data_3a _publ_contact_author_name # Name of author for correspondence ; Prof. Dr. A.L. Spek ; _publ_contact_author_address # Address of author for correspondence ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'a.l.spek@chem.uu.nl' _publ_contact_author_fax '+31 30 2533940' _publ_contact_author_phone '+31 30 2532538' _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ; tris-(2-((dimethylamino)methyl)phenyl)- bis-(tetrahydrofurane)- tin-lithium ; _chemical_formula_moiety 'C35 H52 Li N3 O2 Sn' _chemical_formula_sum 'C35 H52 Li N3 O2 Sn' _chemical_formula_weight 672.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 9.9375(7) _cell_length_b 15.943(2) _cell_length_c 22.152(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3509.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11 _cell_measurement_theta_max 13 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.273 _exptl_crystal_F_000 1408 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_absorpt_coefficient_mu 0.760 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.738 _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_source 'Rotating Anode' _diffrn_measurement_device_type 'Nonius TurboCAD4' _diffrn_measurement_method 'Omega/2theta-scan' _diffrn_reflns_number 6000 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.574 _diffrn_reflns_theta_max 27.504 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5560 _reflns_number_gt 5250 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.792 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Locally modified CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1992)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'PLATON (Spek, 2015)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.1858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct' _atom_sites_solution_secondary 'difmap' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.043(19) _chemical_absolute_configuration ad _refine_ls_number_reflns 5560 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.23309(2) 0.47770(2) 0.64113(2) 0.02110(6) Uani 1 1 d . . . . . O1 O 0.1762(2) 0.68034(16) 0.75339(12) 0.0352(6) Uani 1 1 d . . . . . O2 O -0.0959(2) 0.61078(15) 0.69890(11) 0.0310(5) Uani 1 1 d . . . . . N1 N 0.0858(2) 0.48882(18) 0.79405(12) 0.0257(6) Uani 1 1 d . . . . . N2 N 0.2938(3) 0.68965(19) 0.57980(14) 0.0363(7) Uani 1 1 d . . . . . N3 N 0.0933(3) 0.4172(2) 0.52067(13) 0.0398(8) Uani 1 1 d . . . . . C1 C 0.3703(3) 0.4717(2) 0.72173(13) 0.0218(6) Uani 1 1 d . . . . . C2 C 0.5040(3) 0.50038(19) 0.71905(16) 0.0270(8) Uani 1 1 d . . . . . H2 H 0.5389 0.5187 0.6814 0.032 Uiso 1 1 calc R U . . . C3 C 0.5872(3) 0.5029(2) 0.76966(16) 0.0307(8) Uani 1 1 d . . . . . H3 H 0.6763 0.5241 0.7663 0.037 Uiso 1 1 calc R U . . . C4 C 0.5404(3) 0.4747(3) 0.82437(15) 0.0344(8) Uani 1 1 d . . . . . H4 H 0.5977 0.4744 0.8587 0.041 Uiso 1 1 calc