# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Dominic S Wright' _publ_contact_author_email dsw1000@hermes.cam.ac.uk _publ_section_title ; Oxidative Dehydrocoupling of N-H Bonds Using a Redox-Active Main Group Superbase ; loop_ _publ_author_name R.J.Less V.Naseri M.McPartlin D.S.Wright data_dw1008 _database_code_depnum_ccdc_archive 'CCDC 796653' #TrackingRef '- DW1008.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H50 Li2 N9), C30 H22 N10 Sn7' _chemical_formula_sum 'C78 H122 Li4 N28 Sn7' _chemical_formula_weight 2310.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8673(1) _cell_length_b 18.7128(2) _cell_length_c 20.1729(3) _cell_angle_alpha 97.486(1) _cell_angle_beta 104.430(1) _cell_angle_gamma 103.962(1) _cell_volume 4817.83(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 52773 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 1.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Parts of both C24H50Li2N9 units are disordered and, for the refinment, the disordered C and N atoms were assigned common isotropic displacement parameters (a total of six LS isotropic parameters). Bond length constraints were also applied to these disordered parts. The C30H22N10Sn7 unit may be ever so slightly disordered over two sites: the residual peaks next to the Sn atoms indicate this but no attempt was made to model this disorder in the refinement process. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 56150 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.93 _reflns_number_total 22770 _reflns_number_gt 15857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22770 _refine_ls_number_parameters 997 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.62778(3) 0.86630(2) 0.774920(18) 0.03102(10) Uani 1 1 d . . . Sn2 Sn 0.74564(3) 0.74052(2) 0.70870(2) 0.04091(11) Uani 1 1 d . . . Sn3 Sn 0.75693(3) 0.76669(2) 0.870816(19) 0.03620(11) Uani 1 1 d . . . Sn4 Sn 0.88448(3) 0.91958(2) 0.82036(2) 0.03783(11) Uani 1 1 d . . . Sn5 Sn 0.41201(3) 0.88236(3) 0.64721(2) 0.05399(14) Uani 1 1 d . . . Sn6 Sn 0.55341(3) 1.02325(2) 0.77177(2) 0.04381(12) Uani 1 1 d . . . Sn7 Sn 0.42384(3) 0.87660(2) 0.82807(2) 0.03964(11) Uani 1 1 d . . . N1 N 0.3997(3) 0.9420(3) 0.7464(2) 0.0399(11) Uani 1 1 d . . . N2 N 0.6387(3) 0.7503(3) 0.7707(2) 0.0349(10) Uani 1 1 d . . . N3 N 0.7581(3) 0.8877(3) 0.8697(2) 0.0343(10) Uani 1 1 d . . . N4 N 0.7523(3) 0.8849(3) 0.7286(2) 0.0377(10) Uani 1 1 d . . . N5 N 0.5862(3) 0.9448(3) 0.8461(2) 0.0364(10) Uani 1 1 d . . . N6 N 0.5757(4) 0.9345(3) 0.6988(2) 0.0382(10) Uani 1 1 d . . . N7 N 0.4687(3) 0.8068(3) 0.7563(2) 0.0369(10) Uani 1 1 d . . . N8 N 0.8658(3) 0.8004(3) 0.8096(2) 0.0356(10) Uani 1 1 d . . . N10 N 0.3798(5) 0.9939(4) 0.6318(3) 0.0690(18) Uani 1 1 d . . . H10A H 0.4075 1.0241 0.6072 0.083 Uiso 1 1 calc R . . N80 N 0.7996(4) 0.6574(3) 0.7724(3) 0.0596(16) Uani 1 1 d . . . H80A H 0.7591 0.6160 0.7780 0.071 Uiso 1 1 calc R . . C101 C 0.3178(4) 0.9756(4) 0.7289(3) 0.0439(14) Uani 1 1 d . . . C102 C 0.3114(5) 1.0062(4) 0.6662(3) 0.0528(16) Uani 1 1 d . . . C103 C 0.2324(6) 1.0403(5) 0.6458(4) 0.070(2) Uani 1 1 d . . . H103 H 0.2254 1.0601 0.6044 0.084 Uiso 1 1 calc R . . C104 C 0.1642(6) 1.0456(5) 0.6845(4) 0.074(2) Uani 1 1 d . . . H104 H 0.1126 1.0704 0.6700 0.089 Uiso 1 1 calc R . . C105 C 0.1696(6) 1.0162(6) 0.7431(5) 0.081(3) Uani 1 1 d . . . H105 H 0.1203 1.0184 0.7681 0.097 Uiso 1 1 calc R . . C106 C 0.2471(5) 0.9829(5) 0.7662(4) 0.063(2) Uani 1 1 d . . . H106 H 0.2524 0.9646 0.8083 0.076 Uiso 1 1 calc R . . C201 C 0.5396(4) 0.6992(3) 0.7588(3) 0.0346(11) Uani 1 1 d . . . C202 C 0.4515(4) 0.7288(3) 0.7517(3) 0.0384(12) Uani 1 1 d . . . C203 C 0.3559(4) 0.6794(4) 0.7430(4) 0.0516(16) Uani 1 1 d . . . H203 H 0.2975 0.6984 0.7393 0.062 Uiso 1 1 calc R . . C204 C 0.3417(5) 0.6032(4) 0.7394(4) 0.0610(19) Uani 1 1 d . . . H204 H 0.2745 0.5706 0.7327 0.073 Uiso 1 1 calc R . . C205 C 0.4263(5) 0.5746(4) 0.7455(4) 0.0581(17) Uani 1 1 d . . . H205 H 0.4176 0.5224 0.7436 0.070 Uiso 1 1 calc R . . C206 C 0.5233(5) 0.6228(3) 0.7543(3) 0.0446(14) Uani 1 1 d . . . H206 H 0.5806 0.6028 0.7575 0.054 Uiso 1 1 calc R . . C301 C 0.7474(4) 0.9353(3) 0.9253(3) 0.0324(11) Uani 1 1 d . . . C302 C 0.6590(4) 0.9646(3) 0.9139(3) 0.0337(11) Uani 1 1 d . . . C303 C 0.6484(4) 1.0098(3) 0.9708(3) 0.0390(12) Uani 1 1 d . . . H303 H 0.5896 1.0287 0.9644 0.047 Uiso 1 1 calc R . . C304 C 0.7199(4) 1.0281(3) 1.0357(3) 0.0403(13) Uani 1 1 d . . . H304 H 0.7105 1.0595 1.0732 0.048 Uiso 1 1 calc R . . C305 C 0.8035(5) 1.0015(3) 1.0463(3) 0.0422(13) Uani 1 1 d . . . H305 H 0.8527 1.0139 1.0913 0.051 Uiso 1 1 calc R . . C306 C 0.8178(4) 0.9560(3) 0.9917(3) 0.0403(13) Uani 1 1 d . . . H306 H 0.8777 0.9384 1.0000 0.048 Uiso 1 1 calc R . . C401 C 0.7379(4) 0.9255(3) 0.6748(3) 0.0364(12) Uani 1 1 d . . . C402 C 0.6470(4) 0.9511(3) 0.6596(3) 0.0377(12) Uani 1 1 d . . . C403 C 0.6318(5) 0.9915(4) 0.6063(3) 0.0485(15) Uani 1 1 d . . . H403 H 0.5711 1.0079 0.5951 0.058 Uiso 1 1 calc R . . C404 C 0.7046(6) 1.0083(4) 0.5690(3) 0.0533(16) Uani 1 1 d . . . H404 H 0.6936 1.0365 0.5333 0.064 Uiso 1 1 calc R . . C405 C 0.7915(5) 0.9839(4) 0.5843(4) 0.0556(17) Uani 1 1 d . . . H405 H 0.8404 0.9947 0.5587 0.067 Uiso 1 1 calc R . . C406 C 0.8088(5) 0.9429(4) 0.6376(3) 0.0495(15) Uani 1 1 d . . . H406 H 0.8700 0.9270 0.6482 0.059 Uiso 1 1 calc R . . C801 C 0.9440(4) 0.7632(3) 0.8210(3) 0.0335(11) Uani 1 1 d . . . C802 C 0.9056(4) 0.6829(3) 0.8003(3) 0.0399(13) Uani 1 1 d . . . C803 C 0.9765(5) 0.6414(4) 0.8082(3) 0.0475(14) Uani 1 1 d . . . H803 H 0.9524 0.5882 0.7950 0.057 Uiso 1 1 calc R . . C804 C 1.0813(5) 0.6763(4) 0.8351(4) 0.0546(17) Uani 1 1 d . . . H804 H 1.1285 0.6467 0.8405 0.066 Uiso 1 1 calc R . . C805 C 1.1190(5) 0.7533(4) 0.8542(4) 0.0524(16) Uani 1 1 d . . . H805 H 1.1916 0.7770 0.8720 0.063 Uiso 1 1 calc R . . C806 C 1.0486(4) 0.7960(3) 0.8469(3) 0.0437(14) Uani 1 1 d . . . H806 H 1.0742 0.8493 0.8604 0.052 Uiso 1 1 calc R . . Li1 Li 0.6272(8) 0.3229(6) 0.5802(5) 0.048(2) Uani 1 1 d . . . Li2 Li 0.9923(12) 0.2964(11) 0.4831(8) 0.092(5) Uani 1 1 d . . . N01 N 0.7763(4) 0.3370(4) 0.5852(3) 0.0651(17) Uani 1 1 d . A . N02 N 0.9097(5) 0.3238(6) 0.5406(4) 0.101(3) Uani 1 1 d . A . N03 N 0.8052(7) 0.3092(7) 0.5308(5) 0.127(4) Uani 1 1 d . . . C01 C 0.8696(5) 0.3724(4) 0.6342(4) 0.0561(16) Uani 1 1 d . . . C02 C 0.9517(5) 0.3652(5) 0.6080(4) 0.071(2) Uani 1 1 d . A . C03 C 1.0544(6) 0.3952(6) 0.6467(5) 0.092(3) Uani 1 1 d . . . H03 H 1.1088 0.3911 0.6270 0.110 Uiso 1 1 calc R A . C04 C 1.0754(6) 0.4312(5) 0.7147(5) 0.077(2) Uani 1 1 d . A . H04 H 1.1453 0.4498 0.7436 0.092 Uiso 1 1 calc R . . C05 C 0.9956(7) 0.4406(5) 0.7416(5) 0.081(3) Uani 1 1 d . . . H05 H 1.0125 0.4684 0.7879 0.098 Uiso 1 1 calc R A . C06 C 0.8914(7) 0.4108(5) 0.7032(4) 0.079(2) Uani 1 1 d . A . H06 H 0.8374 0.4162 0.7229 0.094 Uiso 1 1 calc R . . N11 N 0.5308(5) 0.2161(4) 0.5845(3) 0.0647(16) Uani 1 1 d . . . N12 N 0.5825(5) 0.4150(4) 0.6231(3) 0.0677(17) Uani 1 1 d . . . N13 N 0.5167(5) 0.3145(4) 0.4860(3) 0.0663(17) Uani 1 1 d . . . C11 C 0.5118(9) 0.1998(7) 0.6493(5) 0.105(3) Uani 1 1 d . . . H11A H 0.4752 0.1463 0.6424 0.158 Uiso 1 1 calc R . . H11B H 0.4691 0.2302 0.6635 0.158 Uiso 1 1 calc R . . H11C H 0.5781 0.2118 0.6859 0.158 Uiso 1 1 calc R . . C12 C 0.5807(7) 0.1620(5) 0.5587(4) 0.081(3) Uani 1 1 d . . . H12A H 0.5281 0.1140 0.5360 0.121 Uiso 1 1 calc R . . H12B H 0.6326 0.1545 0.5980 0.121 Uiso 1 1 calc R . . H12C H 0.6147 0.1815 0.5250 0.121 Uiso 1 1 calc R . . C13 C 0.4326(6) 0.2061(5) 0.5321(5) 0.077(2) Uani 1 1 d . . . H13A H 0.3902 0.2330 0.5527 0.093 Uiso 1 1 calc R . . H13B H 0.3940 0.1520 0.5184 0.093 Uiso 1 1 calc R . . C14 C 0.4477(6) 0.2348(4) 0.4685(4) 0.072(2) Uani 1 1 d . . . H14A H 0.3792 0.2324 0.4369 0.086 Uiso 1 1 calc R . . H14B H 0.4788 0.2019 0.4433 0.086 Uiso 1 1 calc R . . C15 C 0.4619(7) 0.3677(5) 0.5047(4) 0.077(3) Uani 1 1 d . . . H15A H 0.4049 0.3415 0.5219 0.092 Uiso 1 1 calc R . . H15B H 0.4301 0.3846 0.4621 0.092 Uiso 1 1 calc R . . C16 C 0.5277(9) 0.4337(6) 0.5579(5) 0.110(4) Uani 1 1 d . . . H16A H 0.4843 0.4658 0.5689 0.132 Uiso 1 1 calc R . . H16B H 0.5798 0.4631 0.5386 0.132 Uiso 1 1 calc R . . C17 C 0.5217(14) 0.4007(9) 0.6711(7) 0.168(7) Uani 1 1 d . . . H17A H 0.4901 0.4416 0.6781 0.252 Uiso 1 1 calc R . . H17B H 0.5667 0.3978 0.7160 0.252 Uiso 1 1 calc R . . H17C H 0.4669 0.3530 0.6517 0.252 Uiso 1 1 calc R . . C18 C 0.6683(10) 0.4827(7) 0.6570(8) 0.141(5) Uani 1 1 d . . . H18A H 0.6406 0.5251 0.6670 0.211 Uiso 1 1 calc R . . H18B H 0.7117 0.4938 0.6259 0.211 Uiso 1 1 calc R . . H18C H 0.7102 0.4747 0.7007 0.211 Uiso 1 1 calc R . . C19 C 0.5567(8) 0.3330(7) 0.4285(4) 0.096(3) Uani 1 1 d . . . H19A H 0.5013 0.3398 0.3911 0.144 Uiso 1 1 calc R . . H19B H 0.5819 0.2920 0.4105 0.144 Uiso 1 1 calc R . . H19C H 0.6141 0.3795 0.4450 0.144 Uiso 1 1 calc R . . N21 N 1.0481(8) 0.1935(7) 0.5040(6) 0.0741(12) Uiso 0.60 1 d PD A 1 N22 N 1.1066(9) 0.3803(6) 0.4584(6) 0.0741(12) Uiso 0.60 1 d PD A 1 N23 N 0.9511(9) 0.2454(6) 0.3819(6) 0.0637(13) Uiso 0.60 1 d PD A 1 C21 C 1.0113(15) 0.1625(11) 0.5585(9) 0.1090(18) Uiso 0.60 1 d PD A 1 H21A H 1.0707 0.1665 0.5985 0.164 Uiso 0.60 1 calc PR A 1 H21B H 0.9718 0.1095 