Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Wright, Dominic S.' 'Bond, Andrew D.' 'Harron, Eilis A.' 'Lawson, Gavin T.' 'McPartlin, M.' 'Mosquera, Marta E. G.' _publ_contact_author_name 'Dr Dominic S Wright' _publ_contact_author_address ; Contact Address Dr Dominic S Wright University of Cambridge Lensfiedl Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'DSW1000@CUS.CAM.AC.UK' _publ_section_title ; Nucleophilic Addition to a Sn(II) imido Cubane, [SnNR]4; a New Route to Heteroleptic Stannates ; data_mw0123 _database_code_CSD 185248 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H72 K2 N2 O8 Sn2' _chemical_formula_weight 1024.58 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' 'K' 'K' 0.2009 0.2494 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9548(3) _cell_length_b 12.5067(4) _cell_length_c 16.5675(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.344(2) _cell_angle_gamma 90.00 _cell_volume 2475.02(13) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 17806 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD' _diffrn_reflns_number 22569 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4347 _reflns_number_gt 3677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _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^)+(0.0334P)^2^+1.3796P] 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 4347 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.214032(15) 0.163019(15) 0.966943(11) 0.04733(9) Uani 1 1 d . . . K1 K 0.01745(5) -0.06310(5) 0.89507(3) 0.04679(15) Uani 1 1 d . . . N1 N 0.0740(2) 0.16187(18) 0.88092(14) 0.0483(6) Uiso 1 1 d . . . H1N H 0.0346 0.2181 0.8980 0.054(8) Uiso 1 1 d . . . O1 O 0.2172(2) 0.0359(2) 0.81088(13) 0.0736(7) Uani 1 1 d . . . O3 O 0.09836(16) 0.22669(15) 1.04436(11) 0.0502(5) Uani 1 1 d . . . O2 O 0.17101(14) 0.01156(14) 1.00823(11) 0.0440(4) Uani 1 1 d . . . O4 O -0.0109(2) -0.1195(2) 0.73199(13) 0.0789(7) Uani 1 1 d . . . C1 C 0.1607(3) 0.1064(3) 0.75965(18) 0.0599(8) Uani 1 1 d . . . C2 C 0.0840(3) 0.1726(2) 0.79789(17) 0.0507(7) Uani 1 1 d . . . C3 C 0.0194(3) 0.2438(3) 0.74927(19) 0.0624(8) Uani 1 1 d . . . C4 C 0.0326(4) 0.2447(3) 0.6659(2) 0.0794(11) Uani 1 1 d . . . H4 H -0.0123 0.2905 0.6333 0.095 Uiso 1 1 calc R . . C5 C 0.1094(4) 0.1803(4) 0.6305(2) 0.0875(13) Uani 1 1 d . . . H5 H 0.1173 0.1832 0.5743 0.105 Uiso 1 1 calc R . . C6 C 0.1751(4) 0.1112(3) 0.6768(2) 0.0790(11) Uani 1 1 d . . . H6 H 0.2288 0.0680 0.6528 0.095 Uiso 1 1 calc R . . C7 C -0.0615(3) 0.3180(3) 0.7874(2) 0.0795(11) Uani 1 1 d . . . H7A H -0.0935 0.3660 0.7466 0.119 Uiso 1 1 calc R . . H7B H -0.0226 0.3593 0.8294 0.119 Uiso 1 1 calc R . . H7C H -0.1207 0.2767 0.8108 0.119 Uiso 1 1 calc R . . C8 C 0.3035(4) -0.0270(5) 