 4_556 ? C11 N3 C13 C15 -1.5(19) . . . 4_556 ? C14 N3 C13 C15 -177(3) . . . 4_556 ? C14 N3 C13 C15 3(3) 4_556 . . 4_556 ? C11 N3 C13 C15 -1.5(19) 4_556 . . . ? C11 N3 C13 C15 178.5(19) . . . . ? C14 N3 C13 C15 3(3) . . . . ? C14 N3 C13 C15 -177(3) 4_556 . . . ? C15 N4 C13 N3 -178(8) 4_556 . . . ? C12 N4 C13 N3 4(2) . . . . ? C16 N4 C13 N3 -179.5(13) . . . . ? C15 N4 C13 N4 2(8) 4_556 . . 4_556 ? C12 N4 C13 N4 -176(2) . . . 4_556 ? C16 N4 C13 N4 0.5(13) . . . 4_556 ? C12 N4 C13 C15 -179(10) . . . 4_556 ? C16 N4 C13 C15 -2(8) . . . 4_556 ? C15 N4 C13 C15 3(11) 4_556 . . . ? C12 N4 C13 C15 -175(2) . . . . ? C16 N4 C13 C15 1(4) . . . . ? C13 N3 C14 C11 -12(5) . . . 4_556 ? C11 N3 C14 C11 173(3) . . . 4_556 ? C14 N3 C14 C11 168(5) 4_556 . . 4_556 ? C13 N3 C14 C12 -7.1(19) . . . 4_556 ? C11 N3 C14 C12 5(3) 4_556 . . 4_556 ? C11 N3 C14 C12 178.1(12) . . . 4_556 ? C14 N3 C14 C12 172.9(19) 4_556 . . 4_556 ? N3 C13 C15 N4 3(10) . . . 4_556 ? N4 C13 C15 N4 -178(6) . . . 4_556 ? C15 C13 C15 N4 -177(10) 4_556 . . 4_556 ? N3 C13 C15 C16 178(13) . . . 4_556 ? N4 C13 C15 C16 -3(16) . . . 4_556 ? N4 C13 C15 C16 175(22) 4_556 . . 4_556 ? C15 C13 C15 C16 -2(13) 4_556 . . 4_556 ? N3 C13 C15 C12 4(3) . . . 4_556 ? N4 C13 C15 C12 -177.2(14) . . . 4_556 ? N4 C13 C15 C12 1(7) 4_556 . . 4_556 ? C15 C13 C15 C12 -176(3) 4_556 . . 4_556 ? C13 N4 C16 C15 4(16) . . . 4_556 ? C12 N4 C16 C15 180(100) . . . 4_556 ? C15 N4 C16 C17 37(16) 4_556 . . . ? C13 N4 C16 C17 41(3) . . . . ? C12 N4 C16 C17 -143(3) . . . . ? C15 C16 C17 C18 174(4) 4_556 . . . ? N4 C16 C17 C18 166(3) . . . . ? C13A N3A C11A C12A 1(2) . . . . ? C14A N3A C11A C12A -176(2) . . . . ? C15A N3A C11A C12A 141(8) 4_556 . . . ? C13A N3A C11A C12A -85(3) 4_556 . . . ? N3A C11A C12A N4A -2(2) . . . . ? C13A N4A C12A C11A 2(3) . . . . ? C16A N4A C12A C11A -176.7(17) . . . . ? C12A N4A C13A N3A -1(3) . . . . ? C16A N4A C13A N3A 177.6(17) . . . . ? C12A N4A C13A C15A 179(3) . . . . ? C16A N4A C13A C15A -2(4) . . . . ? C12A N4A C13A C14A 153(2) . . . 4_556 ? C16A N4A C13A C14A -28(3) . . . 4_556 ? C12A N4A C13A N3A 108(2) . . . 4_556 ? C16A N4A C13A N3A -74(3) . . . 4_556 ? C12A N4A C13A C13A 68(4) . . . 4_556 ? C16A N4A C13A C13A -113(3) . . . 4_556 ? C11A N3A C13A N4A 0(2) . . . . ? C14A N3A C13A N4A 177.8(18) . . . . ? C15A N3A C13A N4A -171(3) 4_556 . . . ? C13A N3A C13A N4A 139(2) 4_556 . . . ? C11A N3A C13A C15A 180(2) . . . . ? C14A N3A C13A C15A -2(4) . . . . ? C15A N3A C13A C15A 9(4) 4_556 . . . ? C13A N3A C13A C15A -41(3) 4_556 . . . ? C11A N3A C13A C14A -123(4) . . . 4_556 ? C14A N3A C13A C14A 55(5) . . . 4_556 ? C15A N3A C13A C14A 66(5) 4_556 . . 4_556 ? C13A N3A C13A C14A 16(5) 4_556 . . 4_556 ? C11A N3A C13A N3A -116.6(15) . . . 4_556 ? C14A N3A C13A N3A 61(3) . . . 4_556 ? C15A N3A C13A N3A 73(2) 4_556 . . 4_556 ? C13A N3A C13A N3A 22.3(15) 4_556 . . 4_556 ? C11A N3A C13A C13A -138.8(16) . . . 4_556 ? C14A N3A C13A C13A 39.0(19) . . . 4_556 ? C15A N3A C13A C13A 50.5(12) 4_556 . . 4_556 ? C13A N3A C14A C15A 16(4) . . . 4_556 ? C11A N3A C14A C15A -166(3) . . . 4_556 ? C13A N3A C14A C15A 59(2) 4_556 . . 4_556 ? C13A N3A C14A C13A -42(2) . . . 4_556 ? C11A N3A C14A C13A 135.1(17) . . . 4_556 ? C15A N3A C14A C13A -59(2) 4_556 . . 4_556 ? N4A C13A C15A C14A -39(4) . . . 4_556 ? N3A C13A C15A C14A 142(3) . . . 4_556 ? N3A C13A C15A C14A 59(2) 4_556 . . 4_556 ? C13A C13A C15A C14A 104(3) 4_556 . . 4_556 ? N4A C13A C15A N3A -97(3) . . . 4_556 ? N3A C13A C15A N3A 83(3) . . . 4_556 ? C14A C13A C15A N3A -59(2) 4_556 . . 4_556 ? C13A C13A C15A N3A 45.1(11) 4_556 . . 4_556 ? C13A N4A C16A C17A -91(3) . . . . ? C12A N4A C16A C17A 88(3) . . . . ? N4A C16A C17A C18A -88(3) . . . . ? N4A C16A C17A C18A -72(2) . . . 5_676 ? C16A C17A C18A C18A 44(4) . . . 5_676 ? C16A C17A C18A C17A -14(7) . . . 5_676 ? C18A C17A C18A C17A -58(6) 5_676 . . 5_676 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.140 _refine_diff_density_min -1.271 _refine_diff_density_rms 0.194 data_compound-4_JL7-48E _database_code_depnum_ccdc_archive 'CCDC 903263' #TrackingRef 'compound 1-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Se7 Sn3,2(C9 H17 N2)' _chemical_formula_sum 'C18 H34 N4 Se7 Sn3' _chemical_formula_weight 1215.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 24.538(4) _cell_length_b 13.961(2) _cell_length_c 19.434(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.539(3) _cell_angle_gamma 90.00 _cell_volume 6637(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13845 _cell_measurement_theta_min 3.0098 _cell_measurement_theta_max 27.4835 _exptl_crystal_description lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 9.933 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4964 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 15819 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50421 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.49 _reflns_number_total 15171 _reflns_number_gt 12041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0541P)^2^+10.3742P] 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 15171 _refine_ls_number_parameters 721 _refine_ls_number_restraints 1923 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.379 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.19433(2) 0.33341(3) 0.08713(3) 0.03317(13) Uani 1 1 d . . . Sn2 Sn 0.07345(2) 0.48805(4) 0.02901(3) 0.03731(14) Uani 1 1 d U . . Sn3 Sn 0.20682(2) 0.60078(3) 0.09372(3) 0.03308(13) Uani 1 1 d . . . Sn4 Sn 0.27613(2) 0.82715(4) 0.14058(3) 0.03835(14) Uani 1 1 d . . . Sn5 Sn 0.39426(2) 0.98763(4) 0.17810(3) 0.03725(14) Uani 1 1 d . . . Sn6 Sn 0.26248(2) 1.10628(4) 0.13274(3) 0.04011(15) Uani 1 1 d . . . Se1 Se 0.25376(4) 0.20128(6) 0.02320(5) 0.0447(2) Uani 1 1 d . . . Se2 Se 0.19759(4) 0.22702(6) 0.19294(5) 0.0427(2) Uani 1 1 d . . . Se3 Se 0.13783(3) 0.47478(5) 0.15247(4) 0.03244(17) Uani 1 1 d U . . Se4 Se 0.26769(3) 0.45928(5) 0.06867(5) 0.03852(19) Uani 1 1 d . . . Se5 Se 0.13031(3) 0.63460(6) -0.00078(5) 0.0425(2) Uani 1 1 d . . . Se6 Se -0.01208(3) 0.50517(7) 0.09218(5) 0.0489(2) Uani 1 1 d . . . Se7 Se 0.11425(3) 0.32673(6) -0.00492(4) 0.0423(2) Uani 1 1 d . . . Se8 Se 0.22138(4) 0.69578(6) 0.20511(4) 0.04073(19) Uani 1 1 d . . . Se9 Se 0.27699(4) 0.72368(6) 0.03574(5) 0.0463(2) Uani 1 1 d . . . Se10 Se 0.33771(3) 0.97510(6) 0.06441(4) 0.04101(19) Uani 1 1 d . . . Se11 Se 0.35680(3) 0.83476(6) 0.23160(4) 0.0428(2) Uani 1 1 d . . . Se12 Se 0.20482(3) 0.95784(6) 0.15131(5) 0.0420(2) Uani 1 1 d . . . Se13 Se 0.49249(4) 1.00122(8) 0.18943(7) 0.0655(3) Uani 1 1 d . . . Se14 Se 0.34082(3) 1.12791(6) 0.22562(4) 0.0429(2) Uani 1 1 d . . . N1A N 0.1955(5) 0.4507(8) -0.1492(6) 0.061(2) Uani 0.678(7) 1 d PDU A 1 N2A N 0.2802(5) 0.4749(9) -0.1136(7) 0.067(2) Uani 0.678(7) 1 d PDU A 1 C1A C 0.2170(7) 0.3654(11) -0.1318(9) 0.063(3) Uani 0.678(7) 1 d PDU A 1 H1A H 0.1990 0.3068 -0.1345 0.076 Uiso 0.678(7) 1 calc PR A 1 C2A C 0.2701(7) 0.3804(10) -0.1094(9) 0.067(3) Uani 0.678(7) 1 d PDU A 1 H2A H 0.2951 0.3336 -0.0938 0.081 Uiso 0.678(7) 1 calc PR A 1 C3A C 0.2341(5) 0.5183(9) -0.1380(8) 0.061(2) Uani 0.678(7) 1 d PDU A 1 C4A C 0.1410(6) 0.4645(13) -0.1773(13) 0.068(4) Uani 0.678(7) 1 d PDU A 1 H4A H 0.1319 0.4164 -0.2116 0.102 Uiso 0.678(7) 1 calc PR A 1 H4B H 0.1376 0.5268 -0.1981 0.102 Uiso 0.678(7) 1 calc PR A 1 H4C H 0.1166 0.4597 -0.1412 0.102 Uiso 0.678(7) 1 calc PR A 1 C5A C 0.2274(7) 0.6262(9) -0.1506(9) 0.058(3) Uani 0.678(7) 1 d PDU A 1 H5A H 0.2614 0.6580 -0.1377 0.086 Uiso 0.678(7) 1 calc PR A 1 H5B H 0.1995 0.6507 -0.1234 0.086 Uiso 0.678(7) 1 calc PR A 1 H5C H 0.2171 0.6375 -0.1986 0.086 Uiso 0.678(7) 1 calc PR A 1 C6A C 0.3296(7) 0.5261(12) -0.0950(13) 0.083(3) Uani 0.678(7) 1 d PDU A 1 H6A H 0.3254 0.5647 -0.0543 0.099 Uiso 0.678(7) 1 calc PR A 1 H6B H 0.3381 0.5683 -0.1323 0.099 Uiso 0.678(7) 1 calc PR A 1 C7A C 0.3757(6) 0.4538(13) -0.0805(12) 0.103(3) Uani 0.678(7) 1 d PDU A 1 H7A H 0.3810 0.4157 -0.1212 0.124 Uiso 0.678(7) 1 calc PR A 1 H7B H 0.3680 0.4113 -0.0430 0.124 Uiso 0.678(7) 1 calc PR A 1 C8A C 0.4262(8) 0.5162(16) -0.0605(14) 0.118(4) Uani 0.678(7) 1 d PDU A 1 H8A H 0.4200 0.5809 -0.0774 0.142 Uiso 0.678(7) 1 calc PR A 1 H8B H 0.4328 0.5187 -0.0107 0.142 Uiso 0.678(7) 1 calc PR A 1 C9A C 0.4755(7) 0.4733(19) -0.0920(16) 0.140(7) Uani 0.678(7) 1 d PDU A 1 H9A H 0.5073 0.5109 -0.0786 0.209 Uiso 0.678(7) 1 calc PR A 1 H9B H 0.4692 0.4732 -0.1413 0.209 Uiso 0.678(7) 1 calc PR A 1 H9C H 0.4810 0.4088 -0.0758 0.209 Uiso 0.678(7) 1 calc PR A 1 N1B N 0.1948(10) 0.5169(18) -0.1561(14) 0.061(2) Uani 0.322(7) 1 d PDU A 2 N2B N 0.2812(11) 0.5251(18) -0.1197(16) 0.067(2) Uani 0.322(7) 1 d PDU A 2 C1B C 0.2076(16) 0.610(2) -0.159(2) 0.063(3) Uani 0.322(7) 1 d PDU A 2 H1B H 0.1848 0.6608 -0.1724 0.076 Uiso 0.322(7) 1 calc PR A 2 C2B C 0.2625(15) 0.613(2) -0.1365(18) 0.067(3) Uani 0.322(7) 1 d PDU A 2 H2B H 0.2836 0.6684 -0.1336 0.081 Uiso 0.322(7) 1 calc PR A 2 C3B C 0.2391(10) 0.4662(17) -0.1345(17) 0.061(2) Uani 0.322(7) 1 d PDU A 2 C4B C 0.1385(11) 0.497(3) -0.173(3) 0.068(4) Uani 0.322(7) 1 d PDU A 2 H4D H 0.1325 0.4290 -0.1708 0.102 Uiso 0.322(7) 1 calc PR A 2 H4E H 0.1278 0.5199 -0.2183 0.102 Uiso 0.322(7) 1 calc PR A 2 H4F H 0.1171 0.5282 -0.1400 0.102 Uiso 0.322(7) 1 calc PR A 2 C5B C 0.2411(15) 0.3578(17) -0.124(2) 0.058(3) Uani 0.322(7) 1 d PDU A 2 H5D H 0.2772 0.3393 -0.1060 0.086 Uiso 0.322(7) 1 calc PR A 2 H5E H 0.2319 0.3260 -0.1668 0.086 Uiso 0.322(7) 1 calc PR A 2 H5F H 0.2154 0.3399 -0.0912 0.086 Uiso 0.322(7) 1 calc PR A 2 C6B C 0.3364(17) 0.493(3) -0.104(3) 0.083(3) Uani 0.322(7) 1 d PDU A 2 H6C H 0.3527 0.4751 -0.1456 0.099 Uiso 0.322(7) 1 calc PR A 2 H6D H 0.3365 0.4369 -0.0739 0.099 Uiso 0.322(7) 1 calc PR A 2 C7B C 0.3692(13) 0.574(3) -0.067(2) 0.103(3) Uani 0.322(7) 1 d PDU A 2 H7C H 0.3539 0.5861 -0.0232 0.124 Uiso 0.322(7) 1 calc PR A 2 H7D H 0.3638 0.6315 -0.0947 0.124 Uiso 0.322(7) 1 calc PR A 2 C8B C 0.4312(15) 0.558(4) -0.053(2) 0.118(4) Uani 0.322(7) 1 d PDU A 2 H8C H 0.4492 0.6174 -0.0384 0.142 Uiso 0.322(7) 1 calc PR A 2 H8D H 0.4382 0.5113 -0.0159 0.142 Uiso 0.322(7) 1 calc PR A 2 C9B C 0.4532(18) 0.521(4) -0.120(3) 0.123(9) Uani 0.322(7) 1 d PDU A 2 H9D H 0.4922 0.5156 -0.1134 0.185 Uiso 0.322(7) 1 calc PR A 2 H9E H 0.4433 0.5651 -0.1564 0.185 Uiso 0.322(7) 1 calc PR A 2 H9F H 0.4376 0.4594 -0.1308 0.185 Uiso 0.322(7) 1 calc PR A 2 N3A N 0.5043(6) 0.2405(12) -0.1321(8) 0.069(2) Uani 0.552(7) 1 d PDU B 1 N4A N 0.4886(5) 0.1745(12) -0.0357(8) 0.070(2) Uani 0.552(7) 1 d PDU B 1 C10A C 0.5526(6) 0.2495(16) -0.0972(9) 0.072(3) Uani 0.552(7) 1 d PDU B 1 H10A H 0.5847 0.2778 -0.1097 0.086 Uiso 0.552(7) 1 calc PR B 1 C11A C 0.5404(7) 0.2014(16) -0.0327(12) 0.074(3) Uani 0.552(7) 1 d PDU B 1 H11A H 0.5657 0.1914 0.0049 0.089 Uiso 0.552(7) 1 calc PR B 1 C12A C 0.4664(8) 0.1984(15) -0.0965(8) 0.069(2) Uani 0.552(7) 1 d PDU B 1 C13A C 0.5011(10) 0.276(2) -0.2023(9) 0.088(4) Uani 0.552(7) 1 d PDU B 1 H13A H 