0.5404 0.164 Uiso 0.60 1 calc PR A 1 H21C H 0.9664 0.1905 0.5733 0.164 Uiso 0.60 1 calc PR A 1 C22 C 1.1620(12) 0.2112(9) 0.5189(8) 0.1090(18) Uiso 0.60 1 d PD A 1 H22A H 1.1855 0.1704 0.5374 0.164 Uiso 0.60 1 calc PR A 1 H22B H 1.1952 0.2583 0.5535 0.164 Uiso 0.60 1 calc PR A 1 H22C H 1.1809 0.2165 0.4757 0.164 Uiso 0.60 1 calc PR A 1 C23 C 0.9939(12) 0.1421(8) 0.4357(7) 0.0872(13) Uiso 0.60 1 d PD A 1 H23A H 0.9199 0.1207 0.4326 0.105 Uiso 0.60 1 calc PR A 1 H23B H 1.0253 0.1002 0.4313 0.105 Uiso 0.60 1 calc PR A 1 C24 C 1.0015(12) 0.1843(9) 0.3752(7) 0.0872(13) Uiso 0.60 1 d PD A 1 H24A H 1.0753 0.2057 0.3777 0.105 Uiso 0.60 1 calc PR A 1 H24B H 0.9661 0.1491 0.3297 0.105 Uiso 0.60 1 calc PR A 1 C25 C 0.9898(11) 0.3007(9) 0.3445(8) 0.0872(13) Uiso 0.60 1 d PD A 1 H25A H 0.9371 0.3274 0.3293 0.105 Uiso 0.60 1 calc PR A 1 H25B H 1.0011 0.2752 0.3022 0.105 Uiso 0.60 1 calc PR A 1 C26 C 1.0867(11) 0.3553(9) 0.3871(7) 0.0872(13) Uiso 0.60 1 d PD A 1 H26A H 1.1435 0.3339 0.3811 0.105 Uiso 0.60 1 calc PR A 1 H26B H 1.0940 0.4004 0.3659 0.105 Uiso 0.60 1 calc PR A 1 C27 C 1.2102(12) 0.3844(9) 0.4910(9) 0.1090(18) Uiso 0.60 1 d PD A 1 H27A H 1.2557 0.4146 0.4685 0.164 Uiso 0.60 1 calc PR A 1 H27B H 1.2185 0.3336 0.4868 0.164 Uiso 0.60 1 calc PR A 1 H27C H 1.2289 0.4079 0.5406 0.164 Uiso 0.60 1 calc PR A 1 C28 C 1.0893(15) 0.4573(9) 0.4683(10) 0.1090(18) Uiso 0.60 1 d PD A 1 H28A H 1.1479 0.4944 0.4620 0.164 Uiso 0.60 1 calc PR A 1 H28B H 1.0838 0.4710 0.5155 0.164 Uiso 0.60 1 calc PR A 1 H28C H 1.0249 0.4564 0.4338 0.164 Uiso 0.60 1 calc PR A 1 C29 C 0.8421(10) 0.2080(10) 0.3406(9) 0.092(3) Uiso 0.60 1 d PD A 1 H29A H 0.8369 0.2002 0.2907 0.137 Uiso 0.60 1 calc PR A 1 H29B H 0.7983 0.2395 0.3505 0.137 Uiso 0.60 1 calc PR A 1 H29C H 0.8187 0.1592 0.3532 0.137 Uiso 0.60 1 calc PR A 1 N21' N 1.0159(12) 0.2046(9) 0.5124(8) 0.0741(12) Uiso 0.40 1 d PD A 2 N22' N 1.0602(13) 0.3822(8) 0.4431(8) 0.0741(12) Uiso 0.40 1 d PD A 2 N23' N 0.9471(12) 0.2322(8) 0.3740(9) 0.0637(13) Uiso 0.40 1 d PD A 2 C21' C 0.9237(18) 0.1582(15) 0.5250(11) 0.1090(18) Uiso 0.40 1 d PD A 2 H21D H 0.9307 0.1075 0.5268 0.164 Uiso 0.40 1 calc PR A 2 H21E H 0.8620 0.1552 0.4871 0.164 Uiso 0.40 1 calc PR A 2 H21F H 0.9167 0.1806 0.5696 0.164 Uiso 0.40 1 calc PR A 2 C22' C 1.1175(18) 0.2095(16) 0.5683(12) 0.1090(18) Uiso 0.40 1 d PD A 2 H22D H 1.1311 0.1604 0.5639 0.164 Uiso 0.40 1 calc PR A 2 H22E H 1.1106 0.2242 0.6150 0.164 Uiso 0.40 1 calc PR A 2 H22F H 1.1753 0.2470 0.5616 0.164 Uiso 0.40 1 calc PR A 2 C23' C 1.0294(15) 0.1566(12) 0.4510(9) 0.0872(13) Uiso 0.40 1 d PD A 2 H23C H 1.0207 0.1043 0.4579 0.105 Uiso 0.40 1 calc PR A 2 H23D H 1.0998 0.1765 0.4463 0.105 Uiso 0.40 1 calc PR A 2 C24' C 0.9448(16) 0.1587(11) 0.3835(9) 0.0872(13) Uiso 0.40 1 d PD A 2 H24C H 0.9556 0.1307 0.3421 0.105 Uiso 0.40 1 calc PR A 2 H24D H 0.8752 0.1329 0.3866 0.105 Uiso 0.40 1 calc PR A 2 C25' C 1.0368(14) 0.2737(10) 0.3559(12) 0.0872(13) Uiso 0.40 1 d PD A 2 H25C H 1.0245 0.2593 0.3048 0.105 Uiso 0.40 1 calc PR A 2 H25D H 1.0983 0.2588 0.3794 0.105 Uiso 0.40 1 calc PR A 2 C26' C 1.0598(15) 0.3556(10) 0.3752(9) 0.0872(13) Uiso 0.40 1 d PD A 2 H26C H 1.1286 0.3791 0.3696 0.105 Uiso 0.40 1 calc PR A 2 H26D H 1.0075 0.3719 0.3422 0.105 Uiso 0.40 1 calc PR A 2 C27' C 1.1544(18) 0.4326(14) 0.4891(12) 0.1090(18) Uiso 0.40 1 d PD A 2 H27D H 1.1933 0.4611 0.4620 0.164 Uiso 0.40 1 calc PR A 2 H27E H 1.1963 0.4038 0.5143 0.164 Uiso 0.40 1 calc PR A 2 H27F H 1.1384 0.4673 0.5227 0.164 Uiso 0.40 1 calc PR A 2 C28' C 0.9754(16) 0.4206(12) 0.4351(12) 0.1090(18) Uiso 0.40 1 d PD A 2 H28D H 0.9942 0.4650 0.4149 0.164 Uiso 0.40 1 calc PR A 2 H28E H 0.9666 0.4361 0.4810 0.164 Uiso 0.40 1 calc PR A 2 H28F H 0.9102 0.3857 0.4042 0.164 Uiso 0.40 1 calc PR A 2 C29' C 0.8573(12) 0.2473(10) 0.3295(12) 0.092(3) Uiso 0.40 1 d PD A 2 H29D H 0.8069 0.1997 0.3028 0.137 Uiso 0.40 1 calc PR A 2 H29E H 0.8795 0.2780 0.2973 0.137 Uiso 0.40 1 calc PR A 2 H29F H 0.8252 0.2744 0.3586 0.137 Uiso 0.40 1 calc PR A 2 Li3 Li 0.8835(7) 0.2798(6) 0.8637(5) 0.041(2) Uani 1 1 d . . . Li4 Li 0.4920(8) 0.2936(6) 0.9134(6) 0.052(3) Uani 1 1 d . . . N31 N 0.8947(4) 0.2066(3) 0.7758(3) 0.0501(13) Uani 1 1 d . . . N32 N 1.0122(4) 0.3561(3) 0.9462(3) 0.0457(12) Uani 1 1 d . . . N33 N 0.9130(4) 0.1978(3) 0.9219(3) 0.0528(14) Uani 1 1 d . . . C31 C 0.8068(6) 0.1946(5) 0.7133(4) 0.075(2) Uani 1 1 d . . . H31A H 0.8094 0.1554 0.6770 0.113 Uiso 1 1 calc R . . H31B H 0.8110 0.2415 0.6960 0.113 Uiso 1 1 calc R . . H31C H 0.7415 0.1789 0.7250 0.113 Uiso 1 1 calc R . . C32 C 0.9911(6) 0.2362(5) 0.7582(5) 0.075(2) Uani 1 1 d . . . H32A H 1.0005 0.1973 0.7249 0.112 Uiso 1 1 calc R . . H32B H 1.0500 0.2509 0.8007 0.112 Uiso 1 1 calc R . . H32C H 0.9871 0.2802 0.7372 0.112 Uiso 1 1 calc R . . C33 C 0.8910(7) 0.1384(4) 0.8026(4) 0.070(2) Uani 1 1 d . . . H33A H 0.9156 0.1046 0.7731 0.084 Uiso 1 1 calc R . . H33B H 0.8179 0.1128 0.7987 0.084 Uiso 1 1 calc R . . C34 C 0.9545(6) 0.1509(4) 0.8766(4) 0.069(2) Uani 1 1 d . . . H34A H 1.0279 0.1769 0.8816 0.083 Uiso 1 1 calc R . . H34B H 0.9514 0.1020 0.8911 0.083 Uiso 1 1 calc R . . C35 C 0.9963(5) 0.2367(4) 0.9860(4) 0.0581(18) Uani 1 1 d . . . H35A H 1.0364 0.2018 1.0019 0.070 Uiso 1 1 calc R . . H35B H 0.9654 0.2514 1.0230 0.070 Uiso 1 1 calc R . . C36 C 1.0682(5) 0.3051(4) 0.9760(4) 0.0577(18) Uani 1 1 d . . . H36A H 1.1188 0.3320 1.0216 0.069 Uiso 1 1 calc R . . H36B H 1.1074 0.2898 0.9446 0.069 Uiso 1 1 calc R . . C37 C 0.9609(6) 0.3863(4) 0.9941(4) 0.0636(19) Uani 1 1 d . . . H37A H 1.0119 0.4093 1.0398 0.095 Uiso 1 1 calc R . . H37B H 0.9056 0.3455 0.9993 0.095 Uiso 1 1 calc R . . H37C H 0.9309 0.4244 0.9752 0.095 Uiso 1 1 calc R . . C38 C 1.0877(5) 0.4193(4) 0.9319(4) 0.065(2) Uani 1 1 d . . . H38A H 1.1467 0.4415 0.9739 0.098 Uiso 1 1 calc R . . H38B H 1.0536 0.4577 0.9186 0.098 Uiso 1 1 calc R . . H38C H 1.1126 0.4004 0.8936 0.098 Uiso 1 1 calc R . . C39 C 0.8248(6) 0.1516(5) 0.9390(5) 0.084(3) Uani 1 1 d . . . H39A H 0.8486 0.1180 0.9686 0.126 Uiso 1 1 calc R . . H39B H 0.7725 0.1217 0.8959 0.126 Uiso 1 1 calc R . . H39C H 0.7942 0.1842 0.9641 0.126 Uiso 1 1 calc R . . N41 N 0.3470(13) 0.2898(9) 0.8565(7) 0.0741(12) Uiso 0.50 1 d PD B 3 N42 N 0.5563(11) 0.3482(8) 1.0248(9) 0.0741(12) Uiso 0.50 1 d PD B 3 N43 N 0.4308(12) 0.1976(8) 0.9462(7) 0.0637(13) Uiso 0.50 1 d PD B 3 C41 C 0.3423(18) 0.2549(13) 0.7872(10) 0.1090(18) Uiso 0.50 1 d PD B 3 H41A H 0.2782 0.2134 0.7677 0.164 Uiso 0.50 1 calc PR B 3 H41B H 0.4024 0.2353 0.7896 0.164 Uiso 0.50 1 calc PR B 3 H41C H 0.3432 0.2921 0.7572 0.164 Uiso 0.50 1 calc PR B 3 C42 C 0.305(2) 0.3557(12) 0.8530(12) 0.1090(18) Uiso 0.50 1 d PD B 3 H42A H 0.2318 0.3388 0.8256 0.164 Uiso 0.50 1 calc PR B 3 H42B H 0.3444 0.3910 0.8307 0.164 Uiso 0.50 1 calc PR B 3 H42C H 0.3119 0.3808 0.9004 0.164 Uiso 0.50 1 calc PR B 3 C43 C 0.2827(13) 0.2348(10) 0.8868(10) 0.0872(13) Uiso 0.50 1 d PD B 3 H43A H 0.2813 0.2604 0.9326 0.105 Uiso 0.50 1 calc PR B 3 H43B H 0.2105 0.2173 0.8556 0.105 Uiso 0.50 1 calc PR B 3 C44 C 0.3217(13) 0.1688(10) 0.8966(10) 0.0872(13) Uiso 0.50 1 d PD B 3 H44A H 0.3223 0.1418 0.8513 0.105 Uiso 0.50 1 calc PR B 3 H44B H 0.2765 0.1338 0.9165 0.105 Uiso 0.50 1 calc PR B 3 C45 C 0.4405(15) 0.2231(10) 1.0181(8) 0.0872(13) Uiso 0.50 1 d PD B 3 H45A H 0.4343 0.1797 1.0417 0.105 Uiso 0.50 1 calc PR B 3 H45B H 0.3832 0.2450 1.0214 0.105 Uiso 0.50 1 calc PR B 3 C46 C 0.5405(14) 0.2797(9) 1.0538(9) 0.0872(13) Uiso 0.50 1 d PD B 3 H46A H 0.5973 0.2570 1.0511 0.105 Uiso 0.50 1 calc PR B 3 H46B H 0.5453 0.2938 1.1038 0.105 Uiso 0.50 1 calc PR B 3 C47 C 0.4923(17) 0.3973(13) 1.0456(13) 0.1090(18) Uiso 0.50 1 d PD B 3 H47A H 0.5182 0.4171 1.0962 0.164 Uiso 0.50 1 calc PR B 3 H47B H 0.4195 0.3675 1.0333 0.164 Uiso 0.50 1 calc PR B 3 H47C H 0.4977 0.4392 1.0209 0.164 Uiso 0.50 1 calc PR B 3 C48 C 0.6607(14) 0.3920(13) 1.0459(12) 0.1090(18) Uiso 0.50 1 d PD B 3 H48A H 0.6885 0.4000 1.0968 0.164 Uiso 0.50 1 calc PR B 3 H48B H 0.6652 0.4406 1.0320 0.164 Uiso 0.50 1 calc PR B 3 H48C H 0.7013 0.3658 1.0236 0.164 Uiso 0.50 1 calc PR B 3 C49 C 0.4836(15) 0.1372(11) 0.9399(11) 0.092(3) Uiso 0.50 1 d PD B 3 H49A H 0.4421 0.0910 0.9487 0.137 Uiso 0.50 1 calc PR B 3 H49B H 0.5526 0.1534 0.9741 0.137 Uiso 0.50 1 calc PR B 3 H49C H 0.4908 0.1276 0.8926 0.137 Uiso 0.50 1 calc PR B 3 N41' N 0.3420(14) 0.2894(9) 0.8447(7) 0.0741(12) Uiso 0.50 1 d PD B 4 N42' N 0.5428(11) 0.3399(8) 1.0187(9) 0.0741(12) Uiso 0.50 1 d PD B 4 N43' N 0.4191(11) 0.1935(8) 0.9351(7) 0.0637(13) Uiso 0.50 1 d PD B 4 C41' C 0.3486(18) 0.3011(14) 0.7772(11) 0.1090(18) Uiso 0.50 1 d PD B 4 H41D H 0.3962 0.3508 0.7818 0.164 Uiso 0.50 1 calc PR B 4 H41E H 0.2795 0.2983 0.7475 0.164 Uiso 0.50 1 calc PR B 4 H41F H 0.3745 0.2623 0.7561 0.164 Uiso 0.50 1 calc PR B 4 C42' C 0.304(2) 0.3504(12) 0.8780(12) 0.1090(18) Uiso 0.50 1 d PD B 4 H42D H 0.2357 0.3493 0.8479 0.164 Uiso 0.50 1 calc PR B 4 H42E H 0.3532 0.3996 0.8837 0.164 Uiso 0.50 1 calc PR B 4 H42F H 0.2975 0.3417 0.9238 0.164 Uiso 0.50 1 calc PR B 4 C43' C 0.2787(14) 0.2141(10) 0.8448(10) 0.0872(13) Uiso 0.50 1 d PD B 4 H43C H 0.2051 0.2143 0.8342 0.105 Uiso 0.50 1 calc PR B 4 H43D H 0.2843 0.1779 0.8065 0.105 Uiso 0.50 1 calc PR B 4 C44' C 0.3060(13) 