R U . . . C5 C 0.4092(3) 0.4466(2) 0.82905(15) 0.0298(8) Uani 1 1 d . . . . . H5 H 0.3765 0.4275 0.8669 0.036 Uiso 1 1 calc R U . . . C6 C 0.3245(3) 0.4459(2) 0.77913(14) 0.0219(7) Uani 1 1 d . . . . . C7 C 0.1799(3) 0.4182(2) 0.78704(15) 0.0247(7) Uani 1 1 d . . . . . H7A H 0.1527 0.3846 0.7515 0.030 Uiso 1 1 calc R U . . . H7B H 0.1736 0.3817 0.8231 0.030 Uiso 1 1 calc R U . . . C8 C 0.1141(3) 0.5346(2) 0.85046(14) 0.0305(7) Uani 1 1 d . . . . . H8A H 0.0460 0.5784 0.8563 0.046 Uiso 1 1 calc R U . . . H8B H 0.2034 0.5605 0.8480 0.046 Uiso 1 1 calc R U . . . H8C H 0.1115 0.4955 0.8846 0.046 Uiso 1 1 calc R U . . . C9 C -0.0521(3) 0.4560(3) 0.79702(19) 0.0407(10) Uani 1 1 d . . . . . H9A H -0.1150 0.5023 0.8040 0.061 Uiso 1 1 calc R U . . . H9B H -0.0590 0.4155 0.8302 0.061 Uiso 1 1 calc R U . . . H9C H -0.0744 0.4282 0.7588 0.061 Uiso 1 1 calc R U . . . C10 C 0.3976(3) 0.49794(19) 0.57483(14) 0.0227(7) Uani 1 1 d . . . . . C11 C 0.5054(3) 0.4422(2) 0.57214(15) 0.0290(7) Uani 1 1 d . . . . . H11 H 0.5077 0.3964 0.5995 0.035 Uiso 1 1 calc R U . . . C12 C 0.6102(4) 0.4512(2) 0.53070(17) 0.0359(9) Uani 1 1 d . . . . . H12 H 0.6822 0.4120 0.5301 0.043 Uiso 1 1 calc R U . . . C13 C 0.6086(4) 0.5171(3) 0.49080(16) 0.0376(9) Uani 1 1 d . . . . . H13 H 0.6801 0.5245 0.4628 0.045 Uiso 1 1 calc R U . . . C14 C 0.5014(4) 0.5725(2) 0.49186(15) 0.0330(8) Uani 1 1 d . . . . . H14 H 0.4989 0.6171 0.4634 0.040 Uiso 1 1 calc R U . . . C15 C 0.3978(3) 0.5646(2) 0.53322(14) 0.0273(7) Uani 1 1 d . . . . . C16 C 0.2833(4) 0.6262(2) 0.53262(15) 0.0323(8) Uani 1 1 d . . . . . H16A H 0.2807 0.6544 0.4928 0.039 Uiso 1 1 calc R U . . . H16B H 0.1977 0.5953 0.5377 0.039 Uiso 1 1 calc R U . . . C17 C 0.4036(5) 0.7480(3) 0.5676(2) 0.0524(11) Uani 1 1 d . . . . . H17A H 0.4883 0.7169 0.5642 0.079 Uiso 1 1 calc R U . . . H17B H 0.4102 0.7886 0.6007 0.079 Uiso 1 1 calc R U . . . H17C H 0.3860 0.7777 0.5297 0.079 Uiso 1 1 calc R U . . . C18 C 0.1672(5) 0.7350(3) 0.5859(3) 0.0627(14) Uani 1 1 d . . . . . H18A H 0.1769 0.7788 0.6166 0.094 Uiso 1 1 calc R U . . . H18B H 0.0961 0.6959 0.5981 0.094 Uiso 1 1 calc R U . . . H18C H 0.1435 0.7606 0.5471 0.094 Uiso 1 1 calc R U . . . C19 C 0.2261(3) 0.33962(19) 0.62925(13) 0.0254(7) Uani 1 1 d . . . . . C20 C 0.3188(4) 0.2867(2) 0.65782(16) 0.0335(8) Uani 1 1 d . . . . . H20 H 0.3835 0.3108 0.6842 0.040 Uiso 1 1 calc R U . . . C21 C 0.3199(4) 0.2005(2) 0.64907(18) 0.0403(9) Uani 1 1 d . . . . . H21 H 0.3853 0.1666 0.6686 0.048 Uiso 1 1 calc R U . . . C22 C 0.2255(5) 0.1649(2) 0.61194(17) 0.0452(10) Uani 1 1 d . . . . . H22 H 0.2255 0.1059 0.6058 0.054 Uiso 1 1 calc R U . . . C23 C 0.1311(4) 0.2137(2) 0.58362(18) 0.0394(9) Uani 1 1 d . . . . . H23 H 0.0654 0.1882 0.5585 0.047 Uiso 1 1 calc R U . . . C24 C 0.1305(4) 0.3002(2) 0.59132(15) 0.0308(8) Uani 1 1 d . . . . . C25 C 0.0297(4) 0.3527(3) 0.55767(16) 0.0370(9) Uani 