# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2193 data_dw0026 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 N4 O8 Sn4' _chemical_formula_weight 1079.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c 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 14.0750(4) _cell_length_b 24.3080(10) _cell_length_c 12.3940(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.651(2) _cell_angle_gamma 90.00 _cell_volume 4137.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 18759 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 2.433 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12426 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7131 _reflns_number_gt 5410 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_structure_solution 'SIR-92' _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^)+(0.1105P)^2^+113.0213P] 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 7131 _refine_ls_number_parameters 221 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.2835 _refine_ls_wR_factor_gt 0.2611 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 1.637 _refine_ls_shift/su_mean 0.101 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 0.33388(9) 0.25300(4) 0.65325(11) 0.0561(4) Uani 1 1 d . . . Sn2 Sn 0.46941(9) 0.27888(4) 0.46464(11) 0.0538(4) Uani 1 1 d . . . Sn3 Sn 0.37655(11) 0.38355(4) 0.58833(12) 0.0666(4) Uani 1 1 d . . . Sn4 Sn 0.23022(10) 0.30293(6) 0.40009(13) 0.0716(5) Uani 1 1 d . . . N1 N 0.2533(11) 0.3256(6) 0.5803(13) 0.066(4) Uani 1 1 d . . . N2 N 0.3664(11) 0.3484(5) 0.4202(12) 0.060(4) Uani 1 1 d . . . N3 N 0.4567(10) 0.3060(5) 0.6322(12) 0.055(4) Uani 1 1 d . . . N4 N 0.3321(10) 0.2378(5) 0.4768(12) 0.051(3) Uani 1 1 d . . . O1 O -0.0771(19) 0.4302(12) 0.669(2) 0.0857(17) Uiso 0.50 1 d PD A 1 O2 O 0.200(2) 0.4290(11) 0.504(2) 0.0857(17) Uiso 0.50 1 d PD A 1 C1 C 0.1726(15) 0.3526(10) 0.612(2) 0.0691(12) Uiso 0.50 1 d PG A 1 C2 C 0.1186(18) 0.3253(8) 0.677(2) 0.0691(12) Uiso 0.50 1 d PG A 1 H2 H 0.1393 0.2904 0.7075 0.083 Uiso 0.50 1 calc PR A 1 C3 C 0.0345(17) 0.3492(10) 0.697(2) 0.0691(12) Uiso 0.50 1 d PG A 1 H3 H -0.0024 0.3305 0.7415 0.083 Uiso 0.50 1 calc PR A 1 C4 C 0.0043(15) 0.4004(10) 0.652(2) 0.0691(12) Uiso 0.50 1 d PGD A 1 C5 C 0.0582(18) 0.4277(8) 0.587(2) 0.0691(12) Uiso 0.50 1 d PG A 1 H5 H 0.0376 0.4627 0.5569 0.083 Uiso 0.50 1 calc PR A 1 C6 C 0.1424(17) 0.4038(10) 0.567(2) 0.0691(12) Uiso 0.50 1 d PGD A 1 C7 C -0.126(3) 0.407(2) 0.745(4) 0.104(3) Uiso 0.50 1 d PD A 1 H7A H -0.1302 0.3667 0.7334 0.156 Uiso 0.50 1 calc PR A 1 H7B H -0.1920 0.4219 0.7330 0.156 Uiso 0.50 1 calc PR A 1 H7C H -0.0907 0.4146 0.8203 0.156 Uiso 0.50 1 calc PR A 1 C8 C 0.173(4) 0.4836(14) 0.469(4) 0.104(3) Uiso 0.50 1 d PD A 1 H8A H 0.1191 0.4825 0.4037 0.156 Uiso 0.50 1 calc PR A 1 H8B H 0.2291 0.5020 0.4493 0.156 Uiso 0.50 1 calc PR A 1 H8C H 0.1532 0.5038 0.5283 0.156 Uiso 0.50 1 calc PR A 1 O1' O -0.1110(18) 0.4001(12) 0.642(2) 0.0857(17) Uiso 0.50 1 d PD A 2 O2' O 0.163(2) 0.4090(11) 0.472(2) 0.0857(17) Uiso 0.50 1 d PD A 2 C1' C 0.1546(14) 0.3388(10) 0.598(2) 0.0691(12) Uiso 0.50 1 d PG A 2 C2' C 0.1100(18) 0.3088(8) 0.668(2) 0.0691(12) Uiso 0.50 1 d PG A 2 H2' H 0.1408 0.2769 0.7041 0.083 Uiso 0.50 1 calc PR A 2 C3' C 0.0205(18) 0.3256(10) 0.687(2) 0.0691(12) Uiso 0.50 1 d PG A 2 H3' H -0.0099 0.3052 0.7351 0.083 Uiso 0.50 1 calc PR A 2 C4' C -0.0244(14) 0.3724(10) 0.634(2) 0.0691(12) Uiso 0.50 1 d PGD A 2 C5' C 0.0201(17) 0.4023(9) 0.564(2) 0.0691(12) Uiso 0.50 1 d PG A 2 H5' H -0.0106 0.4343 0.5279 0.083 Uiso 0.50 1 calc PR A 2 C6' C 0.1096(17) 0.3855(10) 0.545(2) 0.0691(12) Uiso 0.50 1 d PGD A 2 C7' C -0.157(3) 0.376(2) 0.721(4) 0.104(3) Uiso 0.50 1 d PD A 2 H7'1 H -0.1660 0.3366 0.7066 0.156 Uiso 0.50 1 calc PR A 2 H7'2 H -0.2209 0.3934 0.7163 0.156 Uiso 0.50 1 calc PR A 2 H7'3 H -0.1168 0.3817 0.7955 0.156 Uiso 0.50 1 calc PR A 2 C8' C 0.138(4) 0.4634(14) 0.437(4) 0.104(3) Uiso 0.50 1 d PD A 2 H8'1 H 0.0675 0.4655 0.4055 0.156 Uiso 0.50 1 calc PR A 2 H8'2 H 0.1736 0.4740 0.3810 0.156 Uiso 0.50 1 calc PR A 2 H8'3 H 0.1544 0.4884 0.5005 0.156 Uiso 0.50 1 calc PR A 2 O3 O 0.4619(10) 0.5190(6) 0.1568(12) 0.0857(17) Uiso 1 1 d D A . O4 O 0.5363(10) 0.4036(6) 0.4755(11) 0.0857(17) Uiso 1 1 d D A . C9 C 0.3880(15) 0.3906(8) 0.3483(16) 0.0691(12) Uiso 1 1 d . A . C10 C 0.3247(15) 0.4029(8) 0.2463(16) 0.0691(12) Uiso 1 1 d . . . H10 H 0.2666 0.3822 0.2217 0.083 Uiso 1 1 calc R A . C11 C 0.3489(14) 0.4465(8) 0.1806(16) 0.0691(12) Uiso 1 1 d . A . H11 H 0.3069 0.4551 0.1117 0.083 Uiso 1 1 calc R . . C12 C 0.4295(14) 0.4750(7) 0.2152(14) 0.0691(12) Uiso 1 1 d D . . C13 C 0.4965(15) 0.4627(8) 0.3137(16) 0.0691(12) Uiso 1 1 d . A . H13 H 0.5551 0.4831 0.3357 0.083 Uiso 1 1 calc R . . C14 C 0.4747(13) 0.4200(8) 0.3780(14) 0.0691(12) Uiso 1 1 d D . . C15 C 0.4032(18) 0.5290(11) 0.0508(15) 0.104(3) Uiso 1 1 d D . . H15A H 0.3935 0.4945 0.0088 0.156 Uiso 1 1 calc R A . H15B H 0.4354 0.5558 0.0119 0.156 Uiso 1 1 calc R . . H15C H 0.3400 0.5435 0.0582 0.156 Uiso 1 1 calc R . . C16 C 0.6232(14) 0.4335(10) 0.513(2) 0.104(3) Uiso 1 1 d D . . H16A H 0.6603 0.4344 0.4548 0.156 Uiso 1 1 calc R A . H16B H 0.6621 0.4156 0.5790 0.156 Uiso 1 1 calc R . . H16C H 0.6074 0.4711 0.5314 0.156 Uiso 1 1 calc R . . O5 O 0.7953(18) 0.2724(11) 0.967(2) 0.0857(17) Uiso 0.50 1 d PD A 1 O6 O 0.541(3) 0.2070(14) 0.662(4) 0.0857(17) Uiso 0.50 1 d PD A 1 C17 C 0.549(2) 0.3006(14) 0.715(3) 0.0691(12) Uiso 0.50 1 d PG A 1 C18 C 0.587(2) 0.3430(10) 0.786(2) 0.0691(12) Uiso 0.50 1 d PG A 1 H18 H 0.5590 0.3786 0.7764 0.083 Uiso 0.50 1 calc PR A 1 C19 C 0.6672(19) 0.3331(9) 0.8721(19) 0.0691(12) Uiso 0.50 1 d PG A 1 H19 H 0.6936 0.3621 0.9210 0.083 Uiso 0.50 1 calc PR A 1 C20 C 0.7085(16) 0.2810(10) 0.8864(18) 0.0691(12) Uiso 0.50 1 d PGD A 1 C21 C 0.670(2) 0.2386(8) 0.815(2) 0.0691(12) Uiso 0.50 1 d PG A 1 H21 H 0.6981 0.2030 0.8245 0.083 Uiso 0.50 1 calc PR A 1 C22 C 0.590(2) 0.2485(11) 0.729(3) 0.0691(12) Uiso 0.50 1 d PGD A 1 C23 C 0.798(3) 0.2217(16) 1.024(4) 0.104(3) Uiso 0.50 1 d PD A 1 H23A H 0.7357 0.2160 1.0457 0.156 Uiso 0.50 1 calc PR A 1 H23B H 0.8508 0.2224 1.0902 0.156 Uiso 0.50 1 calc PR A 1 H23C H 0.8088 0.1917 0.9754 0.156 Uiso 0.50 1 calc PR A 1 C24 C 0.578(5) 0.1532(14) 0.682(5) 0.104(3) Uiso 0.50 1 d PD A 1 H24A H 0.6466 0.1527 0.6775 0.156 Uiso 0.50 1 calc PR A 1 H24B H 0.5408 0.1283 0.6261 0.156 Uiso 0.50 1 calc PR A 1 H24C H 0.5721 0.1413 0.7556 0.156 Uiso 0.50 1 calc PR A 1 O5' O 0.8310(17) 0.2768(11) 0.895(2) 0.0857(17) Uiso 0.50 1 d PD A 2 O6' O 0.529(3) 0.2078(15) 0.649(4) 0.0857(17) Uiso 0.50 1 d PD A 2 C17' C 0.5456(17) 0.2989(14) 0.711(3) 0.0691(12) Uiso 0.50 1 d PG A 2 C18' C 0.6000(19) 0.3420(10) 0.767(2) 0.0691(12) Uiso 0.50 1 d PG A 2 H18' H 0.5731 0.3780 0.7632 0.083 Uiso 0.50 1 calc PR A 2 C19' C 0.6937(17) 0.3326(9) 0.828(2) 0.0691(12) Uiso 0.50 1 d PG A 2 H19' H 0.7309 0.3620 0.8663 0.083 Uiso 0.50 1 calc PR A 2 C20' C 0.7331(14) 0.2799(10) 0.834(2) 0.0691(12) Uiso 0.50 1 d PGD A 2 C21' C 0.679(2) 0.2368(8) 0.778(2) 0.0691(12) Uiso 0.50 1 d PG A 2 H21' H 0.7056 0.2008 0.7817 0.083 Uiso 0.50 1 calc PR A 2 C22' C 0.585(2) 0.2462(12) 0.717(3) 0.0691(12) Uiso 0.50 1 d PGD A 2 C23' C 0.877(3) 0.2253(16) 0.888(4) 0.104(3) Uiso 0.50 1 d PD A 2 H23D H 0.8383 0.1960 0.9122 0.156 Uiso 0.50 1 calc PR A 2 H23E H 0.9423 0.2257 0.9366 0.156 Uiso 0.50 1 calc PR A 2 H23F H 0.8821 0.2186 0.8120 0.156 Uiso 0.50 1 calc PR A 2 C24' C 0.570(5) 0.1538(14) 0.650(5) 0.104(3) Uiso 0.50 1 d PD A 2 H24D H 0.6216 0.1542 0.6075 0.156 Uiso 0.50 1 calc PR A 2 H24E H 0.5194 0.1277 0.6161 0.156 Uiso 0.50 1 calc PR A 2 H24F H 0.5983 0.1426 0.7261 0.156 Uiso 0.50 1 calc PR A 2 O7 O 0.2125(11) 0.0238(6) 0.3392(12) 0.0857(17) Uiso 1 1 d D A . O8 O 0.1663(11) 0.1980(6) 0.5045(12) 0.0857(17) Uiso 1 1 d D A . C25 C 0.3079(15) 0.1822(8) 0.4412(16) 0.0691(12) Uiso 1 1 d . A . C26 C 0.3645(15) 0.1489(8) 0.3924(16) 0.0691(12) Uiso 1 1 d . . . H26 H 0.4250 0.1627 0.3821 0.083 Uiso 1 1 calc R A . C27 C 0.3372(14) 0.0952(8) 0.3567(16) 0.0691(12) Uiso 1 1 d . A . H27 H 0.3781 0.0729 0.3230 0.083 Uiso 1 1 calc R . . C28 C 0.2503(14) 0.0761(7) 0.3720(15) 0.0691(12) Uiso 1 1 d D . . C29 C 0.1917(15) 0.1079(8) 0.4199(16) 0.0691(12) Uiso 1 1 d . A . H29 H 0.1315 0.0934 0.4298 0.083 Uiso 1 1 calc R . . C30 C 0.2172(13) 0.1600(8) 0.4538(16) 0.0691(12) Uiso 1 1 d D . . C31 C 0.2647(18) -0.0064(9) 0.272(2) 0.104(3) Uiso 1 1 d D . . H31A H 0.2696 0.0157 0.2072 0.156 Uiso 1 1 calc R A . H31B H 0.2301 -0.0407 0.2475 0.156 Uiso 1 1 calc R . . H31C H 0.3302 -0.0148 0.3149 0.156 Uiso 1 1 calc R . . C32 C 0.0786(15) 0.1783(11) 0.529(2) 0.104(3) Uiso 1 1 d D . . H32A H 0.0366 0.1637 0.4612 0.156 Uiso 1 1 calc R A . H32B H 0.0452 0.2085 0.5574 0.156 Uiso 1 1 calc R . . H32C H 0.0934 0.1491 0.5843 0.156 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 0.0569(7) 0.0363(6) 0.0859(9) 0.0051(5) 0.0390(7) 0.0066(5) Sn2 0.0600(7) 0.0302(5) 0.0816(8) 0.0078(5) 0.0383(6) 0.0085(5) Sn3 0.0899(10) 0.0310(6) 0.0899(9) 0.0088(6) 0.0439(8) 0.0215(6) Sn4 0.0603(8) 0.0678(9) 0.0932(10) 0.0085(7) 0.0310(7) 0.0207(7) N1 0.064(9) 0.053(8) 0.088(11) 0.015(8) 0.031(8) 0.041(7) N2 0.079(10) 0.032(7) 0.079(10) 0.019(6) 0.040(8) 0.016(7) N3 0.062(9) 0.024(6) 0.087(10) 0.004(6) 0.034(8) 0.007(6) N4 0.054(8) 0.036(7) 0.069(9) 0.008(6) 0.024(7) 0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.185(13) . ? Sn1 N4 2.213(14) . ? Sn1 N3 2.216(13) . ? Sn2 N4 2.209(13) . ? Sn2 N2 2.215(13) . ? Sn2 N3 2.223(14) . ? Sn3 N3 2.204(12) . ? Sn3 N1 2.220(17) . ? Sn3 N2 2.228(15) . ? Sn4 N2 2.179(15) . ? Sn4 N4 2.206(13) . ? Sn4 N1 2.254(16) . ? N1 C1 1.44(2) . ? N1 C1' 1.49(2) . ? N2 C9 1.44(2) . ? N3 C17' 1.42(2) . ? N3 C17 1.47(2) . ? N4 C25 1.44(2) . ? O1 C7 1.40(2) . ? O1 C4 1.411(18) . ? O2 C6 1.383(18) . ? O2 C8 1.421(19) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O1' C4' 1.412(18) . ? O1' C7' 1.42(2) . ? O2' C6' 1.412(18) . ? O2' C8' 1.414(19) . ? C1' C2' 1.3900 . ? C1' C6' 1.3900 . ? C2' C3' 1.3900 . ? C2' H2' 0.9500 . ? C3' C4' 1.3900 . ? C3' H3' 0.9500 . ? C4' C5' 1.3900 . ? C5' C6' 1.3900 . ? C5' H5' 0.9500 . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? O3 C15 1.411(16) . ? O3 C12 1.421(15) . ? O4 C14 1.383(15) . ? O4 C16 1.410(16) . ? C9 C14 1.39(3) . ? C9 C10 1.41(3) . ? C10 C11 1.42(3) . ? C10 H10 0.9500 . ? C11 C12 1.32(3) . ? C11 H11 0.9500 . ? C12 C13 1.40(3) . ? C13 C14 1.38(3) . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O5 C20 1.416(18) . ? O5 C23 1.416(19) . ? O6 C22 1.385(18) . ? O6 C24 1.41(2) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 H19 0.9500 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9801 . ? C24 H24B 0.9803 . ? C24 H24C 0.9803 . ? O5' C23' 1.422(19) . ? O5' C20' 1.422(18) . ? O6' C22' 1.378(18) . ? O6' C24' 1.43(2) . ? C17' C18' 1.3900 . ? C17' C22' 1.3900 . ? C18' C19' 1.3900 . ? C18' H18' 0.9500 . ? C19' C20' 1.3900 . ? C19' H19' 0.9500 . ? C20' C21' 1.3900 . ? C21' C22' 1.3900 . ? C21' H21' 0.9500 . ? C23' H23D 0.9802 . ? C23' H23E 0.9802 . ? C23' H23F 0.9802 . ? C24' H24D 0.9802 . ? C24' H24E 0.9801 . ? C24' H24F 0.9801 . ? O7 C28 1.404(15) . ? O7 C31 1.428(16) . ? O8 C30 1.400(15) . ? O8 C32 1.416(16) . ? C25 C26 1.37(3) . ? C25 C30 1.42(3) . ? C26 C27 1.41(3) . ? C26 H26 0.9500 . ? C27 C28 1.36(3) . ? C27 H27 0.9500 . ? C28 C29 1.36(3) . ? C29 C30 1.36(3) . ? C29 H29 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 N4 80.4(5) . . ? N1 Sn1 N3 80.2(5) . . ? N4 Sn1 N3 79.7(5) . . ? N4 Sn2 N2 80.0(5) . . ? N4 Sn2 N3 79.6(5) . . ? N2 Sn2 N3 79.9(5) . . ? N3 Sn3 N1 79.7(5) . . ? N3 Sn3 N2 80.0(5) . . ? N1 Sn3 N2 79.9(5) . . ? N2 Sn4 N4 80.9(5) . . ? N2 Sn4 N1 80.2(6) . . ? N4 Sn4 N1 79.0(5) . . ? C1 N1 C1' 17.0(16) . . ? C1 N1 Sn1 128.7(14) . . ? C1' N1 Sn1 122.1(13) . . ? C1 N1 Sn3 110.8(13) . . ? C1' N1 Sn3 127.1(13) . . ? Sn1 N1 Sn3 99.4(6) . . ? C1 N1 Sn4 115.6(14) . . ? C1' N1 Sn4 105.1(14) . . ? Sn1 N1 Sn4 99.3(5) . . ? Sn3 N1 Sn4 98.1(6) . . ? C9 N2 Sn4 126.3(12) . . ? C9 N2 Sn2 119.0(11) . . ? Sn4 N2 Sn2 98.8(5) . . ? C9 N2 Sn3 109.1(11) . . ? Sn4 N2 Sn3 100.1(5) . . ? Sn2 N2 Sn3 99.0(6) . . ? C17' N3 C17 2(2) . . ? C17' N3 Sn3 126.9(16) . . ? C17 N3 Sn3 125.0(15) . . ? C17' N3 Sn1 116.1(19) . . ? C17 N3 Sn1 117.3(18) . . ? Sn3 N3 Sn1 99.0(5) . . ? C17' N3 Sn2 111.7(18) . . ? C17 N3 Sn2 112.6(17) . . ? Sn3 N3 Sn2 99.5(6) . . ? Sn1 N3 Sn2 99.3(6) . . ? C25 N4 Sn4 117.0(11) . . ? C25 N4 Sn2 123.7(11) . . ? Sn4 N4 Sn2 98.2(5) . . ? C25 N4 Sn1 114.2(11) . . ? Sn4 N4 Sn1 99.9(5) . . ? Sn2 N4 Sn1 99.9(6) . . ? C7 O1 C4 115(2) . . ? C6 O2 C8 116(2) . . ? C2 C1 C6 120.0 . . ? C2 C1 N1 120.3(17) . . ? C6 C1 N1 119.3(17) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 O1 113.9(18) . . ? C3 C4 O1 126.0(18) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? O2 C6 C5 122.8(19) . . ? O2 C6 C1 117.2(19) . . ? C5 C6 C1 120.0 . . ? C4' O1' C7' 112.6(19) . . ? C6' O2' C8' 116(2) . . ? C2' C1' C6' 120.0 . . ? C2' C1' N1 123.0(17) . . ? C6' C1' N1 116.9(17) . . ? C3' C2' C1' 120.0 . . ? C3' C2' H2' 120.0 . . ? C1' C2' H2' 120.0 . . ? C4' C3' C2' 120.0 . . ? C4' C3' H3' 120.0 . . ? C2' C3' H3' 120.0 . . ? C3' C4' C5' 120.0 . . ? C3' C4' O1' 132.0(18) . . ? C5' C4' O1' 107.9(18) . . ? C6' C5' C4' 120.0 . . ? C6' C5' H5' 120.0 . . ? C4' C5' H5' 120.0 . . ? C5' C6' C1' 120.0 . . ? C5' C6' O2' 127.7(19) . . ? C1' C6' O2' 112.2(19) . . ? O1' C7' H7'1 109.6 . . ? O1' C7' H7'2 109.4 . . ? H7'1 C7' H7'2 109.5 . . ? O1' C7' H7'3 109.4 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? O2' C8' H8'1 109.5 . . ? O2' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? O2' C8' H8'3 109.4 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C15 O3 C12 114.6(14) . . ? C14 O4 C16 118.2(14) . . ? C14 C9 C10 118.4(18) . . ? C14 C9 N2 119.7(17) . . ? C10 C9 N2 121.9(18) . . ? C9 C10 C11 119.1(19) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 120.2(19) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 122.5(17) . . ? C11 C12 O3 125.3(16) . . ? C13 C12 O3 112.0(16) . . ? C14 C13 C12 118.0(18) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? O4 C14 C13 122.9(16) . . ? O4 C14 C9 115.4(17) . . ? C13 C14 C9 121.6(16) . . ? O3 C15 H15A 109.4 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 H16A 109.4 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 O5 C23 113.8(19) . . ? C22 O6 C24 117(2) . . ? C18 C17 C22 120.0 . . ? C18 C17 N3 123(2) . . ? C22 C17 N3 117(2) . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 O5 120(2) . . ? C21 C20 O5 120(2) . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? O6 C22 C21 123(2) . . ? O6 C22 C17 117(2) . . ? C21 C22 C17 120.0 . . ? C23' O5' C20' 114.5(19) . . ? C22' O6' C24' 116(2) . . ? C18' C17' C22' 120.0 . . ? C18' C17' N3 124(2) . . ? C22' C17' N3 115(2) . . ? C17' C18' C19' 120.0 . . ? C17' C18' H18' 120.0 . . ? C19' C18' H18' 120.0 . . ? C20' C19' C18' 120.0 . . ? C20' C19' H19' 120.0 . . ? C18' C19' H19' 120.0 . . ? C21' C20' C19' 120.0 . . ? C21' C20' O5' 126.1(19) . . ? C19' C20' O5' 113.8(19) . . ? C20' C21' C22' 120.0 . . ? C20' C21' H21' 120.0 . . ? C22' C21' H21' 120.0 . . ? O6' C22' C21' 124(2) . . ? O6' C22' C17' 115(2) . . ? C21' C22' C17' 120.0 . . ? O5' C23' H23D 109.5 . . ? O5' C23' H23E 109.4 . . ? H23D C23' H23E 109.5 . . ? O5' C23' H23F 109.5 . . ? H23D C23' H23F 109.4 . . ? H23E C23' H23F 109.4 . . ? O6' C24' H24D 113.0 . . ? O6' C24' H24E 106.5 . . ? H24D C24' H24E 109.6 . . ? O6' C24' H24F 108.8 . . ? H24D C24' H24F 109.4 . . ? H24E C24' H24F 109.4 . . ? C28 O7 C31 115.1(14) . . ? C30 O8 C32 115.3(14) . . ? C26 C25 C30 116.6(18) . . ? C26 C25 N4 124.7(18) . . ? C30 C25 N4 118.6(16) . . ? C25 C26 C27 123(2) . . ? C25 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C28 C27 C26 117.7(18) . . ? C28 C27 H27 121.2 . . ? C26 C27 H27 121.1 . . ? C27 C28 C29 121.2(17) . . ? C27 C28 O7 124.3(16) . . ? C29 C28 O7 114.5(17) . . ? C30 C29 C28 121.4(18) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 O8 128.9(17) . . ? C29 C30 C25 120.1(16) . . ? O8 C30 C25 111.0(16) . . ? O7 C31 H31A 109.5 . . ? O7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O8 C32 H32A 109.5 . . ? O8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 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 N4 Sn1 N1 C1 143(2) . . . . ? N3 Sn1 N1 C1 -136(2) . . . . ? N4 Sn1 N1 C1' 123.3(17) . . . . ? N3 Sn1 N1 C1' -155.6(17) . . . . ? N4 Sn1 N1 Sn3 -91.0(6) . . . . ? N3 Sn1 N1 Sn3 -9.9(5) . . . . ? N4 Sn1 N1 Sn4 8.9(5) . . . . ? N3 Sn1 N1 Sn4 90.0(6) . . . . ? N3 Sn3 N1 C1 147.8(15) . . . . ? N2 Sn3 N1 C1 -130.7(15) . . . . ? N3 Sn3 N1 C1' 153.2(18) . . . . ? N2 Sn3 N1 C1' -125.3(18) . . . . ? N3 Sn3 N1 Sn1 10.0(6) . . . . ? N2 Sn3 N1 Sn1 91.6(6) . . . . ? N3 Sn3 N1 Sn4 -90.9(5) . . . . ? N2 Sn3 N1 Sn4 -9.3(5) . . . . ? N2 Sn4 N1 C1 127.3(14) . . . . ? N4 Sn4 N1 C1 -150.2(15) . . . . ? N2 Sn4 N1 C1' 141.6(13) . . . . ? N4 Sn4 N1 C1' -135.9(13) . . . . ? N2 Sn4 N1 Sn1 -91.5(6) . . . . ? N4 Sn4 N1 Sn1 -9.0(5) . . . . ? N2 Sn4 N1 Sn3 9.5(4) . . . . ? N4 Sn4 N1 Sn3 92.0(5) . . . . ? N4 Sn4 N2 C9 147.2(14) . . . . ? N1 Sn4 N2 C9 -132.4(14) . . . . ? N4 Sn4 N2 Sn2 11.0(5) . . . . ? N1 Sn4 N2 Sn2 91.3(5) . . . . ? N4 Sn4 N2 Sn3 -89.9(5) . . . . ? N1 Sn4 N2 Sn3 -9.5(5) . . . . ? N4 Sn2 N2 C9 -151.4(14) . . . . ? N3 Sn2 N2 C9 127.5(14) . . . . ? N4 Sn2 N2 Sn4 -11.0(5) . . . . ? N3 Sn2 N2 Sn4 -92.1(6) . . . . ? N4 Sn2 N2 Sn3 90.9(6) . . . . ? N3 Sn2 N2 Sn3 9.8(5) . . . . ? N3 Sn3 N2 C9 -134.8(12) . . . . ? N1 Sn3 N2 C9 144.0(12) . . . . ? N3 Sn3 N2 Sn4 90.9(5) . . . . ? N1 Sn3 N2 Sn4 9.7(5) . . . . ? N3 Sn3 N2 Sn2 -9.8(5) . . . . ? N1 Sn3 N2 Sn2 -91.0(5) . . . . ? N1 Sn3 N3 C17' -142(2) . . . . ? N2 Sn3 N3 C17' 136(2) . . . . ? N1 Sn3 N3 C17 -142(2) . . . . ? N2 Sn3 N3 C17 136(2) . . . . ? N1 Sn3 N3 Sn1 -9.8(6) . . . . ? N2 Sn3 N3 Sn1 -91.3(6) . . . . ? N1 Sn3 N3 Sn2 91.3(6) . . . . ? N2 Sn3 N3 Sn2 9.8(5) . . . . ? N1 Sn1 N3 C17' 148.9(18) . . . . ? N4 Sn1 N3 C17' -129.2(18) . . . . ? N1 Sn1 N3 C17 147.2(18) . . . . ? N4 Sn1 N3 C17 -130.9(17) . . . . ? N1 Sn1 N3 Sn3 10.0(6) . . . . ? N4 Sn1 N3 Sn3 91.9(6) . . . . ? N1 Sn1 N3 Sn2 -91.2(6) . . . . ? N4 Sn1 N3 Sn2 -9.3(5) . . . . ? N4 Sn2 N3 C17' 132.4(18) . . . . ? N2 Sn2 N3 C17' -146.0(18) . . . . ? N4 Sn2 N3 C17 134.2(18) . . . . ? N2 Sn2 N3 C17 -144.2(18) . . . . ? N4 Sn2 N3 Sn3 -91.5(5) . . . . ? N2 Sn2 N3 Sn3 -9.9(5) . . . . ? N4 Sn2 N3 Sn1 9.4(5) . . . . ? N2 Sn2 N3 Sn1 90.9(6) . . . . ? N2 Sn4 N4 C25 -145.6(12) . . . . ? N1 Sn4 N4 C25 132.6(12) . . . . ? N2 Sn4 N4 Sn2 -11.0(5) . . . . ? N1 Sn4 N4 Sn2 -92.7(6) . . . . ? N2 Sn4 N4 Sn1 90.6(6) . . . . ? N1 Sn4 N4 Sn1 8.9(5) . . . . ? N2 Sn2 N4 C25 141.2(14) . . . . ? N3 Sn2 N4 C25 -137.4(14) . . . . ? N2 Sn2 N4 Sn4 10.8(5) . . . . ? N3 Sn2 N4 Sn4 92.2(5) . . . . ? N2 Sn2 N4 Sn1 -90.8(5) . . . . ? N3 Sn2 N4 Sn1 -9.4(5) . . . . ? N1 Sn1 N4 C25 -134.8(13) . . . . ? N3 Sn1 N4 C25 143.5(12) . . . . ? N1 Sn1 N4 Sn4 -9.1(6) . . . . ? N3 Sn1 N4 Sn4 -90.8(5) . . . . ? N1 Sn1 N4 Sn2 91.1(6) . . . . ? N3 Sn1 N4 Sn2 9.4(5) . . . . ? C1' N1 C1 C2 55(6) . . . . ? Sn1 N1 C1 C2 -18(3) . . . . ? Sn3 N1 C1 C2 -140.0(13) . . . . ? Sn4 N1 C1 C2 109.5(16) . . . . ? C1' N1 C1 C6 -118(7) . . . . ? Sn1 N1 C1 C6 168.9(13) . . . . ? Sn3 N1 C1 C6 47(2) . . . . ? Sn4 N1 C1 C6 -63(2) . . . . ? C6 C1 C2 C3 0.0 . . . . ? N1 C1 C2 C3 -173(2) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C2 C3 C4 O1 -177(3) . . . . ? C7 O1 C4 C5 -173(3) . . . . ? C7 O1 C4 C3 5(5) . . . . ? C3 C4 C5 C6 0.0 . . . . ? O1 C4 C5 C6 178(3) . . . . ? C8 O2 C6 C5 6(4) . . . . ? C8 O2 C6 C1 -174(3) . . . . ? C4 C5 C6 O2 -179(3) . . . . ? C4 C5 C6 C1 0.0 . . . . ? C2 C1 C6 O2 179(3) . . . . ? N1 C1 C6 O2 -8(3) . . . . ? C2 C1 C6 C5 0.0 . . . . ? N1 C1 C6 C5 173(2) . . . . ? C1 N1 C1' C2' -113(7) . . . . ? Sn1 N1 C1' C2' 6(2) . . . . ? Sn3 N1 C1' C2' -130.2(15) . . . . ? Sn4 N1 C1' C2' 117.0(15) . . . . ? C1 N1 C1' C6' 63(6) . . . . ? Sn1 N1 C1' C6' -178.8(12) . . . . ? Sn3 N1 C1' C6' 45(2) . . . . ? Sn4 N1 C1' C6' -67.3(16) . . . . ? C6' C1' C2' C3' 0.0 . . . . ? N1 C1' C2' C3' 175(2) . . . . ? C1' C2' C3' C4' 0.0 . . . . ? C2' C3' C4' C5' 0.0 . . . . ? C2' C3' C4' O1' -176(3) . . . . ? C7' O1' C4' C3' 3(5) . . . . ? C7' O1' C4' C5' -174(3) . . . . ? C3' C4' C5' C6' 0.0 . . . . ? O1' C4' C5' C6' 177(2) . . . . ? C4' C5' C6' C1' 0.0 . . . . ? C4' C5' C6' O2' 176(3) . . . . ? C2' C1' C6' C5' 0.0 . . . . ? N1 C1' C6' C5' -176(2) . . . . ? C2' C1' C6' O2' -177(3) . . . . ? N1 C1' C6' O2' 7(2) . . . . ? C8' O2' C6' C5' 19(5) . . . . ? C8' O2' C6' C1' -164(3) . . . . ? Sn4 N2 C9 C14 173.4(13) . . . . ? Sn2 N2 C9 C14 -58(2) . . . . ? Sn3 N2 C9 C14 54(2) . . . . ? Sn4 N2 C9 C10 -8(3) . . . . ? Sn2 N2 C9 C10 120.6(18) . . . . ? Sn3 N2 C9 C10 -127.1(17) . . . . ? C14 C9 C10 C11 -3(3) . . . . ? N2 C9 C10 C11 178.0(17) . . . . ? C9 C10 C11 C12 0(3) . . . . ? C10 C11 C12 C13 3(3) . . . . ? C10 C11 C12 O3 179.3(18) . . . . ? C15 O3 C12 C11 -4(3) . . . . ? C15 O3 C12 C13 172.8(19) . . . . ? C11 C12 C13 C14 -2(3) . . . . ? O3 C12 C13 C14 -178.9(17) . . . . ? C16 O4 C14 C13 3(3) . . . . ? C16 O4 C14 C9 -176.9(19) . . . . ? C12 C13 C14 O4 178.7(18) . . . . ? C12 C13 C14 C9 -2(3) . . . . ? C10 C9 C14 O4 -176.0(17) . . . . ? N2 C9 C14 O4 3(3) . . . . ? C10 C9 C14 C13 4(3) . . . . ? N2 C9 C14 C13 -177.0(17) . . . . ? C17' N3 C17 C18 -168(100) . . . . ? Sn3 