0.7787(3) 0.123(2) Uani 1 1 d . . . H8A H 0.2729 -0.0699 0.7343 0.185 Uiso 1 1 calc R . . H8B H 0.3351 -0.0737 0.8205 0.185 Uiso 1 1 calc R . . H8C H 0.3617 0.0194 0.7594 0.185 Uiso 1 1 calc R . . C20 C 0.2478(2) -0.0609(2) 1.04667(17) 0.0510(7) Uani 1 1 d . . . C21 C 0.2352(4) -0.0544(4) 1.1374(2) 0.0876(12) Uani 1 1 d . . . H21A H 0.2517 0.0178 1.1558 0.131 Uiso 1 1 calc R . . H21B H 0.2869 -0.1039 1.1643 0.131 Uiso 1 1 calc R . . H21C H 0.1591 -0.0728 1.1501 0.131 Uiso 1 1 calc R . . C22 C 0.2136(3) -0.1732(3) 1.0179(3) 0.0776(10) Uani 1 1 d . . . H22A H 0.1353 -0.1851 1.0282 0.116 Uiso 1 1 calc R . . H22B H 0.2590 -0.2260 1.0469 0.116 Uiso 1 1 calc R . . H22C H 0.2248 -0.1795 0.9605 0.116 Uiso 1 1 calc R . . C23 C 0.3672(3) -0.0438(4) 1.0234(3) 0.0925(13) Uani 1 1 d . . . H23A H 0.3709 -0.0458 0.9650 0.139 Uiso 1 1 calc R . . H23B H 0.4142 -0.0998 1.0469 0.139 Uiso 1 1 calc R . . H23C H 0.3932 0.0252 1.0432 0.139 Uiso 1 1 calc R . . C30 C 0.1114(3) 0.3279(2) 1.08275(19) 0.0554(7) Uani 1 1 d . . . C31 C 0.1402(4) 0.4141(3) 1.0220(2) 0.0802(11) Uani 1 1 d . . . H31A H 0.2146 0.4012 1.0028 0.120 Uiso 1 1 calc R . . H31B H 0.1382 0.4837 1.0478 0.120 Uiso 1 1 calc R . . H31C H 0.0861 0.4124 0.9768 0.120 Uiso 1 1 calc R . . C32 C 0.2013(4) 0.3211(4) 1.1492(3) 0.0982(14) Uani 1 1 d . . . H32A H 0.1832 0.2643 1.1863 0.147 Uiso 1 1 calc R . . H32B H 0.2057 0.3885 1.1781 0.147 Uiso 1 1 calc R . . H32C H 0.2728 0.3060 1.1259 0.147 Uiso 1 1 calc R . . C33 C -0.0012(4) 0.3545(3) 1.1182(3) 0.0788(11) Uani 1 1 d . . . H33A H -0.0581 0.3595 1.0749 0.118 Uiso 1 1 calc R . . H33B H 0.0043 0.4222 1.1466 0.118 Uiso 1 1 calc R . . H33C H -0.0213 0.2986 1.1555 0.118 Uiso 1 1 calc R . . C42 C -0.0894(3) -0.0539(3) 0.6877(2) 0.0777(10) Uani 1 1 d . A . H42A H -0.0773 0.0214 0.7019 0.093 Uiso 1 1 calc R . . H42B H -0.1659 -0.0734 0.7010 0.093 Uiso 1 1 calc R . . C43 C -0.0738(3) -0.0701(3) 0.6000(2) 0.0787(10) Uani 1 1 d . . . H43A H -0.1407 -0.1021 0.5739 0.094 Uiso 1 1 calc R A . H43B H -0.0581 -0.0020 0.5735 0.094 Uiso 1 1 calc R . . C44 C 0.0235(4) -0.1437(4) 0.5961(2) 0.0935(13) Uani 1 1 d . A . H44A H 0.0924 -0.1040 0.5868 0.112 Uiso 0.88(3) 1 calc PR A 1 H44B H 0.0115 -0.1965 0.5529 0.112 Uiso 0.88(3) 1 calc PR A 1 H44C H 0.0800 -0.1123 0.5620 0.112 Uiso 0.12(3) 1 calc PR A 2 H44D H -0.0008 -0.2117 0.5719 0.112 Uiso 0.12(3) 1 calc PR A 2 C45 C 0.0295(13) -0.1961(8) 0.6761(4) 0.089(3) Uani 0.88(3) 1 d P A 1 H45A H -0.0171 -0.2605 0.6756 0.106 Uiso 0.88(3) 1 calc PR A 1 H45B H 0.1068 -0.2163 0.6910 0.106 Uiso 0.88(3) 1 calc PR A 1 C45' C 0.075(4) -0.164(4) 0.681(2) 0.055(11) Uiso 0.12(3) 1 d P A 2 H45C H 0.0862 -0.2403 0.6912 0.067 Uiso 0.12(3) 1 calc PR A 2 H45D H 0.1465 -0.1263 0.6893 0.067 Uiso 