1 1 d . . . . . H25A H -0.0252 0.3159 0.5314 0.044 Uiso 1 1 calc R U . . . H25B H -0.0316 0.3799 0.5870 0.044 Uiso 1 1 calc R U . . . C26 C 0.1814(5) 0.3813(4) 0.47524(19) 0.0617(14) Uani 1 1 d . . . . . H26A H 0.2511 0.3476 0.4950 0.092 Uiso 1 1 calc R U . . . H26B H 0.2238 0.4265 0.4520 0.092 Uiso 1 1 calc R U . . . H26C H 0.1288 0.3456 0.4480 0.092 Uiso 1 1 calc R U . . . C27 C -0.0068(4) 0.4713(3) 0.49306(18) 0.0550(12) Uani 1 1 d . . . . . H27A H 0.0382 0.5173 0.4718 0.083 Uiso 1 1 calc R U . . . H27B H -0.0657 0.4944 0.5244 0.083 Uiso 1 1 calc R U . . . H27C H -0.0607 0.4387 0.4643 0.083 Uiso 1 1 calc R U . . . C28 C 0.3156(4) 0.6912(3) 0.7368(2) 0.0385(9) Uani 1 1 d . . . . . H28A H 0.3298 0.6782 0.6936 0.046 Uiso 1 1 calc R U . . . H28B H 0.3746 0.6546 0.7614 0.046 Uiso 1 1 calc R U . . . C29 C 0.3432(4) 0.7827(3) 0.7496(2) 0.0549(12) Uani 1 1 d . . . . . H29A H 0.3085 0.8192 0.7169 0.066 Uiso 1 1 calc R U . . . H29B H 0.4405 0.7934 0.7553 0.066 Uiso 1 1 calc R U . . . C30 C 0.2654(5) 0.7949(3) 0.80781(19) 0.0575(12) Uani 1 1 d . . . . . H30A H 0.3164 0.7734 0.8429 0.069 Uiso 1 1 calc R U . . . H30B H 0.2436 0.8548 0.8145 0.069 Uiso 1 1 calc R U . . . C31 C 0.1405(5) 0.7442(3) 0.7969(2) 0.0517(12) Uani 1 1 d . . . . . H31A H 0.1092 0.7181 0.8350 0.062 Uiso 1 1 calc R U . . . H31B H 0.0676 0.7802 0.7809 0.062 Uiso 1 1 calc R U . . . C32 C -0.1482(4) 0.6939(2) 0.70611(18) 0.0364(9) Uani 1 1 d . . . . . H32A H -0.0865 0.7357 0.6880 0.044 Uiso 1 1 calc R U . . . H32B H -0.1603 0.7073 0.7494 0.044 Uiso 1 1 calc R U . . . C33 C -0.2818(4) 0.6940(2) 0.6738(2) 0.0471(10) Uani 1 1 d . . . . . H33A H -0.3067 0.7510 0.6600 0.056 Uiso 1 1 calc R U . . . H33B H -0.3545 0.6713 0.6996 0.056 Uiso 1 1 calc R U . . . C34 C -0.2518(4) 0.6361(2) 0.62056(17) 0.0458(10) Uani 1 1 d . . . . . H34A H -0.3353 0.6107 0.6045 0.055 Uiso 1 1 calc R U . . . H34B H -0.2053 0.6666 0.5877 0.055 Uiso 1 1 calc R U . . . C35 C -0.1619(3) 0.5707(2) 0.64809(17) 0.0360(8) Uani 1 1 d . . . . . H35A H -0.2155 0.5220 0.6618 0.043 Uiso 1 1 calc R U . . . H35B H -0.0947 0.5511 0.6183 0.043 Uiso 1 1 calc R U . . . Li1 Li 0.0851(6) 0.5794(4) 0.7242(3) 0.0284(12) 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 0.02068(9) 0.02152(10) 0.02111(9) 0.00083(9) -0.00051(8) -0.00076(9) O1 0.0390(14) 0.0270(13) 0.0395(14) -0.0065(12) 0.0054(12) -0.0062(11) O2 0.0339(13) 0.0249(12) 0.0341(13) -0.0056(11) -0.0047(11) 0.0044(10) N1 0.0208(12) 0.0284(15) 0.0279(14) 0.0017(13) -0.0003(11) -0.0001(12) N2 0.0398(18) 0.0283(15) 0.0408(17) 0.0009(14) -0.0009(15) 0.0073(14) N3 0.0380(17) 0.060(2) 0.0210(14) 0.0036(15) -0.0036(13) -0.0111(16) C1 0.0213(13) 0.0173(15) 0.0266(15) -0.0025(14) -0.0036(12) 0.0019(15) C2 0.0258(16) 0.0248(19) 0.0306(17) -0.0036(13) -0.0006(14) 0.0021(12) C3 0.0200(15) 0.034(2) 0.0379(19) -0.0102(15) -0.0059(14) 0.0025(13) C4 0.0295(16) 