N3 C17 C18 10(3) . . . . ? Sn1 N3 C17 C18 -115(2) . . . . ? Sn2 N3 C17 C18 130.8(19) . . . . ? C17' N3 C17 C22 3(99) . . . . ? Sn3 N3 C17 C22 -178.2(11) . . . . ? Sn1 N3 C17 C22 57(2) . . . . ? Sn2 N3 C17 C22 -58(2) . . . . ? C22 C17 C18 C19 0.0 . . . . ? N3 C17 C18 C19 171(4) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C18 C19 C20 O5 174(3) . . . . ? C23 O5 C20 C19 142(3) . . . . ? C23 O5 C20 C21 -45(4) . . . . ? C19 C20 C21 C22 0.0 . . . . ? O5 C20 C21 C22 -174(3) . . . . ? C24 O6 C22 C21 -2(8) . . . . ? C24 O6 C22 C17 -175(5) . . . . ? C20 C21 C22 O6 -172(4) . . . . ? C20 C21 C22 C17 0.0 . . . . ? C18 C17 C22 O6 173(4) . . . . ? N3 C17 C22 O6 1(3) . . . . ? C18 C17 C22 C21 0.0 . . . . ? N3 C17 C22 C21 -172(3) . . . . ? C17 N3 C17' C18' -4(98) . . . . ? Sn3 N3 C17' C18' -6(4) . . . . ? Sn1 N3 C17' C18' -131.4(19) . . . . ? Sn2 N3 C17' C18' 116(2) . . . . ? C17 N3 C17' C22' -174(100) . . . . ? Sn3 N3 C17' C22' -175.0(11) . . . . ? Sn1 N3 C17' C22' 59(2) . . . . ? Sn2 N3 C17' C22' -54(2) . . . . ? C22' C17' C18' C19' 0.0 . . . . ? N3 C17' C18' C19' -169(4) . . . . ? C17' C18' C19' C20' 0.0 . . . . ? C18' C19' C20' C21' 0.0 . . . . ? C18' C19' C20' O5' 177(3) . . . . ? C23' O5' C20' C21' 6(5) . . . . ? C23' O5' C20' C19' -171(3) . . . . ? C19' C20' C21' C22' 0.0 . . . . ? O5' C20' C21' C22' -177(3) . . . . ? C24' O6' C22' C21' 4(8) . . . . ? C24' O6' C22' C17' 177(5) . . . . ? C20' C21' C22' O6' 173(4) . . . . ? C20' C21' C22' C17' 0.0 . . . . ? C18' C17' C22' O6' -173(4) . . . . ? N3 C17' C22' O6' -4(3) . . . . ? C18' C17' C22' C21' 0.0 . . . . ? N3 C17' C22' C21' 170(3) . . . . ? Sn4 N4 C25 C26 119.7(18) . . . . ? Sn2 N4 C25 C26 -3(3) . . . . ? Sn1 N4 C25 C26 -124.2(18) . . . . ? Sn4 N4 C25 C30 -58(2) . . . . ? Sn2 N4 C25 C30 179.6(13) . . . . ? Sn1 N4 C25 C30 58(2) . . . . ? C30 C25 C26 C27 -1(3) . . . . ? N4 C25 C26 C27 -178.6(18) . . . . ? C25 C26 C27 C28 0(3) . . . . ? C26 C27 C28 C29 0(3) . . . . ? C26 C27 C28 O7 178.9(18) . . . . ? C31 O7 C28 C27 -9(3) . . . . ? C31 O7 C28 C29 169.6(19) . . . . ? C27 C28 C29 C30 0(3) . . . . ? O7 C28 C29 C30 -178.5(18) . . . . ? C28 C29 C30 O8 -179.8(19) . . . . ? C28 C29 C30 C25 -1(3) . . . . ? C32 O8 C30 C29 4(3) . . . . ? C32 O8 C30 C25 -175.2(18) . . . . ? C26 C25 C30 C29 1(3) . . . . ? N4 C25 C30 C29 179.2(17) . . . . ? C26 C25 C30 O8 -179.9(17) . . . . ? N4 C25 C30 O8 -2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.625 _refine_diff_density_min -1.549 _refine_diff_density_rms 0.266 data_dw0016 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H40 N8 O5 Sn4' _chemical_formula_weight 947.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.8644(3) _cell_length_b 12.4107(4) _cell_length_c 20.7486(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3055.14(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method ? _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.275 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.124 _exptl_absorpt_correction_T_max 0.917 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13472 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6836 _reflns_number_observed 6067 _reflns_observed_criterion >2sigma(I) _computing_data_collection maXus _computing_cell_refinement maXus _computing_data_reduction maXus _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+3.4543P] 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 ? _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 0.00(4) _refine_ls_number_reflns 6822 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_obs 0.0376 _refine_ls_wR_factor_all 0.1140 _refine_ls_wR_factor_obs 0.0778 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 1.438 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sn1 Sn 0.14567(4) 0.75984(4) 0.50070(2) 0.02409(10) Uani 1 d . . Sn2 Sn 0.38766(4) 0.80740(4) 0.58887(2) 0.02634(10) Uani 1 d . . Sn3 Sn 0.39067(4) 0.86457(3) 0.43419(2) 0.02571(10) Uani 1 d . . Sn4 Sn 0.21906(4) 1.01124(4) 0.53348(2) 0.02683(11) Uani 1 d . . N1 N 0.3330(4) 0.7325(4) 0.4976(3) 0.0270(12) Uani 1 d . . N11 N 0.3830(4) 0.6282(4) 0.4843(2) 0.0224(11) Uani 1 d . . C11 C 0.3474(6) 0.5488(5) 0.5330(3) 0.0312(15) Uani 1 d . . H11A H 0.2641(6) 0.5440(5) 0.5334(3) 0.037 Uiso 1 calc R . H11B H 0.3723(6) 0.5728(5) 0.5762(3) 0.037 Uiso 1 calc R . C12 C 0.3964(6) 0.4394(5) 0.5188(4) 0.037(2) Uani 1 d . . H12A H 0.4797(6) 0.4433(5) 0.5208(4) 0.045 Uiso 1 calc R . H12B H 0.3707(6) 0.3874(5) 0.5518(4) 0.045 Uiso 1 calc R . O1 O 0.3625(4) 0.4027(4) 0.4561(2) 0.0383(12) Uani 1 d . . C13 C 0.3957(6) 0.4776(6) 0.4085(3) 0.038(2) Uani 1 d . . H13A H 0.3701(6) 0.4521(6) 0.3658(3) 0.045 Uiso 1 calc R . H13B H 0.4790(6) 0.4822(6) 0.4076(3) 0.045 Uiso 1 calc R . C14 C 0.3472(6) 0.5885(6) 0.4211(3) 0.033(2) Uani 1 d . . H14A H 0.3730(6) 0.6390(6) 0.3872(3) 0.039 Uiso 1 calc R . H14B H 0.2639(6) 0.5851(6) 0.4195(3) 0.039 Uiso 1 calc R . N2 N 0.2038(4) 0.8550(4) 0.5835(2) 0.0228(11) Uani 1 d . . N21 N 0.1306(5) 0.8511(5) 0.6406(2) 0.0291(13) Uani 1 d . . C21 C 0.1622(6) 0.9370(7) 0.6853(3) 0.040(2) Uani 1 d . . H21A H 0.1546(6) 1.0079(7) 0.6638(3) 0.048 Uiso 1 calc R . H21B H 0.2417(6) 0.9280(7) 0.6987(3) 0.048 Uiso 1 calc R . C22 C 0.0860(7) 0.9324(8) 0.7437(3) 0.055(2) Uani 1 d . . H22A H 0.1063(7) 0.9913(8) 0.7737(3) 0.066 Uiso 1 calc R . H22B H 0.0069(7) 0.9436(8) 0.7300(3) 0.066 Uiso 1 calc R . O2 O 0.0950(5) 0.8325(6) 0.7760(2) 0.058(2) Uani 1 d . . C23 C 0.0685(7) 0.7466(8) 0.7327(4) 0.054(2) Uani 1 d . . H23A H -0.0115(7) 0.7523(8) 0.7195(4) 0.064 Uiso 1 calc R . H23B H 0.0787(7) 0.6768(8) 0.7551(4) 0.064 Uiso 1 calc R . C24 C 0.1427(6) 0.7494(7) 0.6733(3) 0.038(2) Uani 1 d . . H24A H 0.2224(6) 0.7389(7) 0.6859(3) 0.046 Uiso 1 calc R . H24B H 0.1213(6) 0.6901(7) 0.6438(3) 0.046 Uiso 1 calc R . N3 N 0.2074(4) 0.9038(4) 0.4498(2) 0.0222(11) Uani 1 d . . N31 N 0.1349(4) 0.9407(4) 0.3970(2) 0.0252(12) Uani 1 d . . C31 C 0.1391(6) 0.8646(6) 0.3431(3) 0.031(2) Uani 1 d . . H31A H 0.1148(6) 0.7925(6) 0.3580(3) 0.038 Uiso 1 calc R . H31B H 0.2175(6) 0.8587(6) 0.3272(3) 0.038 Uiso 1 calc R . C32 C 0.0636(7) 0.9016(7) 0.2893(3) 0.044(2) Uani 1 d . . H32A H 0.0678(7) 0.8494(7) 0.2533(3) 0.053 Uiso 1 calc R . H32B H -0.0153(7) 0.9038(7) 0.3047(3) 0.053 Uiso 1 calc R . O3 O 0.0955(5) 1.0062(4) 0.2665(2) 0.0464(13) Uani 1 d . . C33 C 0.0984(7) 1.0815(7) 0.3183(3) 0.049(2) Uani 1 d . . H33A H 0.0208(7) 1.0923(7) 0.3346(3) 0.058 Uiso 1 calc R . H33B H 0.1259(7) 1.1516(7) 0.3019(3) 0.058 Uiso 1 calc R . C34 C 0.1717(7) 1.0463(6) 0.3726(3) 0.037(2) Uani 1 d . . H34A H 0.2508(7) 1.0415(6) 0.3577(3) 0.045 Uiso 1 calc R . H34B H 0.1682(7) 1.1001(6) 0.4078(3) 0.045 Uiso 1 calc R . N4 N 0.3941(4) 0.9511(4) 0.5266(2) 0.0228(10) Uani 1 d . . N41 N 0.4892(4) 1.0225(4) 0.5373(3) 0.0298(12) Uani 1 d . . C41 C 0.4881(6) 1.0637(6) 0.6032(3) 0.039(2) Uani 1 d . . H41A H 0.4956(6) 1.0029(6) 0.6338(3) 0.046 Uiso 1 calc R . H41B H 0.4151(6) 1.0997(6) 0.6117(3) 0.046 Uiso 1 calc R . C42 C 0.5826(7) 1.1423(7) 0.6138(4) 0.052(2) Uani 1 d . . H42A H 0.5807(7) 1.1684(7) 0.6589(4) 0.063 Uiso 1 calc R . H42B H 0.6557(7) 1.1056(7) 0.6068(4) 0.063 Uiso 1 calc R . O4 O 0.5734(5) 1.2305(4) 0.5715(3) 0.057(2) Uani 1 d . . C43 C 0.5764(7) 1.1931(7) 0.5072(4) 0.050(2) Uani 1 d . . H43A H 0.6494(7) 1.1570(7) 0.4992(4) 0.060 Uiso 1 calc R . H43B H 0.5706(7) 1.2553(7) 0.4776(4) 0.060 Uiso 1 calc R . C44 C 0.4816(6) 1.1152(6) 0.4934(4) 0.044(2) Uani 1 d . . H44A H 0.4082(6) 1.1518(6) 0.4993(4) 0.053 Uiso 1 calc R . H44B H 0.4865(6) 1.0901(6) 0.4482(4) 0.053 Uiso 1 calc R . O51 O 0.6766(9) 1.0864(10) 0.3393(5) 0.138(2) Uiso 1 d . . C52 C 0.7402(14) 1.0273(15) 0.2817(8) 0.138(2) Uiso 0.65(2) d P 1 H52A H 0.7970(14) 0.9754(15) 0.2977(8) 0.166 Uiso 0.65(2) calc PR 1 H52B H 0.6869(14) 0.9900(15) 0.2526(8) 0.166 Uiso 0.65(2) calc PR 1 C53 C 0.7943(15) 1.1233(15) 0.2497(8) 0.138(2) Uiso 0.65(2) d P 1 H53A H 0.8705(15) 1.1050(15) 0.2337(8) 0.166 Uiso 0.65(2) calc PR 1 H53B H 0.7480(15) 1.1489(15) 0.2131(8) 0.166 Uiso 0.65(2) calc PR 1 C54 C 0.8002(26) 1.2027(24) 0.2987(14) 0.138(2) Uiso 0.65(2) d P 1 H54A H 0.8620(26) 1.1855(24) 0.3290(14) 0.166 Uiso 0.65(2) calc PR 1 H54B H 0.8153(26) 1.2743(24) 0.2794(14) 0.166 Uiso 0.65(2) calc PR 1 C55 C 0.7075(16) 1.2038(15) 0.3279(8) 0.138(2) Uiso 0.65(2) d P 1 H55A H 0.6491(16) 1.2399(15) 0.3015(8) 0.166 Uiso 0.65(2) calc PR 1 H55B H 0.7146(16) 1.2425(15) 0.3694(8) 0.166 Uiso 0.65(2) calc PR 1 C62 C 0.7402(14) 1.0273(15) 0.2817(8) 0.138(2) Uiso 0.35(2) d P 2 H62A H 0.7970(47) 0.9754(45) 0.2977(25) 0.166 Uiso 0.35(2) calc PR 2 H62B H 0.6869(47) 0.9900(45) 0.2526(25) 0.166 Uiso 0.35(2) calc PR 2 C63 C 0.7943(15) 1.1233(15) 0.2497(8) 0.138(2) Uiso 0.35(2) d P 2 H63A H 0.8712(47) 1.1344(45) 0.2669(25) 0.166 Uiso 0.35(2) calc PR 2 H63B H 0.8000(47) 1.1111(45) 0.2026(25) 0.166 Uiso 0.35(2) calc PR 2 C64 C 0.7332(47) 1.2067(45) 0.2610(25) 0.138(2) Uiso 0.35(2) d P 2 H64A H 0.6632(47) 1.2043(45) 0.2351(25) 0.166 Uiso 0.35(2) calc PR 2 H64B H 0.7748(47) 1.2734(45) 0.2502(25) 0.166 Uiso 0.35(2) calc PR 2 C65 C 0.7075(16) 1.2038(15) 0.3279(8) 0.138(2) Uiso 0.35(2) d P 2 H65A H 0.6436(17172) 1.2520(17172) 0.3382(25) 0.166 Uiso 0.35(2) calc PR 2 H65B H 0.7736(17172) 1.2250(17172) 0.3541(25) 0.166 Uiso 0.35(2) calc 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 0.0173(2) 0.0269(2) 0.0281(2) 0.0001(2) 0.0004(2) -0.0018(2) Sn2 0.0190(2) 0.0276(2) 0.0324(2) -0.0008(2) -0.0025(2) 0.0003(2) Sn3 0.0198(2) 0.0246(2) 0.0328(2) 0.0003(2) 0.0047(2) 0.0006(2) Sn4 0.0199(2) 0.0267(2) 0.0339(2) -0.0031(2) 0.0013(2) 0.0031(2) N1 0.018(3) 0.026(3) 0.037(3) -0.001(3) 0.004(2) 0.002(2) N11 0.020(3) 0.018(2) 0.029(3) 0.004(2) 0.003(2) -0.001(2) C11 0.030(4) 0.025(3) 0.038(4) 0.001(3) -0.001(3) -0.003(3) C12 0.024(3) 0.029(3) 0.058(5) 0.007(3) 0.002(3) 0.004(3) O1 0.038(3) 0.023(2) 0.053(3) -0.008(2) -0.001(2) -0.004(2) C13 0.035(4) 0.038(4) 0.040(4) -0.006(3) 0.005(3) 0.001(4) C14 0.027(4) 0.038(4) 0.033(4) -0.007(3) -0.002(3) -0.004(3) N2 0.012(3) 0.034(3) 0.022(2) 0.000(2) 0.004(2) 0.004(2) N21 0.021(3) 0.037(3) 0.029(3) -0.004(3) 0.002(2) -0.003(2) C21 0.036(4) 0.046(4) 0.038(4) -0.010(4) 0.001(3) 0.004(4) C22 0.045(5) 0.091(7) 0.029(4) -0.017(4) 0.002(3) 0.010(5) O2 0.054(4) 0.092(5) 0.029(3) -0.002(3) 0.001(3) 0.000(4) C23 0.038(5) 0.084(7) 0.039(4) 0.012(5) 0.006(3) -0.008(5) C24 0.033(4) 0.054(5) 0.028(3) 0.008(4) 0.004(3) 0.001(4) N3 0.016(3) 0.026(3) 0.024(3) 0.003(2) 0.004(2) 0.002(2) N31 0.024(3) 0.027(3) 0.024(3) 0.002(2) -0.001(2) 0.001(2) C31 0.029(4) 0.036(4) 0.029(3) -0.003(3) 0.001(3) 0.000(3) C32 0.044(5) 0.058(5) 0.030(4) 0.004(4) 0.001(3) -0.003(4) O3 0.059(3) 0.048(3) 0.033(2) 0.004(2) 0.005(2) 