0.1873(12) 0.9092(10) 0.0872(13) Uiso 0.50 1 d PD B 4 H44C H 0.2655 0.1341 0.9016 0.105 Uiso 0.50 1 calc PR B 4 H44D H 0.2863 0.2167 0.9455 0.105 Uiso 0.50 1 calc PR B 4 C45' C 0.4456(17) 0.2087(10) 1.0099(8) 0.0872(13) Uiso 0.50 1 d PD B 4 H45C H 0.5041 0.1879 1.0275 0.105 Uiso 0.50 1 calc PR B 4 H45D H 0.3856 0.1802 1.0230 0.105 Uiso 0.50 1 calc PR B 4 C46' C 0.4749(14) 0.2872(9) 1.0475(9) 0.0872(13) Uiso 0.50 1 d PD B 4 H46C H 0.5110 0.2904 1.0972 0.105 Uiso 0.50 1 calc PR B 4 H46D H 0.4111 0.3027 1.0456 0.105 Uiso 0.50 1 calc PR B 4 C47' C 0.5463(16) 0.4206(10) 1.0452(13) 0.1090(18) Uiso 0.50 1 d PD B 4 H47D H 0.5740 0.4331 1.0962 0.164 Uiso 0.50 1 calc PR B 4 H47E H 0.4759 0.4262 1.0314 0.164 Uiso 0.50 1 calc PR B 4 H47F H 0.5910 0.4546 1.0249 0.164 Uiso 0.50 1 calc PR B 4 C48' C 0.6485(14) 0.3405(13) 1.0396(13) 0.1090(18) Uiso 0.50 1 d PD B 4 H48D H 0.6692 0.3383 1.0893 0.164 Uiso 0.50 1 calc PR B 4 H48E H 0.6918 0.3867 1.0322 0.164 Uiso 0.50 1 calc PR B 4 H48F H 0.6575 0.2968 1.0119 0.164 Uiso 0.50 1 calc PR B 4 C49' C 0.4482(15) 0.1291(11) 0.9046(11) 0.092(3) Uiso 0.50 1 d PD B 4 H49D H 0.4054 0.0826 0.9118 0.137 Uiso 0.50 1 calc PR B 4 H49E H 0.5216 0.1347 0.9272 0.137 Uiso 0.50 1 calc PR B 4 H49F H 0.4370 0.1272 0.8544 0.137 Uiso 0.50 1 calc PR B 4 N53 N 0.7560(4) 0.3160(3) 0.8493(3) 0.0447(12) Uani 1 1 d . B . N54 N 0.5959(4) 0.3090(3) 0.8648(3) 0.0564(15) Uani 1 1 d . B . N55 N 0.6677(5) 0.2728(4) 0.8541(4) 0.0695(17) Uani 1 1 d . . . C51 C 0.7738(5) 0.5202(4) 0.8647(3) 0.0526(16) Uani 1 1 d . . . H51 H 0.8182 0.5679 0.8655 0.063 Uiso 1 1 calc R . . C52 C 0.8066(5) 0.4570(4) 0.8556(3) 0.0519(16) Uani 1 1 d . B . H52 H 0.8732 0.4608 0.8494 0.062 Uiso 1 1 calc R . . C53 C 0.7419(4) 0.3873(4) 0.8555(3) 0.0443(14) Uani 1 1 d . . . C54 C 0.6444(4) 0.3824(4) 0.8649(3) 0.0455(14) Uani 1 1 d . B . C55 C 0.6099(6) 0.4463(4) 0.8741(4) 0.0577(17) Uani 1 1 d . . . H55 H 0.5437 0.4430 0.8808 0.069 Uiso 1 1 calc R B . C56 C 0.6755(6) 0.5145(4) 0.8729(4) 0.0563(17) Uani 1 1 d . B . H56 H 0.6531 0.5585 0.8778 0.068 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 0.03056(18) 0.0371(2) 0.03109(19) 0.01072(15) 0.01183(14) 0.01507(15) Sn2 0.0377(2) 0.0554(3) 0.0317(2) 0.00424(18) 0.01068(16) 0.01879(18) Sn3 0.03367(19) 0.0469(2) 0.0339(2) 0.01395(17) 0.01104(15) 0.01786(16) Sn4 0.03278(19) 0.0353(2) 0.0471(2) 0.00703(17) 0.01382(16) 0.01129(16) Sn5 0.0428(2) 0.0667(3) 0.0474(3) -0.0072(2) 0.00821(19) 0.0213(2) Sn6 0.0459(2) 0.0426(2) 0.0494(2) 0.00807(19) 0.02026(19) 0.01860(18) Sn7 0.0363(2) 0.0521(3) 0.0417(2) 0.01721(18) 0.01894(17) 0.02104(18) N1 0.038(2) 0.051(3) 0.040(3) 0.013(2) 0.013(2) 0.025(2) N2 0.032(2) 0.042(3) 0.031(2) 0.0093(19) 0.0054(18) 0.0135(19) N3 0.035(2) 0.038(3) 0.035(2) 0.009(2) 0.0127(19) 0.0161(19) N4 0.038(2) 0.048(3) 0.037(2) 0.015(2) 0.018(2) 0.019(2) N5 0.037(2) 0.041(3) 0.036(2) 0.005(2) 0.0157(19) 0.017(2) N6 0.044(2) 0.044(3) 0.032(2) 0.010(2) 0.013(2) 0.019(2) N7 0.028(2) 0.043(3) 0.040(3) 0.006(2) 0.0096(19) 0.0104(19) N8 0.029(2) 0.044(3) 0.039(2) 0.011(2) 0.0124(19) 0.0166(19) N10 0.078(4) 0.089(5) 0.067(4) 0.041(4) 0.037(3) 0.044(4) N80 0.039(3) 0.038(3) 0.091(4) 0.018(3) 0.003(3) 0.004(2) C101 0.044(3) 0.056(4) 0.035(3) 0.006(3) 0.008(3) 0.026(3) C102 0.047(3) 0.070(5) 0.048(4) 0.022(3) 0.006(3) 0.031(3) C103 0.071(5) 0.092(6) 0.062(5) 0.036(4) 0.012(4) 0.048(4) C104 0.066(4) 0.109(7) 0.066(5) 0.025(5) 0.013(4) 0.063(5) C105 0.070(5) 0.128(8) 0.075(5) 0.026(5) 0.031(4) 0.070(5) C106 0.060(4) 0.095(6) 0.053(4) 0.019(4) 0.023(3) 0.046(4) C201 0.037(3) 0.034(3) 0.034(3) 0.008(2) 0.009(2) 0.010(2) C202 0.030(2) 0.043(3) 0.038(3) 0.007(2) 0.007(2) 0.008(2) C203 0.034(3) 0.050(4) 0.064(4) 0.009(3) 0.008(3) 0.007(3) C204 0.035(3) 0.056(4) 0.081(5) 0.013(4) 0.015(3) -0.005(3) C205 0.062(4) 0.040(4) 0.070(5) 0.011(3) 0.021(4) 0.009(3) C206 0.043(3) 0.044(4) 0.046(3) 0.010(3) 0.014(3) 0.012(3) C301 0.037(3) 0.034(3) 0.033(3) 0.010(2) 0.016(2) 0.015(2) C302 0.033(2) 0.034(3) 0.039(3) 0.007(2) 0.016(2) 0.013(2) C303 0.042(3) 0.039(3) 0.043(3) 0.008(2) 0.022(2) 0.015(2) C304 0.049(3) 0.042(3) 0.032(3) 0.005(2) 0.014(2) 0.015(3) C305 0.053(3) 0.044(3) 0.027(3) 0.005(2) 0.010(2) 0.011(3) C306 0.042(3) 0.039(3) 0.041(3) 0.011(3) 0.013(2) 0.012(2) C401 0.039(3) 0.035(3) 0.039(3) 0.010(2) 0.015(2) 0.012(2) C402 0.048(3) 0.036(3) 0.037(3) 0.013(2) 0.021(2) 0.016(2) C403 0.065(4) 0.054(4) 0.044(3) 0.023(3) 0.028(3) 0.028(3) C404 0.079(4) 0.053(4) 0.044(3) 0.023(3) 0.032(3) 0.027(3) C405 0.065(4) 0.060(4) 0.053(4) 0.023(3) 0.035(3) 0.013(3) C406 0.057(4) 0.064(4) 0.042(3) 0.017(3) 0.025(3) 0.029(3) C801 0.036(3) 0.034(3) 0.037(3) 0.010(2) 0.015(2) 0.016(2) C802 0.042(3) 0.039(3) 0.041(3) 0.008(2) 0.011(2) 0.017(2) C803 0.057(4) 0.044(4) 0.052(4) 0.012(3) 0.019(3) 0.028(3) C804 0.051(4) 0.064(5) 0.068(4) 0.027(4) 0.023(3) 0.038(3) C805 0.034(3) 0.063(4) 0.068(4) 0.018(3) 0.018(3) 0.024(3) C806 0.035(3) 0.039(3) 0.051(3) 0.000(3) 0.010(3) 0.009(2) Li1 0.046(5) 0.058(7) 0.043(5) 0.005(5) 0.015(4) 0.020(5) Li2 0.083(9) 0.145(16) 0.079(10) 0.031(10) 0.055(8) 0.051(10) N01 0.048(3) 0.092(5) 0.050(3) -0.008(3) 0.025(3) 0.014(3) N02 0.063(4) 0.156(8) 0.077(5) -0.017(5) 0.039(4) 0.021(5) N03 0.095(6) 0.195(11) 0.081(6) -0.015(6) 0.034(5) 0.035(7) C01 0.064(4) 0.057(4) 0.051(4) 0.009(3) 0.024(3) 0.017(3) C02 0.052(4) 0.102(7) 0.063(5) 0.024(5) 0.028(4) 0.013(4) C03 0.054(4) 0.125(9) 0.092(7) 0.018(6) 0.032(5) 0.012(5) C04 0.062(5) 0.076(6) 0.078(6) 0.014(5) 0.011(4) 0.006(4) C05 0.086(6) 0.074(6) 0.066(5) -0.008(4) -0.002(5) 0.028(5) C06 0.085(6) 0.093(7) 0.060(5) 0.001(4) 0.014(4) 0.045(5) N11 0.067(4) 0.061(4) 0.068(4) 0.012(3) 0.021(3) 0.019(3) N12 0.080(4) 0.076(4) 0.043(3) -0.005(3) 0.004(3) 0.038(3) N13 0.088(4) 0.075(4) 0.041(3) 0.013(3) 0.009(3) 0.042(4) C11 0.134(9) 0.126(9) 0.094(7) 0.055(7) 0.068(7) 0.055(7) C12 0.095(6) 0.083(6) 0.060(5) 0.010(4) -0.004(4) 0.051(5) C13 0.056(4) 0.069(5) 0.105(7) 0.018(5) 0.014(4) 0.023(4) C14 0.071(5) 0.063(5) 0.063(5) -0.006(4) -0.014(4) 0.031(4) C15 0.101(6) 0.084(6) 0.047(4) -0.001(4) 0.001(4) 0.058(5) C16 0.127(8) 0.084(7) 0.097(7) -0.017(6) -0.019(6) 0.061(6) C17 0.29(2) 0.157(13) 0.155(12) 0.053(11) 0.171(14) 0.125(14) C18 0.136(10) 0.079(8) 0.167(13) -0.035(8) 0.015(9) 0.020(7) C19 0.119(8) 0.138(9) 0.048(5) 0.029(5) 0.028(5) 0.059(7) Li3 0.036(4) 0.049(6) 0.041(5) 0.010(4) 0.011(4) 0.017(4) Li4 0.049(5) 0.053(7) 0.071(7) 0.024(6) 0.031(5) 0.023(5) N31 0.050(3) 0.050(3) 0.050(3) 0.007(2) 0.013(2) 0.015(2) N32 0.044(3) 0.044(3) 0.045(3) 0.007(2) 0.007(2) 0.014(2) N33 0.058(3) 0.048(3) 0.044(3) 0.015(2) 0.004(3) 0.008(3) C31 0.079(5) 0.082(6) 0.049(4) -0.002(4) -0.001(4) 0.021(4) C32 0.066(5) 0.086(6) 0.081(6) 0.011(5) 0.036(4) 0.024(4) C33 0.088(5) 0.046(4) 0.070(5) 0.002(4) 0.009(4) 0.027(4) C34 0.076(5) 0.050(4) 0.074(5) 0.014(4) 0.004(4) 0.026(4) C35 0.059(4) 0.064(5) 0.051(4) 0.023(3) 0.003(3) 0.024(3) C36 0.053(4) 0.055(4) 0.058(4) 0.012(3) 0.000(3) 0.018(3) C37 0.067(4) 0.065(5) 0.053(4) 0.005(3) 0.009(4) 0.021(4) C38 0.052(4) 0.054(4) 0.081(5) 0.010(4) 0.014(4) 0.005(3) C39 0.075(5) 0.080(6) 0.078(6) 0.043(5) 0.004(4) -0.009(4) N53 0.040(2) 0.054(3) 0.049(3) 0.012(2) 0.020(2) 0.020(2) N54 0.047(3) 0.061(4) 0.080(4) 0.029(3) 0.036(3) 0.023(3) N55 0.060(4) 0.076(5) 0.083(5) 0.024(4) 0.029(3) 0.026(3) C51 0.057(4) 0.047(4) 0.051(4) 0.021(3) 0.009(3) 0.011(3) C52 0.039(3) 0.061(4) 0.052(4) 0.019(3) 0.013(3) 0.005(3) C53 0.039(3) 0.053(4) 0.045(3) 0.016(3) 0.016(3) 0.016(3) C54 0.046(3) 0.052(4) 0.052(4) 0.020(3) 0.026(3) 0.023(3) C55 0.063(4) 0.059(4) 0.066(4) 0.021(4) 0.033(4) 0.028(3) C56 0.071(4) 0.053(4) 0.053(4) 0.015(3) 0.016(3) 0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N7 2.131(4) . ? Sn1 N4 2.138(4) . ? Sn1 N3 2.193(4) . ? Sn1 N5 2.196(5) . ? Sn1 N2 2.204(5) . ? Sn1 N6 2.215(4) . ? Sn2 N2 2.189(5) . ? Sn2 N8 2.234(4) . ? Sn2 N80 2.287(5) . ? Sn2 Sn3 3.2015(5) . ? Sn3 N2 2.193(4) . ? Sn3 N8 2.208(4) . ? Sn3 N3 2.263(5) . ? Sn4 N4 2.151(5) . ? Sn4 N8 2.157(5) . ? Sn4 N3 2.222(4) . ? Sn5 N6 2.163(5) . ? Sn5 N1 2.226(5) . ? Sn5 N10 2.281(6) . ? Sn5 Sn6 3.2300(6) . ? Sn6 N1 2.192(5) . ? Sn6 N6 2.204(5) . ? Sn6 N5 2.273(5) . ? Sn7 N7 2.130(5) . ? Sn7 N1 2.184(5) . ? Sn7 N5 2.216(4) . ? N1 C101 1.420(7) . ? N2 C201 1.414(7) . ? N3 C301 1.400(7) . ? N4 C401 1.406(7) . ? N5 C302 1.425(7) . ? N6 C402 1.417(7) . ? N7 C202 1.407(7) . ? N8 C801 1.412(6) . ? N10 C102 1.352(9) . ? N10 H10A 0.8800 . ? N80 C802 1.373(7) . ? N80 H80A 0.8800 . ? C101 C106 1.397(9) . ? C101 C102 1.446(8) . ? C102 C103 1.399(9) . ? C103 C104 1.380(11) . ? C103 H103 0.9500 . ? C104 C105 1.361(11) . ? C104 H104 0.9500 . ? C105 C106 1.380(10) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C201 C206 1.379(8) . ? C201 C202 1.443(8) . ? C202 C203 1.375(8) . ? C203 C204 1.381(10) . ? C203 H203 0.9500 . ? C204 C205 1.387(10) . ? C204 H204 0.9500 . ? C205 C206 1.382(9) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C301 C306 1.389(8) . ? C301 C302 1.440(7) . ? C302 C303 1.395(8) . ? C303 C304 1.375(8) . ? C303 H303 0.9500 . ? C304 C305 1.350(8) . ? C304 H304 0.9500 . ? C305 C306 1.386(8) . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C401 C406 1.384(8) . ? C401 C402 1.432(8) . ? C402 C403 1.394(8) . ? C403 C404 1.405(9) . ? C403 H403 0.9500 . ? C404 C405 1.369(10) . ? C404 H404 0.9500 . ? C405 C406 1.407(9) . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? C801 C806 1.366(7) . ? C801 C802 1.434(8) . ? C802 C803 1.383(8) . ? C803 C804 1.375(9) . ? C803 H803 0.9500 . ? C804 C805 1.374(10) . ? C804 H804 0.9500 . ? C805 C806 1.396(8) . ? C805 H805 0.9500 . ? C806 H806 0.9500 . ? Li1 N01 1.994(11) . ? Li1 N13 2.082(11) . ? Li1 N12 2.123(13) . ? Li1 N11 2.145(13) . ? Li2 N02 1.926(15) . ? Li2 N21' 1.96(2) . ? Li2 N23 2.01(2) . ? Li2 N22' 2.03(2) . ? Li2 N22 2.15(2) . ? Li2 N23' 2.22(2) . ? Li2 N21 2.29(2) . ? Li2 C23' 2.81(3) . ? N01 N03 1.346(10) . ? N01 C01 1.366(9) . ? N02 N03 1.365(11) . ? N02 C02 1.379(11) . ? C01 C02 1.395(10) . ? C01 C06 1.405(11) . ? C02 C03 1.378(11) . ? C03 C04 1.374(13) . ? C03 H03 0.9500 . ? C04 C05 1.385(13) . ? C04 H04 0.9500 . ? C05 C06 1.393(11) . ? C05 H05 0.9500 . ? C06 H06 0.9500 . ? N11 C13 1.454(9) . ? N11 C11 1.454(11) . ? N11 C12 1.466(10) . ? N12 C17 1.443(13) . ? N12 C18 1.459(12) . ? N12 C16 1.476(11) . ? N13 C19 1.452(11) . ? N13 C15 1.457(10) . ? N13 C14 1.505(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.497(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.460(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N21 C21 1.452(17) . ? N21 C22 1.476(17) . ? N21 C23 1.476(15) . ? N22 C26 1.389(14) . ? N22 C27 1.402(17) . ? N22 C28 1.514(18) . ? N23 C25 1.438(15) . ? N23 C29 1.477(14) . ? N23 C24 1.485(16) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.547(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.456(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? N21' C21' 1.463(19) . ? N21' C23' 1.512(18) . ? N21' C22' 1.54(2) . ? N22' C26' 1.394(16) . ? N22' C27' 1.424(19) . ? N22' C28' 1.51(2) . ? N23' C24' 1.406(17) . ? N23' C29' 1.453(16) . ? N23' C25' 1.456(17) . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' C24' 1.572(18) . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? C24' H24C 0.9900 . ? C24' H24D 0.9900 . ? C25' C26' 1.466(19) . ? C25' H25C 0.9900 . ? C25' H25D 0.9900 . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? Li3 N53 2.010(10) . ? Li3 N33 2.105(11) . ? Li3 N31 2.156(12) . ? Li3 N32 2.159(11) . ? Li4 N54 1.922(12) . ? Li4 N41 2.032(19) . ? Li4 N42' 2.06(2) . ? Li4 N43 2.06(2) . ? Li4 N43' 2.06(2) . ? Li4 N41' 2.170(19) . ? Li4 N42 2.20(2) . ? Li4 C46' 2.79(2) . ? N31 C33 1.443(9) . ? N31 C32 1.467(9) . ? N31 C31 1.468(9) . ? N32 C36 1.466(8) . ? N32 C37 1.468(9) . ? N32 C38 1.491(9) . ? N33 C35 1.462(8) . ? N33 C39 1.463(9) . ? N33 C34 1.495(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.489(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.491(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? N41 C41 1.443(19) . ? N41 C42 1.486(17) . ? N41 C43 1.490(16) . ? N42 C48 1.407(17) . ? N42 C46 1.469(17) . ? N42 C47 1.512(18) . ? N43 C45 1.429(15) . ? N43 C49 1.497(16) . ? N43 C44 1.513(15) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.479(17) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.470(18) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? N41' C41' 1.428(18) . ? N41' C43' 1.470(16) . ? N41' C42' 1.519(17) . ? N42' C48' 1.417(17) . ? N42' C46' 1.473(17) . ? N42' C47' 1.521(17) . ? N43' C45' 1.432(16) . ? N43' C49' 1.469(16) . ? N43' C44' 1.495(15) . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42' H42D 0.9800 . ? C42' H42E 0.9800 . ? C42' H42F 0.9800 . ? C43' C44' 1.449(17) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' H44C 0.9900 . ? C44' H44D 0.9900 . ? C45' C46' 1.473(18) . ? C45' H45C 0.9900 . ? C45' H45D 0.9900 . ? C46' H46C 0.9900 . ? C46' H46D 0.9900 . ? C47' H47D 0.9800 . ? C47' H47E 0.9800 . ? C47' H47F 0.9800 . ? C48' H48D 0.9800 . ? C48' H48E 0.9800 . ? C48' H48F 0.9800 . ? C49' H49D 0.9800 . ? C49' H49E 0.9800 . ? C49' H49F 0.9800 . ? N53 N55 1.328(8) . ? N53 C53 1.389(8) . ? N54 N55 1.375(8) . ? N54 C54 1.376(8) . ? C51 C52 1.371(10) . ? C51 C56 1.394(10) . ? C51 H51 0.9500 . ? C52 C53 1.394(9) . ? C52 H52 0.9500 . ? C53 C54 1.395(8) . ? C54 C55 1.397(9) . ? C55 C56 1.384(10) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? 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 N7 Sn1 N4 143.59(19) . . ? N7 Sn1 N3 128.89(17) . . ? N4 Sn1 N3 81.22(17) . . ? N7 Sn1 N5 80.90(18) . . ? N4 Sn1 N5 130.14(18) . . ? N3 Sn1 N5 79.33(17) . . ? N7 Sn1 N2 79.55(17) . . ? N4 Sn1 N2 86.50(18) . . ? N3 Sn1 N2 81.86(16) . . ? N5 Sn1 N2 134.57(17) . . ? N7 Sn1 N6 88.05(17) . . ? N4 Sn1 N6 79.32(17) . . ? N3 Sn1 N6 134.71(17) . . ? N5 Sn1 N6 82.77(17) . . ? N2 Sn1 N6 136.62(17) . . ? N2 Sn2 N8 82.86(16) . . ? N2 Sn2 N80 89.0(2) . . ? N8 Sn2 N80 68.73(18) . . ? N2 Sn2 Sn3 43.12(11) . . ? N8 Sn2 Sn3 43.55(11) . . ? N80 Sn2 Sn3 61.93(17) . . ? N2 Sn3 N8 83.38(16) . . ? N2 Sn3 N3 80.53(16) . . ? N8 Sn3 N3 78.07(17) . . ? N2 Sn3 Sn2 43.03(12) . . ? N8 Sn3 Sn2 44.21(12) . . ? N3 Sn3 Sn2 89.80(11) . . ? N4 Sn4 N8 83.55(17) . . ? N4 Sn4 N3 80.27(16) . . ? N8 Sn4 N3 80.01(17) . . ? N6 Sn5 N1 81.40(17) . . ? N6 Sn5 N10 93.4(2) . . ? N1 Sn5 N10 70.5(2) . . ? N6 Sn5 Sn6 42.79(13) . . ? N1 Sn5 Sn6 42.62(12) . . ? N10 Sn5 Sn6 66.01(17) . . ? N1 Sn6 N6 81.25(18) . . ? N1 Sn6 N5 78.86(16) . . ? N6 Sn6 N5 81.27(16) . . ? N1 Sn6 Sn5 43.44(13) . . ? N6 Sn6 Sn5 41.81(12) . . ? N5 Sn6 Sn5 91.09(12) . . ? N7 Sn7 N1 85.39(18) . . ? N7 Sn7 N5 80.45(17) . . ? N1 Sn7 N5 80.27(17) . . ? C101 N1 Sn7 125.8(4) . . ? C101 N1 Sn6 112.5(4) . . ? Sn7 N1 Sn6 101.56(18) . . ? C101 N1 Sn5 107.7(3) . . ? Sn7 N1 Sn5 110.7(2) . . ? Sn6 N1 Sn5 93.93(18) . . ? C201 N2 Sn2 125.1(4) . . ? C201 N2 Sn3 118.9(3) . . ? Sn2 N2 Sn3 93.86(16) . . ? C201 N2 Sn1 110.8(3) . . ? Sn2 N2 Sn1 104.84(18) . . ? Sn3 N2 Sn1 99.42(18) . . ? C301 N3 Sn1 111.9(3) . . ? C301 N3 Sn4 123.1(3) . . ? Sn1 N3 Sn4 96.96(17) . . ? C301 N3 Sn3 123.2(3) . . ? Sn1 N3 Sn3 97.62(18) . . ? Sn4 N3 Sn3 98.60(17) . . ? C401 N4 Sn1 113.5(3) . . ? C401 N4 Sn4 124.0(4) . . ? Sn1 N4 Sn4 100.84(19) . . ? C302 N5 Sn1 111.1(3) . . ? C302 N5 Sn7 121.0(3) . . ? Sn1 N5 Sn7 96.92(18) . . ? C302 N5 Sn6 126.8(4) . . ? Sn1 N5 Sn6 96.81(17) . . ? Sn7 N5 Sn6 98.11(17) . . ? C402 N6 Sn5 120.8(3) . . ? C402 N6 Sn6 121.7(4) . . ? Sn5 N6 Sn6 95.39(18) . . ? C402 N6 Sn1 110.1(3) . . ? Sn5 N6 Sn1 107.5(2) . . ? Sn6 N6 Sn1 98.27(18) . . ? C202 N7 Sn7 123.9(4) . . ? C202 N7 Sn1 113.3(3) . . ? Sn7 N7 Sn1 101.59(19) . . ? C801 N8 Sn4 128.2(3) . . ? C801 N8 Sn3 111.0(3) . . ? Sn4 N8 Sn3 102.34(19) . . ? C801 N8 Sn2 108.2(3) . . ? Sn4 N8 Sn2 108.90(18) . . ? Sn3 N8 Sn2 92.24(15) . . ? C102 N10 Sn5 109.2(4) . . ? C102 N10 H10A 125.4 . . ? Sn5 N10 H10A 125.4 . . ? C802 N80 Sn2 108.7(4) . . ? C802 N80 H80A 125.6 . . ? Sn2 N80 H80A 125.6 . . ? C106 C101 N1 127.0(5) . . ? C106 C101 C102 118.8(5) . . ? N1 C101 C102 114.2(5) . . ? N10 C102 C103 127.6(6) . . ? N10 C102 C101 114.9(5) . . ? C103 C102 C101 117.3(6) . . ? C104 C103 C102 121.4(7) . . ? C104 C103 H103 119.3 . . ? C102 C103 H103 119.3 . . ? C105 C104 C103 121.2(6) . . ? C105 C104 H104 119.4 . . ? C103 C104 H104 119.4 . . ? C104 C105 C106 119.7(7) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C105 C106 C101 121.5(7) . . ? C105 C106 H106 119.3 . . ? C101 C106 H106 119.3 . . ? C206 C201 N2 123.4(5) . . ? C206 C201 C202 118.4(5) . . ? N2 C201 C202 118.1(5) . . ? C203 C202 N7 123.7(5) . . ? C203 C202 C201 118.1(5) . . ? N7 C202 C201 118.2(4) . . ? C202 C203 C204 122.4(6) . . ? C202 C203 H203 118.8 . . ? C204 C203 H203 118.8 . . ? C203 C204 C205 119.6(6) . . ? C203 C204 H204 120.2 . . ? C205 C204 H204 120.2 . . ? C206 C205 C204 119.3(6) . . ? C206 C205 H205 120.3 . . ? C204 C205 H205 120.3 . . ? C201 C206 C205 122.2(6) . . ? C201 C206 H206 118.9 . . ? C205 C206 H206 118.9 . . ? C306 C301 N3 123.4(5) . . ? C306 C301 C302 117.6(5) . . ? N3 C301 C302 119.0(4) . . ? C303 C302 N5 123.5(5) . . ? C303 C302 C301 117.8(5) . . ? N5 C302 C301 118.6(5) . . ? C304 C303 C302 122.3(5) . . ? C304 C303 H303 118.8 . . ? C302 C303 H303 118.8 . . ? C305 C304 C303 119.9(6) . . ? C305 C304 H304 120.0 . . ? C303 C304 H304 120.0 . . ? C304 C305 C306 120.2(5) . . ? C304 C305 H305 119.9 . . ? C306 C305 H305 119.9 . . ? C305 C306 C301 122.1(5) . . ? C305 C306 H306 119.0 . . ? C301 C306 H306 119.0 . . ? C406 C401 N4 122.7(5) . . ? C406 C401 C402 119.3(5) . . ? N4 C401 C402 118.0(5) . . ? C403 C402 N6 122.4(5) . . ? C403 C402 C401 118.6(5) . . ? N6 C402 C401 119.0(4) . . ? C402 C403 C404 121.3(6) . . ? C402 C403 H403 119.4 . . ? C404 C403 H403 119.4 . . ? C405 C404 C403 119.6(6) . . ? C405 C404 H404 120.2 . . ? C403 C404 H404 120.2 . . ? C404 C405 C406 120.4(6) . . ? C404 C405 H405 119.8 . . ? C406 C405 H405 119.8 . . ? C401 C406 C405 120.8(6) . . ? C401 C406 H406 119.6 . . ? C405 C406 H406 119.6 . . ? C806 C801 N8 126.7(5) . . ? C806 C801 C802 119.1(5) . . ? N8 C801 C802 114.2(4) . . ? N80 C802 C803 128.3(6) . . ? N80 C802 C801 113.2(5) . . ? C803 C802 C801 118.5(5) . . ? C804 C803 C802 120.9(6) . . ? C804 C803 H803 119.5 . . ? C802 C803 H803 119.5 . . ? C805 C804 C803 121.1(5) . . ? C805 C804 H804 119.5 . . ? C803 C804 H804 119.5 . . ? C804 C805 C806 118.8(6) . . ? C804 C805 H805 120.6 . . ? C806 C805 H805 120.6 . . ? C801 C806 C805 121.6(6) . . ? C801 C806 H806 119.2 . . ? C805 C806 H806 119.2 . . ? N01 Li1 N13 121.1(6) . . ? N01 Li1 N12 118.8(6) . . ? N13 Li1 N12 88.3(5) . . ? N01 Li1 N11 120.8(6) . . ? N13 Li1 N11 85.9(5) . . ? N12 Li1 N11 113.0(5) . . ? N02 Li2 N21' 102.1(9) . . ? N02 Li2 N23 130.8(9) . . ? N21' Li2 N23 90.7(10) . . ? N02 Li2 N22' 113.5(11) . . ? N21' Li2 N22' 139.9(10) . . ? N23 Li2 N22' 80.0(8) . . ? N02 Li2 N22 121.4(11) . . ? N21' Li2 N22 124.1(9) . . ? N23 Li2 N22 86.2(7) . . ? N22' Li2 N22 17.6(5) . . ? N02 Li2 N23' 131.3(10) . . ? N21' Li2 N23' 86.5(9) . . ? N23 Li2 N23' 4.2(5) . . ? N22' Li2 N23' 83.7(8) . . ? N22 Li2 N23' 89.1(7) . . ? N02 Li2 N21 114.8(9) . . ? N21' Li2 N21 13.1(5) . . ? N23 Li2 N21 84.5(8) . . ? N22' Li2 N21 127.1(8) . . ? N22 Li2 N21 112.0(7) . . ? N23' Li2 N21 80.5(8) . . ? N02 Li2 C23' 128.4(10) . . ? N21' Li2 C23' 30.9(6) . . ? N23 Li2 C23' 61.8(7) . . ? N22' Li2 C23' 118.1(8) . . ? N22 Li2 C23' 108.1(8) . . ? N23' Li2 C23' 57.8(6) . . ? N21 Li2 C23' 22.8(5) . . ? N03 N01 C01 102.4(6) . . ? N03 N01 Li1 121.8(6) . . ? C01 N01 Li1 135.8(6) . . ? N03 N02 C02 103.2(7) . . ? N03 N02 Li2 133.4(8) . . ? C02 N02 Li2 123.4(8) . . ? N01 N03 N02 116.0(8) . . ? N01 C01 C02 110.8(6) . . ? N01 C01 C06 129.9(7) . . ? C02 C01 C06 119.2(7) . . ? C03 C02 N02 129.4(8) . . ? C03 C02 C01 122.9(8) . . ? N02 C02 C01 107.6(6) . . ? C04 C03 C02 117.7(8) . . ? C04 C03 H03 121.2 . . ? C02 C03 H03 121.2 . . ? C03 C04 C05 120.6(8) . . ? C03 C04 H04 119.7 . . ? C05 C04 H04 119.7 . . ? C04 C05 C06 122.4(8) . . ? C04 C05 H05 118.8 . . ? C06 C05 H05 118.8 . . ? C05 C06 C01 117.1(8) . . ? C05 C06 H06 121.5 . . ? C01 C06 H06 121.5 . . ? C13 N11 C11 109.7(7) . . ? C13 N11 C12 107.8(6) . . ? C11 N11 C12 108.5(7) . . ? C13 N11 Li1 104.7(5) . . ? C11 N11 Li1 121.7(7) . . ? C12 N11 Li1 103.7(6) . . ? C17 N12 C18 107.3(10) . . ? C17 N12 C16 114.6(10) . . ? C18 N12 C16 104.0(9) . . ? C17 N12 Li1 116.3(8) . . ? C18 N12 Li1 114.5(7) . . ? C16 N12 Li1 99.5(6) . . ? C19 N13 C15 110.0(7) . . ? C19 N13 C14 111.3(7) . . ? C15 N13 C14 111.2(7) . . ? C19 N13 Li1 116.1(6) . . ? C15 N13 Li1 102.8(5) . . ? C14 N13 Li1 105.2(5) . . ? N11 C11 H11A 109.5 . . ? N11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N11 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N11 C13 C14 112.0(7) . . ? N11 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? N11 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 N13 112.4(6) . . ? C13 C14 H14A 109.1 . . ? N13 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? N13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N13 C15 C16 114.0(7) . . ? N13 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N13 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 N12 113.5(8) . . ? C15 C16 H16A 108.9 . . ? N12 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? N12 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N12 C17 H17A 109.5 . . ? N12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N12 C18 H18A 109.5 . . ? N12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N13 C19 H19A 109.5 . . ? N13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 N21 C22 112.6(11) . . ? C21 N21 C23 110.0(12) . . ? C22 N21 C23 111.5(12) . . ? C21 N21 Li2 111.2(11) . . ? C22 N21 Li2 111.1(9) . . ? C23 N21 Li2 99.7(9) . . ? C26 N22 C27 107.9(13) . . ? C26 N22 C28 107.1(12) . . ? C27 N22 C28 110.9(12) . . ? C26 N22 Li2 102.1(10) . . ? C27 N22 Li2 115.2(10) . . ? C28 N22 Li2 112.9(11) . . ? C25 N23 C29 105.5(11) . . ? C25 N23 C24 108.5(12) . . ? C29 N23 C24 102.8(11) . . ? C25 N23 Li2 107.3(10) . . ? C29 N23 Li2 122.8(11) . . ? C24 N23 Li2 109.3(9) . . ? N21 C21 H21A 109.5 . . ? N21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N21 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N21 C23 C24 110.7(11) . . ? N21 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? N21 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N23 C24 C23 108.2(12) . . ? N23 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? N23 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? N23 C25 C26 112.0(12) . . ? N23 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? N23 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? N22 C26 C25 122.3(13) . . ? N22 C26 H26A 106.8 . . ? C25 C26 H26A 106.8 . . ? N22 C26 H26B 106.8 . . ? C25 C26 H26B 106.8 . . ? H26A C26 H26B 106.6 . . ? N22 C27 H27A 109.5 . . ? N22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N22 C28 H28A 109.5 . . ? N22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N23 C29 H29A 109.5 . . ? N23 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N23 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C21' N21' C23' 103.8(13) . . ? C21' N21' C22' 112.8(16) . . ? C23' N21' C22' 99.5(15) . . ? C21' N21' Li2 111.6(15) . . ? C23' N21' Li2 107.4(11) . . ? C22' N21' Li2 119.6(15) . . ? C26' N22' C27' 117.5(15) . . ? C26' N22' C28' 105.3(14) . . ? C27' N22' C28' 109.4(15) . . ? C26' N22' Li2 110.1(12) . . ? C27' N22' Li2 115.1(16) . . ? C28' N22' Li2 97.1(13) . . ? C24' N23' C29' 120.8(14) . . ? C24' N23' C25' 116.3(16) . . ? C29' N23' C25' 106.0(13) . . ? C24' N23' Li2 102.6(12) . . ? C29' N23' Li2 112.1(14) . . ? C25' N23' Li2 96.4(12) . . ? N21' C21' H21D 109.5 . . ? N21' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? N21' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? N21' C22' H22D 109.5 . . ? N21' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? N21' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? N21' C23' C24' 107.8(13) . . ? N21' C23' Li2 41.7(8) . . ? C24' C23' Li2 76.3(10) . . ? N21' C23' H23C 110.2 . . ? C24' C23' H23C 110.2 . . ? Li2 C23' H23C 148.8 . . ? N21' C23' H23D 110.2 . . ? C24' C23' H23D 110.2 . . ? Li2 C23' H23D 96.8 . . ? H23C C23' H23D 108.5 . . ? N23' C24' C23' 113.0(15) . . ? N23' C24' H24C 109.0 . . ? C23' C24' H24C 109.0 . . ? N23' C24' H24D 109.0 . . ? C23' C24' H24D 109.0 . . ? H24C C24' H24D 107.8 . . ? N23' C25' C26' 114.0(14) . . ? N23' C25' H25C 108.8 . . ? C26' C25' H25C 108.8 . . ? N23' C25' H25D 108.8 . . ? C26' C25' H25D 108.8 . . ? H25C C25' H25D 107.7 . . ? N22' C26' C25' 114.6(16) . . ? N22' C26' H26C 108.6 . . ? C25' C26' H26C 108.6 . . ? N22' C26' H26D 108.6 . . ? C25' C26' H26D 108.6 . . ? H26C C26' H26D 107.6 . . ? N22' C27' H27D 109.5 . . ? N22' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? N22' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? N22' C28' H28D 109.5 . . ? N22' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? N22' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? N23' C29' H29D 109.5 . . ? N23' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? N23' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? N53 Li3 N33 125.2(5) . . ? N53 Li3 N31 116.9(5) . . ? N33 Li3 N31 86.7(4) . . ? N53 Li3 N32 111.4(5) . . ? N33 Li3 N32 84.5(4) . . ? N31 Li3 N32 126.1(5) . . ? N54 Li4 N41 115.4(7) . . ? N54 Li4 N42' 115.9(7) . . ? N41 Li4 N42' 119.6(8) . . ? N54 Li4 N43 127.4(7) . . ? N41 Li4 N43 89.8(7) . . ? N42' Li4 N43 83.4(7) . . ? N54 Li4 N43' 126.7(7) . . ? N41 Li4 N43' 84.6(7) . . ? N42' Li4 N43' 89.3(7) . . ? N43 Li4 N43' 6.4(6) . . ? N54 Li4 N41' 110.5(7) . . ? N41 Li4 N41' 5.0(7) . . ? N42' Li4 N41' 124.1(8) . . ? N43 Li4 N41' 92.5(7) . . ? N43' Li4 N41' 87.1(7) . . ? N54 Li4 N42 112.0(7) . . ? N41 Li4 N42 122.1(8) . . ? N42' Li4 N42 4.1(7) . . ? N43 Li4 N42 86.8(7) . . ? N43' Li4 N42 92.8(7) . . ? N41' Li4 N42 126.4(8) . . ? N54 Li4 C46' 140.1(7) . . ? N41 Li4 C46' 104.2(7) . . ? N42' Li4 C46' 31.0(5) . . ? N43 Li4 C46' 54.5(6) . . ? N43' Li4 C46' 59.8(6) . . ? N41' Li4 C46' 109.1(7) . . ? N42 Li4 C46' 34.9(6) . . ? C33 N31 C32 113.1(6) . . ? C33 N31 C31 110.9(6) . . ? C32 N31 C31 108.3(6) . . ? C33 N31 Li3 100.6(5) . . ? C32 N31 Li3 111.7(5) . . ? C31 N31 Li3 112.2(5) . . ? C36 N32 C37 111.4(6) . . ? C36 N32 C38 108.7(5) . . ? C37 N32 C38 109.4(6) . . ? C36 N32 Li3 102.3(5) . . ? C37 N32 Li3 103.0(5) . . ? C38 N32 Li3 121.9(5) . . ? C35 N33 C39 110.0(6) . . ? C35 N33 C34 108.6(6) . . ? C39 N33 C34 111.2(7) . . ? C35 N33 Li3 107.2(5) . . ? C39 N33 Li3 116.8(5) . . ? C34 N33 Li3 102.5(5) . . ? N31 C31 H31A 109.5 . . ? N31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 C34 113.9(6) . . ? N31 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? N31 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 N33 109.0(6) . . ? C33 C34 H34A 109.9 . . ? N33 C34 H34A 109.9 . . ? C33 C34 H34B 109.9 . . ? N33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? N33 C35 C36 112.4(5) . . ? N33 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? N33 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? N32 C36 C35 111.9(5) . . ? N32 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? N32 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N32 C37 H37A 109.5 . . ? N32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N32 C38 H38A 109.5 . . ? N32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N33 C39 H39A 109.5 . . ? N33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 N41 C42 109.8(15) . . ? C41 N41 C43 109.5(15) . . ? C42 N41 C43 108.7(14) . . ? C41 N41 Li4 102.4(14) . . ? C42 N41 Li4 124.9(14) . . ? C43 N41 Li4 100.5(9) . . ? C48 