0.043(2) 0.0306(17) -0.0092(19) -0.0124(14) 0.0090(19) C5 0.0316(17) 0.0326(19) 0.0252(16) -0.0010(15) -0.0049(14) 0.0053(15) C6 0.0229(15) 0.0168(15) 0.0260(16) -0.0004(13) -0.0017(13) 0.0036(12) C7 0.0318(17) 0.0200(16) 0.0223(16) 0.0008(14) -0.0021(13) -0.0034(14) C8 0.0342(16) 0.0307(18) 0.0267(17) -0.0009(15) 0.0041(14) 0.0007(14) C9 0.0280(18) 0.048(3) 0.046(2) 0.010(2) -0.0025(17) -0.0078(17) C10 0.0221(14) 0.0246(18) 0.0214(15) -0.0013(12) 0.0004(12) -0.0044(11) C11 0.0291(17) 0.0264(17) 0.0314(17) -0.0032(15) 0.0028(15) -0.0024(15) C12 0.0293(18) 0.037(2) 0.042(2) -0.0145(17) 0.0096(16) -0.0016(15) C13 0.0373(18) 0.045(2) 0.0307(18) -0.007(2) 0.0140(15) -0.011(2) C14 0.044(2) 0.033(2) 0.0211(16) 0.0000(15) 0.0022(15) -0.0157(18) C15 0.0302(17) 0.0292(18) 0.0225(16) -0.0053(15) -0.0021(13) -0.0084(15) C16 0.0350(18) 0.0343(18) 0.0276(16) 0.0105(15) -0.0036(15) -0.0031(16) C17 0.061(3) 0.030(2) 0.066(3) -0.005(2) -0.002(2) 0.000(2) C18 0.056(3) 0.056(3) 0.076(3) -0.003(3) -0.003(3) 0.033(2) C19 0.0297(15) 0.0236(15) 0.0229(15) -0.0018(12) 0.0046(14) -0.0073(14) C20 0.047(2) 0.0241(17) 0.0296(19) -0.0003(15) 0.0008(15) -0.0013(16) C21 0.059(2) 0.0225(17) 0.039(2) 0.0013(17) 0.008(2) 0.0025(16) C22 0.061(3) 0.0260(17) 0.049(2) -0.0100(17) 0.022(2) -0.011(2) C23 0.041(2) 0.036(2) 0.041(2) -0.0151(18) 0.0104(18) -0.0175(18) C24 0.0301(17) 0.037(2) 0.0252(17) -0.0077(16) 0.0096(15) -0.0134(16) C25 0.0294(18) 0.052(3) 0.0298(18) -0.0121(18) -0.0004(15) -0.0177(18) C26 0.057(3) 0.097(4) 0.032(2) -0.004(2) 0.015(2) -0.006(3) C27 0.056(3) 0.075(3) 0.034(2) 0.010(2) -0.0156(19) -0.009(3) C28 0.0308(19) 0.035(2) 0.050(2) -0.0074(19) -0.0018(18) 0.0008(16) C29 0.043(2) 0.040(2) 0.082(3) -0.014(2) -0.011(2) -0.012(2) C30 0.076(3) 0.039(2) 0.057(3) -0.016(2) -0.029(3) 0.003(3) C31 0.063(3) 0.032(2) 0.060(3) -0.014(2) 0.021(2) -0.006(2) C32 0.0334(19) 0.0268(19) 0.049(2) -0.0107(18) -0.0028(18) 0.0048(16) C33 0.037(2) 0.0260(19) 0.078(3) 0.0005(19) -0.015(2) 0.0022(18) C34 0.048(2) 0.042(2) 0.047(2) 0.0042(17) -0.0156(19) -0.004(2) C35 0.0323(17) 0.0355(19) 0.040(2) -0.0122(19) -0.0016(17) 0.0003(15) Li1 0.029(3) 0.026(3) 0.030(3) 0.000(3) 0.001(2) -0.002(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 C19 2.218(3) . ? Sn1 C10 2.221(3) . ? Sn1 C1 2.249(3) . ? Sn1 Li1 2.859(6) . ? O1 C28 1.443(4) . ? O1 C31 1.447(5) . ? O1 Li1 1.957(6) . ? O2 C32 1.432(4) . ? O2 C35 1.451(4) . ? O2 Li1 1.949(6) . ? N1 C9 1.469(4) . ? N1 C7 1.472(4) . ? N1 C8 1.474(4) . ? N1 Li1 2.116(6) . ? N2 C18 1.457(5) . ? N2 C16 1.458(5) . ? N2 C17 1.459(5) . ? N3 C27 1.451(5) . ? N3 C26 1.452(5) . ? N3 C25 1.459(5) . ? C1 C2 1.406(4) . ? C1 C6 1.412(4) . ? C2 C3 1.394(5) . ? C2 H2 0.9500 . ? C3 C4 1.374(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.514(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.393(4) . ? C10 C15 1.407(5) . ? C11 C12 1.396(5) . ? C11 H11 0.9500 . ? C12 C13 1.373(6) . ? C12 H12 0.9500 . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C14 C15 1.384(5) . ? C14 H14 0.9500 . ? C15 C16 1.502(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.400(5) . ? C19 C24 1.416(5) . ? C20 C21 1.389(5) . ? C20 H20 0.9500 . ? C21 C22 1.371(6) . ? C21 H21 0.9500 . ? C22 C23 1.372(6) . ? C22 H22 0.9500 . ? C23 C24 1.389(5) . ? C23 H23 0.9500 . ? C24 C25 1.504(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.512(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.517(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.501(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.509(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.527(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.501(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Sn1 C10 95.10(11) . . ? C19 Sn1 C1 94.08(12) . . ? C10 Sn1 C1 94.85(11) . . ? C19 Sn1 Li1 128.52(14) . . ? C10 Sn1 Li1 136.19(14) . . ? C1 Sn1 Li1 79.93(14) . . ? C28 O1 C31 108.7(3) . . ? C28 O1 Li1 117.3(3) . . ? C31 O1 Li1 133.3(3) . . ? C32 O2 C35 109.2(3) . . ? C32 O2 Li1 122.7(3) . . ? C35 O2 Li1 121.8(3) . . ? C9 N1 C7 109.0(3) . . ? C9 N1 C8 108.4(3) . . ? C7 N1 C8 110.3(3) . . ? C9 N1 Li1 105.8(3) . . ? C7 N1 Li1 116.5(3) . . ? C8 N1 Li1 106.4(3) . . ? C18 N2 C16 110.4(3) . . ? C18 N2 C17 110.3(3) . . ? C16 N2 C17 111.3(3) . . ? C27 N3 C26 110.8(3) . . ? C27 N3 C25 111.0(3) . . ? C26 N3 C25 111.9(4) . . ? C2 C1 C6 115.9(3) . . ? C2 C1 Sn1 121.7(2) . . ? C6 C1 Sn1 122.1(2) . . ? C3 C2 C1 122.4(3) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 121.3(3) . . ? C5 C6 C7 119.0(3) . . ? C1 C6 C7 119.7(3) . . ? N1 C7 C6 113.1(3) . . ? N1 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 116.9(3) . . ? C11 C10 Sn1 120.1(2) . . ? C15 C10 Sn1 122.9(2) . . ? C10 C11 C12 122.4(3) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 119.1(3) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 121.8(3) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C10 120.2(3) . . ? C14 C15 C16 119.9(3) . . ? C10 C15 C16 119.9(3) . . ? N2 C16 C15 113.1(3) . . ? N2 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? N2 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 116.2(3) . . ? C20 C19 Sn1 121.6(2) . . ? C24 C19 Sn1 122.2(3) . . ? C21 C20 C19 122.6(3) . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C22 C21 C20 119.3(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 120.7(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.8(4) . . ? C23 C24 C25 119.6(3) . . ? C19 C24 C25 119.6(3) . . ? N3 C25 C24 112.5(3) . . ? N3 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? N3 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C28 C29 104.0(3) . . ? O1 C28 H28A 111.0 . . ? C29 C28 H28A 111.0 . . ? O1 C28 H28B 111.0 . . ? C29 C28 H28B 111.0 . . ? H28A C28 H28B 109.0 . . ? C28 C29 C30 