0.12(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.04004(13) 0.04959(14) 0.05311(14) 0.00225(9) 0.01115(9) -0.00716(8) K1 0.0471(3) 0.0494(4) 0.0443(3) -0.0001(3) 0.0071(3) -0.0047(3) O1 0.0766(15) 0.0841(16) 0.0624(13) 0.0058(12) 0.0291(12) 0.0182(13) O3 0.0537(11) 0.0448(11) 0.0529(11) -0.0057(9) 0.0117(9) -0.0057(9) O2 0.0362(9) 0.0459(10) 0.0500(10) 0.0043(8) 0.0050(8) 0.0018(8) O4 0.116(2) 0.0717(15) 0.0500(12) -0.0019(12) 0.0122(13) 0.0085(15) C1 0.070(2) 0.064(2) 0.0470(16) 0.0047(15) 0.0164(15) -0.0130(17) C2 0.0599(18) 0.0501(17) 0.0426(15) 0.0066(13) 0.0076(13) -0.0153(14) C3 0.080(2) 0.0535(19) 0.0526(17) 0.0138(14) -0.0062(16) -0.0212(17) C4 0.106(3) 0.071(2) 0.061(2) 0.0217(19) -0.013(2) -0.031(2) C5 0.126(4) 0.093(3) 0.0432(19) 0.012(2) 0.008(2) -0.041(3) C6 0.099(3) 0.087(3) 0.0526(19) -0.0055(19) 0.030(2) -0.030(2) C7 0.088(3) 0.063(2) 0.085(3) 0.0155(19) -0.019(2) 0.0017(19) C8 0.125(4) 0.145(4) 0.104(3) 0.009(3) 0.057(3) 0.063(4) C20 0.0430(14) 0.0592(18) 0.0512(16) 0.0033(13) 0.0067(12) 0.0116(13) C21 0.093(3) 0.111(3) 0.058(2) 0.003(2) -0.0047(19) 0.029(2) C22 0.069(2) 0.071(2) 0.093(3) 0.004(2) 0.008(2) 0.0176(18) C23 0.0454(18) 0.107(3) 0.126(3) 0.037(3) 0.016(2) 0.0144(19) C30 0.067(2) 0.0428(16) 0.0565(17) -0.0051(13) 0.0061(15) -0.0008(14) C31 0.096(3) 0.0500(19) 0.096(3) 0.0052(19) 0.022(2) -0.0049(19) C32 0.113(4) 0.094(3) 0.085(3) -0.023(2) -0.030(3) -0.001(3) C33 0.099(3) 0.050(2) 0.091(3) -0.0109(18) 0.036(2) 0.0047(18) C42 0.090(3) 0.081(3) 0.064(2) -0.0063(19) 0.0194(19) 0.011(2) C43 0.089(3) 0.087(3) 0.061(2) -0.0079(18) 0.0073(19) 0.011(2) C44 0.110(3) 0.111(3) 0.060(2) -0.012(2) 0.013(2) 0.032(3) C45 0.113(7) 0.076(4) 0.078(3) -0.002(3) 0.017(3) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O3 2.0824(18) . ? Sn1 O2 2.0855(17) . ? Sn1 N1 2.154(2) . ? K1 O3 2.6876(19) 3_557 ? K1 O2 2.7342(19) . ? K1 O4 2.799(2) . ? K1 O2 2.8903(17) 3_557 ? K1 N1 2.905(2) . ? K1 O1 3.075(2) . ? N1 C2 1.392(4) . ? O1 C1 1.381(4) . ? O1 C8 1.419(4) . ? O3 C30 1.423(3) . ? O3 K1 2.6876(19) 3_557 ? O2 C20 1.422(3) . ? O2 K1 2.8903(17) 3_557 ? O4 C45 1.430(6) . ? O4 C42 1.427(4) . ? O4 C45' 1.46(4) . ? C1 C2 1.406(4) . ? C1 C6 1.391(4) . ? C2 C3 1.410(4) . ? C3 C4 1.396(5) . ? C3 C7 1.498(5) . ? C4 C5 1.371(6) . ? C5 C6 1.380(6) . ? C20 C23 1.509(4) . ? C20 C21 1.520(4) . ? C20 C22 1.533(5) . ? C30 C32 1.509(5) . ? C30 C31 1.524(4) . ? C30 C33 1.527(5) . ? C42 C43 1.486(5) . ? C43 C44 1.487(5) . ? C44 C45 1.477(7) . ? C44 C45' 1.53(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 O3 Sn1 O2 88.08(7) . . ? O3 Sn1 N1 83.82(8) . . ? O2 Sn1 N1 90.89(8) . . ? O3 K1 O2 110.22(6) 3_557 . ? O3 K1 O4 97.17(7) 3_557 . ? O2 K1 O4 143.05(7) . . ? O3 K1 O2 62.46(5) 3_557 3_557 ? O2 K1 O2 93.47(5) . 