0.5316 0.3173 -0.2081 0.132 Uiso 0.552(7) 1 calc PR B 1 H13B H 0.4676 0.3103 -0.2118 0.132 Uiso 0.552(7) 1 calc PR B 1 H13C H 0.5022 0.2225 -0.2335 0.132 Uiso 0.552(7) 1 calc PR B 1 C14A C 0.4072(10) 0.182(2) -0.1290(13) 0.073(4) Uani 0.552(7) 1 d PU B 1 H14A H 0.3858 0.1524 -0.0958 0.109 Uiso 0.552(7) 1 calc PR B 1 H14B H 0.4080 0.1421 -0.1689 0.109 Uiso 0.552(7) 1 calc PR B 1 H14C H 0.3912 0.2431 -0.1424 0.109 Uiso 0.552(7) 1 calc PR B 1 C15A C 0.4503(8) 0.1396(15) 0.0102(7) 0.082(3) Uani 0.552(7) 1 d PDU B 1 H15A H 0.4553 0.0721 0.0205 0.098 Uiso 0.552(7) 1 calc PR B 1 H15B H 0.4127 0.1517 -0.0068 0.098 Uiso 0.552(7) 1 calc PR B 1 C16A C 0.4698(8) 0.2063(16) 0.0738(11) 0.088(3) Uani 0.552(7) 1 d PDU B 1 H16A H 0.4755 0.1715 0.1169 0.105 Uiso 0.552(7) 1 calc PR B 1 H16B H 0.5018 0.2442 0.0657 0.105 Uiso 0.552(7) 1 calc PR B 1 C17A C 0.4169(9) 0.2646(17) 0.0680(12) 0.089(3) Uani 0.552(7) 1 d PDU B 1 H17A H 0.4137 0.2942 0.0227 0.107 Uiso 0.552(7) 1 calc PR B 1 H17B H 0.3867 0.2197 0.0692 0.107 Uiso 0.552(7) 1 calc PR B 1 C18A C 0.4082(13) 0.343(2) 0.1209(16) 0.086(5) Uani 0.552(7) 1 d PDU B 1 H18A H 0.3741 0.3746 0.1091 0.129 Uiso 0.552(7) 1 calc PR B 1 H18B H 0.4375 0.3886 0.1210 0.129 Uiso 0.552(7) 1 calc PR B 1 H18C H 0.4078 0.3149 0.1660 0.129 Uiso 0.552(7) 1 calc PR B 1 N3B N 0.4661(8) 0.2277(15) -0.1450(9) 0.069(2) Uani 0.448(7) 1 d PDU B 2 N4B N 0.4565(7) 0.1675(15) -0.0483(9) 0.070(2) Uani 0.448(7) 1 d PDU B 2 C10B C 0.4146(10) 0.198(2) -0.1471(15) 0.072(3) Uani 0.448(7) 1 d PDU B 2 H10B H 0.3883 0.2038 -0.1840 0.086 Uiso 0.448(7) 1 calc PR B 2 C11B C 0.4077(8) 0.156(2) -0.0817(13) 0.074(3) Uani 0.448(7) 1 d PDU B 2 H11B H 0.3767 0.1274 -0.0662 0.089 Uiso 0.448(7) 1 calc PR B 2 C12B C 0.4928(9) 0.2089(19) -0.0840(9) 0.069(2) Uani 0.448(7) 1 d PDU B 2 C13B C 0.4820(12) 0.262(3) -0.2110(13) 0.088(4) Uani 0.448(7) 1 d PDU B 2 H13D H 0.4507 0.2626 -0.2439 0.132 Uiso 0.448(7) 1 calc PR B 2 H13E H 0.5095 0.2207 -0.2270 0.132 Uiso 0.448(7) 1 calc PR B 2 H13F H 0.4963 0.3259 -0.2056 0.132 Uiso 0.448(7) 1 calc PR B 2 C14B C 0.5511(11) 0.230(2) -0.0696(15) 0.073(4) Uani 0.448(7) 1 d PU B 2 H14D H 0.5622 0.2135 -0.0225 0.109 Uiso 0.448(7) 1 calc PR B 2 H14E H 0.5576 0.2965 -0.0770 0.109 Uiso 0.448(7) 1 calc PR B 2 H14F H 0.5719 0.1923 -0.0998 0.109 Uiso 0.448(7) 1 calc PR B 2 C15B C 0.4766(10) 0.1450(19) 0.0212(9) 0.082(3) Uani 0.448(7) 1 d PDU B 2 H15C H 0.5108 0.1764 0.0359 0.098 Uiso 0.448(7) 1 calc PR B 2 H15D H 0.4785 0.0769 0.0309 0.098 Uiso 0.448(7) 1 calc PR B 2 C16B C 0.4243(10) 0.1962(19) 0.0475(15) 0.088(3) Uani 0.448(7) 1 d PDU B 2 H16C H 0.4008 0.2224 0.0096 0.105 Uiso 0.448(7) 1 calc PR B 2 H16D H 0.4033 0.1533 0.0745 0.105 Uiso 0.448(7) 1 calc PR B 2 C17B C 0.4523(12) 0.2750(19) 0.0921(15) 0.089(3) Uani 0.448(7) 1 d PDU B 2 H17C H 0.4743 0.3110 0.0618 0.107 Uiso 0.448(7) 1 calc PR B 2 H17D H 0.4778 0.2426 0.1249 0.107 Uiso 0.448(7) 1 calc PR B 2 C18B C 0.4229(15) 0.349(3) 0.134(2) 0.086(5) Uani 0.448(7) 1 d PDU B 2 H18D H 0.4494 0.3871 0.1607 0.129 Uiso 0.448(7) 1 calc PR B 2 H18E H 0.3995 0.3175 0.1636 0.129 Uiso 0.448(7) 1 calc PR B 2 H18F H 0.4014 0.3906 0.1026 0.129 Uiso 0.448(7) 1 calc PR B 2 N5A N 0.3220(7) 0.9901(12) -0.2182(9) 0.066(2) Uani 0.518(8) 1 d PDU C 1 N6A N 0.2628(7) 0.9977(12) -0.1396(8) 0.071(2) Uani 0.518(8) 1 d PDU C 1 C19A C 0.2929(9) 1.0678(14) -0.2384(10) 0.068(3) Uani 0.518(8) 1 d PDU C 1 H19A H 0.2967 1.1084 -0.2756 0.081 Uiso 0.518(8) 1 calc PR C 1 C20A C 0.2517(10) 1.0713(15) -0.1829(11) 0.070(3) Uani 0.518(8) 1 d PDU C 1 H20A H 0.2241 1.1164 -0.1798 0.084 Uiso 0.518(8) 1 calc PR C 1 C21A C 0.3051(8) 0.9492(14) -0.1616(10) 0.068(2) Uani 0.518(8) 1 d PDU C 1 C22A C 0.3640(13) 0.970(2) -0.2620(15) 0.076(4) Uani 0.518(8) 1 d PDU C 1 H22A H 0.3845 0.9154 -0.2449 0.114 Uiso 0.518(8) 1 calc PR C 1 H22B H 0.3879 1.0245 -0.2631 0.114 Uiso 0.518(8) 1 calc PR C 1 H22C H 0.3481 0.9571 -0.3078 0.114 Uiso 0.518(8) 1 calc PR C 1 C23A C 0.3314(12) 0.8588(16) -0.1295(12) 0.072(4) Uani 0.518(8) 1 d PDU C 1 H23A H 0.3129 0.8408 -0.0898 0.108 Uiso 0.518(8) 1 calc PR C 1 H23B H 0.3692 0.8710 -0.1159 0.108 Uiso 0.518(8) 1 calc PR C 1 H23C H 0.3286 0.8078 -0.1628 0.108 Uiso 0.518(8) 1 calc PR C 1 C24A C 0.2310(10) 0.972(3) -0.0842(13) 0.081(3) Uani 0.518(8) 1 d PDU C 1 H24A H 0.2229 1.0291 -0.0584 0.097 Uiso 0.518(8) 1 calc PR C 1 H24B H 0.2519 0.9289 -0.0532 0.097 Uiso 0.518(8) 1 calc PR C 1 C25A C 0.1774(10) 0.923(2) -0.1108(15) 0.096(3) Uani 0.518(8) 1 d PDU C 1 H25A H 0.1834 0.8579 -0.1248 0.115 Uiso 0.518(8) 1 calc PR C 1 H25B H 0.1592 0.9585 -0.1491 0.115 Uiso 0.518(8) 1 calc PR C 1 C26A C 0.1448(14) 0.928(2) -0.0461(15) 0.109(4) Uani 0.518(8) 1 d PDU C 1 H26A H 0.1177 0.8776 -0.0440 0.131 Uiso 0.518(8) 1 calc PR C 1 H26B H 0.1675 0.9324 -0.0031 0.131 Uiso 0.518(8) 1 calc PR C 1 C27A C 0.1207(16) 1.025(2) -0.0717(19) 0.127(6) Uani 0.518(8) 1 d PDU C 1 H27A H 0.0949 1.0470 -0.0407 0.190 Uiso 0.518(8) 1 calc PR C 1 H27B H 0.1027 1.0171 -0.1170 0.190 Uiso 0.518(8) 1 calc PR C 1 H27C H 0.1496 1.0710 -0.0734 0.190 Uiso 0.518(8) 1 calc PR C 1 N5B N 0.3433(7) 0.9427(13) -0.2082(9) 0.066(2) Uani 0.482(8) 1 d PDU C 2 N6B N 0.2872(8) 0.9465(14) -0.1246(10) 0.071(2) Uani 0.482(8) 1 d PDU C 2 C19B C 0.3591(10) 0.8759(15) -0.1608(11) 0.068(3) Uani 0.482(8) 1 d PDU C 2 H19B H 0.3891 0.8354 -0.1626 0.081 Uiso 0.482(8) 1 calc PR C 2 C20B C 0.3244(11) 0.8775(18) -0.1104(14) 0.070(3) Uani 0.482(8) 1 d PDU C 2 H20B H 0.3260 0.8374 -0.0722 0.084 Uiso 0.482(8) 1 calc PR C 2 C21B C 0.2996(9) 0.9831(16) -0.1835(13) 0.068(2) Uani 0.482(8) 1 d PDU C 2 C22B C 0.3652(15) 0.944(2) -0.2739(13) 0.076(4) Uani 0.482(8) 1 d PDU C 2 H22D H 0.3495 0.9956 -0.3010 0.114 Uiso 0.482(8) 1 calc PR C 2 H22E H 0.3566 0.8841 -0.2973 0.114 Uiso 0.482(8) 1 calc PR C 2 H22F H 0.4041 0.9513 -0.2679 0.114 Uiso 0.482(8) 1 calc PR C 2 C23B C 0.2704(11) 1.0704(17) -0.2166(14) 0.072(4) Uani 0.482(8) 1 d PDU C 2 H23D H 0.2855 1.0848 -0.2596 0.108 Uiso 0.482(8) 1 calc PR C 2 H23E H 0.2754 1.1243 -0.1862 0.108 Uiso 0.482(8) 1 calc PR C 2 H23F H 0.2321 1.0568 -0.2250 0.108 Uiso 0.482(8) 1 calc PR C 2 C24B C 0.2432(11) 0.966(3) -0.0831(16) 0.081(3) Uani 0.482(8) 1 d PDU C 2 H24C H 0.2329 1.0331 -0.0888 0.097 Uiso 0.482(8) 1 calc PR C 2 H24D H 0.2556 0.9566 -0.0350 0.097 Uiso 0.482(8) 1 calc PR C 2 C25B C 0.1927(10) 0.903(3) -0.1009(18) 0.096(3) Uani 0.482(8) 1 d PDU C 2 H25C H 0.2050 0.8377 -0.0953 0.115 Uiso 0.482(8) 1 calc PR C 2 H25D H 0.1831 0.9124 -0.1499 0.115 Uiso 0.482(8) 1 calc PR C 2 C26B C 0.1385(13) 0.910(2) -0.0659(18) 0.109(4) Uani 0.482(8) 1 d PDU C 2 H26C H 0.1407 0.8596 -0.0311 0.131 Uiso 0.482(8) 1 calc PR C 2 H26D H 0.1104 0.8894 -0.1008 0.131 Uiso 0.482(8) 1 calc PR C 2 C27B C 0.1140(17) 0.997(2) -0.031(2) 0.127(6) Uani 0.482(8) 1 d PDU C 2 H27D H 0.0793 0.9801 -0.0146 0.190 Uiso 0.482(8) 1 calc PR C 2 H27E H 0.1092 1.0488 -0.0631 0.190 Uiso 0.482(8) 1 calc PR C 2 H27F H 0.1384 1.0169 0.0079 0.190 Uiso 0.482(8) 1 calc PR C 2 N7A N -0.0101(8) 0.2685(19) 0.3282(10) 0.107(3) Uani 0.515(9) 1 d PDU D 1 N8A N 0.0149(9) 0.266(2) 0.2206(9) 0.109(3) Uani 0.515(9) 1 d PDU D 1 C28A C 0.0480(7) 0.272(2) 0.3349(10) 0.113(4) Uani 0.515(9) 1 d PDU D 1 H28A H 0.0709 0.2740 0.3754 0.136 Uiso 0.515(9) 1 calc PR D 1 C29A C 0.0629(8) 0.272(2) 0.2677(14) 0.113(3) Uani 0.515(9) 1 d PDU D 1 H29A H 0.0986 0.2757 0.2550 0.136 Uiso 0.515(9) 1 calc PR D 1 C30A C -0.0309(7) 0.253(2) 0.2593(10) 0.109(3) Uani 0.515(9) 1 d PDU D 1 C31A C -0.0327(11) 0.282(2) 0.3933(13) 0.119(6) Uani 0.515(9) 1 d PDU D 1 H31A H -0.0717 0.2757 0.3874 0.179 Uiso 0.515(9) 1 calc PR D 1 H31B H -0.0234 0.3450 0.4106 0.179 Uiso 0.515(9) 1 calc PR D 1 H31C H -0.0180 0.2349 0.4255 0.179 Uiso 0.515(9) 1 calc PR D 1 C32A C -0.0852(10) 0.223(3) 0.2218(17) 0.127(5) Uani 0.515(9) 1 d PDU D 1 H32A H -0.0806 0.2148 0.1735 0.191 Uiso 0.515(9) 1 calc PR D 1 H32B H -0.1122 0.2710 0.2277 0.191 Uiso 0.515(9) 1 calc PR D 1 H32C H -0.0968 0.1631 0.2405 0.191 Uiso 0.515(9) 1 calc PR D 1 C33A C 0.022(2) 0.247(3) 0.1496(16) 0.119(3) Uani 0.515(9) 1 d PDU D 1 H33A H 0.0589 0.2652 0.1423 0.143 Uiso 0.515(9) 1 calc PR D 1 H33B H -0.0018 0.2926 0.1235 0.143 Uiso 0.515(9) 1 calc PR D 1 C34A C 0.0120(14) 0.1502(18) 0.1136(18) 0.134(4) Uani 0.515(9) 1 d PDU D 1 H34A H -0.0257 0.1290 0.1129 0.160 Uiso 0.515(9) 1 calc PR D 1 H34B H 0.0243 0.1489 0.0675 0.160 Uiso 0.515(9) 1 calc PR D 1 C35A C 0.0501(15) 0.096(2) 0.1663(16) 0.143(4) Uani 0.515(9) 1 d PDU D 1 H35A H 0.0377 0.1028 0.2122 0.171 Uiso 0.515(9) 1 calc PR D 1 H35B H 0.0869 0.1209 0.1666 0.171 Uiso 0.515(9) 1 calc PR D 1 C36A C 0.0497(17) -0.0114(19) 0.146(2) 0.161(6) Uani 0.515(9) 1 d PDU D 1 H36A H 0.0734 -0.0466 0.1783 0.242 Uiso 0.515(9) 1 calc PR D 1 H36B H 0.0622 -0.0181 0.1005 0.242 Uiso 0.515(9) 1 calc PR D 1 H36C H 0.0132 -0.0361 0.1458 0.242 Uiso 0.515(9) 1 calc PR D 1 N7B N -0.0394(8) 0.262(2) 0.3021(11) 0.107(3) Uani 0.485(9) 1 d PDU D 2 N8B N -0.0071(10) 0.264(2) 0.2047(12) 0.109(3) Uani 0.485(9) 1 d PDU D 2 C28B C -0.0825(9) 0.277(3) 0.2495(13) 0.113(4) Uani 0.485(9) 1 d PDU D 2 H28B H -0.1187 0.2899 0.2573 0.136 Uiso 0.485(9) 1 calc PR D 2 C29B C -0.0647(11) 0.269(3) 0.1915(19) 0.113(3) Uani 0.485(9) 1 d PDU D 2 H29B H -0.0847 0.2681 0.1488 0.136 Uiso 0.485(9) 1 calc PR D 2 C30B C 0.0120(8) 0.268(2) 0.2750(12) 0.109(3) Uani 0.485(9) 1 d PDU D 2 C31B C -0.0589(13) 0.242(3) 0.3678(12) 0.119(6) Uani 0.485(9) 1 d PDU D 2 H31D H -0.0285 0.2361 0.4017 0.179 Uiso 0.485(9) 1 calc PR D 2 H31E H -0.0793 0.1834 0.3652 0.179 Uiso 0.485(9) 1 calc PR D 2 H31F H -0.0822 0.2934 0.3806 0.179 Uiso 0.485(9) 1 calc PR D 2 C32B C 0.0689(10) 0.297(3) 0.3038(19) 0.127(5) Uani 0.485(9) 1 d PDU D 2 H32D H 0.0703 0.2987 0.3533 0.191 Uiso 0.485(9) 1 calc PR D 2 H32E H 0.0775 0.3595 0.2868 0.191 Uiso 0.485(9) 1 calc PR D 2 H32F H 0.0950 0.2515 0.2895 0.191 Uiso 0.485(9) 1 calc PR D 2 C33B C 0.030(2) 0.261(3) 0.151(2) 0.119(3) Uani 0.485(9) 1 d PDU D 2 H33C H 0.0644 0.2875 0.1689 0.143 Uiso 0.485(9) 1 calc PR D 2 H33D H 0.0151 0.3019 0.1137 0.143 Uiso 0.485(9) 1 calc PR D 2 C34B C 0.0390(16) 0.1606(19) 0.1226(19) 0.134(4) Uani 0.485(9) 1 d PDU D 2 H34C H 0.0234 0.1693 0.0756 0.160 Uiso 0.485(9) 1 calc PR D 2 H34D H 0.0781 0.1637 0.1188 0.160 Uiso 0.485(9) 1 calc PR D 2 C35B C 0.0322(18) 0.0525(19) 0.1293(17) 0.143(4) Uani 0.485(9) 1 d PDU D 2 H35C H 0.0668 0.0207 0.1242 0.171 Uiso 0.485(9) 1 calc PR D 2 H35D H 0.0057 0.0293 0.0934 0.171 Uiso 0.485(9) 1 calc PR D 2 C36B C 0.0123(19) 0.030(3) 0.2012(19) 0.161(6) Uani 0.485(9) 1 d PDU D 2 H36F H 0.0140 -0.0375 0.2093 0.242 Uiso 0.485(9) 1 calc PR D 2 H36G H -0.0247 0.0518 0.2029 0.242 Uiso 0.485(9) 1 calc PR D 2 H36D H 0.0353 0.0627 0.2361 0.242 Uiso 0.485(9) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0338(3) 0.0228(2) 0.0416(3) 0.0030(2) -0.0051(2) 0.0012(2) Sn2 0.0267(2) 0.0349(3) 0.0497(3) 0.0048(2) -0.0013(2) 0.0021(2) Sn3 0.0339(3) 0.0232(2) 