101.0(4) . . ? C28 C29 H29A 111.6 . . ? C30 C29 H29A 111.6 . . ? C28 C29 H29B 111.6 . . ? C30 C29 H29B 111.6 . . ? H29A C29 H29B 109.4 . . ? C31 C30 C29 102.5(3) . . ? C31 C30 H30A 111.3 . . ? C29 C30 H30A 111.3 . . ? C31 C30 H30B 111.3 . . ? C29 C30 H30B 111.3 . . ? H30A C30 H30B 109.2 . . ? O1 C31 C30 106.4(3) . . ? O1 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? O1 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? O2 C32 C33 105.5(3) . . ? O2 C32 H32A 110.6 . . ? C33 C32 H32A 110.6 . . ? O2 C32 H32B 110.6 . . ? C33 C32 H32B 110.6 . . ? H32A C32 H32B 108.8 . . ? C32 C33 C34 101.2(3) . . ? C32 C33 H33A 111.5 . . ? C34 C33 H33A 111.5 . . ? C32 C33 H33B 111.5 . . ? C34 C33 H33B 111.5 . . ? H33A C33 H33B 109.4 . . ? C35 C34 C33 102.9(3) . . ? C35 C34 H34A 111.2 . . ? C33 C34 H34A 111.2 . . ? C35 C34 H34B 111.2 . . ? C33 C34 H34B 111.2 . . ? H34A C34 H34B 109.1 . . ? O2 C35 C34 106.2(3) . . ? O2 C35 H35A 110.5 . . ? C34 C35 H35A 110.5 . . ? O2 C35 H35B 110.5 . . ? C34 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? O2 Li1 O1 108.1(3) . . ? O2 Li1 N1 112.9(3) . . ? O1 Li1 N1 108.5(3) . . ? O2 Li1 Sn1 115.8(2) . . ? O1 Li1 Sn1 116.2(2) . . ? N1 Li1 Sn1 94.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.4(5) . . . . ? Sn1 C1 C2 C3 175.2(2) . . . . ? C1 C2 C3 C4 1.7(5) . . . . ? C2 C3 C4 C5 -2.2(6) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C4 C5 C6 C1 1.6(5) . . . . ? C4 C5 C6 C7 -177.4(3) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? Sn1 C1 C6 C5 -176.8(2) . . . . ? C2 C1 C6 C7 177.0(3) . . . . ? Sn1 C1 C6 C7 2.3(4) . . . . ? C9 N1 C7 C6 176.0(3) . . . . ? C8 N1 C7 C6 -65.1(3) . . . . ? Li1 N1 C7 C6 56.4(4) . . . . ? C5 C6 C7 N1 97.5(3) . . . . ? C1 C6 C7 N1 -81.6(4) . . . . ? C15 C10 C11 C12 0.3(5) . . . . ? Sn1 C10 C11 C12 178.9(3) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 C14 -1.1(5) . . . . ? C12 C13 C14 C15 1.9(5) . . . . ? C13 C14 C15 C10 -1.5(5) . . . . ? C13 C14 C15 C16 -179.9(3) . . . . ? C11 C10 C15 C14 0.4(5) . . . . ? Sn1 C10 C15 C14 -178.1(2) . . . . ? C11 C10 C15 C16 178.7(3) . . . . ? Sn1 C10 C15 C16 0.3(4) . . . . ? C18 N2 C16 C15 -167.0(3) . . . . ? C17 N2 C16 C15 70.2(4) . . . . ? C14 C15 C16 N2 -101.8(4) . . . . ? C10 C15 C16 N2 79.8(4) . . . . ? C24 C19 C20 C21 1.2(5) . . . . ? Sn1 C19 C20 C21 -177.2(3) . . . . ? C19 C20 C21 C22 -1.2(6) . . . . ? C20 C21 C22 C23 0.1(6) . . . . ? C21 C22 C23 C24 0.9(6) . . . . ? C22 C23 C24 C19 -0.9(5) . . . . ? C22 C23 C24 C25 177.4(3) . . . . ? C20 C19 C24 C23 -0.1(5) . . . . ? Sn1 C19 C24 C23 178.3(3) . . . . ? C20 C19 C24 C25 -178.4(3) . . . . ? Sn1 C19 C24 C25 0.0(4) . . . . ? C27 N3 C25 C24 -175.0(3) . . . . ? C26 N3 C25 C24 60.6(4) . . . . ? C23 C24 C25 N3 -123.2(4) . . . . ? C19 C24 C25 N3 55.1(4) . . . . ? C31 O1 C28 C29 -24.3(4) . . . . ? Li1 O1 C28 C29 164.0(3) . . . . ? O1 C28 C29 C30 39.3(4) . . . . ? C28 C29 C30 