3_557 ? O4 K1 O2 121.65(7) . 3_557 ? O3 K1 N1 153.18(6) 3_557 . ? O2 K1 N1 64.70(6) . . ? O4 K1 N1 100.68(7) . . ? O2 K1 N1 91.03(6) 3_557 . ? O3 K1 O1 153.83(6) 3_557 . ? O2 K1 O1 70.20(6) . . ? O4 K1 O1 74.29(7) . . ? O2 K1 O1 143.04(6) 3_557 . ? N1 K1 O1 52.10(6) . . ? C2 N1 Sn1 123.84(19) . . ? C2 N1 K1 101.72(16) . . ? Sn1 N1 K1 97.48(8) . . ? C1 O1 C8 117.9(3) . . ? C1 O1 K1 99.61(17) . . ? C8 O1 K1 122.5(3) . . ? C30 O3 Sn1 123.51(17) . . ? C30 O3 K1 124.02(16) . 3_557 ? Sn1 O3 K1 107.70(7) . 3_557 ? C20 O2 Sn1 124.22(16) . . ? C20 O2 K1 119.50(16) . . ? Sn1 O2 K1 104.65(7) . . ? C20 O2 K1 113.43(14) . 3_557 ? Sn1 O2 K1 100.81(6) . 3_557 ? K1 O2 K1 86.53(5) . 3_557 ? C45 O4 C42 106.5(4) . . ? C45 O4 C45' 27.1(18) . . ? C42 O4 C45' 112.5(15) . . ? C45 O4 K1 139.7(4) . . ? C42 O4 K1 113.76(18) . . ? C45' O4 K1 126.3(16) . . ? O1 C1 C2 114.2(2) . . ? O1 C1 C6 123.8(3) . . ? C2 C1 C6 121.9(3) . . ? N1 C2 C1 118.2(3) . . ? N1 C2 C3 123.9(3) . . ? C1 C2 C3 117.8(3) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 C7 120.8(3) . . ? C2 C3 C7 119.9(3) . . ? C5 C4 C3 121.5(4) . . ? C4 C5 C6 120.4(3) . . ? C5 C6 C1 119.0(4) . . ? O2 C20 C23 113.3(3) . . ? O2 C20 C21 108.7(2) . . ? C23 C20 C21 112.2(3) . . ? O2 C20 C22 106.6(2) . . ? C23 C20 C22 107.1(3) . . ? C21 C20 C22 108.7(3) . . ? O3 C30 C32 109.7(3) . . ? O3 C30 C31 111.0(3) . . ? C32 C30 C31 110.4(3) . . ? O3 C30 C33 106.4(3) . . ? C32 C30 C33 110.2(3) . . ? C31 C30 C33 109.0(3) . . ? O4 C42 C43 108.5(3) . . ? C44 C43 C42 104.9(3) . . ? C43 C44 C45 104.1(4) . . ? C43 C44 C45' 110.3(14) . . ? C45 C44 C45' 26.0(17) . . ? O4 C45 C44 106.2(4) . . ? O4 C45' C44 102(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.661 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.055 data_mw0144 _database_code_CSD 185249 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H17 Li N3 O Sn' _chemical_formula_weight 344.92 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' 'Li' 'Li' -0.0003 0.0001 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3386(2) _cell_length_b 9.7200(3) _cell_length_c 17.1794(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.946(2) _cell_angle_gamma 90.00 _cell_volume 1544.42(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7204 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.645 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD' _diffrn_reflns_number 13564 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3505 _reflns_number_gt 2914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _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^)+(0.0360P)^2^+0.7752P] 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 3505 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.008 