0.009(3) C33 0.056(5) 0.056(5) 0.034(4) 0.008(4) 0.004(4) 0.029(5) C34 0.048(5) 0.028(4) 0.035(4) -0.001(3) 0.002(3) 0.011(3) N4 0.014(2) 0.020(2) 0.035(3) -0.005(2) 0.004(2) 0.001(2) N41 0.019(3) 0.021(3) 0.050(3) -0.006(3) -0.002(2) -0.006(2) C41 0.038(4) 0.038(4) 0.039(4) -0.013(3) -0.005(3) -0.004(4) C42 0.040(5) 0.047(5) 0.069(5) -0.026(5) -0.013(4) -0.006(4) O4 0.049(4) 0.031(3) 0.090(4) -0.020(3) -0.001(3) -0.007(3) C43 0.045(5) 0.031(4) 0.075(6) 0.002(4) 0.009(4) -0.011(4) C44 0.034(4) 0.023(4) 0.075(6) 0.006(4) 0.002(4) -0.008(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 N2 2.196(5) . ? Sn1 N3 2.201(5) . ? Sn1 N1 2.250(5) . ? Sn2 N4 2.204(5) . ? Sn2 N1 2.207(5) . ? Sn2 N2 2.262(5) . ? Sn2 Sn3 3.2870(6) . ? Sn3 N4 2.197(5) . ? Sn3 N1 2.210(5) . ? Sn3 N3 2.252(5) . ? Sn4 N3 2.194(5) . ? Sn4 N2 2.208(5) . ? Sn4 N4 2.211(5) . ? N1 N11 1.450(7) . ? N11 C14 1.464(8) . ? N11 C11 1.473(8) . ? C11 C12 1.506(9) . ? C12 O1 1.436(9) . ? O1 C13 1.412(8) . ? C13 C14 1.515(10) . ? N2 N21 1.469(7) . ? N21 C24 1.440(9) . ? N21 C21 1.461(9) . ? C21 C22 1.514(10) . ? C22 O2 1.413(11) . ? O2 C23 1.429(11) . ? C23 C24 1.515(10) . ? N3 N31 1.465(7) . ? N31 C31 1.465(8) . ? N31 C34 1.471(8) . ? C31 C32 1.503(10) . ? C32 O3 1.432(10) . ? O3 C33 1.425(9) . ? C33 C34 1.489(10) . ? N4 N41 1.451(6) . ? N41 C41 1.460(9) . ? N41 C44 1.469(9) . ? C41 C42 1.503(10) . ? C42 O4 1.407(10) . ? O4 C43 1.412(10) . ? C43 C44 1.511(10) . ? O51 C65 1.52(2) . ? O51 C55 1.52(2) . ? O51 C52 1.59(2) . ? O51 C62 1.59(2) . ? C52 C53 1.51(2) . ? C53 C54 1.42(3) . ? C54 C55 1.26(3) . ? C62 C63 1.51(2) . ? C63 C64 1.29(5) . ? C64 C65 1.42(5) . ? 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 N2 Sn1 N3 80.5(2) . . ? N2 Sn1 N1 78.1(2) . . ? N3 Sn1 N1 77.3(2) . . ? N4 Sn2 N1 81.2(2) . . ? N4 Sn2 N2 78.1(2) . . ? N1 Sn2 N2 77.6(2) . . ? N4 Sn2 Sn3 41.61(12) . . ? N1 Sn2 Sn3 41.95(14) . . ? N2 Sn2 Sn3 84.63(12) . . ? N4 Sn3 N1 81.3(2) . . ? N4 Sn3 N3 77.7(2) . . ? N1 Sn3 N3 77.1(2) . . ? N4 Sn3 Sn2 41.76(13) . . ? N1 Sn3 Sn2 41.87(14) . . ? N3 Sn3 Sn2 84.02(12) . . ? N3 Sn4 N2 80.4(2) . . ? N3 Sn4 N4 78.6(2) . . ? N2 Sn4 N4 79.1(2) . . ? N11 N1 Sn2 114.8(4) . . ? N11 N1 Sn3 115.0(3) . . ? Sn2 N1 Sn3 96.2(2) . . ? N11 N1 Sn1 123.0(4) . . ? Sn2 N1 Sn1 101.7(2) . . ? Sn3 N1 Sn1 102.2(2) . . ? N1 N11 C14 110.6(5) . . ? N1 N11 C11 110.5(5) . . ? C14 N11 C11 107.8(5) . . ? N11 C11 C12 111.0(5) . . ? O1 C12 C11 110.7(6) . . ? C13 O1 C12 110.3(5) . . ? O1 C13 C14 111.8(5) . . ? N11 C14 C13 110.5(6) . . ? N21 N2 Sn1 115.3(4) . . ? N21 N2 Sn4 117.1(4) . . ? Sn1 N2 Sn4 97.5(2) . . ? N21 N2 Sn2 121.5(4) . . ? Sn1 N2 Sn2 101.6(2) . . ? Sn4 N2 Sn2 100.0(2) . . ? C24 N21 C21 108.4(5) . . ? C24 N21 N2 110.4(5) . . ? C21 N21 N2 109.6(5) . . ? N21 C21 C22 109.1(6) . . ? O2 C22 C21 111.5(7) . . ? C22 O2 C23 109.9(6) . . ? O2 C23 C24 111.5(7) . . ? N21 C24 C23 110.2(7) . . ? N31 N3 Sn4 116.0(3) . . ? N31 N3 Sn1 114.7(4) . . ? Sn4 N3 Sn1 97.7(2) . . ? N31 N3 Sn3 121.8(3) . . ? Sn4 N3 Sn3 100.6(2) . . ? Sn1 N3 Sn3 102.4(2) . . ? C31 N31 N3 110.5(5) . . ? C31 N31 C34 107.5(5) . . ? N3 N31 C34 111.2(5) . . ? N31 C31 C32 110.5(6) . . ? O3 C32 C31 111.4(6) . . ? C33 O3 C32 110.6(5) . . ? O3 C33 C34 113.1(6) . . ? N31 C34 C33 110.4(7) . . ? N41 N4 Sn3 116.5(3) . . ? N41 N4 Sn2 115.5(4) . . ? Sn3 N4 Sn2 96.6(2) . . ? N41 N4 Sn4 120.9(3) . . ? Sn3 N4 Sn4 101.8(2) . . ? Sn2 N4 Sn4 101.7(2) . . ? N4 N41 C41 110.5(5) . . ? N4 N41 C44 109.6(5) . . ? C41 N41 C44 107.8(6) . . ? N41 C41 C42 111.0(6) . . ? O4 C42 C41 110.8(6) . . ? C42 O4 C43 109.4(6) . . ? O4 C43 C44 111.8(7) . . ? N41 C44 C43 109.8(6) . . ? C55 O51 C52 102.1(12) . . ? C65 O51 C62 102.1(12) . . ? C53 C52 O51 99.7(14) . . ? C54 C53 C52 104.7(17) . . ? C55 C54 C53 108.1(26) . . ? C54 C55 O51 106.1(21) . . ? C63 C62 O51 99.7(14) . . ? C64 C63 C62 108.3(28) . . ? C63 C64 C65 106.3(41) . . ? C64 C65 O51 103.2(27) . . ? _refine_diff_density_max 0.761 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.137 data_dw0008 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H48 N4 O4 Sn4' _chemical_formula_weight 1153.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c 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 13.7720(17) _cell_length_b 27.577(3) _cell_length_c 12.388(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.489(9) _cell_angle_gamma 90.00 _cell_volume 4377.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 33964 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2252 _exptl_absorpt_coefficient_mu 2.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25437 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7518 _reflns_number_gt 6511 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+187.1381P] 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 7518 _refine_ls_number_parameters 477 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2043 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.253 _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 0.55667(8) 0.86215(4) 0.66650(9) 0.0261(3) Uani 1 1 d . . . Sn2 Sn 0.64265(8) 0.76883(4) 0.85464(9) 0.0278(3) Uani 1 1 d . . . Sn3 Sn 0.49987(7) 0.75035(4) 0.56861(9) 0.0230(2) Uani 1 1 d . . . Sn4 Sn 0.39235(7) 0.79586(4) 0.75276(9) 0.0237(3) Uani 1 1 d . . . O1 O 0.0327(9) 0.8654(5) 0.2376(10) 0.046(3) Uani 1 1 d . . . O2 O 0.6136(11) 0.9783(5) 1.1690(12) 0.060(4) Uani 1 1 d . . . O3 O 0.4012(16) 0.5474(5) 0.8567(14) 0.076(5) Uani 1 1 d . . . O4 O 1.0119(9) 0.7720(5) 0.5957(11) 0.049(3) Uani 1 1 d . . . N1 N 0.4167(9) 0.8161(4) 0.5910(10) 0.022(3) Uani 1 1 d . . . N2 N 0.5424(9) 0.8337(4) 0.8283(9) 0.022(3) Uani 1 1 d . . . N3 N 0.4918(9) 0.7346(4) 0.7401(9) 0.022(3) Uani 1 1 d . . . N4 N 0.6360(8) 0.7913(4) 0.6783(11) 0.024(3) Uani 1 1 d . . . C1 C 0.3212(10) 0.8307(5) 0.4976(12) 0.022(3) Uani 1 1 d . . . C2 C 0.2675(11) 0.7993(5) 0.4066(12) 0.024(3) Uani 1 1 d . . . H2A H 0.2972 0.7686 0.4027 0.029 Uiso 1 1 calc R . . C3 C 0.1717(11) 0.8115(6) 0.3212(14) 0.033(4) Uani 1 1 d . . . H3A H 0.1372 0.7891 0.2611 0.040 Uiso 1 1 calc R . . C4 C 0.1271(11) 0.8562(6) 0.3240(12) 0.030(4) Uani 1 1 d . . . C5 C 0.1777(12) 0.8879(6) 0.4151(14) 0.032(4) Uani 1 1 d . . . H5A H 0.1469 0.9184 0.4184 0.039 Uiso 1 1 calc R . . C6 C 0.2732(11) 0.8754(6) 0.5018(13) 0.030(3) Uani 1 1 d . . . C7 C 0.3222(13) 0.9126(6) 0.5949(15) 0.039(4) Uani 1 1 d . . . H7A H 0.2762 0.9408 0.5819 0.059 Uiso 1 1 calc R . . H7B H 0.3896 0.9226 0.5924 0.059 Uiso 1 1 calc R . . H7C H 0.3328 0.8984 0.6710 0.059 Uiso 1 1 calc R . . C8 C -0.0173(16) 0.9089(8) 0.247(2) 0.072(7) Uani 1 1 d . . . H8A H -0.0837 0.9117 0.1812 0.108 Uiso 1 1 calc R . . H8B H 0.0274 0.9365 0.2468 0.108 Uiso 1 1 calc R . . H8C H -0.0305 0.9088 0.3196 0.108 Uiso 1 1 calc R . . C9 C 0.5620(11) 0.8686(6) 0.9208(12) 0.029(4) Uani 1 1 d . . . C10 C 0.4844(12) 0.8822(6) 0.9605(12) 0.029(3) Uani 1 1 d . . . H10A H 0.4183 0.8668 0.9280 0.035 Uiso 1 1 calc R . . C11 C 0.4979(14) 0.9171(6) 1.0450(12) 0.035(4) Uani 1 1 d . . . H11A H 0.4437 0.9247 1.0723 0.042 Uiso 1 1 calc R . . C12 C 0.5929(14) 0.9406(6) 1.0882(13) 0.037(4) Uani 1 1 d . . . C13 C 0.6723(13) 0.9275(6) 1.0513(15) 0.041(4) Uani 1 1 d . . . H13A H 0.7376 0.9436 1.0836 0.049 Uiso 1 1 calc R . . C14 C 0.6608(13) 0.8925(7) 0.9709(16) 0.042(4) Uani 1 1 d . . . C15 C 0.7542(12) 0.8801(7) 0.9416(16) 0.045(5) Uani 1 1 d . . . H15A H 0.8134 0.9004 0.9875 0.068 Uiso 1 1 calc R . . H15B H 0.7383 0.8858 0.8589 0.068 Uiso 1 1 calc R . . H15C H 0.7721 0.8458 0.9594 0.068 Uiso 1 1 calc R . . C16 C 0.5272(18) 0.9982(7) 1.1875(17) 0.056(6) Uani 1 1 d . . . H16A H 0.5505 1.0241 1.2452 0.084 Uiso 1 1 calc R . . H16B H 0.4925 0.9728 1.2156 0.084 Uiso 1 1 calc R . . H16C H 0.4781 1.0114 1.1144 0.084 Uiso 1 1 calc R . . C17 C 0.4676(11) 0.6868(5) 0.7666(11) 0.024(3) Uani 1 1 d . . . C18 C 0.5399(15) 0.6590(7) 0.8522(16) 0.045(4) Uani 1 1 d . . . H18A H 0.6071 0.6724 0.8918 0.054 Uiso 1 1 calc R . . C19 C 0.520(2) 0.6119(7) 0.8840(18) 0.059(6) Uani 1 1 d . . . H19A H 0.5706 0.5945 0.9446 0.071 Uiso 1 1 calc R . . C20 C 0.4223(19) 0.5923(7) 0.8229(17) 0.052(6) Uani 1 1 d . . . C21 C 0.3482(17) 0.6179(7) 0.7344(17) 0.048(5) Uani 1 1 d . . . H21A H 0.2821 0.6039 0.6923 0.058 Uiso 1 1 calc R . . C22 C 0.3715(13) 0.6641(6) 0.7079(15) 0.035(4) Uani 1 1 d . . . C23 C 0.2875(13) 0.6893(7) 0.6052(15) 0.045(5) Uani 1 1 d . . . H23A H 0.2257 0.6685 0.5753 0.068 Uiso 1 1 calc R . . H23B H 0.3149 0.6953 0.5436 0.068 Uiso 1 1 calc R . . H23C H 0.2685 0.7203 0.6310 0.068 Uiso 1 1 calc R . . C24 C 0.296(3) 0.5242(13) 0.779(4) 0.149(17) Uani 1 1 d . . . H24A H 0.2883 0.4923 0.8101 0.224 Uiso 1 1 calc R . . H24B H 0.2940 0.5205 0.6998 0.224 Uiso 1 1 calc R . . H24C H 0.2379 0.5451 0.7785 0.224 Uiso 1 1 calc R . . C25 C 0.7322(11) 0.7863(6) 0.6546(14) 0.028(3) Uani 1 1 d . . . C26 C 0.7718(11) 0.8251(6) 0.6131(14) 0.031(4) Uani 1 1 d . . . H26A H 0.7358 0.8552 0.6015 0.037 Uiso 1 1 calc R . . C27 C 0.8625(11) 0.8221(7) 0.5874(14) 0.034(4) Uani 1 1 d . . . H27A H 0.8852 0.8490 0.5549 0.041 Uiso 1 1 calc R . . C28 C 0.9179(12) 0.7795(7) 0.6101(14) 0.037(4) Uani 1 1 d . . . C29 C 0.8796(12) 0.7406(6) 0.6512(14) 0.035(4) Uani 1 1 d . . . H29A H 0.9176 0.7111 0.6643 0.042 Uiso 1 1 calc R . . C30 C 0.7886(11) 0.7421(6) 0.6747(14) 0.032(4) Uani 1 1 d . . . C31 C 0.7514(13) 0.6963(6) 0.7123(15) 0.036(4) Uani 1 1 d . . . H31A H 0.6866 0.7028 0.7252 0.055 Uiso 1 1 calc R . . H31B H 0.8047 0.6846 0.7844 0.055 Uiso 1 1 calc R . . H31C H 0.7387 0.6716 0.6517 0.055 Uiso 1 1 calc R . . C32 C 1.0395(15) 0.8086(9) 0.529(2) 0.063(6) Uani 1 1 d . . . H32A H 1.1072 0.8007 0.5245 0.095 Uiso 1 1 calc R . . H32B H 1.0437 0.8402 0.5667 0.095 Uiso 1 1 calc R . . H32C H 0.9862 0.8099 0.4507 0.095 Uiso 1 1 calc R . . C50 C -0.0074(19) 0.6704(12) 0.416(2) 0.096(10) Uani 1 1 d . . . H50A H 0.0275 0.7019 0.4236 0.144 Uiso 1 1 calc R . . H50B H -0.0236 0.6643 0.4859 0.144 Uiso 1 1 calc R . . H50C H -0.0722 0.6707 0.3480 0.144 Uiso 1 1 calc R . . C51 C 0.0628(14) 0.6314(9) 0.4036(14) 0.050(5) Uani 1 1 d . . . C52 C 0.1171(15) 0.6383(9) 0.3324(18) 0.058(6) Uani 1 1 d . . . H52 H 0.1069 0.6677 0.2896 0.070 Uiso 1 1 calc R . . C56 C 0.077(3) 0.5874(12) 0.464(2) 0.089(9) Uani 1 1 d . . . H56 H 0.0395 0.5807 0.5130 0.107 Uiso 1 1 calc R . . C53 C 0.1847(19) 0.6053(11) 0.319(2) 0.075(7) Uani 1 1 d . . . H53 H 0.2211 0.6113 0.2687 0.090 Uiso 1 1 calc R . . C54 C 0.199(2) 0.5645(13) 0.379(3) 0.097(10) Uani 1 1 d . . . H54 H 0.2478 0.5419 0.3712 0.116 Uiso 1 1 calc R . . C55 C 0.149(3) 0.5528(13) 0.450(3) 0.123(15) Uani 1 1 d . . . H55 H 0.1606 0.5226 0.4902 0.148 Uiso 1 1 calc R . . C60 C 0.797(8) 0.952(3) 0.470(6) 0.183(12) Uiso 0.50 1 d