N42 C46 112.9(15) . . ? C48 N42 C47 107.9(15) . . ? C46 N42 C47 111.4(15) . . ? C48 N42 Li4 115.8(15) . . ? C46 N42 Li4 97.6(10) . . ? C47 N42 Li4 111.0(13) . . ? C45 N43 C49 109.4(13) . . ? C45 N43 C44 116.8(14) . . ? C49 N43 C44 108.3(12) . . ? C45 N43 Li4 104.3(11) . . ? C49 N43 Li4 115.5(13) . . ? C44 N43 Li4 102.5(10) . . ? N41 C41 H41A 109.5 . . ? N41 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N41 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N41 113.1(14) . . ? C44 C43 H43A 109.0 . . ? N41 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? N41 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 N43 107.4(13) . . ? C43 C44 H44A 110.2 . . ? N43 C44 H44A 110.2 . . ? C43 C44 H44B 110.2 . . ? N43 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? N43 C45 C46 111.6(15) . . ? N43 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? N43 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45 C46 N42 114.0(14) . . ? C45 C46 H46A 108.7 . . ? N42 C46 H46A 108.7 . . ? C45 C46 H46B 108.7 . . ? N42 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? N42 C47 H47A 109.5 . . ? N42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N42 C48 H48A 109.5 . . ? N42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N43 C49 H49A 109.5 . . ? N43 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N43 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C41' N41' C43' 114.2(15) . . ? C41' N41' C42' 109.4(15) . . ? C43' N41' C42' 111.3(15) . . ? C41' N41' Li4 111.6(14) . . ? C43' N41' Li4 101.8(10) . . ? C42' N41' Li4 108.1(13) . . ? C48' N42' C46' 114.1(15) . . ? C48' N42' C47' 103.6(12) . . ? C46' N42' C47' 110.8(15) . . ? C48' N42' Li4 104.5(14) . . ? C46' N42' Li4 103.1(10) . . ? C47' N42' Li4 121.0(13) . . ? C45' N43' C49' 114.7(13) . . ? C45' N43' C44' 106.3(14) . . ? C49' N43' C44' 114.1(13) . . ? C45' N43' Li4 103.4(11) . . ? C49' N43' Li4 113.1(13) . . ? C44' N43' Li4 104.2(10) . . ? N41' C41' H41D 109.5 . . ? N41' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? N41' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? N41' C42' H42D 109.5 . . ? N41' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? N41' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C44' C43' N41' 115.6(14) . . ? C44' C43' H43C 108.4 . . ? N41' C43' H43C 108.4 . . ? C44' C43' H43D 108.4 . . ? N41' C43' H43D 108.4 . . ? H43C C43' H43D 107.4 . . ? C43' C44' N43' 113.2(14) . . ? C43' C44' H44C 108.9 . . ? N43' C44' H44C 108.9 . . ? C43' C44' H44D 108.9 . . ? N43' C44' H44D 108.9 . . ? H44C C44' H44D 107.8 . . ? N43' C45' C46' 118.7(14) . . ? N43' C45' H45C 107.6 . . ? C46' C45' H45C 107.6 . . ? N43' C45' H45D 107.6 . . ? C46' C45' H45D 107.6 . . ? H45C C45' H45D 107.1 . . ? C45' C46' N42' 113.2(14) . . ? C45' C46' Li4 73.9(10) . . ? N42' C46' Li4 46.0(8) . . ? C45' C46' H46C 108.9 . . ? N42' C46' H46C 108.9 . . ? Li4 C46' H46C 147.2 . . ? C45' C46' H46D 108.9 . . ? N42' C46' H46D 108.9 . . ? Li4 C46' H46D 101.6 . . ? H46C C46' H46D 107.8 . . ? N42' C47' H47D 109.5 . . ? N42' C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? N42' C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? N42' C48' H48D 109.5 . . ? N42' C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? N42' C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? N43' C49' H49D 109.5 . . ? N43' C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? N43' C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? N55 N53 C53 103.5(5) . . ? N55 N53 Li3 120.6(5) . . ? C53 N53 Li3 132.8(5) . . ? N55 N54 C54 102.5(5) . . ? N55 N54 Li4 134.7(6) . . ? C54 N54 Li4 116.4(6) . . ? N53 N55 N54 116.1(6) . . ? C52 C51 C56 120.1(6) . . ? C52 C51 H51 119.9 . . ? C56 C51 H51 119.9 . . ? C51 C52 C53 119.8(6) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? N53 C53 C52 131.7(6) . . ? N53 C53 C54 108.6(5) . . ? C52 C53 C54 119.6(6) . . ? N54 C54 C53 109.3(5) . . ? N54 C54 C55 129.5(6) . . ? C53 C54 C55 121.2(6) . . ? C56 C55 C54 117.7(6) . . ? C56 C55 H55 121.1 . . ? C54 C55 H55 121.1 . . ? C55 C56 C51 121.5(7) . . ? C55 C56 H56 119.2 . . ? C51 C56 H56 119.2 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 4.328 _refine_diff_density_min -3.333 _refine_diff_density_rms 0.362 # Attachment '- dw0801.cif' data_dw0801 _database_code_depnum_ccdc_archive 'CCDC 796654' #TrackingRef '- dw0801.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H56 Li2 N10 Sn2' _chemical_formula_sum 'C30 H56 Li2 N10 Sn2' _chemical_formula_weight 808.11 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9707(3) _cell_length_b 9.3155(2) _cell_length_c 14.8029(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.888(1) _cell_angle_gamma 90.00 _cell_volume 1843.43(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 14869 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; the coordinated molecule of PMDETA was disordered and modelled as an isotropic 75:25 mixture with geometric restraints. The amido hydrogen atom (H1A) was located in the difference Fourier map and refined; all other hydrogens were placed in geometrically idealized positions. ; _diffrn_ambient_temperature 180(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 23029 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3760 _reflns_number_gt 2872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0371P)^2^+2.0076P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3760 _refine_ls_number_parameters 183 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.047 _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 0.52973(2) 0.64610(3) 0.058707(17) 0.03523(11) Uani 1 1 d . . . N1 N 0.3806(3) 0.7214(4) -0.0016(3) 0.0484(9) Uani 1 1 d D . . H1A H 0.365(3) 0.8093(17) -0.005(3) 0.049(13) Uiso 1 1 d D . . N2 N 0.4428(2) 0.4558(3) 0.06455(19) 0.0330(7) Uani 1 1 d . . . C1 C 0.3077(3) 0.6309(4) 0.0109(3) 0.0388(9) Uani 1 1 d . . . C2 C 0.2072(3) 0.6663(5) -0.0060(3) 0.0486(11) Uani 1 1 d . . . H2A H 0.1845 0.7585 -0.0303 0.058 Uiso 1 1 calc R . . C3 C 0.1399(3) 0.5701(6) 0.0120(3) 0.0516(11) Uani 1 1 d . . . H3A H 0.0719 0.5973 0.0010 0.062 Uiso 1 1 calc R . . C4 C 0.1704(3) 0.4363(5) 0.0454(3) 0.0495(11) Uani 1 1 d . . . H4A H 0.1239 0.3703 0.0579 0.059 Uiso 1 1 calc R . . C5 C 0.2702(3) 0.3969(5) 0.0612(3) 0.0416(9) Uani 1 1 d . . . H5A H 0.2904 0.3028 0.0833 0.050 Uiso 1 1 calc R . . C6 C 0.3411(3) 0.4907(4) 0.0457(2) 0.0342(8) Uani 1 1 d . A . Li1 Li 0.4765(4) 0.3554(6) 0.1889(4) 0.0382(14) Uiso 1 1 d D . . N3 N 0.4363(4) 0.4890(5) 0.2927(3) 0.0401(14) Uiso 0.75 1 d PD A 1 N4 N 0.6180(4) 0.3331(6) 0.2885(4) 0.0452(11) Uiso 0.75 1 d PD A 1 N5 N 0.4618(5) 0.1252(6) 0.2037(4) 0.042(3) Uiso 0.75 1 d PD A 1 C7 C 0.3835(5) 0.6240(6) 0.2561(4) 0.0500(14) Uiso 0.75 1 d PD A 1 H7A H 0.3873 0.6896 0.3088 0.075 Uiso 0.75 1 calc PR A 1 H7B H 0.3132 0.6031 0.2233 0.075 Uiso 0.75 1 calc PR A 1 H7C H 0.4149 0.6688 0.2120 0.075 Uiso 0.75 1 calc PR A 1 C8 C 0.3761(7) 0.4071(11) 0.3420(7) 0.059(3) Uiso 0.75 1 d PD A 1 H8A H 0.3611 0.4680 0.3901 0.088 Uiso 0.75 1 calc PR A 1 H8B H 0.4138 0.3226 0.3722 0.088 Uiso 0.75 1 calc PR A 1 H8C H 0.3135 0.3764 0.2963 0.088 Uiso 0.75 1 calc PR A 1 C9 C 0.5355(4) 0.5221(7) 0.3556(4) 0.0524(15) Uiso 0.75 1 d PD A 1 H9A H 0.5287 0.5598 0.4160 0.063 Uiso 0.75 1 calc PR A 1 H9B H 0.5665 0.5981 0.3266 0.063 Uiso 0.75 1 calc PR A 1 C10 C 0.6035(6) 0.3920(7) 0.3755(4) 0.0510(15) Uiso 0.75 1 d PD A 1 H10A H 0.6692 0.4194 0.4191 0.061 Uiso 0.75 1 calc PR A 1 H10B H 0.5741 0.3173 0.4069 0.061 Uiso 0.75 1 calc PR A 1 C11 C 0.6987(5) 0.4099(7) 0.2630(5) 0.0585(16) Uiso 0.75 1 d PD A 1 H11A H 0.7622 0.3935 0.3117 0.088 Uiso 0.75 1 calc PR A 1 H11B H 0.6838 0.5129 0.2581 0.088 Uiso 0.75 1 calc PR A 1 H11C H 0.7035 0.3742 0.2022 0.088 Uiso 0.75 1 calc PR A 1 C12 C 0.6377(7) 0.1761(7) 0.2933(7) 0.050(3) Uiso 0.75 1 d PD A 1 H12A H 0.6891 0.1534 0.3534 0.060 Uiso 0.75 1 calc PR A 1 H12B H 0.6643 0.1479 0.2408 0.060 Uiso 0.75 1 calc PR A 1 C13 C 0.5446(4) 0.0911(7) 0.2873(4) 0.0492(14) Uiso 0.75 1 d PD A 1 H13A H 0.5602 -0.0124 0.2866 0.059 Uiso 0.75 1 calc PR A 1 H13B H 0.5233 0.1101 0.3444 0.059 Uiso 0.75 1 calc PR A 1 C14 C 0.4841(5) 0.0700(7) 0.1187(4) 0.0533(15) Uiso 0.75 1 d PD A 1 H14A H 0.4798 -0.0350 0.1178 0.080 Uiso 0.75 1 calc PR A 1 H14B H 0.5518 0.0992 0.1197 0.080 Uiso 0.75 1 calc PR A 1 H14C H 0.4357 0.1091 0.0623 0.080 Uiso 0.75 1 calc PR A 1 C15 C 0.3709(5) 0.0535(7) 0.2105(5) 0.0603(16) Uiso 0.75 1 d PD A 1 H15A H 0.3813 -0.0506 0.2135 0.090 Uiso 0.75 1 calc PR A 1 H15B H 0.3151 0.0773 0.1550 0.090 Uiso 0.75 1 calc PR A 1 H15C H 0.3554 0.0858 0.2677 0.090 Uiso 0.75 1 calc PR A 1 N3' N 0.4644(12) 0.4746(14) 0.3087(9) 0.045(5) Uiso 0.25 1 d PD A 2 N4' N 0.6307(9) 0.3333(17) 0.2745(10) 0.0452(11) Uiso 0.25 1 d PD A 2 N5' N 0.4762(12) 0.1219(14) 0.1998(11) 0.044(9) Uiso 0.25 1 d PD A 2 C7' C 0.4479(15) 0.6278(15) 0.2785(13) 0.0500(14) Uiso 0.25 1 d PD A 2 H7D H 0.4426 0.6865 0.3318 0.075 Uiso 0.25 1 calc PR A 2 H7E H 0.3859 0.6359 0.2265 0.075 Uiso 0.25 1 calc PR A 2 H7F H 0.5043 0.6615 0.2574 0.075 Uiso 0.25 1 calc PR A 2 C8' C 0.3700(19) 0.440(3) 0.333(3) 0.071(11) Uiso 0.25 1 d PD A 2 H8D H 0.3673 0.4967 0.3877 0.107 Uiso 0.25 1 calc PR A 2 H8E H 0.3686 0.3379 0.3468 0.107 Uiso 0.25 1 calc