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 0.621559(18) 0.109887(19) 0.785293(10) 0.02798(8) Uani 1 1 d . . . O1 O 0.4018(2) -0.1357(2) 0.74584(12) 0.0362(5) Uani 1 1 d . . . N1 N 0.6361(3) -0.0939(2) 0.84324(14) 0.0278(5) Uani 1 1 d . . . H1N H 0.707(3) -0.094(3) 0.8772(17) 0.027(8) Uiso 1 1 d . . . N2 N 0.8522(2) 0.1340(2) 0.80733(14) 0.0301(5) Uani 1 1 d . . . N3 N 0.6773(2) 0.0062(2) 0.68270(12) 0.0328(5) Uani 1 1 d . . . C1 C 0.9224(3) 0.1322(4) 0.89023(19) 0.0459(8) Uani 1 1 d . . . C2 C 0.9153(3) 0.0292(3) 0.76108(17) 0.0366(7) Uani 1 1 d . . . H2A H 0.9105 -0.0620 0.7863 0.044 Uiso 1 1 calc R . . H2B H 1.0181 0.0510 0.7587 0.044 Uiso 1 1 calc R . . C3 C 0.8326(3) 0.0253(3) 0.67875(17) 0.0387(7) Uani 1 1 d . . . H3A H 0.8478 0.1125 0.6512 0.046 Uiso 1 1 calc R . . H3B H 0.8688 -0.0512 0.6488 0.046 Uiso 1 1 calc R . . C4 C 0.5930(4) 0.0392(4) 0.60614(18) 0.0537(9) Uani 1 1 d . . . H4A H 0.6128 0.1342 0.5918 0.081 Uiso 1 1 calc R . . H4B H 0.4896 0.0288 0.6096 0.081 Uiso 1 1 calc R . . H4C H 0.6203 -0.0235 0.5660 0.081 Uiso 1 1 calc R . . C11 C 0.5158(3) -0.1426(3) 0.87575(16) 0.0294(6) Uani 1 1 d . . . C12 C 0.3878(3) -0.1631(3) 0.82437(16) 0.0346(6) Uani 1 1 d . . . C13 C 0.2630(3) -0.2109(4) 0.8493(2) 0.0518(9) Uani 1 1 d . . . H13 H 0.1770 -0.2221 0.8133 0.062 Uiso 1 1 calc R . . C14 C 0.2659(4) -0.2424(4) 0.9285(2) 0.0624(11) Uani 1 1 d . . . H14 H 0.1810 -0.2752 0.9472 0.075 Uiso 1 1 calc R . . C15 C 0.3905(4) -0.2262(4) 0.97962(19) 0.0532(9) Uani 1 1 d . . . H15 H 0.3916 -0.2506 1.0332 0.064 Uiso 1 1 calc R . . C16 C 0.5157(3) -0.1749(3) 0.95511(16) 0.0373(6) Uani 1 1 d . . . C17 C 0.6517(4) -0.1552(4) 1.01263(17) 0.0486(8) Uani 1 1 d . . . H17A H 0.6302 -0.1699 1.0662 0.073 Uiso 1 1 calc R . . H17B H 0.6881 -0.0615 1.0078 0.073 Uiso 1 1 calc R . . H17C H 0.7251 -0.2214 1.0012 0.073 Uiso 1 1 calc R . . C18 C 0.2734(4) -0.1428(5) 0.6901(2) 0.0663(12) Uani 1 1 d . . . H18A H 0.2303 -0.2344 0.6918 0.099 Uiso 1 1 calc R . . H18B H 0.2976 -0.1254 0.6372 0.099 Uiso 1 1 calc R . . H18C H 0.2043 -0.0733 0.7029 0.099 Uiso 1 1 calc R . . Li1 Li 0.6155(5) -0.1729(5) 0.7307(3) 0.0323(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02568(12) 0.02337(12) 0.03487(12) 0.00041(7) 0.00412(8) 0.00245(7) O1 0.0247(10) 0.0506(14) 0.0327(10) -0.0076(9) 0.0017(8) -0.0007(8) N1 0.0229(12) 0.0310(14) 0.0286(11) 0.0024(9) 0.0005(10) -0.0013(9) N2 0.0259(11) 0.0267(13) 0.0376(13) 0.0007(9) 0.0043(10) -0.0004(9) N3 0.0409(13) 0.0297(13) 0.0273(11) 0.0013(9) 0.0031(10) -0.0003(10) C1 0.0346(17) 0.058(2) 0.0419(17) 0.0036(15) -0.0060(14) -0.0071(14) C2 0.0280(14) 0.0291(16) 0.0544(18) -0.0020(13) 0.0116(13) 0.0025(12) C3 0.0490(17) 0.0295(17) 0.0408(16) -0.0058(13) 