0.0415(3) -0.0040(2) -0.0011(2) -0.0004(2) Sn4 0.0399(3) 0.0242(3) 0.0494(3) -0.0064(2) -0.0064(2) 0.0015(2) Sn5 0.0308(3) 0.0323(3) 0.0477(3) -0.0010(2) -0.0026(2) -0.0011(2) Sn6 0.0459(3) 0.0232(3) 0.0489(3) 0.0054(2) -0.0112(3) -0.0007(2) Se1 0.0615(5) 0.0300(4) 0.0425(5) 0.0012(3) 0.0045(4) 0.0119(4) Se2 0.0508(5) 0.0326(4) 0.0451(5) 0.0071(4) 0.0051(4) 0.0084(4) Se3 0.0319(4) 0.0282(4) 0.0370(4) 0.0007(3) 0.0012(3) 0.0006(3) Se4 0.0334(4) 0.0286(4) 0.0544(5) -0.0046(3) 0.0082(4) 0.0001(3) Se5 0.0415(4) 0.0388(4) 0.0462(5) 0.0129(4) -0.0034(4) -0.0020(4) Se6 0.0313(4) 0.0708(6) 0.0441(5) 0.0071(4) -0.0010(4) 0.0051(4) Se7 0.0415(4) 0.0391(5) 0.0441(5) -0.0079(4) -0.0102(4) 0.0032(4) Se8 0.0513(5) 0.0306(4) 0.0404(4) -0.0043(3) 0.0044(4) -0.0059(4) Se9 0.0592(5) 0.0338(4) 0.0477(5) -0.0067(4) 0.0162(4) -0.0138(4) Se10 0.0431(4) 0.0414(5) 0.0381(4) -0.0012(4) -0.0001(4) 0.0028(4) Se11 0.0450(4) 0.0373(4) 0.0445(5) 0.0091(4) -0.0062(4) -0.0021(4) Se12 0.0356(4) 0.0290(4) 0.0620(6) 0.0013(4) 0.0082(4) 0.0010(3) Se13 0.0322(4) 0.0617(6) 0.1014(9) -0.0155(6) -0.0025(5) -0.0027(4) Se14 0.0443(4) 0.0391(5) 0.0439(5) -0.0111(4) -0.0061(4) 0.0033(4) N1A 0.068(4) 0.065(4) 0.052(4) 0.001(4) 0.015(3) 0.000(4) N2A 0.073(4) 0.069(4) 0.058(4) 0.001(4) 0.011(3) 0.002(4) C1A 0.072(5) 0.062(4) 0.057(4) 0.002(4) 0.015(4) 0.001(4) C2A 0.075(5) 0.065(4) 0.062(4) 0.003(4) 0.011(4) 0.003(4) C3A 0.068(4) 0.065(4) 0.052(3) 0.001(4) 0.014(3) 0.001(4) C4A 0.067(5) 0.072(8) 0.067(6) -0.003(6) 0.009(5) -0.001(5) C5A 0.061(6) 0.057(6) 0.055(6) 0.003(5) 0.006(5) -0.006(5) C6A 0.085(4) 0.085(5) 0.078(4) 0.002(4) 0.005(4) 0.002(4) C7A 0.102(5) 0.105(5) 0.101(5) -0.005(5) -0.002(5) 0.002(5) C8A 0.116(6) 0.117(6) 0.120(6) -0.005(5) -0.005(5) -0.003(5) C9A 0.143(10) 0.138(11) 0.139(11) -0.008(9) 0.020(9) 0.005(9) N1B 0.068(4) 0.065(4) 0.052(4) 0.001(4) 0.015(3) 0.000(4) N2B 0.073(4) 0.069(4) 0.058(4) 0.001(4) 0.011(3) 0.002(4) C1B 0.072(5) 0.062(4) 0.057(4) 0.002(4) 0.015(4) 0.001(4) C2B 0.075(5) 0.065(4) 0.062(4) 0.003(4) 0.011(4) 0.003(4) C3B 0.068(4) 0.065(4) 0.052(3) 0.001(4) 0.014(3) 0.001(4) C4B 0.067(5) 0.072(8) 0.067(6) -0.003(6) 0.009(5) -0.001(5) C5B 0.061(6) 0.057(6) 0.055(6) 0.003(5) 0.006(5) -0.006(5) C6B 0.085(4) 0.085(5) 0.078(4) 0.002(4) 0.005(4) 0.002(4) C7B 0.102(5) 0.105(5) 0.101(5) -0.005(5) -0.002(5) 0.002(5) C8B 0.116(6) 0.117(6) 0.120(6) -0.005(5) -0.005(5) -0.003(5) C9B 0.121(12) 0.124(12) 0.124(12) 0.000(10) 0.004(10) 0.002(10) N3A 0.077(4) 0.063(4) 0.068(4) 0.001(4) 0.012(4) 0.008(4) N4A 0.080(4) 0.065(4) 0.065(4) 0.000(3) 0.017(4) 0.005(4) C10A 0.075(5) 0.070(5) 0.072(5) 0.000(4) 0.013(4) 0.005(4) C11A 0.076(5) 0.074(5) 0.072(5) -0.001(4) 0.007(4) 0.005(4) C12A 0.075(4) 0.065(4) 0.068(4) -0.003(3) 0.015(4) 0.007(4) C13A 0.097(8) 0.084(7) 0.082(6) 0.010(6) 0.007(6) 0.004(6) C14A 0.071(6) 0.072(6) 0.078(7) 0.003(6) 0.015(5) 0.003(5) C15A 0.088(5) 0.078(4) 0.080(4) -0.008(4) 0.016(4) 0.004(4) C16A 0.092(5) 0.087(5) 0.086(5) -0.003(4) 0.016(4) 0.002(4) C17A 0.091(5) 0.092(5) 0.086(5) -0.004(5) 0.018(5) 0.003(5) C18A 0.087(8) 0.087(7) 0.086(7) -0.007(6) 0.019(6) 0.006(6) N3B 0.077(4) 0.063(4) 0.068(4) 0.001(4) 0.012(4) 0.008(4) N4B 0.080(4) 0.065(4) 0.065(4) 0.000(3) 0.017(4) 0.005(4) C10B 0.075(5) 0.070(5) 0.072(5) 0.000(4) 0.013(4) 0.005(4) C11B 0.076(5) 0.074(5) 0.072(5) -0.001(4) 0.007(4) 0.005(4) C12B 0.075(4) 0.065(4) 0.068(4) -0.003(3) 0.015(4) 0.007(4) C13B 0.097(8) 0.084(7) 0.082(6) 0.010(6) 0.007(6) 0.004(6) C14B 0.071(6) 0.072(6) 0.078(7) 0.003(6) 0.015(5) 0.003(5) C15B 0.088(5) 0.078(4) 0.080(4) -0.008(4) 0.016(4) 0.004(4) C16B 0.092(5) 0.087(5) 0.086(5) -0.003(4) 0.016(4) 0.002(4) C17B 0.091(5) 0.092(5) 0.086(5) -0.004(5) 0.018(5) 0.003(5) C18B 0.087(8) 0.087(7) 0.086(7) -0.007(6) 0.019(6) 0.006(6) N5A 0.067(4) 0.061(4) 0.066(4) -0.002(4) -0.013(4) -0.007(4) N6A 0.074(4) 0.067(4) 0.070(4) -0.009(4) -0.007(4) 0.002(4) C19A 0.072(5) 0.063(5) 0.066(5) 0.004(4) -0.006(4) 0.000(4) C20A 0.074(5) 0.065(5) 0.070(5) 0.000(4) -0.003(4) 0.007(4) C21A 0.070(4) 0.063(4) 0.067(4) -0.004(4) -0.011(4) -0.003(4) C22A 0.078(6) 0.073(8) 0.075(7) 0.001(6) -0.002(5) -0.005(6) C23A 0.078(6) 0.065(6) 0.073(6) 0.005(5) -0.002(6) 0.010(5) C24A 0.083(5) 0.080(4) 0.079(4) -0.018(4) -0.002(4) 0.005(4) C25A 0.097(5) 0.096(5) 0.094(5) -0.015(4) 0.002(4) 0.000(4) C26A 0.109(5) 0.110(5) 0.107(6) -0.014(5) 0.002(5) 0.000(5) C27A 0.126(8) 0.128(8) 0.126(8) -0.002(7) 0.006(7) 0.001(7) N5B 0.067(4) 0.061(4) 0.066(4) -0.002(4) -0.013(4) -0.007(4) N6B 0.074(4) 0.067(4) 0.070(4) -0.009(4) -0.007(4) 0.002(4) C19B 0.072(5) 0.063(5) 0.066(5) 0.004(4) -0.006(4) 0.000(4) C20B 0.074(5) 0.065(5) 0.070(5) 0.000(4) -0.003(4) 0.007(4) C21B 0.070(4) 0.063(4) 0.067(4) -0.004(4) -0.011(4) -0.003(4) C22B 0.078(6) 0.073(8) 0.075(7) 0.001(6) -0.002(5) -0.005(6) C23B 0.078(6) 0.065(6) 0.073(6) 0.005(5) -0.002(6) 0.010(5) C24B 0.083(5) 0.080(4) 0.079(4) -0.018(4) -0.002(4) 0.005(4) C25B 0.097(5) 0.096(5) 0.094(5) -0.015(4) 0.002(4) 0.000(4) C26B 0.109(5) 0.110(5) 0.107(6) -0.014(5) 0.002(5) 0.000(5) C27B 0.126(8) 0.128(8) 0.126(8) -0.002(7) 0.006(7) 0.001(7) N7A 0.114(5) 0.097(5) 0.111(5) 0.013(4) 0.017(4) 0.001(5) N8A 0.110(5) 0.101(4) 0.118(4) 0.008(4) 0.012(4) -0.002(4) C28A 0.112(5) 0.109(5) 0.118(5) 0.006(5) 0.012(5) 0.000(5) C29A 0.112(5) 0.110(5) 0.118(5) 0.004(5) 0.012(5) -0.001(5) C30A 0.112(4) 0.101(4) 0.116(4) 0.007(4) 0.014(4) 0.002(4) C31A 0.127(8) 0.112(8) 0.121(8) 0.006(7) 0.027(7) 0.001(7) C32A 0.123(8) 0.128(8) 0.131(8) 0.005(7) 0.012(7) -0.002(7) C33A 0.119(5) 0.114(5) 0.123(5) 0.007(4) 0.008(4) -0.003(4) C34A 0.132(5) 0.129(5) 0.139(5) 0.004(5) 0.005(5) -0.005(5) C35A 0.141(6) 0.138(6) 0.147(6) 0.002(5) 0.004(5) -0.004(5) C36A 0.161(9) 0.158(9) 0.164(9) 0.001(7) 0.010(7) 0.003(7) N7B 0.114(5) 0.097(5) 0.111(5) 0.013(4) 0.017(4) 0.001(5) N8B 0.110(5) 0.101(4) 0.118(4) 0.008(4) 0.012(4) -0.002(4) C28B 0.112(5) 0.109(5) 0.118(5) 0.006(5) 0.012(5) 0.000(5) C29B 0.112(5) 0.110(5) 0.118(5) 0.004(5) 0.012(5) -0.001(5) C30B 0.112(4) 0.101(4) 0.116(4) 0.007(4) 0.014(4) 0.002(4) C31B 0.127(8) 0.112(8) 0.121(8) 0.006(7) 0.027(7) 0.001(7) C32B 0.123(8) 0.128(8) 0.131(8) 0.005(7) 0.012(7) -0.002(7) C33B 0.119(5) 0.114(5) 0.123(5) 0.007(4) 0.008(4) -0.003(4) C34B 0.132(5) 0.129(5) 0.139(5) 0.004(5) 0.005(5) -0.005(5) C35B 0.141(6) 0.138(6) 0.147(6) 0.002(5) 0.004(5) -0.004(5) C36B 0.161(9) 0.158(9) 0.164(9) 0.001(7) 0.010(7) 0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Se2 2.5327(10) . ? Sn1 Se7 2.5522(10) . ? Sn1 Se4 2.5613(9) . ? Sn1 Se1 2.7129(10) . ? Sn1 Se3 2.7765(9) . ? Sn2 Se6 2.5252(11) . ? Sn2 Se5 2.5684(10) . ? Sn2 Se7 2.5719(10) . ? Sn2 Se6 2.6948(11) 3_565 ? Sn2 Se3 2.7726(10) . ? Sn3 Se8 2.5399(10) . ? Sn3 Se4 2.5468(9) . ? Sn3 Se5 2.5641(10) . ? Sn3 Se9 2.7360(10) . ? Sn3 Se3 2.7513(9) . ? Sn4 Se9 2.4992(11) . ? Sn4 Se12 2.5479(10) . ? Sn4 Se11 2.5504(10) . ? Sn4 Se8 2.6473(10) . ? Sn4 Se10 3.0158(11) . ? Sn5 Se13 2.4104(11) . ? Sn5 Se10 2.5205(11) . ? Sn5 Se14 2.5689(10) . ? Sn5 Se11 2.5753(10) . ? Sn6 Se1 2.5030(11) 1_565 ? Sn6 Se14 2.5486(10) . ? Sn6 Se12 2.5511(10) . ? Sn6 Se2 2.6534(10) 1_565 ? Sn6 Se10 2.9855(11) . ? Se1 Sn6 2.5030(11) 1_545 ? Se2 Sn6 2.6534(10) 1_545 ? Se6 Sn2 2.6948(11) 3_565 ? N1A C1A 1.336(11) . ? N1A C3A 1.342(10) . ? N1A C4A 1.418(15) . ? N2A C3A 1.339(10) . ? N2A C2A 1.346(11) . ? N2A C6A 1.429(16) . ? C1A C2A 1.36(2) . ? C1A H1A 0.9300 . ? C2A H2A 0.9300 . ? C3A C5A 1.533(11) . ? C4A H4A 0.9600 . ? C4A H4B 0.9600 . ? C4A H4C 0.9600 . ? C5A H5A 0.9600 . ? C5A H5B 0.9600 . ? C5A H5C 0.9600 . ? C6A C7A 1.525(12) . ? C6A H6A 0.9700 . ? C6A H6B 0.9700 . ? C7A C8A 1.539(12) . ? C7A H7A 0.9700 . ? C7A H7B 0.9700 . ? C8A C9A 1.520(12) . ? C8A H8A 0.9700 . ? C8A H8B 0.9700 . ? C9A H9A 0.9600 . ? C9A H9B 0.9600 . ? C9A H9C 0.9600 . ? N1B C3B 1.336(12) . ? N1B C1B 1.338(12) . ? N1B C4B 1.421(17) . ? N2B C3B 1.335(12) . ? N2B C2B 1.341(12) . ? N2B C6B 1.44(5) . ? C1B C2B 1.38(5) . ? C1B H1B 0.9300 . ? C2B H2B 0.9300 . ? C3B C5B 1.529(12) . ? C4B H4D 0.9600 . ? C4B H4E 0.9600 . ? C4B H4F 0.9600 . ? C5B H5D 0.9600 . ? C5B H5E 0.9600 . ? C5B H5F 0.9600 . ? C6B C7B 1.534(13) . ? C6B H6C 0.9700 . ? C6B H6D 0.9700 . ? C7B C8B 1.543(13) . ? C7B H7C 0.9700 . ? C7B H7D 0.9700 . ? C8B C9B 1.536(13) . ? C8B H8C 0.9700 . ? C8B H8D 0.9700 . ? C9B H9D 0.9600 . ? C9B H9E 0.9600 . ? C9B H9F 0.9600 . ? N3A C10A 1.325(11) . ? N3A C12A 1.337(11) . ? N3A C13A 1.446(13) . ? N4A C12A 1.305(11) . ? N4A C11A 1.324(11) . ? N4A C15A 1.430(12) . ? C10A C11A 1.47(2) . ? C10A H10A 0.9300 . ? C11A H11A 0.9300 . ? C12A C14A 1.55(3) . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C15A C16A 1.590(12) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A C17A 1.529(12) . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C17A C18A 1.528(12) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? N3B C10B 1.326(12) . ? N3B C12B 1.335(11) . ? N3B C13B 1.452(13) . ? N4B C12B 1.306(11) . ? N4B C11B 1.325(12) . ? N4B C15B 1.436(13) . ? C10B C11B 1.42(4) . ? C10B H10B 0.9300 . ? C11B H11B 0.9300 . ? C12B C14B 1.47(3) . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15B C16B 1.590(12) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B C17B 1.529(12) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C18B 1.533(12) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? N5A C21A 1.334(12) . ? N5A C19A 1.340(12) . ? N5A C22A 1.415(15) . ? N6A C21A 1.338(12) . ? N6A C20A 1.342(12) . ? N6A C24A 1.424(15) . ? C19A C20A 1.54(3) . ? C19A H19A 0.9300 . ? C20A H20A 0.9300 . ? C21A C23A 1.528(12) . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C24A C25A 1.532(12) . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? C25A C26A 1.545(12) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C26A C27A 1.543(12) . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? N5B C21B 1.334(12) . ? N5B C19B 1.346(12) . ? N5B C22B 1.424(15) . ? N6B C21B 1.31(3) . ? N6B C20B 1.341(12) . ? N6B C24B 1.425(15) . ? C19B C20B 1.35(4) . ? C19B H19B 0.9300 . ? C20B H20B 0.9300 . ? C21B C23B 1.530(12) . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23B H23D 0.9600 . ? C23B H23E 0.9600 . ? C23B H23F 0.9600 . ? C24B C25B 1.535(12) . ? C24B H24C 0.9700 . ? C24B H24D 0.9700 . ? C25B C26B 1.544(12) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26B C27B 1.545(12) . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? N7A C30A 1.411(11) . ? N7A C28A 1.424(11) . ? N7A C31A 1.435(17) . ? N8A C30A 1.413(11) . ? N8A C33A 1.427(17) . ? N8A C29A 1.435(11) . ? C28A C29A 1.38(3) . ? C28A H28A 0.9300 . ? C29A H29A 0.9300 . ? C30A C32A 1.526(12) . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C33A C34A 1.534(12) . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C34A C35A 1.534(12) . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C35A C36A 1.545(13) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? N7B C30B 1.406(11) . ? N7B C28B 1.428(11) . ? N7B C31B 1.426(17) . ? N8B C30B 1.410(11) . ? N8B C29B 1.419(12) . ? N8B C33B 1.427(17) . ? C28B C29B 1.25(4) . ? C28B H28B 0.9300 . ? C29B H29B 0.9300 . ? C30B C32B 1.518(12) . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33B C34B 1.534(13) . ? C33B H33C 0.9700 . ? C33B H33D 0.9700 . ? C34B C35B 1.525(13) . ? C34B H34C 0.9700 . ? C34B H34D 0.9700 . ? C35B C36B 1.548(13) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C36B H36F 0.9600 . ? C36B H36G 0.9600 . ? C36B H36D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se7 121.39(4) . . ? Se2 Sn1 Se4 122.59(4) . . ? Se7 Sn1 Se4 115.95(4) . . ? Se2 Sn1 Se1 89.40(3) . . ? Se7 Sn1 Se1 93.79(3) . . ? Se4 Sn1 Se1 89.61(3) . . ? Se2 Sn1 Se3 91.74(3) . . ? Se7 Sn1 Se3 87.82(3) . . ? Se4 Sn1 Se3 87.60(3) . . ? Se1 Sn1 Se3 177.18(3) . . ? Se6 Sn2 Se5 121.43(4) . . ? Se6 Sn2 Se7 124.26(4) . . ? Se5 Sn2 Se7 114.23(4) . . ? Se6 Sn2 Se6 89.61(4) . 3_565 ? Se5 Sn2 Se6 92.92(3) . 3_565 ? Se7 Sn2 Se6 90.49(3) . 3_565 ? Se6 Sn2 Se3 91.39(3) . . ? Se5 Sn2 Se3 88.04(3) . . ? Se7 Sn2 Se3 87.52(3) . . ? Se6 Sn2 Se3 178.00(3) 3_565 . ? Se8 Sn3 Se4 121.52(4) . . ? Se8 Sn3 Se5 124.06(4) . . ? Se4 Sn3 Se5 114.41(4) . . ? Se8 Sn3 Se9 88.44(3) . . ? Se4 Sn3 Se9 90.57(3) . . ? Se5 Sn3 Se9 92.21(3) . . ? Se8 Sn3 Se3 91.71(3) . . ? Se4 Sn3 Se3 88.44(3) . . ? Se5 Sn3 Se3 88.59(3) . . ? Se9 Sn3 Se3 178.92(3) . . ? Se9 Sn4 Se12 122.06(4) . . ? Se9 Sn4 Se11 122.23(4) . . ? Se12 Sn4 Se11 114.44(4) . . ? Se9 Sn4 Se8 91.32(3) . . ? Se12 Sn4 Se8 94.58(3) . . ? Se11 Sn4 Se8 95.47(3) . . ? Se9 Sn4 Se10 87.64(3) . . ? Se12 Sn4 Se10 85.62(3) . . ? Se11 Sn4 Se10 85.43(3) . . ? Se8 Sn4 Se10 178.88(3) . . ? Se13 Sn5 Se10 124.24(4) . . ? Se13 Sn5 Se14 116.25(4) . . ? Se10 Sn5 Se14 96.13(3) . . ? Se13 Sn5 Se11 114.49(4) . . ? Se10 Sn5 Se11 96.14(3) . . ? Se14 Sn5 Se11 106.15(4) . . ? Se1 Sn6 Se14 123.27(4) 1_565 . ? Se1 Sn6 Se12 122.66(4) 1_565 . ? Se14 Sn6 Se12 113.06(4) . . ? Se1 Sn6 Se2 91.40(3) 1_565 1_565 ? Se14 Sn6 Se2 93.31(3) . 1_565 ? Se12 Sn6 Se2 95.44(3) . 1_565 ? Se1 Sn6 Se10 87.77(3) 1_565 . ? Se14 Sn6 Se10 85.96(3) . . ? Se12 Sn6 Se10 86.21(3) . . ? Se2 Sn6 Se10 178.35(3) 1_565 . ? Sn6 Se1 Sn1 89.06(3) 1_545 . ? Sn1 Se2 Sn6 89.78(3) . 1_545 ? Sn3 Se3 Sn2 85.72(3) . . ? Sn3 Se3 Sn1 85.35(3) . . ? Sn2 Se3 Sn1 85.56(3) . . ? Sn3 Se4 Sn1 94.36(3) . . ? Sn3 Se5 Sn2 94.12(3) . . ? Sn2 Se6 Sn2 90.39(4) . 3_565 ? Sn1 Se7 Sn2 94.71(3) . . ? Sn3 Se8 Sn4 90.03(3) . . ? Sn4 Se9 Sn3 88.88(3) . . ? Sn5 Se10 Sn6 83.36(3) . . ? Sn5 Se10 Sn4 83.09(3) . . ? Sn6 Se10 Sn4 81.40(3) . . ? Sn4 Se11 Sn5 92.11(3) . . ? Sn4 Se12 Sn6 100.25(3) . . ? Sn6 Se14 Sn5 91.89(3) . . ? C1A N1A C3A 109.0(13) . . ? C1A N1A C4A 124.2(14) . . ? C3A N1A C4A 126.8(13) . . ? C3A N2A C2A 108.1(13) . . ? C3A N2A C6A 122.7(12) . . ? C2A N2A C6A 129.3(14) . . ? N1A C1A C2A 107.1(14) . . ? N1A C1A H1A 126.4 . . ? C2A C1A H1A 126.4 . . ? N2A C2A C1A 108.0(14) . . ? N2A C2A H2A 126.0 . . ? C1A C2A H2A 126.0 . . ? N2A C3A N1A 107.8(12) . . ? N2A C3A C5A 125.3(11) . . ? N1A C3A C5A 126.9(12) . . ? C3A C5A H5A 109.5 . . ? C3A C5A H5B 109.5 . . ? H5A C5A H5B 109.5 . . ? C3A C5A H5C 109.5 . . ? H5A C5A H5C 109.5 . . ? H5B C5A H5C 109.5 . . ? N2A C6A C7A 108.5(13) . . ? N2A C6A H6A 110.0 . . ? C7A C6A H6A 110.0 . . ? N2A C6A H6B 110.0 . . ? C7A C6A H6B 110.0 . . ? H6A C6A H6B 108.4 . . ? C6A C7A C8A 104.0(16) . . ? C6A C7A H7A 111.0 . . ? C8A C7A H7A 111.0 . . ? C6A C7A H7B 111.0 . . ? C8A C7A H7B 111.0 . . ? H7A C7A H7B 109.0 . . ? C9A C8A C7A 109.0(11) . . ? C9A C8A H8A 109.9 . . ? C7A C8A H8A 109.9 . . ? C9A C8A H8B 109.9 . . ? C7A C8A H8B 109.9 . . ? H8A C8A H8B 108.3 . . ? C8A C9A H9A 109.5 . . ? C8A C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? C8A C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? C3B N1B C1B 110(3) . . ? C3B N1B C4B 136(3) . . ? C1B N1B C4B 114(3) . . ? C3B N2B C2B 106(3) . . ? C3B N2B C6B 124(3) . . ? C2B N2B C6B 130(3) . . ? N1B C1B C2B 104(3) . . ? N1B C1B H1B 127.9 . . ? C2B C1B H1B 127.9 . . ? N2B C2B C1B 111(3) . . ? N2B C2B H2B 124.7 . . ? C1B C2B H2B 124.7 . . ? N2B C3B N1B 110(2) . . ? N2B C3B C5B 124(2) . . ? N1B C3B C5B 126(2) . . ? N1B C4B H4D 109.5 . . ? N1B C4B H4E 109.5 . . ? H4D C4B H4E 109.5 . . ? N1B C4B H4F 109.5 . . ? H4D C4B H4F 109.5 . . ? H4E C4B H4F 109.5 . . ? C3B C5B H5D 109.5 . . ? C3B C5B H5E 109.5 . . ? H5D C5B H5E 109.5 . . ? C3B C5B H5F 109.5 . . ? H5D C5B H5F 109.5 . . ? H5E C5B H5F 109.5 . . ? N2B C6B C7B 109(3) . . ? N2B C6B H6C 110.0 . . ? C7B C6B H6C 110.0 . . ? N2B C6B H6D 110.0 . . ? C7B C6B H6D 110.0 . . ? H6C C6B H6D 108.4 . . ? C6B C7B C8B 117(3) . . ? C6B C7B H7C 108.1 . . ? C8B C7B H7C 108.1 . . ? C6B C7B H7D 108.1 . . ? C8B C7B H7D 108.1 . . ? H7C C7B H7D 107.3 . . ? C9B C8B C7B 107.6(12) . . ? C9B C8B H8C 110.2 . . ? C7B C8B H8C 110.2 . . ? C9B C8B H8D 110.2 . . ? C7B C8B H8D 110.2 . . ? H8C C8B H8D 108.5 . . ? C8B C9B H9D 109.5 . . ? C8B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C8B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C10A N3A C12A 114.1(15) . . ? C10A N3A C13A 115.5(11) . . ? C12A N3A C13A 130.5(16) . . ? C12A N4A C11A 107.3(15) . . ? C12A N4A C15A 113.8(9) . . ? C11A N4A C15A 138.2(16) . . ? N3A C10A C11A 99.2(10) . . ? N3A C10A H10A 130.4 . . ? C11A C10A H10A 130.4 . . ? N4A C11A C10A 110.5(15) . . ? N4A C11A H11A 124.7 . . ? C10A C11A H11A 124.7 . . ? N4A C12A N3A 108.9(16) . . ? N4A C12A C14A 129.9(13) . . ? N3A C12A C14A 121.2(15) . . ? C12A C14A H14A 109.5 . . ? C12A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C12A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? N4A C15A C16A 96.4(15) . . ? N4A C15A H15A 112.5 . . ? C16A C15A H15A 112.5 . . ? N4A C15A H15B 112.5 . . ? C16A C15A H15B 112.5 . . ? H15A C15A H15B 110.0 . . ? C17A C16A C15A 93.0(16) . . ? C17A C16A H16A 113.1 . . ? C15A C16A H16A 113.1 . . ? C17A C16A H16B 113.1 . . ? C15A C16A H16B 113.1 . . ? H16A C16A H16B 110.5 . . ? C18A C17A C16A 120(2) . . ? C18A C17A H17A 107.4 . . ? C16A C17A H17A 107.4 . . ? C18A C17A H17B 107.4 . . ? C16A C17A H17B 107.4 . . ? H17A C17A H17B 107.0 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C10B N3B C12B 111(2) . . ? C10B N3B C13B 113.5(13) . . ? C12B N3B C13B 135(2) . . ? C12B N4B C11B 115(2) . . ? C12B N4B C15B 113.4(10) . . ? C11B N4B C15B 132(2) . . ? N3B C10B C11B 106(2) . . ? N3B C10B H10B 126.8 . . ? C11B C10B H10B 126.8 . . ? N4B C11B C10B 103(2) . . ? N4B C11B H11B 128.7 . . ? C10B C11B H11B 128.7 . . ? N4B C12B N3B 104.5(18) . . ? N4B C12B C14B 133.1(17) . . ? N3B C12B C14B 122.3(19) . . ? N3B C13B H13D 109.5 . . ? N3B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? N3B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? N4B C15B C16B 88.7(18) . . ? N4B C15B H15C 113.9 . . ? C16B C15B H15C 113.9 . . ? N4B C15B H15D 113.9 . . ? C16B C15B H15D 113.9 . . ? H15C C15B H15D 111.1 . . ? C17B C16B C15B 100(2) . . ? C17B C16B H16C 111.9 . . ? C15B C16B H16C 111.9 . . ? C17B C16B H16D 111.9 . . ? C15B C16B H16D 111.9 . . ? H16C C16B H16D 109.6 . . ? C16B C17B C18B 125(3) . . ? C16B C17B H17C 106.0 . . ? C18B C17B H17C 106.0 . . ? C16B C17B H17D 106.0 . . ? C18B C17B H17D 106.0 . . ? H17C C17B H17D 106.3 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C21A N5A C19A 113.3(17) . . ? C21A N5A C22A 135(2) . . ? C19A N5A C22A 112.2(19) . . ? C21A N6A C20A 108.1(16) . . ? C21A N6A C24A 127(2) . . ? C20A N6A C24A 125(2) . . ? N5A C19A C20A 100.7(13) . . ? N5A C19A H19A 129.7 . . ? C20A C19A H19A 129.7 . . ? N6A C20A C19A 107.6(15) . . ? N6A C20A H20A 126.2 . . ? C19A C20A H20A 126.2 . . ? N5A C21A N6A 110.3(17) . . ? N5A C21A C23A 122.8(17) . . ? N6A C21A C23A 126.9(18) . . ? N5A C22A H22A 109.5 . . ? N5A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? N5A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C21A C23A H23A 109.5 . . ? C21A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C21A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? N6A C24A C25A 111(2) . . ? N6A C24A H24A 109.4 . . ? C25A C24A H24A 109.4 . . ? N6A C24A H24B 109.4 . . ? C25A C24A H24B 109.4 . . ? H24A C24A H24B 108.0 . . ? C24A C25A C26A 101(2) . . ? C24A C25A H25A 111.5 . . ? C26A C25A H25A 111.5 . . ? C24A C25A H25B 111.5 . . ? C26A C25A H25B 111.5 . . ? H25A C25A H25B 109.4 . . ? C27A C26A C25A 89(2) . . ? C27A C26A H26A 113.8 . . ? C25A C26A H26A 113.8 . . ? C27A C26A H26B 113.8 . . ? C25A C26A H26B 113.8 . . ? H26A C26A H26B 111.0 . . ? C26A C27A H27A 109.5 . . ? C26A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C26A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C21B N5B C19B 104.0(19) . . ? C21B N5B C22B 134(2) . . ? C19B N5B C22B 121(2) . . ? C21B N6B C20B 105(2) . . ? C21B N6B C24B 131(2) . . ? C20B N6B C24B 124(3) . . ? N5B C19B C20B 109(2) . . ? N5B C19B H19B 125.7 . . ? C20B C19B H19B 125.7 . . ? N6B C20B C19B 109(2) . . ? N6B C20B H20B 125.6 . . ? C19B C20B H20B 125.6 . . ? N6B C21B N5B 113.5(19) . . ? N6B C21B C23B 123.0(18) . . ? N5B C21B C23B 123(2) . . ? N5B C22B H22D 109.5 . . ? N5B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? N5B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C21B C23B H23D 109.5 . . ? C21B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C21B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N6B C24B C25B 113(2) . . ? N6B C24B H24C 108.9 . . ? C25B C24B H24C 108.9 . . ? N6B C24B H24D 108.9 . . ? C25B C24B H24D 108.9 . . ? H24C C24B H24D 107.7 . . ? C24B C25B C26B 125(3) . . ? C24B C25B H25C 106.0 . . ? C26B C25B H25C 106.0 . . ? C24B C25B H25D 106.0 . . ? C26B C25B H25D 106.0 . . ? H25C C25B H25D 106.3 . . ? C25B C26B C27B 128(3) . . ? C25B C26B H26C 105.2 . . ? C27B C26B H26C 105.2 . . ? C25B C26B H26D 105.2 . . ? C27B C26B H26D 105.2 . . ? H26C C26B H26D 106.0 . . ? C26B C27B H27D 109.5 . . ? C26B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C30A N7A C28A 112.1(12) . . ? C30A N7A C31A 136.3(17) . . ? C28A N7A C31A 111.6(12) . . ? C30A N8A C33A 130(3) . . ? C30A N8A C29A 108.3(12) . . ? C33A N8A C29A 119(3) . . ? C29A C28A N7A 104.5(10) . . ? C29A C28A H28A 127.8 . . ? N7A C28A H28A 127.8 . . ? C28A C29A N8A 109.8(13) . . ? C28A C29A H29A 125.1 . . ? N8A C29A H29A 125.1 . . ? N7A C30A N8A 104.0(10) . . ? N7A C30A C32A 137(2) . . ? N8A C30A C32A 119(2) . . ? N7A C31A H31A 109.5 . . ? N7A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? N7A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C30A C32A H32A 109.5 . . ? C30A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? N8A C33A C34A 125(3) . . ? N8A C33A H33A 106.0 . . ? C34A C33A H33A 106.0 . . ? N8A C33A H33B 106.0 . . ? C34A C33A H33B 106.0 . . ? H33A C33A H33B 106.3 . . ? C35A C34A C33A 94(3) . . ? C35A C34A H34A 112.9 . . ? C33A C34A H34A 112.9 . . ? C35A C34A H34B 112.9 . . ? C33A C34A H34B 112.9 . . ? H34A C34A H34B 110.3 . . ? C34A C35A C36A 108.5(12) . . ? C34A C35A H35A 110.0 . . ? C36A C35A H35A 110.0 . . ? C34A