PD . . C61 C 0.896(2) 0.9735(12) 0.483(3) 0.183(12) Uiso 1 1 d D . . C62 C 0.990(3) 0.9678(16) 0.597(3) 0.183(12) Uiso 1 1 d D . . C63 C 0.909(3) 1.0038(17) 0.385(3) 0.183(12) 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 Sn1 0.0219(5) 0.0243(6) 0.0318(6) -0.0029(4) 0.0095(4) -0.0023(4) Sn2 0.0220(5) 0.0291(6) 0.0276(5) -0.0022(4) 0.0036(4) 0.0011(4) Sn3 0.0192(5) 0.0240(5) 0.0247(5) -0.0023(4) 0.0068(4) 0.0003(4) Sn4 0.0200(5) 0.0267(6) 0.0243(5) -0.0037(4) 0.0082(4) -0.0022(4) O1 0.031(6) 0.051(8) 0.040(7) -0.004(6) -0.006(5) 0.012(6) O2 0.070(9) 0.043(8) 0.061(9) -0.035(7) 0.016(7) -0.009(7) O3 0.151(16) 0.029(8) 0.068(10) -0.012(7) 0.062(11) -0.033(9) O4 0.029(6) 0.062(9) 0.060(8) 0.009(7) 0.022(6) 0.004(6) N1 0.020(6) 0.016(6) 0.031(7) -0.007(5) 0.011(5) 0.005(5) N2 0.022(6) 0.030(7) 0.012(5) 0.001(5) 0.005(5) -0.001(5) N3 0.029(6) 0.028(7) 0.006(5) -0.004(5) 0.005(5) -0.005(5) N4 0.015(6) 0.024(7) 0.034(7) -0.003(6) 0.009(5) -0.003(5) C1 0.018(7) 0.026(8) 0.024(7) -0.009(6) 0.011(6) -0.006(6) C2 0.024(7) 0.020(8) 0.021(7) -0.005(6) 0.001(6) 0.003(6) C3 0.022(8) 0.031(9) 0.035(9) -0.003(7) -0.001(7) -0.002(7) C4 0.027(8) 0.039(9) 0.019(7) -0.001(7) 0.001(6) 0.008(7) C5 0.033(8) 0.031(9) 0.036(9) -0.007(7) 0.016(7) 0.008(7) C6 0.025(8) 0.028(9) 0.031(8) -0.010(7) 0.003(6) 0.001(6) C7 0.033(9) 0.028(9) 0.050(11) 0.000(8) 0.009(8) 0.010(7) C8 0.046(12) 0.064(15) 0.075(15) -0.013(12) -0.015(11) 0.029(11) C9 0.021(7) 0.029(8) 0.019(7) -0.006(6) -0.014(6) 0.002(6) C10 0.030(8) 0.030(9) 0.022(8) -0.009(7) 0.004(6) 0.003(7) C11 0.061(11) 0.028(9) 0.015(7) -0.002(6) 0.012(7) -0.004(8) C12 0.051(10) 0.034(9) 0.019(8) -0.008(7) 0.004(7) 0.004(8) C13 0.030(9) 0.034(10) 0.039(10) -0.005(8) -0.011(7) 0.001(7) C14 0.030(9) 0.038(10) 0.054(11) -0.018(9) 0.010(8) -0.004(8) C15 0.024(8) 0.052(12) 0.049(11) -0.018(9) 0.001(8) -0.006(8) C16 0.103(17) 0.030(10) 0.046(11) -0.013(9) 0.040(12) -0.015(11) C17 0.033(8) 0.026(8) 0.012(6) -0.001(6) 0.006(6) 0.000(6) C18 0.056(11) 0.036(10) 0.049(11) -0.009(9) 0.026(9) 0.004(9) C19 0.116(19) 0.021(10) 0.046(12) -0.003(9) 0.037(12) 0.001(11) C20 0.109(18) 0.025(10) 0.047(11) 0.002(9) 0.057(13) -0.012(11) C21 0.076(14) 0.029(10) 0.051(11) -0.016(9) 0.036(11) -0.018(9) C22 0.047(10) 0.030(9) 0.041(9) -0.018(8) 0.033(8) -0.013(8) C23 0.042(10) 0.052(12) 0.045(10) -0.018(9) 0.019(8) -0.030(9) C24 0.24(5) 0.09(3) 0.16(4) 0.00(3) 0.12(4) -0.03(3) C25 0.018(7) 0.026(8) 0.038(9) -0.010(7) 0.007(6) -0.002(6) C26 0.023(7) 0.029(9) 0.039(9) -0.005(7) 0.010(7) 0.002(6) C27 0.021(8) 0.049(11) 0.034(9) -0.004(8) 0.011(7) -0.005(7) C28 0.020(8) 0.059(12) 0.036(9) -0.004(8) 0.016(7) 0.001(8) C29 0.023(8) 0.041(10) 0.034(9) -0.010(8) 0.003(7) 0.001(7) C30 0.022(7) 0.026(9) 0.042(9) -0.003(7) 0.004(7) 0.002(6) C31 0.039(9) 0.032(9) 0.042(10) 0.003(8) 0.018(8) 0.011(7) C32 0.042(11) 0.085(17) 0.076(15) 0.008(13) 0.038(11) 0.003(11) C50 0.061(15) 0.14(3) 0.085(19) -0.055(19) 0.025(14) -0.008(16) C51 0.038(10) 0.087(16) 0.019(8) -0.024(10) 0.004(7) -0.020(10) C52 0.045(11) 0.073(15) 0.056(13) -0.015(11) 0.019(10) -0.006(11) C56 0.13(3) 0.08(2) 0.048(14) -0.011(14) 0.031(16) -0.05(2) C53 0.062(15) 0.09(2) 0.079(18) -0.008(16) 0.030(13) -0.012(14) C54 0.09(2) 0.10(3) 0.08(2) -0.03(2) 0.009(18) -0.004(19) C55 0.17(4) 0.08(2) 0.07(2) 0.000(18) -0.03(2) 0.00(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.210(12) . ? Sn1 N4 2.218(12) . ? Sn1 N2 2.228(11) . ? Sn2 N2 2.210(12) . ? Sn2 N4 2.239(12) . ? Sn2 N3 2.250(11) . ? Sn2 Sn4 3.2930(14) . ? Sn3 N4 2.183(11) . ? Sn3 N3 2.211(11) . ? Sn3 N1 2.216(11) . ? Sn4 N2 2.194(11) . ? Sn4 N3 2.217(12) . ? Sn4 N1 2.221(12) . ? O1 C4 1.372(17) . ? O1 C8 1.41(2) . ? O2 C12 1.399(19) . ? O2 C16 1.40(2) . ? O3 C20 1.37(2) . ? O3 C24 1.56(4) . ? O4 C28 1.385(18) . ? O4 C32 1.44(2) . ? N1 C1 1.455(18) . ? N2 C9 1.445(18) . ? N3 C17 1.426(19) . ? N4 C25 1.465(18) . ? C1 C2 1.399(19) . ? C1 C6 1.41(2) . ? C2 C3 1.40(2) . ? C2 H2A 0.9500 . ? C3 C4 1.38(2) . ? C3 H3A 0.9500 . ? C4 C5 1.40(2) . ? C5 C6 1.40(2) . ? C5 H5A 0.9500 . ? C6 C7 1.51(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.38(2) . ? C9 C14 1.43(2) . ? C10 C11 1.38(2) . ? C10 H10A 0.9500 . ? C11 C12 1.38(2) . ? C11 H11A 0.9500 . ? C12 C13 1.38(2) . ? C13 C14 1.35(2) . ? C13 H13A 0.9500 . ? C14 C15 1.50(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.39(2) . ? C17 C22 1.40(2) . ? C18 C19 1.41(3) . ? C18 H18A 0.9500 . ? C19 C20 1.39(3) . ? C19 H19A 0.9500 . ? C20 C21 1.39(3) . ? C21 C22 1.38(2) . ? C21 H21A 0.9500 . ? C22 C23 1.54(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.38(2) . ? C25 C30 1.42(2) . ? C26 C27 1.40(2) . ? C26 H26A 0.9500 . ? C27 C28 1.37(2) . ? C27 H27A 0.9500 . ? C28 C29 1.37(2) . ? C29 C30 1.39(2) . ? C29 H29A 0.9500 . ? C30 C31 1.50(2) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C50 C51 1.49(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.36(3) . ? C51 C56 1.40(4) . ? C52 C53 1.35(3) . ? C52 H52 0.9500 . ? C56 C55 1.43(5) . ? C56 H56 0.9500 . ? C53 C54 1.32(4) . ? C53 H53 0.9500 . ? C54 C55 1.34(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C60 C61 1.44(10) . ? C61 C62 1.53(3) . ? C61 C63 1.54(3) . ? C62 C63 1.54(3) 3_776 ? C63 C62 1.54(3) 3_776 ? 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 N4 81.6(4) . . ? N1 Sn1 N2 80.1(4) . . ? N4 Sn1 N2 80.4(4) . . ? N2 Sn2 N4 80.3(4) . . ? N2 Sn2 N3 82.2(4) . . ? N4 Sn2 N3 78.6(4) . . ? N2 Sn2 Sn4 41.4(3) . . ? N4 Sn2 Sn4 84.3(3) . . ? N3 Sn2 Sn4 42.1(3) . . ? N4 Sn3 N3 80.6(4) . . ? N4 Sn3 N1 82.2(4) . . ? N3 Sn3 N1 80.3(4) . . ? N2 Sn4 N3 83.3(4) . . ? N2 Sn4 N1 80.5(4) . . ? N3 Sn4 N1 80.0(4) . . ? N2 Sn4 Sn2 41.8(3) . . ? N3 Sn4 Sn2 42.9(3) . . ? N1 Sn4 Sn2 85.4(3) . . ? C4 O1 C8 116.5(14) . . ? C12 O2 C16 116.3(15) . . ? C20 O3 C24 116(2) . . ? C28 O4 C32 115.1(14) . . ? C1 N1 Sn1 124.9(9) . . ? C1 N1 Sn3 119.0(8) . . ? Sn1 N1 Sn3 96.4(4) . . ? C1 N1 Sn4 113.3(8) . . ? Sn1 N1 Sn4 99.2(5) . . ? Sn3 N1 Sn4 99.4(5) . . ? C9 N2 Sn4 121.9(9) . . ? C9 N2 Sn2 119.8(8) . . ? Sn4 N2 Sn2 96.8(5) . . ? C9 N2 Sn1 115.2(9) . . ? Sn4 N2 Sn1 99.4(4) . . ? Sn2 N2 Sn1 99.3(4) . . ? C17 N3 Sn3 120.1(8) . . ? C17 N3 Sn4 119.0(9) . . ? Sn3 N3 Sn4 99.6(5) . . ? C17 N3 Sn2 118.8(9) . . ? Sn3 N3 Sn2 99.4(5) . . ? Sn4 N3 Sn2 95.0(4) . . ? C25 N4 Sn3 117.4(9) . . ? C25 N4 Sn1 122.0(9) . . ? Sn3 N4 Sn1 97.2(4) . . ? C25 N4 Sn2 116.9(9) . . ? Sn3 N4 Sn2 100.6(5) . . ? Sn1 N4 Sn2 98.7(5) . . ? C2 C1 C6 117.0(13) . . ? C2 C1 N1 121.8(13) . . ? C6 C1 N1 120.8(12) . . ? C3 C2 C1 122.4(14) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C4 C3 C2 120.0(14) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? O1 C4 C3 116.7(14) . . ? O1 C4 C5 124.3(14) . . ? C3 C4 C5 119.0(14) . . ? C4 C5 C6 121.0(14) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 120.5(13) . . ? C5 C6 C7 116.9(14) . . ? C1 C6 C7 122.6(13) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 117.2(14) . . ? C10 C9 N2 121.2(13) . . ? C14 C9 N2 121.5(14) . . ? C9 C10 C11 123.4(15) . . ? C9 C10 H10A 118.3 . . ? C11 C10 H10A 118.3 . . ? C12 C11 C10 117.8(16) . . ? C12 C11 H11A 121.1 . . ? C10 C11 H11A 121.1 . . ? C11 C12 C13 120.2(15) . . ? C11 C12 O2 122.9(16) . . ? C13 C12 O2 116.9(16) . . ? C14 C13 C12 122.4(16) . . ? C14 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? C13 C14 C9 118.9(16) . . ? C13 C14 C15 117.5(15) . . ? C9 C14 C15 123.6(15) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 115.1(15) . . ? C18 C17 N3 121.6(14) . . ? C22 C17 N3 123.3(13) . . ? C17 C18 C19 124.1(19) . . ? C17 C18 H18A 117.9 . . ? C19 C18 H18A 117.9 . . ? C20 C19 C18 117(2) . . ? C20 C19 H19A 121.4 . . ? C18 C19 H19A 121.4 . . ? O3 C20 C19 117(2) . . ? O3 C20 C21 122(2) . . ? C19 C20 C21 121.1(17) . . ? C22 C21 C20 119.4(19) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C17 123.0(18) . . ? C21 C22 C23 116.4(16) . . ? C17 C22 C23 120.5(14) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 H24A 109.5 . . ? O3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 117.7(14) . . ? C26 C25 N4 120.7(13) . . ? C30 C25 N4 121.6(14) . . ? C25 C26 C27 123.0(15) . . ? C25 C26 H26A 118.5 . . ? C27 C26 H26A 118.5 . . ? C28 C27 C26 118.6(16) . . ? C28 C27 H27A 120.7 . . ? C26 C27 H27A 120.7 . . ? C29 C28 C27 118.9(14) . . ? C29 C28 O4 115.9(16) . . ? C27 C28 O4 125.2(16) . . ? C28 C29 C30 123.7(16) . . ? C28 C29 H29A 118.1 . . ? C30 C29 H29A 118.1 . . ? C29 C30 C25 117.9(15) . . ? C29 C30 C31 118.6(14) . . ? C25 C30 C31 123.4(14) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C56 118(2) . . ? C52 C51 C50 120(2) . . ? C56 C51 C50 123(2) . . ? C53 C52 C51 123(3) . . ? C53 C52 H52 118.4 . . ? C51 C52 H52 118.4 . . ? C51 C56 C55 119(3) . . ? C51 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C54 C53 C52 118(3) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? C53 C54 C55 125(4) . . ? C53 C54 H54 117.7 . . ? C55 C54 H54 117.7 . . ? C54 C55 C56 117(3) . . ? C54 C55 H55 121.3 . . ? C56 C55 H55 121.3 . . ? C60 C61 C62 121.0(16) . . ? C60 C61 C63 120.6(16) . . ? C62 C61 C63 118.4(15) . . ? C61 C62 C63 120.0(16) . 