0.0179(14) -0.0024(13) C4 0.071(2) 0.052(2) 0.0355(16) 0.0091(16) -0.0019(15) -0.0014(19) C11 0.0309(14) 0.0221(14) 0.0364(14) -0.0027(11) 0.0089(12) -0.0029(11) C12 0.0311(14) 0.0392(17) 0.0349(14) -0.0093(13) 0.0095(11) -0.0030(13) C13 0.0396(18) 0.063(2) 0.0555(19) -0.0229(17) 0.0153(15) -0.0202(16) C14 0.062(2) 0.075(3) 0.057(2) -0.0206(19) 0.0344(18) -0.036(2) C15 0.066(2) 0.055(2) 0.0428(18) -0.0034(16) 0.0251(17) -0.0185(18) C16 0.0480(17) 0.0303(16) 0.0352(15) 0.0003(13) 0.0113(13) -0.0011(14) C17 0.060(2) 0.055(2) 0.0303(15) 0.0078(15) 0.0049(14) 0.0051(17) C18 0.0322(18) 0.120(4) 0.0437(19) -0.015(2) -0.0065(15) -0.002(2) Li1 0.032(2) 0.030(3) 0.035(2) 0.000(2) 0.0078(19) -0.001(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 2.147(2) . ? Sn1 N3 2.156(2) . ? Sn1 N1 2.213(2) . ? Sn1 Li1 3.278(5) 2_656 ? O1 C12 1.399(3) . ? O1 C18 1.429(4) . ? O1 Li1 2.080(5) . ? N1 C11 1.404(3) . ? N1 Li1 2.065(5) . ? N2 C2 1.465(3) . ? N2 C1 1.483(4) . ? N2 Li1 2.023(5) 2_656 ? N3 C3 1.473(4) . ? N3 C4 1.472(4) . ? N3 Li1 2.043(5) . ? C2 C3 1.515(4) . ? C11 C16 1.399(4) . ? C11 C12 1.399(4) . ? C12 C13 1.376(4) . ? C13 C14 1.392(5) . ? C14 C15 1.366(5) . ? C15 C16 1.389(4) . ? C16 C17 1.510(4) . ? Li1 N2 2.023(5) 2_646 ? Li1 Sn1 3.278(5) 2_646 ? 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 81.11(8) . . ? N2 Sn1 N1 91.19(9) . . ? N3 Sn1 N1 86.70(8) . . ? N2 Sn1 Li1 36.86(10) . 2_656 ? N3 Sn1 Li1 87.96(10) . 2_656 ? N1 Sn1 Li1 127.88(11) . 2_656 ? C12 O1 C18 117.1(2) . . ? C12 O1 Li1 107.9(2) . . ? C18 O1 Li1 129.6(2) . . ? C11 N1 Li1 105.7(2) . . ? C11 N1 Sn1 118.56(17) . . ? Li1 N1 Sn1 85.39(16) . . ? C2 N2 C1 110.8(2) . . ? C2 N2 Li1 112.4(2) . 2_656 ? C1 N2 Li1 104.7(2) . 2_656 ? C2 N2 Sn1 107.30(16) . . ? C1 N2 Sn1 117.87(18) . . ? Li1 N2 Sn1 103.60(16) 2_656 . ? C3 N3 C4 109.9(2) . . ? C3 N3 Li1 117.5(2) . . ? C4 N3 Li1 113.6(2) . . ? C3 N3 Sn1 109.22(16) . . ? C4 N3 Sn1 117.9(2) . . ? Li1 N3 Sn1 87.43(15) . . ? N2 C2 C3 109.4(2) . . ? N3 C3 C2 109.8(2) . . ? N1 C11 C16 124.9(3) . . ? N1 C11 C12 117.3(2) . . ? C16 C11 C12 117.8(2) . . ? C13 C12 O1 124.1(3) . . ? C13 C12 C11 122.6(3) . . ? O1 C12 C11 113.3(2) . . ? C12 C13 C14 118.4(3) . . ? C15 C14 C13 120.2(3) . . ? C14 C15 C16 121.6(3) . . ? C15 C16 C11 119.4(3) . . ? C15 C16 C17 121.0(3) . . ? C11 C16 C17 119.7(3) . . ? N3 Li1 N2 126.7(2) . 2_646 ? N3 Li1 N1 93.8(2) . . ? N2 Li1 N1 130.4(3) 2_646 . ? N3 Li1 O1 103.4(2) . . ? N2 Li1 O1 113.0(2) 2_646 . ? N1 Li1 O1 77.57(18) . . ? N3 Li1 Sn1 104.97(17) . 2_646 ? N2 Li1 Sn1 39.54(11) 2_646 2_646 ? N1 Li1 Sn1 110.12(19) . 2_646 ? O1 Li1 Sn1 149.9(2) . 2_646 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.720 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.083