C35A H35B 110.0 . . ? C36A C35A H35B 110.0 . . ? H35A C35A H35B 108.4 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C30B N7B C28B 111.0(13) . . ? C30B N7B C31B 136.2(17) . . ? C28B N7B C31B 112.7(12) . . ? C30B N8B C29B 115(2) . . ? C30B N8B C33B 122(3) . . ? C29B N8B C33B 123(3) . . ? C29B C28B N7B 110(2) . . ? C29B C28B H28B 125.0 . . ? N7B C28B H28B 125.0 . . ? C28B C29B N8B 105(3) . . ? C28B C29B H29B 127.5 . . ? N8B C29B H29B 127.5 . . ? N7B C30B N8B 97.0(16) . . ? N7B C30B C32B 135(2) . . ? N8B C30B C32B 126(2) . . ? N7B C31B H31D 109.5 . . ? N7B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? N7B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C30B C32B H32D 109.5 . . ? C30B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N8B C33B C34B 114(3) . . ? N8B C33B H33C 108.7 . . ? C34B C33B H33C 108.7 . . ? N8B C33B H33D 108.7 . . ? C34B C33B H33D 108.7 . . ? H33C C33B H33D 107.6 . . ? C35B C34B C33B 149(3) . . ? C35B C34B H34C 99.6 . . ? C33B C34B H34C 99.6 . . ? C35B C34B H34D 99.6 . . ? C33B C34B H34D 99.6 . . ? H34C C34B H34D 104.1 . . ? C34B C35B C36B 108.7(12) . . ? C34B C35B H35C 109.9 . . ? C36B C35B H35C 109.9 . . ? C34B C35B H35D 109.9 . . ? C36B C35B H35D 109.9 . . ? H35C C35B H35D 108.3 . . ? C35B C36B H36F 109.5 . . ? C35B C36B H36G 109.5 . . ? H36F C36B H36G 109.5 . . ? C35B C36B H36D 109.5 . . ? H36F C36B H36D 109.5 . . ? H36G C36B H36D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.212 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.156 data_compound-5_JL7-47D _database_code_depnum_ccdc_archive 'CCDC 903264' #TrackingRef 'compound 1-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Sn3 Se7, 2(C9 H17 N2)' _chemical_formula_sum 'C18 H34 N4 Se7 Sn3' _chemical_formula_weight 1215.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_space_group_name_Hall 'P 31 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' '-x, -x+y, -z+1/3' 'x-y, -y, -z+2/3' _cell_length_a 13.9329(9) _cell_length_b 13.9329(9) _cell_length_c 28.159(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4734.0(7) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9333 _cell_measurement_theta_min 2.2229 _cell_measurement_theta_max 27.4779 _exptl_crystal_description Lathe _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3348 _exptl_absorpt_coefficient_mu 10.444 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5901 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 4107 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34501 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.59 _reflns_number_total 7278 _reflns_number_gt 5214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.430(15) _refine_ls_number_reflns 7278 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.66778(5) 0.56983(5) 0.33505(2) 0.03998(14) Uani 1 1 d . . . Sn2 Sn 0.40396(5) 0.58416(5) 0.33743(2) 0.04259(16) Uani 1 1 d . . . Sn3 Sn 0.68268(5) 0.84599(5) 0.33537(2) 0.04582(17) Uani 1 1 d . . . Se1 Se 0.58581(7) 0.66721(7) 0.27454(3) 0.04120(19) Uani 1 1 d . . . Se2 Se 0.47469(8) 0.46176(8) 0.37210(4) 0.0483(2) Uani 1 1 d . . . Se3 Se 0.72913(9) 0.49479(9) 0.26714(3) 0.0502(2) Uani 1 1 d . . . Se4 Se 0.49102(8) 0.77996(8) 0.37089(4) 0.0521(3) Uani 1 1 d . . . Se5 Se 0.78834(8) 0.75953(8) 0.37240(4) 0.0555(3) Uani 1 1 d . . . Se6 Se 0.74842(9) 0.47894(9) 0.39703(3) 0.0499(2) Uani 1 1 d . . . Se7 Se 0.77369(10) 1.01627(8) 0.39808(4) 0.0592(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0322(3) 0.0395(3) 0.0564(3) -0.0020(3) 0.0010(3) 0.0240(3) Sn2 0.0276(3) 0.0371(3) 0.0650(4) -0.0032(3) -0.0057(3) 0.0176(3) Sn3 0.0350(3) 0.0348(4) 0.0672(4) 0.0077(3) 0.0007(3) 0.0171(3) Se1 0.0319(4) 0.0379(5) 0.0558(5) 0.0005(4) -0.0031(4) 0.0189(4) Se2 0.0424(5) 0.0457(5) 0.0659(6) 0.0129(4) 0.0130(5) 0.0288(5) Se3 0.0516(6) 0.0666(7) 0.0517(5) -0.0020(5) -0.0010(5) 0.0439(5) Se4 0.0407(6) 0.0422(5) 0.0754(7) -0.0090(5) 0.0049(5) 0.0224(5) Se5 0.0482(5) 0.0457(6) 0.0774(7) -0.0131(5) -0.0252(5) 0.0270(5) Se6 0.0560(6) 0.0605(6) 0.0537(5) 0.0000(5) -0.0023(5) 0.0446(5) Se7 0.0731(7) 0.0356(5) 0.0581(6) 0.0018(5) -0.0023(6) 0.0190(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Se3 2.5247(11) . ? Sn1 Se5 2.5444(11) . ? Sn1 Se2 2.5579(11) . ? Sn1 Se6 2.7084(10) . ? Sn1 Se1 2.7565(10) . ? Sn2 Se6 2.5062(11) 6_565 ? Sn2 Se4 2.5481(11) . ? Sn2 Se2 2.5520(11) . ? Sn2 Se3 2.6932(11) 6_565 ? Sn2 Se1 2.8218(10) . ? Sn3 Se7 2.5110(12) 6_675 ? Sn3 Se5 2.5454(11) . ? Sn3 Se4 2.5536(11) . ? Sn3 Se7 2.7104(12) . ? Sn3 Se1 2.7566(11) . ? Se3 Sn2 2.6932(11) 6_665 ? Se6 Sn2 2.5062(11) 6_665 ? Se7 Sn3 2.5110(12) 6_675 ? 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 Sn1 Se5 123.98(4) . . ? Se3 Sn1 Se2 122.65(4) . . ? Se5 Sn1 Se2 113.37(4) . . ? Se3 Sn1 Se6 89.37(3) . . ? Se5 Sn1 Se6 90.38(4) . . ? Se2 Sn1 Se6 91.26(3) . . ? Se3 Sn1 Se1 92.58(3) . . ? Se5 Sn1 Se1 87.99(3) . . ? Se2 Sn1 Se1 88.23(3) . . ? Se6 Sn1 Se1 177.94(4) . . ? Se6 Sn2 Se4 121.97(4) 6_565 . ? Se6 Sn2 Se2 121.86(4) 6_565 . ? Se4 Sn2 Se2 115.97(4) . . ? Se6 Sn2 Se3 90.11(3) 6_565 6_565 ? Se4 Sn2 Se3 92.75(4) . 6_565 ? Se2 Sn2 Se3 91.83(4) . 6_565 ? Se6 Sn2 Se1 91.51(3) 6_565 . ? Se4 Sn2 Se1 86.78(3) . . ? Se2 Sn2 Se1 86.94(3) . . ? Se3 Sn2 Se1 178.33(4) 6_565 . ? Se7 Sn3 Se5 123.47(4) 6_675 . ? Se7 Sn3 Se4 121.88(4) 6_675 . ? Se5 Sn3 Se4 114.65(4) . . ? Se7 Sn3 Se7 89.15(4) 6_675 . ? Se5 Sn3 Se7 91.10(4) . . ? Se4 Sn3 Se7 90.43(4) . . ? Se7 Sn3 Se1 93.09(4) 6_675 . ? Se5 Sn3 Se1 87.97(3) . . ? Se4 Sn3 Se1 88.08(3) . . ? Se7 Sn3 Se1 177.73(4) . . ? Sn1 Se1 Sn3 85.67(3) . . ? Sn1 Se1 Sn2 85.31(3) . . ? Sn3 Se1 Sn2 85.07(3) . . ? Sn2 Se2 Sn1 95.42(3) . . ? Sn1 Se3 Sn2 90.14(3) . 6_665 ? Sn2 Se4 Sn3 95.34(3) . . ? Sn1 Se5 Sn3 94.86(3) . . ? Sn2 Se6 Sn1 90.19(3) 6_665 . ? Sn3 Se7 Sn3 90.74(4) 6_675 . ? 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 Sn1 Se1 Sn3 -137.47(4) . . . . ? Se5 Sn1 Se1 Sn3 -13.54(3) . . . . ? Se2 Sn1 Se1 Sn3 99.92(3) . . . . ? Se6 Sn1 Se1 Sn3 24.1(11) . . . . ? Se3 Sn1 Se1 Sn2 137.13(4) . . . . ? Se5 Sn1 Se1 Sn2 -98.94(4) . . . . ? Se2 Sn1 Se1 Sn2 14.52(3) . . . . ? Se6 Sn1 Se1 Sn2 -61.3(11) . . . . ? Se7 Sn3 Se1 Sn1 136.95(4) 6_675 . . . ? Se5 Sn3 Se1 Sn1 13.53(3) . . . . ? Se4 Sn3 Se1 Sn1 -101.23(3) . . . . ? Se7 Sn3 Se1 Sn1 -52.3(10) . . . . ? Se7 Sn3 Se1 Sn2 -137.40(4) 6_675 . . . ? Se5 Sn3 Se1 Sn2 99.19(3) . . . . ? Se4 Sn3 Se1 Sn2 -15.57(3) . . . . ? Se7 Sn3 Se1 Sn2 33.3(10) . . . . ? Se6 Sn2 Se1 Sn1 -136.40(4) 6_565 . . . ? Se4 Sn2 Se1 Sn1 101.67(3) . . . . ? Se2 Sn2 Se1 Sn1 -14.57(3) . . . . ? Se3 Sn2 Se1 Sn1 27.9(13) 6_565 . . . ? Se6 Sn2 Se1 Sn3 137.56(4) 6_565 . . . ? Se4 Sn2 Se1 Sn3 15.62(3) . . . . ? Se2 Sn2 Se1 Sn3 -100.62(3) . . . . ? Se3 Sn2 Se1 Sn3 -58.1(13) 6_565 . . . ? Se6 Sn2 Se2 Sn1 105.62(5) 6_565 . . . ? Se4 Sn2 Se2 Sn1 -69.17(5) . . . . ? Se3 Sn2 Se2 Sn1 -163.12(4) 6_565 . . . ? Se1 Sn2 Se2 Sn1 15.75(3) . . . . ? Se3 Sn1 Se2 Sn2 -108.05(4) . . . . ? Se5 Sn1 Se2 Sn2 70.93(5) . . . . ? Se6 Sn1 Se2 Sn2 161.89(4) . . . . ? Se1 Sn1 Se2 Sn2 -16.12(4) . . . . ? Se5 Sn1 Se3 Sn2 86.80(5) . . . 6_665 ? Se2 Sn1 Se3 Sn2 -94.33(4) . . . 6_665 ? Se6 Sn1 Se3 Sn2 -3.23(4) . . . 6_665 ? Se1 Sn1 Se3 Sn2 176.12(3) . . . 6_665 ? Se6 Sn2 Se4 Sn3 -106.68(4) 6_565 . . . ? Se2 Sn2 Se4 Sn3 68.11(5) . . . . ? Se3 Sn2 Se4 Sn3 161.48(4) 6_565 . . . ? Se1 Sn2 Se4 Sn3 -16.91(3) . . . . ? Se7 Sn3 Se4 Sn2 109.75(5) 6_675 . . . ? Se5 Sn3 Se4 Sn2 -69.58(5) . . . . ? Se7 Sn3 Se4 Sn2 -160.99(4) . . . . ? Se1 Sn3 Se4 Sn2 17.31(4) . . . . ? Se3 Sn1 Se5 Sn3 106.46(4) . . . . ? Se2 Sn1 Se5 Sn3 -72.51(5) . . . . ? Se6 Sn1 Se5 Sn3 -164.05(4) . . . . ? Se1 Sn1 Se5 Sn3 14.70(4) . . . . ? Se7 Sn3 Se5 Sn1 -107.05(5) 6_675 . . . ? Se4 Sn3 Se5 Sn1 72.26(5) . . . . ? Se7 Sn3 Se5 Sn1 163.24(4) . . . . ? Se1 Sn3 Se5 Sn1 -14.69(4) . . . . ? Se3 Sn1 Se6 Sn2 3.47(4) . . . 6_665 ? Se5 Sn1 Se6 Sn2 -120.50(4) . . . 6_665 ? Se2 Sn1 Se6 Sn2 126.11(4) . . . 6_665 ? Se1 Sn1 Se6 Sn2 -158.1(11) . . . 6_665 ? Se7 Sn3 Se7 Sn3 3.74(6) 6_675 . . 6_675 ? Se5 Sn3 Se7 Sn3 127.20(4) . . . 6_675 ? Se4 Sn3 Se7 Sn3 -118.14(4) . . . 6_675 ? Se1 Sn3 Se7 Sn3 -167.0(10) . . . 6_675 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.934 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.154 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.034 -0.025 -0.008 3116.8 232.1 _platon_squeeze_details ; ? ; data_compound-6_WX11-46B _database_code_depnum_ccdc_archive 'CCDC 903265' #TrackingRef 'compound 1-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag Se28 Sn12,C63 H119 N14' _chemical_formula_sum 'C63 H119 Ag N14 Se28 Sn12' _chemical_formula_weight 4815.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8983(4) _cell_length_b 13.5554(6) _cell_length_c 23.0906(10) _cell_angle_alpha 88.904(3) _cell_angle_beta 86.700(3) _cell_angle_gamma 68.230(4) _cell_volume 3162.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5701 _cell_measurement_theta_min 2.2824 _cell_measurement_theta_max 28.8863 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2194 _exptl_absorpt_coefficient_mu 10.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.39933 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21587 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12155 _reflns_number_gt 8734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0420P)^2^+2.6055P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12155 _refine_ls_number_parameters 896 _refine_ls_number_restraints 2164 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.006 _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 Ag1 Ag 0.5000 0.5000 0.0000 0.0771(4) Uani 1 2 d S . . Sn1 Sn 0.71706(5) -0.03868(4) 0.28015(2) 0.02943(13) Uani 1 1 d . . . Sn2 Sn 0.51803(5) 0.02995(4) 0.42285(2) 0.03651(14) Uani 1 1 d . . . Sn3 Sn 0.44245(5) 0.22224(4) 0.29920(2) 0.03335(13) Uani 1 1 d . . . Sn4 Sn 0.28705(6) 0.47606(4) 0.23120(3) 0.04847(17) Uani 1 1 d . . . Sn5 Sn 0.00528(5) 0.75929(4) 0.20729(2) 0.03677(14) Uani 1 1 d . . . Sn6 Sn 0.21883(5) 0.60879(4) 0.09028(2) 0.04248(15) Uani 1 1 d . . . Se1 Se 0.76374(8) -0.20563(6) 0.20685(4) 0.0412(2) Uani 1 1 d . . . Se2 Se 0.95870(8) -0.06476(6) 0.26684(4) 0.0443(2) Uani 1 1 d . . . Se3 Se 0.54262(8) 0.08744(6) 0.21670(3) 0.0396(2) Uani 1 1 d . . . Se4 Se 0.63236(8) -0.13486(6) 0.35922(4) 0.0402(2) Uani 1 1 d . . . Se5 Se 0.66625(7) 0.12616(6) 0.35592(3) 0.03364(18) Uani 1 1 d . . . Se6 Se 0.38137(9) -0.06294(8) 0.48781(4) 0.0521(2) Uani 1 1 d . . . Se7 Se 0.31189(8) 0.16832(7) 0.38076(4) 0.0470(2) Uani 1 1 d . . . Se8 Se 0.22385(9) 0.31710(6) 0.23877(4) 0.0470(2) Uani 1 1 d . . . Se9 Se 0.47949(9) 0.39691(6) 0.30003(4) 0.0551(3) Uani 1 1 d . . . Se10 Se 0.15306(8) 0.64721(6) 0.28456(4) 0.0427(2) Uani 1 1 d . . . Se11 Se 0.42562(8) 0.50256(7) 0.14327(4) 0.0511(2) Uani 1 1 d . . . Se12 Se 0.05085(8) 0.55670(7) 0.14593(4) 0.0467(2) Uani 1 1 d . . . Se13 Se 0.13604(9) 0.80245(7) 0.12173(4) 0.0542(3) Uani 1 1 d . . . Se14 Se 0.26144(11) 