3_776 ? C62 C63 C61 121.3(16) 3_776 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Sn2 Sn4 N2 -81.9(5) . . . . ? N3 Sn2 Sn4 N2 -161.2(6) . . . . ? N2 Sn2 Sn4 N3 161.2(6) . . . . ? N4 Sn2 Sn4 N3 79.3(5) . . . . ? N2 Sn2 Sn4 N1 80.9(5) . . . . ? N4 Sn2 Sn4 N1 -1.0(4) . . . . ? N3 Sn2 Sn4 N1 -80.3(5) . . . . ? N4 Sn1 N1 C1 -144.4(11) . . . . ? N2 Sn1 N1 C1 133.9(10) . . . . ? N4 Sn1 N1 Sn3 -12.1(4) . . . . ? N2 Sn1 N1 Sn3 -93.7(5) . . . . ? N4 Sn1 N1 Sn4 88.5(5) . . . . ? N2 Sn1 N1 Sn4 6.9(4) . . . . ? N4 Sn3 N1 C1 148.4(10) . . . . ? N3 Sn3 N1 C1 -129.8(10) . . . . ? N4 Sn3 N1 Sn1 12.2(5) . . . . ? N3 Sn3 N1 Sn1 94.0(5) . . . . ? N4 Sn3 N1 Sn4 -88.2(5) . . . . ? N3 Sn3 N1 Sn4 -6.4(4) . . . . ? N2 Sn4 N1 C1 -141.5(9) . . . . ? N3 Sn4 N1 C1 133.7(9) . . . . ? Sn2 Sn4 N1 C1 176.7(9) . . . . ? N2 Sn4 N1 Sn1 -7.0(4) . . . . ? N3 Sn4 N1 Sn1 -91.7(4) . . . . ? Sn2 Sn4 N1 Sn1 -48.8(3) . . . . ? N2 Sn4 N1 Sn3 91.2(5) . . . . ? N3 Sn4 N1 Sn3 6.4(4) . . . . ? Sn2 Sn4 N1 Sn3 49.3(3) . . . . ? N3 Sn4 N2 C9 -144.4(11) . . . . ? N1 Sn4 N2 C9 134.6(11) . . . . ? Sn2 Sn4 N2 C9 -131.6(12) . . . . ? N3 Sn4 N2 Sn2 -12.8(4) . . . . ? N1 Sn4 N2 Sn2 -93.7(4) . . . . ? N3 Sn4 N2 Sn1 87.9(5) . . . . ? N1 Sn4 N2 Sn1 6.9(4) . . . . ? Sn2 Sn4 N2 Sn1 100.6(5) . . . . ? N4 Sn2 N2 C9 -134.7(11) . . . . ? N3 Sn2 N2 C9 145.6(11) . . . . ? Sn4 Sn2 N2 C9 133.0(12) . . . . ? N4 Sn2 N2 Sn4 92.3(4) . . . . ? N3 Sn2 N2 Sn4 12.6(4) . . . . ? N4 Sn2 N2 Sn1 -8.4(4) . . . . ? N3 Sn2 N2 Sn1 -88.1(4) . . . . ? Sn4 Sn2 N2 Sn1 -100.7(5) . . . . ? N1 Sn1 N2 C9 -139.1(10) . . . . ? N4 Sn1 N2 C9 137.9(10) . . . . ? N1 Sn1 N2 Sn4 -7.0(4) . . . . ? N4 Sn1 N2 Sn4 -90.0(5) . . . . ? N1 Sn1 N2 Sn2 91.6(5) . . . . ? N4 Sn1 N2 Sn2 8.5(4) . . . . ? N4 Sn3 N3 C17 -138.1(11) . . . . ? N1 Sn3 N3 C17 138.3(11) . . . . ? N4 Sn3 N3 Sn4 90.1(5) . . . . ? N1 Sn3 N3 Sn4 6.4(4) . . . . ? N4 Sn3 N3 Sn2 -6.7(4) . . . . ? N1 Sn3 N3 Sn2 -90.3(5) . . . . ? N2 Sn4 N3 C17 139.5(9) . . . . ? N1 Sn4 N3 C17 -139.0(10) . . . . ? Sn2 Sn4 N3 C17 127.0(10) . . . . ? N2 Sn4 N3 Sn3 -88.0(5) . . . . ? N1 Sn4 N3 Sn3 -6.4(4) . . . . ? Sn2 Sn4 N3 Sn3 -100.5(5) . . . . ? N2 Sn4 N3 Sn2 12.5(4) . . . . ? N1 Sn4 N3 Sn2 94.0(4) . . . . ? N2 Sn2 N3 C17 -139.6(10) . . . . ? N4 Sn2 N3 C17 138.8(10) . . . . ? Sn4 Sn2 N3 C17 -127.1(11) . . . . ? N2 Sn2 N3 Sn3 88.2(5) . . . . ? N4 Sn2 N3 Sn3 6.6(4) . . . . ? Sn4 Sn2 N3 Sn3 100.7(5) . . . . ? N2 Sn2 N3 Sn4 -12.4(4) . . . . ? N4 Sn2 N3 Sn4 -94.1(5) . . . . ? N3 Sn3 N4 C25 134.7(11) . . . . ? N1 Sn3 N4 C25 -144.0(11) . . . . ? N3 Sn3 N4 Sn1 -93.5(5) . . . . ? N1 Sn3 N4 Sn1 -12.2(4) . . . . ? N3 Sn3 N4 Sn2 6.7(5) . . . . ? N1 Sn3 N4 Sn2 88.1(5) . . . . ? N1 Sn1 N4 C25 140.9(11) . . . . ? N2 Sn1 N4 C25 -137.8(11) . . . . ? N1 Sn1 N4 Sn3 12.3(4) . . . . ? N2 Sn1 N4 Sn3 93.5(5) . . . . ? N1 Sn1 N4 Sn2 -89.6(5) . . . . ? N2 Sn1 N4 Sn2 -8.4(4) . . . . ? N2 Sn2 N4 C25 141.2(10) . . . . ? N3 Sn2 N4 C25 -134.9(10) . . . . ? Sn4 Sn2 N4 C25 -177.2(10) . . . . ? N2 Sn2 N4 Sn3 -90.6(5) . . . . ? N3 Sn2 N4 Sn3 -6.7(4) . . . . ? Sn4 Sn2 N4 Sn3 -48.9(4) . . . . ? N2 Sn2 N4 Sn1 8.5(4) . . . . ? N3 Sn2 N4 Sn1 92.4(5) . . . . ? Sn4 Sn2 N4 Sn1 50.1(3) . . . . ? Sn1 N1 C1 C2 137.9(12) . . . . ? Sn3 N1 C1 C2 15.0(17) . . . . ? Sn4 N1 C1 C2 -101.3(13) . . . . ? Sn1 N1 C1 C6 -48.9(17) . . . . ? Sn3 N1 C1 C6 -171.8(11) . . . . ? Sn4 N1 C1 C6 72.0(15) . . . . ? C6 C1 C2 C3 2(2) . . . . ? N1 C1 C2 C3 175.0(14) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C8 O1 C4 C3 174.0(18) . . . . ? C8 O1 C4 C5 -4(3) . . . . ? C2 C3 C4 O1 -179.7(15) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? O1 C4 C5 C6 178.6(16) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C4 C5 C6 C1 1(2) . . . . ? C4 C5 C6 C7 178.9(15) . . . . ? C2 C1 C6 C5 -2(2) . . . . ? N1 C1 C6 C5 -175.9(14) . . . . ? C2 C1 C6 C7 180.0(15) . . . . ? N1 C1 C6 C7 6(2) . . . . ? Sn4 N2 C9 C10 -4.5(19) . . . . ? Sn2 N2 C9 C10 -125.7(13) . . . . ? Sn1 N2 C9 C10 115.9(14) . . . . ? Sn4 N2 C9 C14 178.9(12) . . . . ? Sn2 N2 C9 C14 57.7(18) . . . . ? Sn1 N2 C9 C14 -60.6(17) . . . . ? C14 C9 C10 C11 0(2) . . . . ? N2 C9 C10 C11 -176.9(14) . . . . ? C9 C10 C11 C12 2(2) . . . . ? C10 C11 C12 C13 -3(2) . . . . ? C10 C11 C12 O2 176.4(15) . . . . ? C16 O2 C12 C11 -12(3) . . . . ? C16 O2 C12 C13 167.0(16) . . . . ? C11 C12 C13 C14 1(3) . . . . ? O2 C12 C13 C14 -178.1(17) . . . . ? C12 C13 C14 C9 1(3) . . . . ? C12 C13 C14 C15 -177.4(17) . . . . ? C10 C9 C14 C13 -2(3) . . . . ? N2 C9 C14 C13 175.2(16) . . . . ? C10 C9 C14 C15 176.7(17) . . . . ? N2 C9 C14 C15 -7(3) . . . . ? Sn3 N3 C17 C18 114.4(14) . . . . ? Sn4 N3 C17 C18 -122.7(14) . . . . ? Sn2 N3 C17 C18 -7.9(18) . . . . ? Sn3 N3 C17 C22 -64.1(17) . . . . ? Sn4 N3 C17 C22 58.8(16) . . . . ? Sn2 N3 C17 C22 173.5(11) . . . . ? C22 C17 C18 C19 -3(2) . . . . ? N3 C17 C18 C19 178.6(15) . . . . ? C17 C18 C19 C20 2(3) . . . . ? C24 O3 C20 C19 -174(2) . . . . ? C24 O3 C20 C21 8(3) . . . . ? C18 C19 C20 O3 -177.6(16) . . . . ? C18 C19 C20 C21 0(3) . . . . ? O3 C20 C21 C22 176.5(16) . . . . ? C19 C20 C21 C22 -1(3) . . . . ? C20 C21 C22 C17 0(3) . . . . ? C20 C21 C22 C23 177.3(16) . . . . ? C18 C17 C22 C21 2(2) . . . . ? N3 C17 C22 C21 -179.7(14) . . . . ? C18 C17 C22 C23 -175.4(14) . . . . ? N3 C17 C22 C23 3(2) . . . . ? Sn3 N4 C25 C26 113.1(14) . . . . ? Sn1 N4 C25 C26 -6.2(19) . . . . ? Sn2 N4 C25 C26 -127.3(13) . . . . ? Sn3 N4 C25 C30 -67.8(17) . . . . ? Sn1 N4 C25 C30 172.9(11) . . . . ? Sn2 N4 C25 C30 51.8(17) . . . . ? C30 C25 C26 C27 2(2) . . . . ? N4 C25 C26 C27 -179.0(14) . . . . ? C25 C26 C27 C28 -4(2) . . . . ? C26 C27 C28 C29 3(2) . . . . ? C26 C27 C28 O4 -176.0(15) . . . . ? C32 O4 C28 C29 166.7(17) . . . . ? C32 O4 C28 C27 -14(3) . . . . ? C27 C28 C29 C30 -2(3) . . . . ? O4 C28 C29 C30 177.7(15) . . . . ? C28 C29 C30 C25 0(2) . . . . ? C28 C29 C30 C31 176.2(15) . . . . ? C26 C25 C30 C29 0(2) . . . . ? N4 C25 C30 C29 -179.2(14) . . . . ? C26 C25 C30 C31 -176.0(15) . . . . ? N4 C25 C30 C31 5(2) . . . . ? C56 C51 C52 C53 -1(3) . . . . ? C50 C51 C52 C53 178(2) . . . . ? C52 C51 C56 C55 2(3) . . . . ? C50 C51 C56 C55 -177(2) . . . . ? C51 C52 C53 C54 0(4) . . . . ? C52 C53 C54 C55 2(5) . . . . ? C53 C54 C55 C56 -1(5) . . . . ? C51 C56 C55 C54 0(4) . . . . ? C60 C61 C62 C63 -173(6) . . . 3_776 ? C63 C61 C62 C63 6(6) . . . 3_776 ? C60 C61 C63 C62 172(6) . . . 3_776 ? C62 C61 C63 C62 -6(6) . . . 3_776 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.018 _refine_diff_density_min -1.968 _refine_diff_density_rms 0.231 data_dw0001 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H28 N4 O4 Sn4' _chemical_formula_weight 959.30 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 12.7836(7) _cell_length_b 12.7836(7) _cell_length_c 9.5220(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1556.09(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colurless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method ? _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 3.212 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.056 _exptl_absorpt_correction_T_max 0.966 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7211 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1381 _reflns_number_observed 1278 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'teXsan' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0126P)^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 ? _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 -0.01(4) _refine_ls_number_reflns 1377 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_obs 0.0198 _refine_ls_wR_factor_all 0.0443 _refine_ls_wR_factor_obs 0.0419 _refine_ls_goodness_of_fit_all 1.087 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.108 _refine_ls_restrained_S_obs 1.091 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sn1 Sn 0.38330(2) 0.43870(2) 0.12241(3) 0.02671(10) Uani 1 d . . O1 O 0.6912(3) 0.1025(2) 0.4970(3) 0.0416(7) Uani 1 d . . N1 N 0.5512(2) 0.4005(2) 0.1051(3) 0.0267(7) Uani 1 d . . C1 C 0.5884(3) 0.3248(3) 0.2043(4) 0.0249(9) Uani 1 d . . C2 C 0.6287(3) 0.2280(3) 0.1634(4) 0.0279(9) Uani 1 d . . H2 H 0.6341(3) 0.2118(3) 0.0663(4) 0.034 Uiso 1 calc R . C3 C 0.6611(3) 0.1550(3) 0.2625(4) 0.0315(9) Uani 1 d . . H3 H 0.6877(3) 0.0893(3) 0.2328(4) 0.038 Uiso 1 calc R . C4 C 0.6549(3) 0.1779(3) 0.4047(4) 0.0305(10) Uani 1 d . . C5 C 0.6174(4) 0.2736(4) 0.4468(4) 0.0376(11) Uani 1 d . . H5 H 0.6139(4) 0.2899(4) 0.5441(4) 0.045 Uiso 1 calc R . C6 C 0.5845(4) 0.3466(3) 0.3482(5) 0.0355(11) Uani 1 d . . H6 H 0.5588(4) 0.4124(3) 0.3790(5) 0.043 Uiso 1 calc R . C7 C 0.6434(4) 0.1035(4) 0.6309(6) 0.0604(15) Uani 1 d . . H7A H 0.6672(23) 0.0428(16) 0.6851(15) 0.091 Uiso 1 calc R . H7B H 0.5672(4) 0.1004(29) 0.6199(6) 0.091 Uiso 1 calc R . H7C H 0.6625(23) 0.1679(14) 0.6805(16) 0.091 Uiso 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 0.0274(2) 0.0266(2) 0.0261(2) 0.00108(13) 0.00316(14) -0.00129(12) O1 0.050(2) 0.039(2) 0.036(2) 0.0104(15) 0.004(2) 0.0191(15) N1 0.028(2) 0.024(2) 0.028(2) -0.0007(15) 0.002(2) 0.0004(14) C1 0.021(2) 0.025(2) 0.028(2) 0.004(2) -0.001(2) 0.000(2) C2 0.030(2) 0.026(2) 0.028(2) 0.000(2) 0.001(2) 0.004(2) C3 0.028(2) 0.024(2) 0.042(2) -0.002(2) 0.003(2) 0.007(2) C4 0.031(2) 0.031(2) 0.029(3) 0.001(2) 0.001(2) 0.010(2) C5 0.048(3) 0.038(3) 0.026(3) 0.001(2) 0.000(2) 0.008(2) C6 0.044(3) 0.025(2) 0.037(3) 0.000(2) 0.006(2) 0.009(2) C7 0.062(3) 0.066(3) 0.053(4) 0.030(3) 0.023(3) 0.022(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 N1 2.182(3) 3_565 ? Sn1 N1 2.207(3) . ? Sn1 N1 2.226(3) 2_665 ? O1 C4 1.384(5) . ? O1 C7 1.415(6) . ? N1 C1 1.434(5) . ? N1 Sn1 2.182(3) 4_655 ? N1 Sn1 2.226(3) 2_665 ? C1 C2 1.395(5) . ? C1 C6 1.399(6) . ? C2 C3 1.390(6) . ? C3 C4 1.387(6) . ? C4 C5 1.374(6) . ? C5 C6 1.389(6) . ? 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 N1 80.85(12) 3_565 . ? N1 Sn1 N1 80.44(13) 3_565 2_665 ? N1 Sn1 N1 80.38(12) . 2_665 ? C4 O1 C7 114.9(3) . . ? C1 N1 Sn1 124.5(2) . 4_655 ? C1 N1 Sn1 115.0(2) . . ? Sn1 N1 Sn1 98.85(12) 4_655 . ? C1 N1 Sn1 116.8(2) . 2_665 ? Sn1 N1 Sn1 98.30(12) 4_655 2_665 ? Sn1 N1 Sn1 98.98(12) . 2_665 ? C2 C1 C6 117.6(4) . . ? C2 C1 N1 122.5(4) . . ? C6 C1 N1 119.9(3) . . ? C3 C2 C1 121.0(4) . . ? C4 C3 C2 120.3(4) . . ? C5 C4 O1 123.5(4) . . ? C5 C4 C3 119.5(4) . . ? O1 C4 C3 117.0(3) . . ? C4 C5 C6 120.4(4) . . ? C5 C6 C1 121.2(4) . . ? _refine_diff_density_max 0.320 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.069 data_dw9960 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H52 N4 O8 Sn4' _chemical_formula_weight 1263.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.6406(15) _cell_length_b 8.9310(3) _cell_length_c 18.6514(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.982(2) _cell_angle_gamma 90.00 _cell_volume 4815.