PR A 2 H8F H 0.3123 0.4644 0.2788 0.107 Uiso 0.25 1 calc PR A 2 C9' C 0.5550(12) 0.443(2) 0.3846(11) 0.050(4) Uiso 0.25 1 d PD A 2 H9C H 0.5651 0.5189 0.4331 0.060 Uiso 0.25 1 calc PR A 2 H9D H 0.5453 0.3509 0.4146 0.060 Uiso 0.25 1 calc PR A 2 C10' C 0.6433(16) 0.432(2) 0.3545(12) 0.060(5) Uiso 0.25 1 d PD A 2 H10C H 0.6994 0.3979 0.4080 0.072 Uiso 0.25 1 calc PR A 2 H10D H 0.6609 0.5282 0.3362 0.072 Uiso 0.25 1 calc PR A 2 C11' C 0.7111(14) 0.365(2) 0.2292(15) 0.0585(16) Uiso 0.25 1 d PD A 2 H11D H 0.7767 0.3495 0.2751 0.088 Uiso 0.25 1 calc PR A 2 H11E H 0.7057 0.4654 0.2081 0.088 Uiso 0.25 1 calc PR A 2 H11F H 0.7037 0.3017 0.1748 0.088 Uiso 0.25 1 calc PR A 2 C12' C 0.639(2) 0.189(2) 0.3134(19) 0.054(9) Uiso 0.25 1 d PD A 2 H12C H 0.6083 0.1845 0.3660 0.065 Uiso 0.25 1 calc PR A 2 H12D H 0.7099 0.1602 0.3377 0.065 Uiso 0.25 1 calc PR A 2 C13' C 0.5830(11) 0.089(2) 0.2330(12) 0.052(4) Uiso 0.25 1 d PD A 2 H13C H 0.6122 0.0992 0.1798 0.062 Uiso 0.25 1 calc PR A 2 H13D H 0.5922 -0.0114 0.2551 0.062 Uiso 0.25 1 calc PR A 2 C14' C 0.4272(16) 0.055(2) 0.1066(11) 0.058(5) Uiso 0.25 1 d PD A 2 H14D H 0.4279 -0.0495 0.1134 0.086 Uiso 0.25 1 calc PR A 2 H14E H 0.4636 0.0822 0.0616 0.086 Uiso 0.25 1 calc PR A 2 H14F H 0.3579 0.0888 0.0834 0.086 Uiso 0.25 1 calc PR A 2 C15' C 0.4250(16) 0.072(2) 0.2699(14) 0.069(6) Uiso 0.25 1 d PD A 2 H15D H 0.4254 -0.0332 0.2720 0.104 Uiso 0.25 1 calc PR A 2 H15E H 0.3558 0.1065 0.2512 0.104 Uiso 0.25 1 calc PR A 2 H15F H 0.4603 0.1099 0.3325 0.104 Uiso 0.25 1 calc PR A 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 0.03568(17) 0.03448(16) 0.03432(15) -0.00343(12) 0.00824(11) -0.00085(12) N1 0.048(2) 0.035(2) 0.067(2) 0.0139(18) 0.0228(18) 0.0130(17) N2 0.0285(17) 0.0380(17) 0.0295(14) 0.0011(13) 0.0039(12) 0.0018(14) C1 0.034(2) 0.046(2) 0.038(2) 0.0034(18) 0.0121(16) 0.0070(18) C2 0.044(3) 0.056(3) 0.046(2) 0.008(2) 0.0142(19) 0.021(2) C3 0.031(2) 0.079(3) 0.045(2) -0.005(2) 0.0120(18) 0.010(2) C4 0.039(2) 0.065(3) 0.048(2) -0.007(2) 0.0172(19) -0.002(2) C5 0.037(2) 0.049(2) 0.037(2) 0.0004(18) 0.0098(17) -0.0014(19) C6 0.033(2) 0.041(2) 0.0277(17) 0.0012(16) 0.0078(15) 0.0019(17) _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 N1 2.132(4) . ? Sn1 N2 2.165(3) . ? Sn1 N2 2.188(3) 3_665 ? Sn1 Sn1 3.2065(7) 3_665 ? N1 C1 1.375(5) . ? N2 C6 1.404(5) . ? N2 Li1 1.995(7) . ? N2 Sn1 2.188(3) 3_665 ? C1 C2 1.393(6) . ? C1 C6 1.431(5) . ? C2 C3 1.380(7) . ? C3 C4 1.363(7) . ? C4 C5 1.395(6) . ? C5 C6 1.389(5) . ? C6 Li1 2.708(7) . ? Li1 N4 2.105(8) . ? Li1 N3' 2.141(12) . ? Li1 N4' 2.168(13) . ? Li1 N5 2.171(8) . ? Li1 N3 2.174(7) . ? Li1 N5' 2.182(13) . ? N3 C9 1.461(6) . ? N3 C8 1.475(7) . ? N3 C7 1.479(6) . ? N4 C10 1.468(6) . ? N4 C11 1.473(7) . ? N4 C12 1.486(6) . ? N5 C13 1.462(7) . ? N5 C15 1.465(7) . ? N5 C14 1.474(7) . ? C9 C10 1.515(9) . ? C12 C13 1.503(11) . ? N3' C9' 1.458(10) . ? N3' C7' 1.493(9) . ? N3' C8' 1.495(10) . ? N4' C12' 1.454(10) . ? N4' C10' 1.469(10) . ? N4' C11' 1.496(10) . ? N5' C13' 1.461(10) . ? N5' C14' 1.486(10) . ? N5' C15' 1.496(10) . ? C9' C10' 1.43(3) . ? C12' C13' 1.53(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 N2 78.16(12) . . ? N1 Sn1 N2 100.38(13) . 3_665 ? N2 Sn1 N2 85.10(11) . 3_665 ? N1 Sn1 Sn1 89.11(11) . 3_665 ? N2 Sn1 Sn1 42.82(8) . 3_665 ? N2 Sn1 Sn1 42.27(8) 3_665 3_665 ? C1 N1 Sn1 114.4(3) . . ? C6 N2 Li1 104.3(3) . . ? C6 N2 Sn1 110.5(2) . . ? Li1 N2 Sn1 115.8(2) . . ? C6 N2 Sn1 110.3(2) . 3_665 ? Li1 N2 Sn1 120.9(2) . 3_665 ? Sn1 N2 Sn1 94.90(11) . 3_665 ? N1 C1 C2 125.4(4) . . ? N1 C1 C6 115.6(3) . . ? C2 C1 C6 119.1(4) . . ? C3 C2 C1 121.4(4) . . ? C4 C3 C2 120.3(4) . . ? C3 C4 C5 119.6(4) . . ? C6 C5 C4 122.2(4) . . ? C5 C6 N2 123.4(4) . . ? C5 C6 C1 117.5(4) . . ? N2 C6 C1 119.2(3) . . ? C5 C6 Li1 87.0(3) . . ? N2 C6 Li1 45.6(2) . . ? C1 C6 Li1 141.9(3) . . ? N2 Li1 N4 127.9(3) . . ? N2 Li1 N3' 117.8(4) . . ? N4 Li1 N3' 75.8(5) . . ? N2 Li1 N4' 120.8(5) . . ? N4 Li1 N4' 8.1(5) . . ? N3' Li1 N4' 82.5(6) . . ? N2 Li1 N5 123.5(3) . . ? N4 Li1 N5 85.9(3) . . ? N3' Li1 N5 113.3(5) . . ? N4' Li1 N5 87.4(5) . . ? N2 Li1 N3 110.1(3) . . ? N4 Li1 N3 86.8(3) . . ? N3' Li1 N3 11.1(4) . . ? N4' Li1 N3 93.4(5) . . ? N5 Li1 N3 116.2(3) . . ? N2 Li1 N5' 122.0(5) . . ? N4 Li1 N5' 82.6(5) . . ? N3' Li1 N5' 117.0(6) . . ? N4' Li1 N5' 83.4(6) . . ? N5 Li1 N5' 6.0(5) . . ? N3 Li1 N5' 120.8(5) . . ? N2 Li1 C6 30.17(15) . . ? N4 Li1 C6 153.5(3) . . ? N3' Li1 C6 101.6(4) . . ? N4' Li1 C6 148.4(5) . . ? N5 Li1 C6 118.3(3) . . ? N3 Li1 C6 91.2(3) . . ? N5' Li1 C6 120.4(5) . . ? C9 N3 C8 111.4(6) . . ? C9 N3 C7 109.5(5) . . ? C8 N3 C7 109.0(6) . . ? C9 N3 Li1 100.3(4) . . ? C8 N3 Li1 110.8(5) . . ? C7 N3 Li1 115.6(4) . . ? C10 N4 C11 110.7(5) . . ? C10 N4 C12 113.3(6) . . ? C11 N4 C12 110.2(6) . . ? C10 N4 Li1 103.7(4) . . ? C11 N4 Li1 113.9(4) . . ? C12 N4 Li1 104.7(5) . . ? C13 N5 C15 109.3(5) . . ? C13 N5 C14 109.6(6) . . ? C15 N5 C14 107.6(5) . . ? C13 N5 Li1 103.0(4) . . ? C15 N5 Li1 124.5(5) . . ? C14 N5 Li1 102.1(4) . . ? N3 C9 C10 112.4(5) . . ? N4 C10 C9 111.5(5) . . ? N4 C12 C13 111.8(6) . . ? N5 C13 C12 113.2(5) . . ? C9' N3' C7' 116.8(15) . . ? C9' N3' C8' 113.7(18) . . ? C7' N3' C8' 101.8(17) . . ? C9' N3' Li1 105.8(10) . . ? C7' N3' Li1 106.9(10) . . ? C8' N3' Li1 111.9(15) . . ? C12' N4' C10' 106.3(17) . . ? C12' N4' C11' 112.3(17) . . ? C10' N4' C11' 107.9(15) . . ? C12' N4' Li1 105.6(13) . . ? C10' N4' Li1 106.1(11) . . ? C11' N4' Li1 117.8(12) . . ? C13' N5' C14' 112.0(15) . . ? C13' N5' C15' 110.5(15) . . ? C14' N5' C15' 109.3(15) . . ? C13' N5' Li1 102.0(10) . . ? C14' N5' Li1 111.0(11) . . ? C15' N5' Li1 111.9(12) . . ? C10' C9' N3' 114.1(14) . . ? C9' C10' N4' 112.5(16) . . ? N4' C12' C13' 106.8(18) . . ? N5' C13' C12' 112.0(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.447 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.087 # Attachment '- dw1048.cif' data_dw1048 _database_code_depnum_ccdc_archive 'CCDC 796655' #TrackingRef '- dw1048.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 N4 1+, C12 H10 N4, 7(H2 O), Cl 1-' _chemical_formula_sum 'C24 H35 Cl N8 O7' _chemical_formula_weight 583.05 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 7.0826(2) _cell_length_b 12.5439(4) _cell_length_c 16.0868(6) _cell_angle_alpha 82.669(1) _cell_angle_beta 78.708(2) _cell_angle_gamma 84.163(2) _cell_volume 1385.75(8) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10043 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 1.002 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 14267 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6208 _reflns_number_gt 4150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1219P)^2^+1.8119P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6208 _refine_ls_number_parameters 404 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2071 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.20155(17) 1.05951(9) 0.83555(7) 0.0570(3) Uani 1 1 d . . . N1 N -0.1995(4) 1.1427(2) 0.43778(16) 0.0278(6) Uani 1 1 d . . . C1 C -0.1143(4) 0.8602(3) 0.39901(19) 0.0272(7) Uani 1 1 d . . . N2 N -0.3719(4) 1.0440(2) 0.59617(16) 0.0267(6) Uani 1 1 d . . . H2N H -0.4272 1.0133 0.6460 0.032 Uiso 1 1 calc R . . C2 C -0.1147(4) 0.9708(3) 0.38696(19) 0.0277(7) Uani 1 1 d . . . H2 H -0.0549 1.0045 0.3333 0.033 Uiso 1 1 calc R . . N3 N -0.2024(4) 0.6991(2) 0.49471(18) 0.0331(6) Uani 1 1 d . . . H3A H -0.2552 0.6668 0.5444 0.040 Uiso 1 1 calc R . . H3B H -0.1477 0.6606 0.4531 0.040 Uiso 1 1 calc R . . C3 C -0.2008(4) 1.0355(3) 0.45148(19) 0.0260(6) Uani 1 1 d . . . N4 N -0.0338(4) 0.7992(2) 0.33589(17) 0.0341(6) Uani 1 1 d . . . H4A H 0.0198 0.8301 0.2858 0.041 Uiso 1 1 calc R . . H4B H -0.0350 0.7285 0.3449 0.041 Uiso 1 1 calc R . . C4 C -0.2812(4) 1.2033(2) 0.50188(19) 0.0262(6) Uani 1 1 d . . . C5 C -0.2804(5) 1.3164(3) 0.4887(2) 0.0329(7) Uani 1 1 d . . . H5 H -0.2222 1.3505 0.4350 0.040 Uiso 1 1 calc R . . C6 C -0.3632(5) 1.3771(3) 0.5530(2) 0.0341(7) Uani 1 1 d . . . H6 H -0.3616 1.4533 0.5437 0.041 Uiso 1 1 calc R . . C7 C -0.4510(5) 1.3279(3) 0.6332(2) 0.0343(7) Uani 1 1 d . . . H7 H -0.5095 1.3712 0.6770 0.041 Uiso 1 1 calc R . . C8 C -0.4525(4) 1.2179(3) 0.6480(2) 0.0310(7) Uani 1 1 d . . . H8 H -0.5098 1.1851 0.7024 0.037 Uiso 1 1 calc R . . C9 C -0.3687(4) 1.1530(3) 0.58231(19) 0.0261(6) Uani 1 1 d . . . C10 C -0.2913(4) 0.9837(3) 0.53437(19) 0.0252(6) Uani 1 1 d . . . C11 C -0.2900(4) 0.8704(2) 0.54618(19) 0.0269(6) Uani 1 1 d . . . H11 H -0.3490 0.8362 0.5997 0.032 Uiso 1 1 calc R . . C12 C -0.2054(4) 0.8076(2) 0.4823(2) 0.0267(6) Uani 1 1 d . . . N1' N -0.2246(3) 0.5480(2) 1.09965(16) 0.0266(6) Uani 1 1 d . . . C1' C -0.2307(4) 0.3170(3) 0.9837(2) 0.0269(6) Uani 1 1 d . . . N2' N -0.2879(4) 0.6527(2) 0.94186(17) 0.0297(6) Uani 1 1 d . . . C2' C -0.2189(4) 0.3769(3) 1.0481(2) 0.0284(7) Uani 1 1 d . . . H2' H -0.1992 0.3407 1.1017 0.034 Uiso 1 1 calc R . . N3' N -0.2691(4) 0.3126(2) 0.83719(18) 0.0374(7) Uani 1 1 d . . . H3'A H -0.2868 0.3451 0.7872 0.045 Uiso 1 1 calc R . . H3'B H -0.2576 0.2417 0.8458 0.045 Uiso 1 1 calc R . . C3' C -0.2355(4) 0.4907(2) 1.03672(19) 0.0251(6) Uani 1 1 d . . . N4' N -0.2163(4) 0.2076(2) 0.99507(18) 0.0338(6) Uani 1 1 d . . . H4'A H -0.1991 0.1733 