0.58696(10) -0.01542(4) 0.0767(3) Uani 1 1 d . . . N1 N 0.2671(14) 0.3034(14) -0.0005(7) 0.077(5) Uani 0.50 1 d PDU A 1 N2 N 0.4560(14) 0.2364(14) 0.0379(7) 0.085(5) Uani 0.50 1 d PDU A 1 C1 C 0.2436(17) 0.304(2) 0.0595(7) 0.101(5) Uani 0.50 1 d PDU A 1 H1A H 0.1612 0.3277 0.0794 0.121 Uiso 0.50 1 calc PR A 1 C2 C 0.3596(18) 0.264(2) 0.0830(7) 0.098(4) Uani 0.50 1 d PDU A 1 H2A H 0.3739 0.2554 0.1224 0.117 Uiso 0.50 1 calc PR A 1 C3 C 0.3968(16) 0.263(2) -0.0116(6) 0.096(4) Uani 0.50 1 d PDU A 1 C4 C 0.165(2) 0.343(2) -0.0406(9) 0.105(6) Uani 0.50 1 d PDU A 1 H4A H 0.2005 0.3634 -0.0760 0.157 Uiso 0.50 1 calc PR A 1 H4B H 0.0948 0.4044 -0.0242 0.157 Uiso 0.50 1 calc PR A 1 H4C H 0.1312 0.2894 -0.0487 0.157 Uiso 0.50 1 calc PR A 1 C5 C 0.464(2) 0.246(2) -0.0696(7) 0.103(6) Uani 0.50 1 d PDU A 1 H5A H 0.5580 0.2161 -0.0661 0.154 Uiso 0.50 1 calc PR A 1 H5B H 0.4406 0.3127 -0.0897 0.154 Uiso 0.50 1 calc PR A 1 H5C H 0.4370 0.1982 -0.0910 0.154 Uiso 0.50 1 calc PR A 1 C6 C 0.5987(15) 0.1866(14) 0.0458(10) 0.103(4) Uani 0.50 1 d PDU A 1 H6A H 0.6457 0.2097 0.0148 0.124 Uiso 0.50 1 calc PR A 1 H6B H 0.6178 0.2111 0.0822 0.124 Uiso 0.50 1 calc PR A 1 C7 C 0.6480(19) 0.0710(14) 0.0462(12) 0.108(4) Uani 0.50 1 d PDU A 1 H7A H 0.6043 0.0481 0.0167 0.130 Uiso 0.50 1 calc PR A 1 H7B H 0.6220 0.0484 0.0834 0.130 Uiso 0.50 1 calc PR A 1 C8 C 0.796(2) 0.0140(16) 0.0357(14) 0.128(6) Uani 0.50 1 d PDU A 1 H8A H 0.8431 0.0279 0.0670 0.154 Uiso 0.50 1 calc PR A 1 H8B H 0.8267 0.0370 -0.0005 0.154 Uiso 0.50 1 calc PR A 1 C9 C 0.819(3) -0.1038(15) 0.0330(14) 0.148(8) Uani 0.50 1 d PDU A 1 H9A H 0.9083 -0.1453 0.0414 0.222 Uiso 0.50 1 calc PR A 1 H9B H 0.8019 -0.1212 -0.0052 0.222 Uiso 0.50 1 calc PR A 1 H9C H 0.7594 -0.1191 0.0609 0.222 Uiso 0.50 1 calc PR A 1 N3 N 0.821(2) 0.3293(14) 0.2232(9) 0.087(6) Uani 0.50 1 d PDU B 1 N4 N 0.847(2) 0.4619(13) 0.2654(8) 0.088(5) Uani 0.50 1 d PDU B 1 C11 C 0.779(3) 0.4165(17) 0.1862(10) 0.107(4) Uani 0.50 1 d PDU B 1 H11A H 0.7453 0.4182 0.1500 0.129 Uiso 0.50 1 calc PR B 1 C12 C 0.796(3) 0.4957(15) 0.2119(10) 0.109(4) Uani 0.50 1 d PDU B 1 H12A H 0.7766 0.5634 0.1967 0.131 Uiso 0.50 1 calc PR B 1 C13 C 0.862(3) 0.3594(14) 0.2707(10) 0.105(4) Uani 0.50 1 d PDU B 1 C14 C 0.815(3) 0.2281(16) 0.2096(13) 0.111(6) Uani 0.50 1 d PDU B 1 H14A H 0.8734 0.1741 0.2335 0.167 Uiso 0.50 1 calc PR B 1 H14B H 0.8420 0.2115 0.1695 0.167 Uiso 0.50 1 calc PR B 1 H14C H 0.7263 0.2311 0.2168 0.167 Uiso 0.50 1 calc PR B 1 C15 C 0.914(3) 0.2914(17) 0.3205(10) 0.112(6) Uani 0.50 1 d PDU B 1 H15A H 0.9642 0.2204 0.3073 0.168 Uiso 0.50 1 calc PR B 1 H15B H 0.8413 0.2908 0.3462 0.168 Uiso 0.50 1 calc PR B 1 H15C H 0.9693 0.3182 0.3408 0.168 Uiso 0.50 1 calc PR B 1 C16 C 0.885(3) 0.5255(18) 0.3047(9) 0.123(5) Uani 0.50 1 d PDU B 1 H16A H 0.8477 0.5987 0.2917 0.148 Uiso 0.50 1 calc PR B 1 H16B H 0.9802 0.5036 0.3009 0.148 Uiso 0.50 1 calc PR B 1 C17 C 0.847(3) 0.524(2) 0.3666(9) 0.142(5) Uani 0.50 1 d PDU B 1 H17A H 0.8772 0.4499 0.3787 0.170 Uiso 0.50 1 calc PR B 1 H17B H 0.7507 0.5512 0.3707 0.170 Uiso 0.50 1 calc PR B 1 C18 C 0.895(3) 0.583(2) 0.4080(11) 0.174(7) Uani 0.50 1 d PDU . 1 H18A H 0.8328 0.6032 0.4415 0.208 Uiso 0.50 1 calc PR . 1 H18B H 0.8948 0.6477 0.3894 0.208 Uiso 0.50 1 calc PR . 1 C19 C 1.034(3) 0.521(3) 0.4290(14) 0.181(7) Uani 0.50 1 d PDU . 1 H19A H 1.0532 0.5698 0.4532 0.272 Uiso 0.50 1 d PR . 1 H19B H 1.0340 0.4608 0.4515 0.272 Uiso 0.50 1 d PR . 1 H19C H 1.0993 0.4982 0.3975 0.272 Uiso 0.50 1 d PR . 1 N5 N 0.3670(16) 0.7601(13) 0.3464(8) 0.100(6) Uani 0.50 1 d PDU C 1 N6 N 0.3421(15) 0.8655(12) 0.2728(8) 0.106(6) Uani 0.50 1 d PDU C 1 C21 C 0.281(2) 0.8587(17) 0.3641(9) 0.132(5) Uani 0.50 1 d PDU C 1 H21A H 0.2367 0.8760 0.4003 0.158 Uiso 0.50 1 calc PR C 1 C22 C 0.273(3) 0.9252(14) 0.3201(10) 0.138(5) Uani 0.50 1 d PDU C 1 H22A H 0.2281 0.9985 0.3210 0.165 Uiso 0.50 1 calc PR C 1 C23 C 0.403(3) 0.7675(14) 0.2908(9) 0.133(5) Uani 0.50 1 d PDU C 1 C24 C 0.413(3) 0.6625(19) 0.3814(13) 0.157(7) Uani 0.50 1 d PDU C 1 H24A H 0.3872 0.6096 0.3646 0.235 Uiso 0.50 1 calc PR C 1 H24B H 0.3752 0.6778 0.4203 0.235 Uiso 0.50 1 calc PR C 1 H24C H 0.5081 0.6366 0.3821 0.235 Uiso 0.50 1 calc PR C 1 C25 C 0.492(3) 0.6826(19) 0.2526(12) 0.123(6) Uani 0.50 1 d PDU C 1 H25A H 0.4519 0.6838 0.2166 0.185 Uiso 0.50 1 calc PR C 1 H25B H 0.5099 0.6151 0.2711 0.185 Uiso 0.50 1 calc PR C 1 H25C H 0.5740 0.6936 0.2451 0.185 Uiso 0.50 1 calc PR C 1 C26 C 0.350(3) 0.9096(19) 0.2149(10) 0.140(5) Uani 0.50 1 d PDU C 1 H26A H 0.3413 0.8616 0.1863 0.168 Uiso 0.50 1 calc PR C 1 H26B H 0.4375 0.9128 0.2081 0.168 Uiso 0.50 1 calc PR C 1 C27 C 0.250(3) 1.0161(18) 0.2058(10) 0.161(6) Uani 0.50 1 d PDU C 1 H27A H 0.2756 1.0675 0.2257 0.194 Uiso 0.50 1 calc PR C 1 H27B H 0.1665 1.0186 0.2237 0.194 Uiso 0.50 1 calc PR C 1 C28 C 0.230(3) 1.050(2) 0.1426(11) 0.164(8) Uani 0.50 1 d PDU C 1 H28A H 0.2956 1.0784 0.1284 0.197 Uiso 0.50 1 calc PR C 1 H28B H 0.2377 0.9898 0.1186 0.197 Uiso 0.50 1 calc PR C 1 C29 C 0.091(3) 1.135(3) 0.1404(15) 0.183(11) Uani 0.50 1 d PDU C 1 H29A H 0.0465 1.1199 0.1091 0.274 Uiso 0.50 1 calc PR C 1 H29B H 0.0974 1.2034 0.1343 0.274 Uiso 0.50 1 calc PR C 1 H29C H 0.0421 1.1357 0.1764 0.274 Uiso 0.50 1 calc PR C 1 N1B N 0.2463(15) 0.3124(15) 0.0201(7) 0.081(5) Uani 0.50 1 d PDU D 2 N2B N 0.4602(14) 0.2433(13) 0.0195(7) 0.081(5) Uani 0.50 1 d PDU D 2 C1B C 0.2803(18) 0.291(2) 0.0770(7) 0.091(4) Uani 0.50 1 d PDU D 2 H1B H 0.2218 0.3037 0.1094 0.109 Uiso 0.50 1 calc PR D 2 C2B C 0.4115(19) 0.249(2) 0.0770(7) 0.098(4) Uani 0.50 1 d PDU D 2 H2B H 0.4616 0.2275 0.1095 0.118 Uiso 0.50 1 calc PR D 2 C3B C 0.3582(16) 0.281(2) -0.0132(7) 0.092(4) Uani 0.50 1 d PDU D 2 C4B C 0.1136(16) 0.3580(18) 0.0012(9) 0.098(6) Uani 0.50 1 d PDU D 2 H4D H 0.1078 0.4129 -0.0266 0.147 Uiso 0.50 1 calc PR D 2 H4E H 0.0535 0.3878 0.0340 0.147 Uiso 0.50 1 calc PR D 2 H4F H 0.0908 0.3039 -0.0163 0.147 Uiso 0.50 1 calc PR D 2 C5B C 0.364(2) 0.293(2) -0.0763(7) 0.108(6) Uani 0.50 1 d PDU D 2 H5D H 0.4107 0.3397 -0.0867 0.162 Uiso 0.50 1 calc PR D 2 H5E H 0.2763 0.3232 -0.0896 0.162 Uiso 0.50 1 calc PR D 2 H5F H 0.4102 0.2251 -0.0940 0.162 Uiso 0.50 1 calc PR D 2 C6B C 0.6010(16) 0.2000(14) 0.0025(10) 0.107(4) Uani 0.50 1 d PDU D 2 H6C H 0.6504 0.2073 0.0347 0.129 Uiso 0.50 1 calc PR D 2 H6D H 0.6180 0.2411 -0.0296 0.129 Uiso 0.50 1 calc PR D 2 C7B C 0.650(2) 0.0847(15) -0.0152(8) 0.123(5) Uani 0.50 1 d PDU D 2 H7C H 0.5936 0.0750 -0.0437 0.147 Uiso 0.50 1 calc PR D 2 H7D H 0.7391 0.0636 -0.0327 0.147 Uiso 0.50 1 calc PR D 2 C8B C 0.650(3) 0.0164(17) 0.0367(11) 0.115(5) Uani 0.50 1 d PDU D 2 H8C H 0.5734 0.0534 0.0625 0.138 Uiso 0.50 1 calc PR D 2 H8D H 0.6417 -0.0487 0.0241 0.138 Uiso 0.50 1 calc PR D 2 C9B C 0.773(3) -0.010(2) 0.0692(11) 0.128(8) Uani 0.50 1 d PDU D 2 H9D H 0.7916 -0.0777 0.0881 0.193 Uiso 0.50 1 calc PR D 2 H9E H 0.7604 0.0436 0.0977 0.193 Uiso 0.50 1 calc PR D 2 H9F H 0.8455 -0.0143 0.0426 0.193 Uiso 0.50 1 calc PR D 2 N3B N 0.8702(19) 0.4380(13) 0.2793(8) 0.092(5) Uani 0.50 1 d PDU E 2 N4B N 0.812(2) 0.3392(14) 0.2228(9) 0.088(6) Uani 0.50 1 d PDU E 2 C11B C 0.811(3) 0.4992(15) 0.2320(10) 0.115(4) Uani 0.50 1 d PDU E 2 H11B H 0.7974 0.5705 0.2261 0.138 Uiso 0.50 1 calc PR E 2 C12B C 0.778(3) 0.4386(17) 0.1973(10) 0.110(4) Uani 0.50 1 d PDU E 2 H12B H 0.7395 0.4587 0.1619 0.132 Uiso 0.50 1 calc PR E 2 C13B C 0.868(3) 0.3421(14) 0.2720(10) 0.104(4) Uani 0.50 1 d PDU E 2 C14B C 0.926(2) 0.4749(17) 0.3246(9) 0.112(6) Uani 0.50 1 d PDU E 2 H14D H 0.9293 0.4326 0.3587 0.167 Uiso 0.50 1 calc PR E 2 H14E H 0.8730 0.5478 0.3332 0.167 Uiso 0.50 1 calc PR E 2 H14F H 1.0144 0.4692 0.3123 0.167 Uiso 0.50 1 calc PR E 2 C15B C 0.923(3) 0.2494(16) 0.3103(11) 0.111(6) Uani 0.50 1 d PDU E 2 H15D H 0.8917 0.2695 0.3497 0.166 Uiso 0.50 1 calc PR E 2 H15E H 1.0178 0.2247 0.3075 0.166 Uiso 0.50 1 calc PR E 2 H15F H 0.8951 0.1937 0.2987 0.166 Uiso 0.50 1 calc PR E 2 C16B C 0.786(2) 0.2517(18) 0.1994(12) 0.112(5) Uani 0.50 1 d PDU E 2 H16C H 0.6964 0.2789 0.1861 0.134 Uiso 0.50 1 calc PR E 2 H16D H 0.7880 0.2023 0.2306 0.134 Uiso 0.50 1 calc PR E 2 C17B C 0.877(2) 0.1914(17) 0.1508(10) 0.107(5) Uani 0.50 1 d PDU E 2 H17C H 0.8714 0.1217 0.1489 0.129 Uiso 0.50 1 calc PR E 2 H17D H 0.8453 0.2276 0.1148 0.129 Uiso 0.50 1 calc PR E 2 C18B C 1.015(2) 0.177(2) 0.1538(12) 0.123(5) Uani 0.50 1 d PDU E 2 H18C H 1.0437 0.1470 0.1913 0.148 Uiso 0.50 1 calc PR E 2 H18D H 1.0206 0.2471 0.1524 0.148 Uiso 0.50 1 calc PR E 2 C19B C 1.110(2) 0.110(2) 0.1080(13) 0.146(10) Uani 0.50 1 d PDU E 2 H19D H 1.1927 0.1197 0.1087 0.219 Uiso 0.50 1 calc PR E 2 H19E H 1.0744 0.1292 0.0706 0.219 Uiso 0.50 1 calc PR E 2 H19F H 1.1247 0.0362 0.1153 0.219 Uiso 0.50 1 calc PR E 2 N5B N 0.3972(16) 0.7991(12) 0.2640(8) 0.094(5) Uani 0.50 1 d PDU F 2 N6B N 0.4271(16) 0.7082(13) 0.3441(8) 0.100(6) Uani 0.50 1 d PDU F 2 C21B C 0.488(3) 0.6979(17) 0.2514(9) 0.129(5) Uani 0.50 1 d PDU F 2 H21B H 0.5293 0.6728 0.2153 0.155 Uiso 0.50 1 calc PR F 2 C22B C 0.506(2) 0.6432(14) 0.3012(10) 0.129(5) Uani 0.50 1 d PDU F 2 H22B H 0.5622 0.5729 0.3058 0.154 Uiso 0.50 1 calc PR F 2 C23B C 0.362(2) 0.8033(14) 0.3200(9) 0.127(5) Uani 0.50 1 d PDU F 2 C24B C 0.354(3) 0.882(2) 0.2206(12) 0.143(7) Uani 0.50 1 d PDU F 2 H24D H 0.2589 0.9080 0.2201 0.215 Uiso 0.50 1 calc PR F 2 H24E H 0.3917 0.8530 0.1832 0.215 Uiso 0.50 1 calc PR F 2 H24F H 0.3815 0.9386 0.2299 0.215 Uiso 0.50 1 calc PR F 2 C25B C 0.268(3) 0.8962(17) 0.3503(12) 0.123(6) Uani 0.50 1 d PDU F 2 H25D H 0.2244 0.9496 0.3226 0.184 Uiso 0.50 1 calc PR F 2 H25E H 0.3141 0.9237 0.3758 0.184 Uiso 0.50 1 calc PR F 2 H25F H 0.2033 0.8765 0.3724 0.184 Uiso 0.50 1 calc PR F 2 C26B C 0.410(2) 0.682(2) 0.4045(9) 0.147(5) Uani 0.50 1 d PDU F 2 H26C H 0.3573 0.6380 0.4064 0.176 Uiso 0.50 1 calc PR F 2 H26D H 0.3584 0.7478 0.4249 0.176 Uiso 0.50 1 calc PR F 2 C27B C 0.531(2) 0.627(2) 0.4368(10) 0.155(6) Uani 0.50 1 d PDU F 2 H27C H 0.5909 0.6653 0.4313 0.186 Uiso 0.50 1 calc PR F 2 H27D H 0.5762 0.5559 0.4215 0.186 Uiso 0.50 1 calc PR F 2 C28B C 0.496(3) 0.622(3) 0.5023(10) 0.193(8) Uani 0.50 1 d PDU F 2 H28C H 0.5455 0.5516 0.5169 0.232 Uiso 0.50 1 calc PR F 2 H28D H 0.5190 0.6730 0.5232 0.232 Uiso 0.50 1 calc PR F 2 C29B C 0.346(3) 0.646(3) 0.5124(15) 0.206(11) Uani 0.50 1 d PDU F 2 H29D H 0.3326 0.5976 0.5409 0.310 Uiso 0.50 1 calc PR F 2 H29E H 0.3103 0.6369 0.4767 0.310 Uiso 0.50 1 calc PR F 2 H29F H 0.3020 0.7174 0.5260 0.310 Uiso 0.50 1 calc PR F 2 N7 N 0.979(3) -0.053(2) 0.4684(13) 0.099(8) Uani 0.50 1 d PDU . . N8 N 1.029(3) 0.070(2) 0.5077(9) 0.106(9) Uani 0.50 1 d PDU . . C31 C 0.982(3) 0.018(2) 0.4254(10) 0.144(7) Uani 0.50 1 d PDU . . H31A H 0.9652 0.0143 0.3853 0.173 Uiso 0.50 1 d PR . . C32 C 1.012(4) 0.095(2) 0.4495(11) 0.145(6) Uani 0.50 1 d PDU . . H32A H 1.0190 0.1565 0.4307 0.173 Uiso 0.50 1 d PR . . C33 C 1.006(4) -0.017(2) 0.5175(11) 0.143(7) Uani 0.50 1 d PDU . . C34 C 0.928(4) -0.125(3) 0.447(2) 