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method ? _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 2.105 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.041 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995); _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10524 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4581 _reflns_number_observed 3746 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'teXsan' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+27.8130P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4569 _refine_ls_number_parameters 257 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_obs 0.0420 _refine_ls_wR_factor_all 0.1345 _refine_ls_wR_factor_obs 0.1142 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.105 _refine_ls_restrained_S_all 1.171 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max 0.520 _refine_ls_shift/esd_mean 0.023 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sn1 Sn -0.013022(13) 0.18222(4) 0.82859(2) 0.02497(13) Uani 1 d . . Sn2 Sn 0.056077(13) 0.44630(4) 0.81163(2) 0.02569(13) Uani 1 d . . N1 N 0.04889(15) 0.2020(5) 0.8021(2) 0.0221(9) Uani 1 d . . N2 N -0.0118(2) 0.4254(5) 0.8162(3) 0.0242(10) Uani 1 d . . C1 C 0.0864(2) 0.1007(6) 0.8390(3) 0.0244(11) Uani 1 d . . C2 C 0.1268(2) 0.1464(6) 0.9021(3) 0.0298(12) Uani 1 d . . H2 H 0.1293(2) 0.2466(6) 0.9205(3) 0.036 Uiso 1 calc R . C3 C 0.1629(2) 0.0485(7) 0.9379(3) 0.0334(13) Uani 1 d . . C4 C 0.1601(2) -0.0991(7) 0.9095(4) 0.0344(14) Uani 1 d . . C5 C 0.1205(2) -0.1438(6) 0.8494(4) 0.0351(14) Uani 1 d . . H5 H 0.1179(2) -0.2440(6) 0.8309(4) 0.042 Uiso 1 calc R . C6 C 0.0839(2) -0.0451(6) 0.8143(4) 0.0320(13) Uani 1 d . . H6 H 0.0565(2) -0.0793(6) 0.7725(4) 0.038 Uiso 1 calc R . O7 O 0.2029(2) 0.0841(5) 1.0005(3) 0.0500(12) Uani 1 d . . C7 C 0.2052(3) 0.2290(10) 1.0350(5) 0.075(3) Uani 1 d . . H7A H 0.2335(12) 0.2363(29) 1.0833(22) 0.112 Uiso 1 calc R . H7B H 0.1782(12) 0.2434(31) 1.0472(36) 0.112 Uiso 1 calc R . H7C H 0.2056(23) 0.3063(11) 0.9979(16) 0.112 Uiso 1 calc R . O8 O 0.1984(2) -0.1879(5) 0.9485(3) 0.0472(12) Uani 1 d . . C8 C 0.1963(3) -0.3356(7) 0.9174(5) 0.053(2) Uani 1 d . . H8A H 0.2262(6) -0.3855(23) 0.9445(22) 0.080 Uiso 1 calc R . H8B H 0.1891(18) -0.3295(8) 0.8612(8) 0.080 Uiso 1 calc R . H8C H 0.1721(13) -0.3931(20) 0.9253(28) 0.080 Uiso 1 calc R . C9 C -0.0263(2) 0.5246(6) 0.8622(3) 0.0244(11) Uani 1 d . . C10 C -0.0479(2) 0.4727(6) 0.9093(3) 0.0280(12) Uani 1 d . . H10 H -0.0517(2) 0.3678(6) 0.9128(3) 0.034 Uiso 1 calc R . C11 C -0.0640(2) 0.5675(6) 0.9511(3) 0.0262(12) Uani 1 d . . C12 C -0.0585(2) 0.7236(6) 0.9473(3) 0.0285(12) Uani 1 d . . C13 C -0.0370(2) 0.7764(6) 0.9010(3) 0.0328(13) Uani 1 d . . H13 H -0.0331(2) 0.8813(6) 0.8976(3) 0.039 Uiso 1 calc R . C14 C -0.0209(2) 0.6790(6) 0.8590(3) 0.0308(13) Uani 1 d . . H14 H -0.0061(2) 0.7185(6) 0.8279(3) 0.037 Uiso 1 calc R . O15 O -0.0859(2) 0.5220(4) 0.9975(2) 0.0349(10) Uani 1 d . . C15 C -0.0947(3) 0.3637(6) 0.9963(4) 0.040(2) Uani 1 d . . H15A H -0.1141(13) 0.3434(9) 1.0249(23) 0.059 Uiso 1 calc R . H15B H -0.0653(3) 0.3099(7) 1.0214(24) 0.059 Uiso 1 calc R . H15C H -0.1107(14) 0.3299(12) 0.9419(4) 0.059 Uiso 1 calc R . O16 O -0.0750(2) 0.8110(4) 0.9906(2) 0.0353(10) Uani 1 d . . C16 C -0.0745(3) 0.9687(6) 0.9787(4) 0.040(2) Uani 1 d . . H16A H -0.0877(14) 1.0204(7) 1.0112(20) 0.060 Uiso 1 calc R . H16B H -0.0929(13) 0.9919(8) 0.9233(7) 0.060 Uiso 1 calc R . H16C H -0.0426(3) 1.0022(10) 0.9933(24) 0.060 Uiso 1 calc R . C100 C -0.1780(5) -0.0523(14) 0.8059(8) 0.118(2) Uiso 1 d D . H10B H -0.1515(21) -0.0740(15) 0.7931(58) 0.177 Uiso 1 calc R . H10C H -0.2057(13) -0.1005(18) 0.7672(41) 0.177 Uiso 1 calc R . H10D H -0.1719(35) -0.0910(22) 0.8583(18) 0.177 Uiso 1 calc R . C101 C -0.1849(5) 0.1023(16) 0.8044(8) 0.118(2) Uiso 1 d G . C102 C -0.1682(5) 0.1788(15) 0.7564(8) 0.118(2) Uiso 1 d GD . H102 H -0.1564(38) 0.1247(29) 0.7248(55) 0.142 Uiso 1 calc R . C103 C -0.1687(5) 0.3206(16) 0.7549(8) 0.118(2) Uiso 1 d G . H103 H -0.1553(5) 0.3687(16) 0.7238(8) 0.142 Uiso 1 calc R . C104 C -0.1879(5) 0.4137(16) 0.7961(8) 0.118(2) Uiso 1 d G . H104 H -0.1875(5) 0.5199(16) 0.7939(8) 0.142 Uiso 1 calc R . C105 C -0.2076(5) 0.3334(16) 0.8411(8) 0.118(2) Uiso 1 d G . H105 H -0.2229(5) 0.3855(16) 0.8680(8) 0.142 Uiso 1 calc R . C106 C -0.2043(5) 0.1827(15) 0.8450(8) 0.118(2) Uiso 1 d GD . H106 H -0.2160(5) 0.1307(15) 0.8775(8) 0.142 Uiso 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 0.0294(2) 0.0210(2) 0.0269(2) 0.00178(14) 0.0139(2) -0.00081(14) Sn2 0.0282(2) 0.0227(2) 0.0281(2) -0.00209(14) 0.0134(2) -0.00311(15) N1 0.019(2) 0.022(2) 0.025(2) 0.000(2) 0.008(2) 0.000(2) N2 0.028(2) 0.023(2) 0.025(2) -0.002(2) 0.014(2) -0.002(2) C1 0.026(3) 0.022(3) 0.028(3) 0.004(2) 0.014(2) 0.003(2) C2 0.031(3) 0.027(3) 0.033(3) -0.001(2) 0.015(3) -0.003(2) C3 0.025(3) 0.041(3) 0.033(3) 0.002(3) 0.010(3) -0.002(2) C4 0.024(3) 0.031(3) 0.042(3) 0.003(3) 0.007(3) 0.005(2) C5 0.033(3) 0.021(3) 0.050(4) 0.000(3) 0.014(3) 0.002(2) C6 0.024(3) 0.029(3) 0.037(3) 0.000(2) 0.006(3) -0.002(2) O7 0.031(2) 0.046(3) 0.054(3) -0.009(2) -0.002(2) 0.005(2) C7 0.049(5) 0.076(6) 0.066(5) -0.027(5) -0.011(4) 0.003(4) O8 0.030(2) 0.041(3) 0.060(3) 0.003(2) 0.007(2) 0.010(2) C8 0.039(4) 0.040(4) 0.079(5) 0.005(4) 0.023(4) 0.015(3) C9 0.026(3) 0.026(3) 0.023(3) 0.003(2) 0.012(2) -0.001(2) C10 0.035(3) 0.020(3) 0.032(3) 0.000(2) 0.017(3) 0.000(2) C11 0.026(3) 0.030(3) 0.025(3) 0.001(2) 0.013(2) -0.004(2) C12 0.036(3) 0.025(3) 0.026(3) -0.001(2) 0.014(3) 0.006(2) C13 0.048(4) 0.018(3) 0.039(3) -0.002(2) 0.025(3) -0.003(3) C14 0.042(3) 0.028(3) 0.029(3) 0.003(2) 0.022(3) -0.001(2) O15 0.047(3) 0.027(2) 0.044(2) -0.002(2) 0.033(2) -0.006(2) C15 0.061(5) 0.026(3) 0.043(4) -0.005(3) 0.033(3) -0.009(3) O16 0.049(3) 0.024(2) 0.045(2) -0.006(2) 0.032(2) 0.000(2) C16 0.055(4) 0.024(3) 0.051(4) 0.002(3) 0.032(3) 0.003(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 N2 2.186(4) . ? Sn1 N1 2.213(4) . ? Sn1 N1 2.239(4) 2_556 ? Sn2 N2 2.190(5) . ? Sn2 N1 2.193(4) . ? Sn2 N2 2.229(4) 2_556 ? N1 C1 1.427(7) . ? N1 Sn1 2.239(4) 2_556 ? N2 C9 1.434(7) . ? N2 Sn2 2.229(4) 2_556 ? C1 C6 1.373(8) . ? C1 C2 1.400(8) . ? C2 C3 1.378(8) . ? C3 O7 1.366(7) . ? C3 C4 1.410(8) . ? C4 C5 1.359(8) . ? C4 O8 1.382(7) . ? C5 C6 1.391(8) . ? O7 C7 1.434(9) . ? O8 C8 1.431(8) . ? C9 C10 1.393(8) . ? C9 C14 1.393(7) . ? C10 C11 1.381(8) . ? C11 O15 1.372(6) . ? C11 C12 1.411(8) . ? C12 O16 1.371(7) . ? C12 C13 1.382(8) . ? C13 C14 1.397(8) . ? O15 C15 1.440(7) . ? O16 C16 1.427(7) . ? C100 C101 1.40(2) . ? C101 C102 1.39 . ? C101 C106 1.36(2) . ? C102 C103 1.267(15) . ? C103 C104 1.42(2) . ? C104 C105 1.43(2) . ? C105 C106 1.35(2) . ? 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 N2 Sn1 N1 80.9(2) . . ? N2 Sn1 N1 80.2(2) . 2_556 ? N1 Sn1 N1 81.6(2) . 2_556 ? N2 Sn2 N1 81.2(2) . . ? N2 Sn2 N2 80.4(2) . 2_556 ? N1 Sn2 N2 80.3(2) . 2_556 ? C1 N1 Sn2 123.6(3) . . ? C1 N1 Sn1 118.7(3) . . ? Sn2 N1 Sn1 97.7(2) . . ? C1 N1 Sn1 115.4(3) . 2_556 ? Sn2 N1 Sn1 99.0(2) . 2_556 ? Sn1 N1 Sn1 97.7(2) . 2_556 ? C9 N2 Sn1 121.8(3) . . ? C9 N2 Sn2 122.0(3) . . ? Sn1 N2 Sn2 98.6(2) . . ? C9 N2 Sn2 111.9(3) . 2_556 ? Sn1 N2 Sn2 99.5(2) . 2_556 ? Sn2 N2 Sn2 98.7(2) . 2_556 ? C6 C1 C2 117.9(5) . . ? C6 C1 N1 121.1(5) . . ? C2 C1 N1 121.1(5) . . ? C3 C2 C1 121.1(5) . . ? O7 C3 C2 124.5(5) . . ? O7 C3 C4 115.7(5) . . ? C2 C3 C4 119.9(5) . . ? C5 C4 O8 125.6(5) . . ? C5 C4 C3 118.8(5) . . ? O8 C4 C3 115.6(5) . . ? C4 C5 C6 121.0(5) . . ? C1 C6 C5 121.3(5) . . ? C3 O7 C7 116.9(5) . . ? C4 O8 C8 115.5(5) . . ? C10 C9 C14 117.1(5) . . ? C10 C9 N2 122.1(5) . . ? C14 C9 N2 120.8(5) . . ? C11 C10 C9 122.7(5) . . ? O15 C11 C10 124.9(5) . . ? O15 C11 C12 115.4(5) . . ? C10 C11 C12 119.7(5) . . ? O16 C12 C13 125.2(5) . . ? O16 C12 C11 116.7(5) . . ? C13 C12 C11 118.1(5) . . ? C12 C13 C14 121.4(5) . . ? C9 C14 C13 120.9(5) . . ? C11 O15 C15 115.1(4) . . ? C12 O16 C16 116.0(4) . . ? C100 C101 C102 113.6(12) . . ? C100 C101 C106 128.0(12) . . ? C102 C101 C106 118.4(14) . . ? C103 C102 C101 120.1(15) . . ? C102 C103 C104 125.2(15) . . ? C105 C104 C103 114.1(13) . . ? C104 C105 C106 119.4(15) . . ? C105 C106 C101 122.7(15) . . ? _refine_diff_density_max 1.467 _refine_diff_density_min -1.767 _refine_diff_density_rms 0.145 data_dw9959 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H30 N4 O2 Sn3' _chemical_formula_weight 714.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c 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 12.2482(2) _cell_length_b 13.7235(2) _cell_length_c 14.4319(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.9670(10) _cell_angle_gamma 90.00 _cell_volume 2396.18(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method ? _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 3.125 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.079 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995); _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37964 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5493 _reflns_number_observed 4778 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'maXus' _computing_cell_refinement 'maXus' _computing_data_reduction 'maXus' _computing_structure_solution 'teXsan' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+3.4897P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5480 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_obs 0.0257 _refine_ls_wR_factor_all 0.0571 _refine_ls_wR_factor_obs 0.0530 _refine_ls_goodness_of_fit_all 1.066 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_restrained_S_all 1.101 _refine_ls_restrained_S_obs 1.100 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sn1 Sn 0.88924(2) 0.092665(15) 0.206834(14) 0.02238(6) Uani 1 d . . Sn2 Sn 0.64231(2) 0.06379(2) 0.082251(14) 0.02562(6) Uani 1 d . . Sn3 Sn 0.69602(2) -0.03390(2) 0.304229(15) 0.02828(6) Uani 1 d . . O1 O 0.8468(2) 0.0140(2) 0.0215(2) 0.0344(5) Uani 1 d . . O2 O 0.5515(2) 0.2283(2) 0.0612(2) 0.0386(6) Uani 1 d . . N1 N 0.7727(2) -0.0325(2) 0.1775(2) 0.0236(5) Uani 1 d . . N2 N 0.7503(2) 0.1737(2) 0.1461(2) 0.0257(6) Uani 1 d . . N3 N 0.8195(2) 0.0837(2) 0.3433(2) 0.0252(5) Uani 1 d . . N4 N 0.5621(2) 0.0457(2) 0.2131(2) 0.0327(6) Uani 1 d . . C1 C 0.8449(3) -0.0851(2) 0.0375(2) 0.0258(7) Uani 1 d . . C2 C 0.8075(2) -0.1093(2) 0.1230(2) 0.0226(6) Uani 1 d . . C3 C 0.8067(2) -0.2093(2) 0.1448(2) 0.0268(7) Uani 1 d . . C4 C 0.8411(3) -0.2774(2) 0.0835(2) 0.0330(7) Uani 1 d . . H4 H 0.8399(3) -0.3446(2) 0.0991(2) 0.040 Uiso 1 calc R . C5 C 0.8764(3) -0.2508(2) 0.0017(2) 0.0351(8) Uani 1 d . . H5 H 0.8996(3) -0.2989(2) -0.0383(2) 0.042 Uiso 1 calc R . C6 C 0.8779(3) -0.1528(2) -0.0224(2) 0.0314(7) Uani 1 d . . H6 H 0.9014(3) -0.1331(2) -0.0793(2) 0.038 Uiso 1 calc R . C7 C 0.8560(3) 0.0458(3) -0.0704(2) 0.0407(9) Uani 1 d . . H7A H 0.8450(20) 0.1165(4) -0.0746(5) 0.061 Uiso 1 calc R . H7B H 0.7997(14) 0.0133(14) -0.1156(3) 0.061 Uiso 1 calc R . H7C H 0.9296(8) 0.0296(16) -0.0844(7) 0.061 Uiso 1 calc R . C8 C 0.7688(3) -0.2468(3) 0.2318(3) 0.0440(9) Uani 1 d . . H8A H 0.6908(7) -0.2299(16) 0.2307(9) 0.066 Uiso 1 calc R . H8B H 0.8133(14) -0.2172(14) 0.2870(3) 0.066 Uiso 1 calc R . H8C H 0.7774(20) -0.3178(3) 0.2348(9) 0.066 Uiso 1 calc R . C9 C 0.6245(3) 0.3041(2) 0.0872(2) 0.0289(7) Uani 1 d . . C10 C 0.5977(3) 0.4005(2) 0.0686(2) 0.0338(8) Uani 1 d . . H10 H 0.5266(3) 0.4177(2) 0.0365(2) 0.041 Uiso 1 calc R . C11 C 0.6758(3) 0.4721(2) 0.0972(3) 0.0377(8) Uani 1 d . . H11 H 0.6594(3) 0.5388(2) 0.0841(3) 0.045 Uiso 1 calc R . C12 C 0.7779(3) 0.4446(2) 0.1450(2) 0.0341(8) Uani 1 d . . H12 H 0.8304(3) 0.4938(2) 0.1664(2) 0.041 Uiso 1 calc R . C13 C 0.8066(3) 0.3473(2) 0.1630(2) 0.0274(7) Uani 1 d . . C14 C 0.7302(2) 0.2721(2) 0.1332(2) 0.0247(6) Uani 1 d . . C15 C 0.4433(3) 0.2499(3) 0.0128(3) 0.0455(9) Uani 1 d . . H15A H 0.4071(9) 0.2965(15) 0.0495(9) 0.068 Uiso 1 calc R . H15B H 0.3997(8) 0.1898(4) 0.0042(16) 0.068 Uiso 1 calc R . H15C H 0.4491(3) 0.2782(18) -0.0487(8) 0.068 Uiso 1 calc R . C16 C 0.9220(3) 0.3251(2) 0.2113(3) 0.0364(8) Uani 1 d . . H16A H 0.9604(7) 0.3861(3) 