1.0446 0.041 Uiso 1 1 calc R . . H4'B H -0.2243 0.1709 0.9529 0.041 Uiso 1 1 calc R . . C4' C -0.2410(4) 0.6584(2) 1.08606(19) 0.0263(6) Uani 1 1 d . . . C5' C -0.2228(4) 0.7202(3) 1.1503(2) 0.0306(7) Uani 1 1 d . . . H5' H -0.1970 0.6857 1.2034 0.037 Uiso 1 1 calc R . . C6' C -0.2421(5) 0.8305(3) 1.1362(2) 0.0345(7) Uani 1 1 d . . . H6' H -0.2289 0.8722 1.1798 0.041 Uiso 1 1 calc R . . C7' C -0.2816(5) 0.8830(3) 1.0575(2) 0.0383(8) Uani 1 1 d . . . H7' H -0.2977 0.9594 1.0492 0.046 Uiso 1 1 calc R . . C8' C -0.2966(5) 0.8248(3) 0.9936(2) 0.0348(8) Uani 1 1 d . . . H8' H -0.3214 0.8607 0.9407 0.042 Uiso 1 1 calc R . . C9' C -0.2751(4) 0.7102(3) 1.0062(2) 0.0281(7) Uani 1 1 d . . . C10' C -0.2660(4) 0.5446(2) 0.95436(19) 0.0261(6) Uani 1 1 d . . . C11' C -0.2771(5) 0.4828(3) 0.8894(2) 0.0309(7) Uani 1 1 d . . . H11' H -0.2974 0.5185 0.8357 0.037 Uiso 1 1 calc R . . C12' C -0.2596(4) 0.3716(3) 0.9008(2) 0.0282(7) Uani 1 1 d . . . O10W O 0.1480(4) 0.8990(2) 0.83582(16) 0.0413(6) Uani 1 1 d D . . H11W H 0.044(6) 0.954(4) 0.853(4) 0.116(6) Uiso 1 1 d D . . H12W H 0.109(8) 0.845(4) 0.805(4) 0.116(6) Uiso 1 1 d D . . O20W O -0.4818(4) 0.95039(19) 0.76355(16) 0.0416(6) Uani 1 1 d D . . H22W H -0.406(6) 1.007(4) 0.773(4) 0.116(6) Uiso 1 1 d D . . H21W H -0.619(3) 0.960(4) 0.789(4) 0.116(6) Uiso 1 1 d D . . O30W O 0.0021(3) 0.55301(17) 0.35078(15) 0.0313(5) Uani 1 1 d D . . H31W H -0.096(6) 0.532(5) 0.327(4) 0.116(6) Uiso 1 1 d D . . H32W H 0.130(4) 0.521(5) 0.338(4) 0.116(6) Uiso 1 1 d D . . O40W O -0.3631(3) 0.58839(17) 0.67226(13) 0.0267(5) Uani 1 1 d D . . H41W H -0.350(8) 0.645(4) 0.705(4) 0.116(6) Uiso 1 1 d D . . H42W H -0.489(4) 0.569(5) 0.674(4) 0.116(6) Uiso 1 1 d D . . O50W O -0.2392(4) 0.45047(19) 1.26768(15) 0.0396(6) Uani 1 1 d D . . H51W H -0.167(9) 0.378(3) 1.270(3) 0.116(6) Uiso 1 1 d D . . H52W H -0.218(9) 0.484(4) 1.2071(18) 0.116(6) Uiso 1 1 d D . . O60W O 0.0764(4) 0.75904(19) 0.72678(15) 0.0380(6) Uani 1 1 d D . . H61W H -0.061(4) 0.744(5) 0.738(3) 0.116(6) Uiso 1 1 d D . . H62W H 0.118(8) 0.786(5) 0.6654(17) 0.116(6) Uiso 1 1 d D . . O70W O -0.3127(4) 0.74311(19) 0.77693(15) 0.0379(6) Uani 1 1 d D . . H71W H -0.381(9) 0.817(3) 0.778(3) 0.116(6) Uiso 1 1 d D . . H72W H -0.298(9) 0.712(4) 0.8350(19) 0.116(6) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0622(7) 0.0506(6) 0.0564(7) -0.0059(5) -0.0067(5) -0.0052(5) N1 0.0267(13) 0.0295(14) 0.0266(13) 0.0011(11) -0.0046(10) -0.0059(10) C1 0.0227(14) 0.0347(17) 0.0249(15) -0.0023(13) -0.0058(12) -0.0048(12) N2 0.0237(12) 0.0321(14) 0.0225(12) 0.0004(10) -0.0012(10) -0.0040(10) C2 0.0266(15) 0.0322(16) 0.0230(15) 0.0009(12) -0.0019(12) -0.0065(12) N3 0.0392(15) 0.0278(14) 0.0304(15) -0.0018(11) -0.0020(12) -0.0038(11) C3 0.0217(14) 0.0324(16) 0.0237(15) 0.0012(12) -0.0048(11) -0.0055(12) N4 0.0397(15) 0.0344(15) 0.0263(14) -0.0041(11) -0.0003(11) -0.0040(12) C4 0.0245(14) 0.0301(16) 0.0249(15) -0.0023(12) -0.0057(12) -0.0047(12) C5 0.0357(17) 0.0333(17) 0.0299(17) 0.0000(13) -0.0065(13) -0.0064(14) C6 0.0360(17) 0.0295(17) 0.0382(19) -0.0016(14) -0.0104(14) -0.0047(13) C7 0.0324(17) 0.0350(18) 0.0365(18) -0.0101(14) -0.0062(14) -0.0006(14) C8 0.0275(16) 0.0354(18) 0.0287(16) -0.0035(13) -0.0020(12) -0.0018(13) C9 0.0199(14) 0.0310(16) 0.0269(15) -0.0016(12) -0.0037(11) -0.0020(11) C10 0.0191(13) 0.0341(16) 0.0219(15) -0.0002(12) -0.0036(11) -0.0035(11) C11 0.0247(14) 0.0299(16) 0.0248(15) 0.0029(12) -0.0034(11) -0.0056(12) C12 0.0235(14) 0.0299(16) 0.0268(15) 0.0010(12) -0.0061(12) -0.0049(12) N1' 0.0226(12) 0.0299(14) 0.0253(13) -0.0011(11) -0.0008(10) -0.0026(10) C1' 0.0221(14) 0.0295(16) 0.0269(16) 0.0006(12) -0.0019(11) -0.0015(11) N2' 0.0263(13) 0.0338(15) 0.0276(14) 0.0010(11) -0.0051(10) -0.0003(11) C2' 0.0271(15) 0.0293(16) 0.0264(16) 0.0029(12) -0.0032(12) -0.0018(12) N3' 0.0453(17) 0.0381(16) 0.0298(15) -0.0032(12) -0.0103(12) -0.0017(13) C3' 0.0193(13) 0.0313(16) 0.0226(15) 0.0006(12) -0.0014(11) -0.0014(11) N4' 0.0422(16) 0.0314(15) 0.0278(14) -0.0016(11) -0.0066(12) -0.0043(12) C4' 0.0196(14) 0.0288(16) 0.0272(15) -0.0011(12) 0.0020(11) -0.0008(11) C5' 0.0280(15) 0.0370(18) 0.0256(16) -0.0020(13) -0.0013(12) -0.0060(13) C6' 0.0325(17) 0.0347(18) 0.0350(18) -0.0091(14) 0.0018(14) -0.0064(14) C7' 0.0378(18) 0.0288(17) 0.045(2) -0.0027(15) 0.0010(15) -0.0041(14) C8' 0.0327(17) 0.0336(18) 0.0350(18) 0.0016(14) -0.0030(14) -0.0013(13) C9' 0.0232(14) 0.0308(16) 0.0274(16) 0.0002(13) -0.0005(12) -0.0013(12) C10' 0.0204(14) 0.0311(16) 0.0246(15) 0.0016(12) -0.0024(11) -0.0015(11) C11' 0.0307(16) 0.0365(18) 0.0239(15) 0.0024(13) -0.0059(12) 0.0003(13) C12' 0.0219(14) 0.0363(17) 0.0253(15) -0.0036(13) -0.0028(12) -0.0005(12) O10W 0.0504(15) 0.0401(14) 0.0328(13) -0.0043(11) -0.0041(11) -0.0070(11) O20W 0.0469(15) 0.0336(13) 0.0356(14) 0.0040(11) 0.0062(11) 0.0017(11) O30W 0.0431(13) 0.0214(11) 0.0349(13) -0.0070(9) -0.0168(10) -0.0051(9) O40W 0.0313(11) 0.0318(12) 0.0189(10) -0.0079(8) -0.0028(8) -0.0085(9) O50W 0.0541(15) 0.0322(13) 0.0302(12) 0.0026(10) -0.0074(11) -0.0002(11) O60W 0.0440(14) 0.0363(13) 0.0293(12) 0.0018(10) 0.0012(10) -0.0053(11) O70W 0.0467(14) 0.0335(13) 0.0321(13) 0.0038(10) -0.0085(11) -0.0030(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C3 1.336(4) . ? N1 C4 1.361(4) . ? C1 N4 1.351(4) . ? C1 C2 1.376(4) . ? C1 C12 1.473(4) . ? N2 C10 1.329(4) . ? N2 C9 1.359(4) . ? N2 H2N 0.8800 . ? C2 C3 1.405(4) . ? C2 H2 0.9500 . ? N3 C12 1.349(4) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? C3 C10 1.463(4) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? C4 C5 1.408(4) . ? C4 C9 1.419(4) . ? C5 C6 1.366(5) . ? C5 H5 0.9500 . ? C6 C7 1.411(5) . ? C6 H6 0.9500 . ? C7 C8 1.371(5) . ? C7 H7 0.9500 . ? C8 C9 1.416(4) . ? C8 H8 0.9500 . ? C10 C11 1.409(4) . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? N1' C3' 1.332(4) . ? N1' C4' 1.370(4) . ? C1' N4' 1.358(4) . ? C1' C2' 1.374(5) . ? C1' C12' 1.461(4) . ? N2' C10' 1.342(4) . ? N2' C9' 1.357(4) . ? C2' C3' 1.412(4) . ? C2' H2' 0.9500 . ? N3' C12' 1.353(4) . ? N3' H3'A 0.8800 . ? N3' H3'B 0.8800 . ? C3' C10' 1.454(4) . ? N4' H4'A 0.8800 . ? N4' H4'B 0.8800 . ? C4' C5' 1.401(5) . ? C4' C9' 1.417(4) . ? C5' C6' 1.370(5) . ? C5' H5' 0.9500 . ? C6' C7' 1.416(5) . ? C6' H6' 0.9500 . ? C7' C8' 1.359(5) . ? C7' H7' 0.9500 . ? C8' C9' 1.423(5) . ? C8' H8' 0.9500 . ? C10' C11' 1.397(5) . ? C11' C12' 1.380(5) . ? C11' H11' 0.9500 . ? O10W H11W 0.981(19) . ? O10W H12W 0.978(19) . ? O20W H22W 0.978(14) . ? O20W H21W 0.979(14) . ? O30W H31W 0.937(19) . ? O30W H32W 0.950(19) . ? O40W H41W 0.961(19) . ? O40W H42W 0.939(19) . ? O50W H51W 0.999(19) . ? O50W H52W 0.999(19) . ? O60W H61W 0.99(2) . ? O60W H62W 0.999(19) . ? O70W H71W 1.005(19) . ? O70W H72W 0.985(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 N1 C4 119.4(3) . . ? N4 C1 C2 121.4(3) . . ? N4 C1 C12 119.5(3) . . ? C2 C1 C12 119.1(3) . . ? C10 N2 C9 120.0(3) . . ? C10 N2 H2N 120.0 . . ? C9 N2 H2N 120.0 . . ? C1 C2 C3 122.1(3) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C12 N3 H3A 120.0 . . ? C12 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N1 C3 C2 120.7(3) . . ? N1 C3 C10 120.2(3) . . ? C2 C3 C10 119.1(3) . . ? C1 N4 H4A 120.0 . . ? C1 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? N1 C4 C5 120.2(3) . . ? N1 C4 C9 120.3(3) . . ? C5 C4 C9 119.5(3) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.8(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? N2 C9 C8 120.4(3) . . ? N2 C9 C4 120.4(3) . . ? C8 C9 C4 119.2(3) . . ? N2 C10 C11 121.9(3) . . ? N2 C10 C3 119.6(3) . . ? C11 C10 C3 118.5(3) . . ? C12 C11 C10 122.0(3) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? N3 C12 C11 121.5(3) . . ? N3 C12 C1 119.2(3) . . ? C11 C12 C1 119.3(3) . . ? C3' N1' C4' 119.5(3) . . ? N4' C1' C2' 121.6(3) . . ? N4' C1' C12' 118.7(3) . . ? C2' C1' C12' 119.7(3) . . ? C10' N2' C9' 119.0(3) . . ? C1' C2' C3' 121.7(3) . . ? C1' C2' H2' 119.2 . . ? C3' C2' H2' 119.2 . . ? C12' N3' H3'A 120.0 . . ? C12' N3' H3'B 120.0 . . ? H3'A N3' H3'B 120.0 . . ? N1' C3' C2' 121.2(3) . . ? N1' C3' C10' 120.4(3) . . ? C2' C3' C10' 118.4(3) . . ? C1' N4' H4'A 120.0 . . ? C1' N4' H4'B 120.0 . . ? H4'A N4' H4'B 120.0 . . ? N1' C4' C5' 120.5(3) . . ? N1' C4' C9' 119.7(3) . . ? C5' C4' C9' 119.8(3) . . ? C6' C5' C4' 119.9(3) . . ? C6' C5' H5' 120.0 . . ? C4' C5' H5' 120.0 . . ? C5' C6' C7' 120.6(3) . . ? C5' C6' H6' 119.7 . . ? C7' C6' H6' 119.7 . . ? C8' C7' C6' 120.6(3) . . ? C8' C7' H7' 119.7 . . ? C6' C7' H7' 119.7 . . ? C7' C8' C9' 119.9(3) . . ? C7' C8' H8' 120.1 . . ? C9' C8' H8' 120.1 . . ? N2' C9' C4' 121.3(3) . . ? N2' C9' C8' 119.6(3) . . ? C4' C9' C8' 119.1(3) . . ? N2' C10' C11' 120.5(3) . . ? N2' C10' C3' 120.1(3) . . ? C11' C10' C3' 119.4(3) . . ? C12' C11' C10' 121.9(3) . . ? C12' C11' H11' 119.0 . . ? C10' C11' H11' 119.0 . . ? N3' C12' C11' 121.5(3) . . ? N3' C12' C1' 119.6(3) . . ? C11' C12' C1' 118.9(3) . . ? H11W O10W H12W 113(3) . . ? H22W O20W H21W 114(2) . . ? H31W O30W H32W 121(3) . . ? H41W O40W H42W 117(3) . . ? H51W O50W H52W 108(3) . . ? H61W O60W H62W 110(3) . . ? H71W O70W H72W 111(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.526 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.082