0.138(7) Uani 0.50 1 d PU . . H34A H 0.9286 -0.1731 0.4782 0.206 Uiso 0.50 1 d PR . . H34B H 0.8389 -0.0877 0.4363 0.206 Uiso 0.50 1 d PR . . H34C H 0.9812 -0.1633 0.4146 0.206 Uiso 0.50 1 d PR . . C35 C 1.012(5) -0.082(3) 0.5699(16) 0.142(7) Uani 0.50 1 d PU . . H35A H 1.0337 -0.0487 0.6020 0.212 Uiso 0.50 1 d PR . . H35B H 0.9266 -0.0864 0.5779 0.212 Uiso 0.50 1 d PR . . H35C H 1.0773 -0.1524 0.5644 0.212 Uiso 0.50 1 d PR . . C36 C 1.062(4) 0.137(2) 0.5477(17) 0.153(6) Uani 0.50 1 d PDU . . H36A H 1.1464 0.1400 0.5357 0.183 Uiso 0.50 1 d PR . . H36B H 1.0685 0.1061 0.5856 0.183 Uiso 0.50 1 d PR . . C37 C 0.959(2) 0.248(2) 0.5503(14) 0.155(7) Uani 0.50 1 d PDU . . H37A H 0.8933 0.2509 0.5806 0.186 Uiso 0.50 1 d PR . . H37B H 0.9153 0.2625 0.5143 0.186 Uiso 0.50 1 d PR . . C38 C 1.005(3) 0.334(2) 0.5576(14) 0.169(8) Uani 0.50 1 d PDU . . H38A H 1.0372 0.3234 0.5959 0.203 Uiso 0.50 1 d PR . . H38B H 0.9312 0.4006 0.5580 0.203 Uiso 0.50 1 d PR . . C39 C 1.114(3) 0.344(2) 0.5199(15) 0.189(8) Uani 0.50 1 d PDU . . H39A H 1.1361 0.4017 0.5326 0.283 Uiso 0.50 1 d PR . . H39B H 1.1905 0.2793 0.5199 0.283 Uiso 0.50 1 d PR . . H39C H 1.0827 0.3577 0.4813 0.283 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0612(7) 0.0872(8) 0.0726(8) -0.0215(7) 0.0288(6) -0.0190(6) Sn1 0.0266(3) 0.0269(3) 0.0310(3) 0.0014(2) 0.0008(2) -0.0059(2) Sn2 0.0390(3) 0.0458(3) 0.0227(3) 0.0041(2) -0.0013(2) -0.0136(3) Sn3 0.0344(3) 0.0264(3) 0.0344(3) 0.0036(2) 0.0008(2) -0.0062(2) Sn4 0.0479(4) 0.0277(3) 0.0551(4) 0.0070(3) 0.0143(3) 0.0003(3) Sn5 0.0278(3) 0.0325(3) 0.0422(3) 0.0034(2) 0.0063(2) -0.0035(2) Sn6 0.0357(3) 0.0484(3) 0.0351(3) 0.0007(3) 0.0083(3) -0.0074(3) Se1 0.0325(4) 0.0368(4) 0.0520(5) -0.0136(4) 0.0005(4) -0.0101(4) Se2 0.0304(4) 0.0376(4) 0.0654(6) -0.0111(4) 0.0034(4) -0.0134(4) Se3 0.0446(5) 0.0355(4) 0.0299(4) 0.0000(4) -0.0077(4) -0.0036(4) Se4 0.0481(5) 0.0336(4) 0.0411(5) 0.0048(4) 0.0023(4) -0.0184(4) Se5 0.0341(4) 0.0337(4) 0.0330(4) 0.0003(3) -0.0024(3) -0.0123(3) Se6 0.0618(6) 0.0820(7) 0.0291(5) 0.0059(5) -0.0040(4) -0.0459(5) Se7 0.0310(4) 0.0565(5) 0.0470(5) 0.0122(4) 0.0047(4) -0.0101(4) Se8 0.0415(5) 0.0409(5) 0.0532(5) 0.0083(4) -0.0118(4) -0.0080(4) Se9 0.0565(6) 0.0327(4) 0.0764(7) 0.0057(5) -0.0139(5) -0.0158(4) Se10 0.0417(5) 0.0380(4) 0.0395(5) -0.0042(4) -0.0038(4) -0.0039(4) Se11 0.0299(5) 0.0609(6) 0.0523(6) 0.0058(5) 0.0071(4) -0.0063(4) Se12 0.0419(5) 0.0540(5) 0.0445(5) -0.0049(4) 0.0072(4) -0.0193(4) Se13 0.0578(6) 0.0429(5) 0.0591(6) 0.0063(5) 0.0187(5) -0.0186(4) Se14 0.0704(7) 0.1122(9) 0.0364(5) -0.0049(6) 0.0108(5) -0.0226(7) N1 0.086(9) 0.076(8) 0.076(11) 0.007(8) -0.020(9) -0.035(8) N2 0.090(9) 0.080(9) 0.085(11) 0.004(9) -0.015(9) -0.029(8) C1 0.115(9) 0.106(8) 0.086(8) -0.001(8) -0.009(8) -0.044(8) C2 0.117(8) 0.105(7) 0.081(7) -0.001(7) -0.012(7) -0.052(8) C3 0.116(8) 0.103(7) 0.080(7) 0.001(7) -0.014(7) -0.054(7) C4 0.115(12) 0.116(11) 0.086(11) -0.003(11) -0.023(11) -0.043(11) C5 0.113(11) 0.118(11) 0.077(10) -0.005(10) -0.009(10) -0.043(10) C6 0.116(8) 0.111(7) 0.092(7) 0.002(7) -0.015(7) -0.050(7) C7 0.118(8) 0.114(8) 0.093(7) -0.006(7) -0.014(7) -0.043(8) C8 0.136(10) 0.127(10) 0.108(9) 0.001(9) -0.021(9) -0.030(9) C9 0.156(15) 0.137(14) 0.126(14) 0.011(13) -0.031(13) -0.023(14) N3 0.059(9) 0.065(9) 0.135(11) 0.008(9) 0.031(9) -0.026(8) N4 0.059(9) 0.073(9) 0.135(11) -0.007(9) 0.028(9) -0.031(8) C11 0.085(7) 0.088(7) 0.159(8) -0.003(7) 0.035(7) -0.049(6) C12 0.086(6) 0.092(7) 0.162(8) -0.014(7) 0.031(7) -0.054(6) C13 0.084(7) 0.088(7) 0.158(8) -0.004(7) 0.036(7) -0.054(6) C14 0.096(10) 0.086(10) 0.166(12) -0.007(10) 0.017(10) -0.054(9) C15 0.098(10) 0.093(11) 0.155(12) -0.010(10) 0.029(10) -0.052(10) C16 0.098(7) 0.106(8) 0.165(9) -0.013(7) 0.028(7) -0.042(7) C17 0.117(8) 0.120(8) 0.184(9) -0.010(8) 0.023(8) -0.042(7) C18 0.139(12) 0.149(12) 0.201(13) -0.016(11) 0.016(12) -0.019(11) C19 0.145(11) 0.162(11) 0.197(11) -0.012(10) 0.021(10) -0.014(10) N5 0.039(10) 0.119(14) 0.155(12) -0.096(11) 0.019(10) -0.044(10) N6 0.046(9) 0.124(14) 0.158(13) -0.096(11) 0.023(10) -0.043(10) C21 0.103(8) 0.124(8) 0.186(10) -0.055(8) 0.006(8) -0.061(7) C22 0.107(8) 0.125(8) 0.190(10) -0.053(8) 0.008(8) -0.054(7) C23 0.106(8) 0.123(8) 0.190(10) -0.052(8) 0.006(8) -0.063(7) C24 0.124(11) 0.144(12) 0.199(13) -0.046(12) 0.008(11) -0.044(11) C25 0.096(9) 0.107(9) 0.181(11) -0.064(10) 0.036(10) -0.058(9) C26 0.113(8) 0.127(9) 0.197(10) -0.054(8) 0.003(8) -0.065(8) C27 0.129(9) 0.150(10) 0.205(11) -0.043(10) 0.006(10) -0.052(9) C28 0.145(13) 0.154(13) 0.203(14) -0.057(13) -0.004(13) -0.065(12) C29 0.17(2) 0.144(19) 0.24(2) -0.091(19) 0.00(2) -0.063(17) N1B 0.081(9) 0.080(9) 0.080(12) 0.007(9) -0.029(9) -0.025(8) N2B 0.082(9) 0.079(9) 0.090(11) 0.000(9) -0.012(9) -0.038(8) C1B 0.111(9) 0.101(8) 0.072(7) -0.004(7) -0.007(8) -0.051(8) C2B 0.116(8) 0.106(7) 0.085(7) 0.001(7) -0.015(7) -0.054(7) C3B 0.112(8) 0.100(8) 0.078(7) -0.003(7) -0.013(7) -0.055(7) C4B 0.097(12) 0.117(12) 0.078(11) -0.002(11) -0.029(10) -0.034(11) C5B 0.134(12) 0.118(11) 0.070(10) 0.002(10) -0.020(10) -0.042(11) C6B 0.119(8) 0.112(7) 0.097(7) -0.001(7) -0.008(7) -0.049(7) C7B 0.128(8) 0.127(8) 0.105(8) 0.006(8) -0.008(8) -0.037(8) C8B 0.124(8) 0.121(8) 0.103(8) 0.005(8) -0.012(8) -0.048(8) C9B 0.129(14) 0.138(14) 0.100(13) 0.027(12) -0.011(13) -0.029(13) N3B 0.059(9) 0.079(9) 0.139(11) 0.001(9) 0.043(9) -0.034(8) N4B 0.064(9) 0.067(9) 0.135(11) 0.004(9) 0.035(9) -0.033(8) C11B 0.090(7) 0.095(7) 0.170(8) -0.012(7) 0.033(7) -0.051(6) C12B 0.085(7) 0.093(7) 0.159(8) -0.003(7) 0.035(7) -0.047(6) C13B 0.084(7) 0.085(7) 0.158(8) -0.005(7) 0.036(7) -0.056(6) C14B 0.095(10) 0.097(10) 0.157(12) -0.026(10) 0.056(10) -0.059(9) C15B 0.090(10) 0.099(10) 0.157(11) 0.005(10) 0.028(10) -0.056(9) C16B 0.090(7) 0.090(8) 0.166(9) -0.008(7) 0.027(7) -0.049(7) C17B 0.096(8) 0.087(8) 0.152(9) -0.011(8) 0.026(8) -0.053(7) C18B 0.101(8) 0.099(8) 0.168(9) -0.017(8) 0.044(8) -0.042(8) C19B 0.155(19) 0.096(16) 0.166(19) -0.023(16) 0.065(17) -0.030(15) N5B 0.044(9) 0.104(13) 0.156(13) -0.082(11) 0.027(10) -0.052(9) N6B 0.049(10) 0.113(14) 0.152(13) -0.076(11) 0.038(10) -0.049(10) C21B 0.102(7) 0.116(8) 0.185(9) -0.048(7) 0.021(7) -0.059(7) C22B 0.103(7) 0.113(7) 0.185(9) -0.042(7) 0.014(8) -0.058(7) C23B 0.101(8) 0.116(8) 0.188(10) -0.051(8) 0.009(8) -0.068(7) C24B 0.109(11) 0.136(12) 0.201(13) -0.047(12) 0.003(11) -0.065(10) C25B 0.090(10) 0.116(11) 0.174(12) -0.056(10) -0.003(10) -0.049(9) C26B 0.121(8) 0.130(8) 0.191(10) -0.045(8) 0.009(8) -0.050(7) C27B 0.132(9) 0.134(9) 0.198(10) -0.032(9) 0.019(9) -0.049(8) C28B 0.173(13) 0.154(13) 0.223(14) -0.024(13) 0.015(13) -0.029(13) C29B 0.167(18) 0.161(17) 0.25(2) -0.011(18) 0.038(18) -0.022(17) N7 0.043(10) 0.157(18) 0.07(2) 0.008(15) 0.012(14) -0.013(11) N8 0.056(11) 0.160(18) 0.06(2) -0.002(16) 0.022(14) -0.001(12) C31 0.095(10) 0.176(14) 0.137(12) -0.029(12) -0.012(10) -0.018(11) C32 0.096(10) 0.169(12) 0.145(12) -0.024(11) -0.002(10) -0.022(10) C33 0.093(10) 0.171(13) 0.142(12) -0.029(12) -0.005(11) -0.021(10) C34 0.088(11) 0.168(13) 0.142(13) -0.033(12) -0.017(11) -0.027(11) C35 0.094(10) 0.170(13) 0.139(12) -0.021(12) -0.008(10) -0.023(11) C36 0.107(10) 0.176(12) 0.153(11) -0.036(11) -0.005(9) -0.025(10) C37 0.118(11) 0.172(13) 0.155(12) -0.041(12) 0.000(11) -0.029(10) C38 0.130(13) 0.184(14) 0.171(14) -0.048(13) 0.014(12) -0.033(13) C39 0.149(12) 0.187(13) 0.181(13) -0.037(12) 0.016(11) -0.007(11) _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 Ag1 Se14 2.4684(12) 2_665 ? Ag1 Se14 2.4684(12) . ? Sn1 Se2 2.5249(9) . ? Sn1 Se4 2.5481(9) . ? Sn1 Se3 2.5491(9) . ? Sn1 Se1 2.7273(8) . ? Sn1 Se5 2.7351(8) . ? Sn2 Se6 2.5133(10) 2_656 ? Sn2 Se4 2.5599(9) . ? Sn2 Se7 2.5623(10) . ? Sn2 Se6 2.6675(10) . ? Sn2 Se5 2.8102(9) . ? Sn3 Se9 2.5458(10) . ? Sn3 Se7 2.5528(10) . ? Sn3 Se3 2.5639(9) . ? Sn3 Se5 2.7031(9) . ? Sn3 Se8 2.7052(10) . ? Sn4 Se8 2.4942(11) . ? Sn4 Se10 2.5343(9) . ? Sn4 Se11 2.5600(10) . ? Sn4 Se9 2.5932(12) . ? Sn5 Se1 2.4960(10) 1_465 ? Sn5 Se10 2.5490(10) . ? Sn5 Se13 2.5548(10) . ? Sn5 Se2 2.6428(9) 1_465 ? Sn5 Se12 2.9752(10) . ? Sn6 Se14 2.4607(11) . ? Sn6 Se12 2.4809(10) . ? Sn6 Se13 2.5443(10) . ? Sn6 Se11 2.5480(11) . ? Se1 Sn5 2.4960(10) 1_645 ? Se2 Sn5 2.6428(9) 1_645 ? Se6 Sn2 2.5133(10) 2_656 ? N1 C3 1.324(13) . ? N1 C1 1.393(14) . ? N1 C4 1.430(13) . ? N2 C3 1.323(13) . ? N2 C2 1.387(14) . ? N2 C6 1.468(13) . ? C1 C2 1.321(15) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C5 1.469(13) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.456(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.517(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.525(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N3 C13 1.331(13) . ? N3 C11 1.393(14) . ? N3 C14 1.440(13) . ? N4 C13 1.341(13) . ? N4 C12 1.383(14) . ? N4 C16 1.439(13) . ? C11 C12 1.311(15) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C15 1.463(13) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.468(17) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.497(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.534(17) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9598 . ? C19 H19C 0.9601 . ? N5 C23 1.334(14) . ? N5 C21 1.371(14) . ? N5 C24 1.472(15) . ? N6 C23 1.316(14) . ? N6 C22 1.381(14) . ? N6 C26 1.466(15) . ? C21 C22 1.328(15) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C25 1.470(14) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.471(17) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.527(17) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.527(17) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? N1B C3B 1.334(13) . ? N1B C1B 1.381(14) . ? N1B C4B 1.436(13) . ? N2B C3B 1.316(13) . ? N2B C2B 1.395(14) . ? N2B C6B 1.457(13) . ? C1B C2B 1.328(15) . ? C1B H1B 0.9300 . ? C2B H2B 0.9300 . ? C3B C5B 1.463(13) . ? C4B H4D 0.9600 . ? C4B H4E 0.9600 . ? C4B H4F 0.9600 . ? C5B H5D 0.9600 . ? C5B H5E 0.9600 . ? C5B H5F 0.9600 . ? C6B C7B 1.508(15) . ? C6B H6C 0.9700 . ? C6B H6D 0.9700 . ? C7B C8B 1.501(17) . ? C7B H7C 0.9700 . ? C7B H7D 0.9700 . ? C8B C9B 1.496(17) . ? C8B H8C 0.9700 . ? C8B H8D 0.9700 . ? C9B H9D 0.9600 . ? C9B H9E 0.9600 . ? C9B H9F 0.9600 . ? N3B C13B 1.323(13) . ? N3B C11B 1.396(14) . ? N3B C14B 1.427(13) . ? N4B C13B 1.330(13) . ? N4B C12B 1.387(14) . ? N4B C16B 1.441(13) . ? C11B C12B 1.312(15) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C15B 1.476(13) . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B C17B 1.489(15) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C18B 1.450(17) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B C19B 1.501(16) . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? N5B C23B 1.324(14) . ? N5B C21B 1.387(14) . ? N5B C24B 1.448(15) . ? N6B C23B 1.348(14) . ? N6B C22B 1.367(14) . ? N6B C26B 1.452(14) . ? C21B C22B 1.340(16) . ? C21B H21B 0.9300 . ? C22B H22B 0.9300 . ? C23B C25B 1.455(14) . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? C25B H25D 0.9600 . ? C25B H25E 0.9600 . ? C25B H25F 0.9600 . ? C26B C27B 1.491(17) . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C27B C28B 1.547(16) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29B 1.544(17) . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? N7 C33 1.332(15) . ? N7 C31 1.376(16) . ? N7 C34 1.39(3) . ? N8 C33 1.314(15) . ? N8 C32 1.386(15) . ? N8 C36 1.458(14) . ? C31 C32 1.344(16) . ? C31 H31A 0.9601 . ? C32 H32A 0.9600 . ? C33 C35 1.47(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9599 . ? C35 H35A 0.9601 . ? C35 H35B 0.9600 . ? C35 H35C 0.9601 . ? C36 C37 1.503(18) . ? C36 H36A 0.9601 . ? C36 H36B 0.9600 . ? C37 C38 1.446(16) . ? C37 H37A 0.9599 . ? C37 H37B 0.9601 . ? C38 C39 1.476(17) . ? C38 H38A 0.9599 . ? C38 H38B 0.9601 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? 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 Se14 Ag1 Se14 180.00(4) 2_665 . ? Se2 Sn1 Se4 121.85(4) . . ? Se2 Sn1 Se3 122.21(3) . . ? Se4 Sn1 Se3 115.94(3) . . ? Se2 Sn1 Se1 88.82(3) . . ? Se4 Sn1 Se1 89.78(3) . . ? Se3 Sn1 Se1 92.37(3) . . ? Se2 Sn1 Se5 92.33(3) . . ? Se4 Sn1 Se5 88.54(3) . . ? Se3 Sn1 Se5 88.09(3) . . ? Se1 Sn1 Se5 178.29(3) . . ? Se6 Sn2 Se4 122.02(4) 2_656 . ? Se6 Sn2 Se7 122.94(4) 2_656 . ? Se4 Sn2 Se7 114.54(3) . . ? Se6 Sn2 Se6 89.83(3) 2_656 . ? Se4 Sn2 Se6 93.27(3) . . ? Se7 Sn2 Se6 94.14(3) . . ? Se6 Sn2 Se5 89.21(3) 2_656 . ? Se4 Sn2 Se5 86.68(3) . . ? Se7 Sn2 Se5 86.93(3) . . ? Se6 Sn2 Se5 178.84(3) . . ? Se9 Sn3 Se7 122.59(4) . . ? Se9 Sn3 Se3 121.06(4) . . ? Se7 Sn3 Se3 116.32(3) . . ? Se9 Sn3 Se5 90.29(3) . . ? Se7 Sn3 Se5 89.45(3) . . ? Se3 Sn3 Se5 88.48(3) . . ? Se9 Sn3 Se8 89.51(3) . . ? Se7 Sn3 Se8 92.40(3) . . ? Se3 Sn3 Se8 89.85(3) . . ? Se5 Sn3 Se8 177.92(3) . . ? Se8 Sn4 Se10 121.58(4) . . ? Se8 Sn4 Se11 120.99(4) . . ? Se10 Sn4 Se11 113.36(3) . . ? Se8 Sn4 Se9 93.26(3) . . ? Se10 Sn4 Se9 100.06(4) . . ? Se11 Sn4 Se9 97.11(4) . . ? Se1 Sn5 Se10 123.02(4) 1_465 . ? Se1 Sn5 Se13 123.21(4) 1_465 . ? Se10 Sn5 Se13 112.88(4) . . ? Se1 Sn5 Se2 91.37(3) 1_465 1_465 ? Se10 Sn5 Se2 91.36(3) . 1_465 ? Se13 Sn5 Se2 96.79(3) . 1_465 ? Se1 Sn5 Se12 87.13(3) 1_465 . ? Se10 Sn5 Se12 87.05(3) . . ? Se13 Sn5 Se12 86.44(3) . . ? Se2 Sn5 Se12 176.75(3) 1_465 . ? Se14 Sn6 Se12 123.63(4) . . ? Se14 Sn6 Se13 112.52(4) . . ? Se12 Sn6 Se13 98.23(3) . . ? Se14 Sn6 Se11 110.86(4) . . ? Se12 Sn6 Se11 100.60(4) . . ? Se13 Sn6 Se11 109.62(4) . . ? Sn5 Se1 Sn1 88.81(3) 1_645 . ? Sn1 Se2 Sn5 90.11(3) . 1_645 ? Sn1 Se3 Sn3 92.82(3) . . ? Sn1 Se4 Sn2 95.19(3) . . ? Sn3 Se5 Sn1 85.84(3) . . ? Sn3 Se5 Sn2 85.53(3) . . ? Sn1 Se5 Sn2 85.70(3) . . ? Sn2 Se6 Sn2 90.17(3) 2_656 . ? Sn3 Se7 Sn2 94.11(3) . . ? Sn4 Se8 Sn3 87.49(3) . . ? Sn3 Se9 Sn4 88.88(3) . . ? Sn4 Se10 Sn5 103.08(3) . . ? Sn6 Se11 Sn4 91.73(3) . . ? Sn6 Se12 Sn5 81.57(3) . . ? Sn6 Se13 Sn5 89.31(3) . . ? Sn6 Se14 Ag1 89.02(4) . . ? C3 N1 C1 107.8(9) . . ? C3 N1 C4 128.3(13) . . ? C1 N1 C4 123.9(13) . . ? C3 N2 C2 108.3(9) . . ? C3 N2 C6 127.4(13) . . ? C2 N2 C6 124.3(13) . . ? C2 C1 N1 107.6(10) . . ? C2 C1 H1A 126.2 . . ? N1 C1 H1A 126.2 . . ? C1 C2 N2 107.3(10) . . ? C1 C2 H2A 126.3 . . ? N2 C2 H2A 126.3 . . ? N2 C3 N1 109.0(10) . . ? N2 C3 C5 125.5(12) . . ? N1 C3 C5 125.5(12) . . ? C7 C6 N2 113.6(13) . . ? C7 C6 H6A 108.8 . . ? N2 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? N2 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 C8 116.5(16) . . ? C6 C7 H7A 108.2 . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7B 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C7 C8 C9 105.5(15) . . ? C7 C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? C7 C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.8 . . ? C13 N3 C11 107.8(9) . . ? C13 N3 C14 129.2(14) . . ? C11 N3 C14 123.0(14) . . ? C13 N4 C12 107.1(9) . . ? C13 N4 C16 128.1(13) . . ? C12 N4 C16 124.7(13) . . ? C12 C11 N3 107.4(10) . . ? C12 C11 H11A 126.3 . . ? N3 C11 H11A 126.3 . . ? C11 C12 N4 108.8(10) . . ? C11 C12 H12A 125.6 . . ? N4 C12 H12A 125.6 . . ? N3 C13 N4 108.9(10) . . ? N3 C13 C15 125.2(13) . . ? N4 C13 C15 125.9(13) . . ? N4 C16 C17 118.3(15) . . ? N4 C16 H16A 107.7 . . ? C17 C16 H16A 107.7 . . ? N4 C16 H16B 107.7 . . ? C17 C16 H16B 107.7 . . ? H16A C16 H16B 107.1 . . ? C16 C17 C18 118.3(18) . . ? C16 C17 H17A 107.7 . . ? C18 C17 H17A 107.7 . . ? C16 C17 H17B 107.7 . . ? C18 C17 H17B 107.7 . . ? H17A C17 H17B 107.1 . . ? C17 C18 C19 114.8(16) . . ? C17 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? C17 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? C18 C19 H19A 105.7 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 112.3 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 N5 C21 107.5(10) . . ? C23 N5 C24 125.2(15) . . ? C21 N5 C24 127.3(15) . . ? C23 N6 C22 107.6(10) . . ? C23 N6 C26 128.4(13) . . ? C22 N6 C26 123.9(13) . . ? C22 C21 N5 107.7(11) . . ? C22 C21 H21A 126.2 . . ? N5 C21 H21A 126.2 . . ? C21 C22 N6 107.4(10) . . ? C21 C22 H22A 126.3 . . ? N6 C22 H22A 126.3 . . ? N6 C23 N5 109.4(10) . . ? N6 C23 C25 122.8(16) . . ? N5 C23 C25 127.8(16) . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C26 C27 114.5(16) . . ? N6 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? N6 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C26 C27 C28 115.3(17) . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27B 108.5 . . ? C28 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C29 C28 C27 107.0(16) . . ? C29 C28 H28A 110.3 . . ? C27 C28 H28A 110.3 . . ? C29 C28 H28B 110.3 . . ? C27 C28 H28B 110.3 . . ? H28A C28 H28B 108.6 . . ? C3B N1B C1B 107.6(9) . . ? C3B N1B C4B 127.0(13) . . ? C1B N1B C4B 125.3(13) . . ? C3B N2B C2B 107.6(9) . . ? C3B N2B C6B 129.3(13) . . ? C2B N2B C6B 123.0(13) . . ? C2B C1B N1B 107.7(10) . . ? C2B C1B H1B 126.2 . . ? N1B C1B H1B 126.2 . . ? C1B C2B N2B 107.4(10) . . ? C1B C2B H2B 126.3 . . ? N2B C2B H2B 126.3 . . ? N2B C3B N1B 109.6(10) . . ? N2B C3B C5B 125.9(12) . . ? N1B C3B C5B 124.4(12) . . ? N1B C4B H4D 109.5 . . ? N1B C4B H4E 109.5 . . ? H4D C4B H4E 109.5 . . ? N1B C4B H4F 109.5 . . ? H4D C4B H4F 109.5 . . ? H4E C4B H4F 109.5 . . ? C3B C5B H5D 109.5 . . ? C3B C5B H5E 109.5 . . ? H5D C5B H5E 109.5 . . ? C3B C5B H5F 109.5 . . ? H5D C5B H5F 109.5 . . ? H5E C5B H5F 109.5 . . ? N2B C6B C7B 113.1(13) . . ? N2B C6B H6C 109.0 . . ? C7B C6B H6C 109.0 . . ? N2B C6B H6D 109.0 . . ? C7B C6B H6D 109.0 . . ? H6C C6B H6D 107.8 . . ? C8B C7B C6B 110.2(14) . . ? C8B C7B H7C 109.6 . . ? C6B C7B H7C 109.6 . . ? C8B C7B H7D 109.6 . . ? C6B C7B H7D 109.6 . . ? H7C C7B H7D 108.1 . . ? C9B C8B C7B 112.0(16) . . ? C9B C8B H8C 109.2 . . ? C7B C8B H8C 109.2 . . ? C9B C8B H8D 109.2 . . ? C7B C8B H8D 109.2 . . ? H8C C8B H8D 107.9 . . ? C8B C9B H9D 109.5 . . ? C8B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C8B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C13B N3B C11B 107.1(10) . . ? C13B N3B C14B 128.5(13) . . ? C11B N3B C14B 124.3(13) . . ? C13B N4B C12B 107.6(9) . . ? C13B N4B C16B 127.7(13) . . ? C12B N4B C16B 124.7(14) . . ? C12B C11B N3B 108.1(10) . . ? C12B C11B H11B 126.0 . . ? N3B C11B H11B 126.0 . . ? C11B C12B N4B 107.7(10) . . ? C11B C12B H12B 126.2 . . ? N4B C12B H12B 126.2 . . ? N3B C13B N4B 109.5(10) . . ? N3B C13B C15B 126.7(13) . . ? N4B C13B C15B 123.8(13) . . ? N3B C14B H14D 109.5 . . ? N3B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? N3B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13B C15B H15D 109.5 . . ? C13B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C13B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N4B C16B C17B 116.6(12) . . ? N4B C16B H16C 108.1 . . ? C17B C16B H16C 108.1 . . ? N4B C16B H16D 108.1 . . ? C17B C16B H16D 108.1 . . ? H16C C16B H16D 107.3 . . ? C18B C17B C16B 116.2(15) . . ? C18B C17B H17C 108.2 . . ? C16B C17B H17C 108.2 . . ? C18B C17B H17D 108.2 . . ? C16B C17B H17D 108.2 . . ? H17C C17B H17D 107.4 . . ? C17B C18B C19B 117.1(18) . . ? C17B C18B H18C 108.0 . . ? C19B C18B H18C 108.0 . . ? C17B C18B H18D 108.0 . . ? C19B C18B H18D 108.0 . . ? H18C C18B H18D 107.3 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C23B N5B C21B 108.2(10) . . ? C23B N5B C24B 128.9(15) . . ? C21B N5B C24B 122.9(15) . . ? C23B N6B C22B 107.5(10) . . ? C23B N6B C26B 124.4(14) . . ? C22B N6B C26B 128.0(14) . . ? C22B C21B N5B 106.9(10) . . ? C22B C21B H21B 126.5 . . ? N5B C21B H21B 126.5 . . ? C21B C22B N6B 108.4(10) . . ? C21B C22B H22B 125.8 . . ? N6B C22B H22B 125.8 . . ? N5B C23B N6B 109.0(10) . . ? N5B C23B C25B 125.2(16) . . ? N6B C23B C25B 125.8(16) . . ? N5B C24B H24D 109.5 . . ? N5B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? N5B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C23B C25B H25D 109.5 . . ? C23B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C23B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? N6B C26B C27B 117.7(16) . . ? N6B C26B H26C 107.9 . . ? C27B C26B H26C 107.9 . . ? N6B C26B H26D 107.9 . . ? C27B C26B H26D 107.9 . . ? H26C C26B H26D 107.2 . . ? C26B C27B C28B 110.7(14) . . ? C26B C27B H27C 109.5 . . ? C28B C27B H27C 109.5 . . ? C26B C27B H27D 109.5 . . ? C28B C27B H27D 109.5 . . ? H27C C27B H27D 108.1 . . ? C29B C28B C27B 110.2(14) . . ? C29B C28B H28C 109.6 . . ? C27B C28B H28C 109.6 . . ? C29B C28B H28D 109.6 . . ? C27B C28B H28D 109.6 . . ? H28C C28B H28D 108.1 . . ? C28B C29B H29D 109.5 . . ? C28B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C28B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C33 N7 C31 107.1(11) . . ? C33 N7 C34 142(4) . . ? C31 N7 C34 110(3) . . ? C33 N8 C32 107.9(10) . . ? C33 N8 C36 130.1(16) . . ? C32 N8 C36 122.0(15) . . ? C32 C31 N7 108.0(11) . . ? C32 C31 H31A 125.0 . . ? N7 C31 H31A 126.9 . . ? C31 C32 N8 106.8(11) . . ? C31 C32 H32A 127.4 . . ? N8 C32 H32A 125.8 . . ? N8 C33 N7 110.2(11) . . ? N8 C33 C35 132(2) . . ? N7 C33 C35 117(2) . . ? N7 C34 H34A 107.0 . . ? N7 C34 H34B 110.1 . . ? H34A C34 H34B 109.5 . . ? N7 C34 H34C 111.3 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.3 . . ? C33 C35 H35B 108.3 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 110.9 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N8 C36 C37 111.8(16) . . ? N8 C36 H36A 109.3 . . ? C37 C36 H36A 109.7 . . ? N8 C36 H36B 108.6 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 116.9(18) . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37A 108.7 . . ? C38 C37 H37B 105.1 . . ? C36 C37 H37B 108.7 . . ? H37A C37 H37B 107.5 . . ? C37 C38 C39 121.3(18) . . ? C37 C38 H38A 104.0 . . ? C39 C38 H38A 105.1 . . ? C37 C38 H38B 109.8 . . ? C39 C38 H38B 108.7 . . ? H38A C38 H38B 106.9 . . ? C38 C39 H39A 110.3 . . ? C38 C39 H39B 110.9 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 107.1 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.918 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.158 #===END