0.2308(15) 0.055 Uiso 1 calc R . H16B H 0.9623(7) 0.2902(15) 0.1680(6) 0.055 Uiso 1 calc R . H16C H 0.9183(3) 0.2845(14) 0.2666(9) 0.055 Uiso 1 calc R . C17 C 0.7844(3) 0.1756(2) 0.3821(2) 0.0374(8) Uani 1 d . . H17A H 0.7396(16) 0.1613(2) 0.4311(12) 0.056 Uiso 1 calc R . H17B H 0.7404(17) 0.2134(8) 0.3320(4) 0.056 Uiso 1 calc R . H17C H 0.8497(3) 0.2132(8) 0.4089(15) 0.056 Uiso 1 calc R . C18 C 0.9034(3) 0.0370(3) 0.4156(2) 0.0363(8) Uani 1 d . . H18A H 0.8704(6) 0.0234(16) 0.4719(7) 0.054 Uiso 1 calc R . H18B H 0.9666(9) 0.0810(8) 0.4317(13) 0.054 Uiso 1 calc R . H18C H 0.9284(15) -0.0242(9) 0.3908(6) 0.054 Uiso 1 calc R . C19 C 0.5191(3) 0.1338(3) 0.2524(3) 0.0548(11) Uani 1 d . . H19A H 0.4991(23) 0.1187(6) 0.3140(9) 0.082 Uiso 1 calc R . H19B H 0.4535(15) 0.1567(13) 0.2104(10) 0.082 Uiso 1 calc R . H19C H 0.5759(9) 0.1847(8) 0.2592(19) 0.082 Uiso 1 calc R . C20 C 0.4722(3) -0.0283(4) 0.1920(3) 0.0559(12) Uani 1 d . . H20A H 0.4470(18) -0.0480(17) 0.2504(4) 0.084 Uiso 1 calc R . H20B H 0.5004(7) -0.0854(10) 0.1625(19) 0.084 Uiso 1 calc R . H20C H 0.4102(10) -0.0001(8) 0.1492(17) 0.084 Uiso 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 0.02133(11) 0.02198(11) 0.02396(11) 0.00015(8) 0.00399(8) 0.00002(8) Sn2 0.02323(11) 0.03239(13) 0.02079(11) -0.00173(9) 0.00204(8) 0.00029(9) Sn3 0.03005(12) 0.03149(13) 0.02407(11) 0.00169(9) 0.00666(9) -0.00542(9) O1 0.0493(14) 0.0228(12) 0.0344(13) 0.0024(10) 0.0174(11) -0.0007(10) O2 0.0282(12) 0.0367(14) 0.0466(14) 0.0028(11) -0.0078(10) 0.0055(10) N1 0.0252(13) 0.0215(13) 0.0244(13) -0.0027(10) 0.0047(10) -0.0015(10) N2 0.0271(13) 0.0224(13) 0.0266(13) 0.0004(10) 0.0013(10) 0.0027(11) N3 0.0307(14) 0.0250(13) 0.0196(12) -0.0005(10) 0.0032(10) 0.0014(11) N4 0.0214(13) 0.051(2) 0.0270(14) -0.0043(12) 0.0062(11) 0.0004(12) C1 0.028(2) 0.0176(15) 0.031(2) -0.0030(12) 0.0038(13) -0.0006(12) C2 0.0192(14) 0.023(2) 0.0247(15) -0.0042(12) 0.0005(11) -0.0008(12) C3 0.025(2) 0.025(2) 0.029(2) -0.0001(13) -0.0013(12) -0.0034(13) C4 0.038(2) 0.021(2) 0.039(2) -0.0009(14) -0.0004(15) 0.0042(14) C5 0.042(2) 0.029(2) 0.035(2) -0.0092(14) 0.0082(15) 0.0042(15) C6 0.041(2) 0.028(2) 0.027(2) -0.0016(13) 0.0107(14) -0.0004(14) C7 0.051(2) 0.036(2) 0.039(2) 0.004(2) 0.017(2) 0.001(2) C8 0.054(2) 0.040(2) 0.039(2) 0.001(2) 0.010(2) 0.000(2) C9 0.029(2) 0.029(2) 0.029(2) 0.0040(13) 0.0076(13) 0.0027(14) C10 0.032(2) 0.035(2) 0.036(2) 0.0081(15) 0.0088(14) 0.0128(15) C11 0.045(2) 0.024(2) 0.046(2) 0.0087(15) 0.013(2) 0.010(2) C12 0.040(2) 0.026(2) 0.038(2) 0.0034(14) 0.014(2) 0.0028(15) C13 0.032(2) 0.026(2) 0.026(2) 0.0036(13) 0.0087(13) 0.0020(13) C14 0.028(2) 0.026(2) 0.0215(15) 0.0062(12) 0.0064(12) 0.0068(13) C15 0.031(2) 0.050(2) 0.050(2) 0.000(2) -0.010(2) 0.007(2) C16 0.035(2) 0.026(2) 0.046(2) 0.0038(15) 0.001(2) -0.0030(14) C17 0.051(2) 0.034(2) 0.029(2) -0.0075(14) 0.011(2) -0.002(2) C18 0.036(2) 0.044(2) 0.025(2) 0.0046(15) -0.0048(14) -0.003(2) C19 0.047(2) 0.078(3) 0.043(2) -0.002(2) 0.015(2) 0.030(2) C20 0.031(2) 0.103(4) 0.035(2) -0.001(2) 0.008(2) -0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N2 2.106(2) . ? Sn1 N1 2.232(2) . ? Sn1 N3 2.269(2) . ? Sn1 Sn2 3.2926(3) . ? Sn2 N2 2.120(2) . ? Sn2 N4 2.274(3) . ? Sn2 N1 2.346(2) . ? Sn2 O2 2.515(2) . ? Sn3 N1 2.182(2) . ? Sn3 N4 2.223(3) . ? Sn3 N3 2.224(3) . ? O1 C1 1.380(4) . ? O1 C7 1.416(4) . ? O2 C9 1.384(4) . ? O2 C15 1.429(4) . ? N1 C2 1.419(4) . ? N2 C14 1.379(4) . ? N3 C17 1.471(4) . ? N3 C18 1.491(4) . ? N4 C19 1.468(5) . ? N4 C20 1.494(5) . ? C1 C6 1.373(4) . ? C1 C2 1.421(4) . ? C2 C3 1.409(4) . ? C3 C4 1.396(4) . ? C3 C8 1.497(5) . ? C4 C5 1.369(5) . ? C5 C6 1.389(5) . ? C9 C10 1.380(5) . ? C9 C14 1.429(4) . ? C10 C11 1.389(5) . ? C11 C12 1.383(5) . ? C12 C13 1.395(4) . ? C13 C14 1.415(4) . ? C13 C16 1.506(4) . ? 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 N2 Sn1 N1 82.89(9) . . ? N2 Sn1 N3 90.03(9) . . ? N1 Sn1 N3 78.84(9) . . ? N2 Sn1 Sn2 38.98(7) . . ? N1 Sn1 Sn2 45.40(6) . . ? N3 Sn1 Sn2 91.69(6) . . ? N2 Sn2 N4 92.17(10) . . ? N2 Sn2 N1 79.91(9) . . ? N4 Sn2 N1 78.14(9) . . ? N2 Sn2 O2 69.37(8) . . ? N4 Sn2 O2 87.60(9) . . ? N1 Sn2 O2 145.56(8) . . ? N2 Sn2 Sn1 38.68(7) . . ? N4 Sn2 Sn1 92.23(7) . . ? N1 Sn2 Sn1 42.65(6) . . ? O2 Sn2 Sn1 108.02(5) . . ? N1 Sn3 N4 82.76(9) . . ? N1 Sn3 N3 80.90(9) . . ? N4 Sn3 N3 101.74(10) . . ? C1 O1 C7 117.8(3) . . ? C9 O2 C15 119.2(3) . . ? C9 O2 Sn2 112.7(2) . . ? C15 O2 Sn2 127.2(2) . . ? C2 N1 Sn3 131.6(2) . . ? C2 N1 Sn1 115.9(2) . . ? Sn3 N1 Sn1 101.17(10) . . ? C2 N1 Sn2 109.2(2) . . ? Sn3 N1 Sn2 98.84(9) . . ? Sn1 N1 Sn2 91.95(9) . . ? C14 N2 Sn1 133.5(2) . . ? C14 N2 Sn2 123.5(2) . . ? Sn1 N2 Sn2 102.35(10) . . ? C17 N3 C18 108.2(2) . . ? C17 N3 Sn3 119.4(2) . . ? C18 N3 Sn3 103.5(2) . . ? C17 N3 Sn1 117.1(2) . . ? C18 N3 Sn1 108.6(2) . . ? Sn3 N3 Sn1 98.77(9) . . ? C19 N4 C20 110.0(3) . . ? C19 N4 Sn3 116.8(2) . . ? C20 N4 Sn3 103.8(2) . . ? C19 N4 Sn2 117.3(2) . . ? C20 N4 Sn2 107.8(2) . . ? Sn3 N4 Sn2 99.82(10) . . ? C6 C1 O1 123.2(3) . . ? C6 C1 C2 123.8(3) . . ? O1 C1 C2 113.0(3) . . ? C3 C2 N1 125.8(3) . . ? C3 C2 C1 115.8(3) . . ? N1 C2 C1 118.3(3) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 C8 117.7(3) . . ? C2 C3 C8 122.4(3) . . ? C5 C4 C3 122.3(3) . . ? C4 C5 C6 119.6(3) . . ? C1 C6 C5 118.7(3) . . ? C10 C9 O2 122.9(3) . . ? C10 C9 C14 123.8(3) . . ? O2 C9 C14 113.3(3) . . ? C9 C10 C11 119.2(3) . . ? C12 C11 C10 118.9(3) . . ? C11 C12 C13 122.4(3) . . ? C12 C13 C14 120.4(3) . . ? C12 C13 C16 118.1(3) . . ? C14 C13 C16 121.4(3) . . ? N2 C14 C13 125.3(3) . . ? N2 C14 C9 119.5(3) . . ? C13 C14 C9 115.2(3) . . ? _refine_diff_density_max 0.884 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.100 data_Mx427 _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'c32 h36 n4 o4 sn4' _chemical_formula_weight 1015.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'c' 'c' 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'h' 'h' 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'n' 'n' 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'o' 'o' 0.0106 0.0060 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'sn' 'sn' -0.6537 1.4246 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_h-m P-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' _cell_length_a 9.9679(16) _cell_length_b 9.9679(16) _cell_length_c 8.505(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 845.0(4) _cell_formula_units_z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.75 _cell_measurement_theta_max 12.96 _exptl_crystal_description ? _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.38mm _exptl_crystal_size_mid 0.34mm _exptl_crystal_size_min 0.28mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 488 _exptl_absorpt_coefficient_mu 2.963 _exptl_absorpt_correction_type Difabs _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1270 _diffrn_reflns_av_r_equivalents 0.0408 _diffrn_reflns_av_sigmai/neti 0.0329 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1125 _reflns_number_gt 1069 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0369P)^2^+2.3584P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(9) _refine_ls_number_reflns 1125 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 1.827 _refine_ls_shift/su_mean 0.024 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 0.65471(6) 0.42424(6) 0.36606(7) 0.03126(18) Uani 1 1 d . . . N1 N 0.4390(7) 0.3721(7) 0.3723(8) 0.0317(14) Uani 1 1 d . . . C1 C 0.3636(9) 0.2771(9) 0.2861(10) 0.036(2) Uani 1 1 d . . . C2 C 0.4063(10) 0.2078(9) 0.1539(11) 0.041(2) Uani 1 1 d . . . C21 C 0.5434(11) 0.2304(10) 0.0828(11) 0.051(2) Uani 1 1 d . . . H21A H 0.5553 0.3251 0.0608 0.077 Uiso 1 1 calc R . . H21B H 0.5511 0.1797 -0.0141 0.077 Uiso 1 1 calc R . . H21C H 0.6118 0.2009 0.1562 0.077 Uiso 1 1 calc R . . C3 C 0.3211(12) 0.1185(10) 0.0803(13) 0.052(3) Uani 1 1 d . . . H3 H 0.3525 0.0698 -0.0069 0.062 Uiso 1 1 calc R . . C4 C 0.1924(13) 0.0990(10) 0.1309(17) 0.064(3) Uani 1 1 d . . . H4 H 0.1366 0.0372 0.0790 0.076 Uiso 1 1 calc R . . C5 C 0.1452(11) 0.1696(11) 0.2569(13) 0.054(3) Uani 1 1 d . . . H5 H 0.0565 0.1573 0.2916 0.064 Uiso 1 1 calc R . . C6 C 0.2286(9) 0.2592(9) 0.3331(11) 0.035(2) Uani 1 1 d . . . O61 O 0.1890(6) 0.3355(7) 0.4595(8) 0.0470(17) Uani 1 1 d . . . C62 C 0.0580(11) 0.3196(17) 0.5153(17) 0.083(4) Uani 1 1 d . . . H62A H -0.0051 0.3416 0.4324 0.124 Uiso 1 1 calc R . . H62B H 0.0436 0.3788 0.6042 0.124 Uiso 1 1 calc R . . H62C H 0.0446 0.2274 0.5480 0.124 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 0.0298(3) 0.0322(3) 0.0317(3) -0.0014(3) 0.0037(3) 0.0016(3) N1 0.031(3) 0.037(3) 0.027(3) -0.006(4) -0.001(4) -0.007(3) C1 0.041(5) 0.036(5) 0.031(4) 0.001(4) -0.010(4) 0.000(4) C2 0.056(5) 0.038(4) 0.029(5) -0.002(4) -0.006(5) 0.006(4) C21 0.074(7) 0.047(5) 0.032(5) -0.014(5) -0.003(5) 0.007(6) C3 0.072(7) 0.035(5) 0.049(6) -0.013(5) -0.025(6) 0.006(5) C4 0.081(8) 0.039(5) 0.071(8) -0.014(6) -0.044(8) -0.006(5) C5 0.049(6) 0.053(6) 0.059(6) 0.011(6) -0.021(5) -0.003(5) C6 0.038(5) 0.029(4) 0.038(6) 0.004(4) -0.007(4) 0.001(4) O61 0.035(3) 0.054(4) 0.053(4) -0.008(4) 0.002(3) -0.002(3) C62 0.036(6) 0.135(13) 0.077(9) -0.018(10) 0.013(6) -0.009(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 N1 2.213(6) . ? Sn1 N1 2.235(7) 2_665 ? Sn1 N1 2.246(7) 4_656 ? N1 C1 1.414(10) . ? N1 Sn1 2.235(7) 2_665 ? N1 Sn1 2.246(7) 3_566 ? C1 C2 1.387(13) . ? C1 C6 1.414(13) . ? C2 C3 1.381(13) . ? C2 C21 1.511(15) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C3 C4 1.367(17) . ? C3 H3 0.9400 . ? C4 C5 1.366(17) . ? C4 H4 0.9400 . ? C5 C6 1.382(13) . ? C5 H5 0.9400 . ? C6 O61 1.375(11) . ? O61 C62 1.398(12) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? 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 N1 78.8(3) . 2_665 ? N1 Sn1 N1 82.9(3) . 4_656 ? N1 Sn1 N1 82.4(3) 2_665 4_656 ? C1 N1 Sn1 131.4(6) . . ? C1 N1 Sn1 111.9(5) . 2_665 ? Sn1 N1 Sn1 101.1(3) . 2_665 ? C1 N1 Sn1 113.5(5) . 3_566 ? Sn1 N1 Sn1 96.6(3) . 3_566 ? Sn1 N1 Sn1 96.0(3) 2_665 3_566 ? C2 C1 C6 117.3(9) . . ? C2 C1 N1 126.2(9) . . ? C6 C1 N1 116.3(8) . . ? C1 C2 C3 120.0(10) . . ? C1 C2 C21 121.9(9) . . ? C3 C2 C21 118.1(9) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C3 C4 121.8(11) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 119.8(10) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.6(11) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? O61 C6 C5 123.4(9) . . ? O61 C6 C1 115.1(8) . . ? C5 C6 C1 121.4(9) . . ? C6 O61 C62 118.1(9) . . ? O61 C62 H62A 109.5 . . ? O61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.674 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.108