C31 -39.3(4) . . . . ? C28 O1 C31 C30 -1.0(5) . . . . ? Li1 O1 C31 C30 168.8(4) . . . . ? C29 C30 C31 O1 25.7(5) . . . . ? C35 O2 C32 C33 20.1(4) . . . . ? Li1 O2 C32 C33 172.8(3) . . . . ? O2 C32 C33 C34 -35.6(4) . . . . ? C32 C33 C34 C35 37.4(4) . . . . ? C32 O2 C35 C34 4.3(4) . . . . ? Li1 O2 C35 C34 -148.6(3) . . . . ? C33 C34 C35 O2 -26.4(4) . . . . ? _refine_diff_density_max 0.441 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.057 _shelx_res_file ; s827b_sx.res created by SHELXL-2014/7 TITL shelxl R = 0.02 CELL 0.71073 9.9375 15.9430 22.1520 90.000 90.000 90.000 ZERR 1 0.0007 0.0020 0.0030 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H Li N O Sn UNIT 140 208 4 12 8 4 TEMP -120 L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H CONF TWIN WGHT 0.038100 0.185800 BASF -0.04307 FVAR 9.95200 SN1 6 0.233089 0.477697 0.641127 11.00000 0.02068 0.02152 = 0.02111 0.00083 -0.00051 -0.00076 O1 5 0.176230 0.680336 0.753390 11.00000 0.03903 0.02698 = 0.03953 -0.00654 0.00538 -0.00616 O2 5 -0.095882 0.610779 0.698896 11.00000 0.03392 0.02490 = 0.03410 -0.00562 -0.00467 0.00443 N1 4 0.085812 0.488825 0.794052 11.00000 0.02077 0.02838 = 0.02790 0.00166 -0.00030 -0.00014 N2 4 0.293831 0.689653 0.579800 11.00000 0.03984 0.02829 = 0.04080 0.00092 -0.00087 0.00728 N3 4 0.093288 0.417244 0.520666 11.00000 0.03802 0.06029 = 0.02096 0.00359 -0.00360 -0.01110 C1 1 0.370345 0.471747 0.721732 11.00000 0.02134 0.01730 = 0.02661 -0.00246 -0.00363 0.00191 C2 1 0.504003 0.500383 0.719047 11.00000 0.02576 0.02478 = 0.03059 -0.00363 -0.00062 0.00211 AFIX 43 H2 2 0.538883 0.518704 0.681358 11.00000 -1.20000 AFIX 0 C3 1 0.587218 0.502874 0.769665 11.00000 0.01998 0.03433 = 0.03792 -0.01016 -0.00591 0.00253 AFIX 43 H3 2 0.676259 0.524062 0.766339 11.00000 -1.20000 AFIX 0 C4 1 0.540386 0.474669 0.824367 11.00000 0.02955 0.04300 = 0.03063 -0.00924 -0.01244 0.00896 AFIX 43 H4 2 0.597694 0.474444 0.858692 11.00000 -1.20000 AFIX 0 C5 1 0.409210 0.446627 0.829050 11.00000 0.03158 0.03262 = 0.02523 -0.00105 -0.00492 0.00527 AFIX 43 H5 2 0.376464 0.427545 0.866928 11.00000 -1.20000 AFIX 0 C6 1 0.324543 0.445950 0.779129 11.00000 0.02285 0.01678 = 0.02599 -0.00043 -0.00170 0.00359 C7 1 0.179899 0.418195 0.787040 11.00000 0.03176 0.02004 = 0.02233 0.00077 -0.00210 -0.00341 AFIX 23 H7A 2 0.152737 0.384564 0.751502 11.00000 -1.20000 H7B 2 0.173622 0.381658 0.823067 11.00000 -1.20000 AFIX 0 C8 1 0.114051 0.534624 0.850460 11.00000 0.03425 0.03067 = 0.02667 -0.00088 0.00410 0.00074 AFIX 137 H8A 2 0.046007 0.578366 0.856317 11.00000 -1.50000 H8B 2 0.203372 0.560451 0.847998 11.00000 -1.50000 H8C 2 0.111546 0.495501 0.884564 11.00000 -1.50000 AFIX 0 C9 1 -0.052146 0.455973 0.797016 11.00000 0.02803 0.04841 = 0.04580 0.01014 -0.00246 -0.00779 AFIX 137 H9A 2 -0.115028 0.502315 0.804014 11.00000 -1.50000 H9B 2 -0.059027 0.415503 0.830172 11.00000 -1.50000 H9C 2 -0.074415 0.428184 0.758840 11.00000 -1.50000 AFIX 0 C10 1 0.397632 0.497943 0.574835 11.00000 0.02208 0.02460 = 0.02141 -0.00129 0.00040 -0.00441 C11 1 0.505446 0.442237 0.572144 11.00000 0.02907 0.02643 = 0.03145 -0.00322 0.00280 -0.00239 AFIX 43 H11 2 0.507741 0.396418 0.599543 11.00000 -1.20000 AFIX 0 C12 1 0.610221 0.451229 0.530696 11.00000 0.02929 0.03662 = 0.04173 -0.01455 0.00958 -0.00164 AFIX 43 H12 2 0.682200 0.412025 0.530100 11.00000 -1.20000 AFIX 0 C13 1 0.608586 0.517086 0.490798 11.00000 0.03733 0.04484 = 0.03069 -0.00725 0.01397 -0.01079 AFIX 43 H13 2 0.680065 0.524541 0.462831 11.00000 -1.20000 AFIX 0 C14 1 0.501427 0.572464 0.491864 11.00000 0.04434 0.03342 = 0.02115 0.00003 0.00216 -0.01574 AFIX 43 H14 2 0.498902 0.617056 0.463441 11.00000 -1.20000 AFIX 0 C15 1 0.397829 0.564643 0.533220 11.00000 0.03022 0.02918 = 0.02248 -0.00532 -0.00208 -0.00844 C16 1 0.283342 0.626192 0.532617 11.00000 0.03504 0.03432 = 0.02758 0.01053 -0.00357 -0.00313 AFIX 23 H16A 2 0.280683 0.654405 0.492823 11.00000 -1.20000 H16B 2 0.197696 0.595279 0.537728 11.00000 -1.20000 AFIX 0 C17 1 0.403587 0.747987 0.567589 11.00000 0.06137 0.03029 = 0.06553 -0.00457 -0.00242 -0.00025 AFIX 137 H17A 2 0.488291 0.716853 0.564244 11.00000 -1.50000 H17B 2 0.410243 0.788619 0.600651 11.00000 -1.50000 H17C 2 0.385967 0.777681 0.529669 11.00000 -1.50000 AFIX 0 C18 1 0.167222 0.734953 0.585895 11.00000 0.05578 0.05612 = 0.07605 -0.00295 -0.00338 0.03320 AFIX 137 H18A 2 0.176883 0.778804 0.616593 11.00000 -1.50000 H18B 2 0.096083 0.695881 0.598058 11.00000 -1.50000 H18C 2 0.143542 0.760644 0.547134 11.00000 -1.50000 AFIX 0 C19 1 0.226116 0.339622 0.629254 11.00000 0.02975 0.02357 = 0.02285 -0.00184 0.00464 -0.00732 C20 1 0.318818 0.286744 0.657822 11.00000 0.04671 0.02409 = 0.02965 -0.00026 0.00081 -0.00134 AFIX 43 H20 2 0.383504 0.310804 0.684228 11.00000 -1.20000 AFIX 0 C21 1 0.319913 0.200499 0.649071 11.00000 0.05907 0.02247 = 0.03935 0.00134 0.00766 0.00249 AFIX 43 H21 2 0.385347 0.166570 0.668596 11.00000 -1.20000 AFIX 0 C22 1 0.225506 0.164866 0.611937 11.00000 0.06062 0.02602 = 0.04899 -0.01002 0.02245 -0.01138 AFIX 43 H22 2 0.225499 0.105897 0.605775 11.00000 -1.20000 AFIX 0 C23 1 0.131061 0.213732 0.583616 11.00000 0.04126 0.03633 = 0.04074 -0.01509 0.01042 -0.01746 AFIX 43 H23 2 0.065355 0.188181 0.558473 11.00000 -1.20000 AFIX 0 C24 1 0.130514 0.300163 0.591322 11.00000 0.03012 0.03710 = 0.02523 -0.00775 0.00960 -0.01344 C25 1 0.029657 0.352732 0.557667 11.00000 0.02940 0.05196 = 0.02978 -0.01207 -0.00042 -0.01765 AFIX 23 H25A 2 -0.025217 0.315883 0.531438 11.00000 -1.20000 H25B 2 -0.031553 0.379865 0.587027 11.00000 -1.20000 AFIX 0 C26 1 0.181420 0.381323 0.475244 11.00000 0.05650 0.09691 = 0.03156 -0.00440 0.01537 -0.00647 AFIX 137 H26A 2 0.251138 0.347612 0.495000 11.00000 -1.50000 H26B 2 0.223818 0.426482 0.452025 11.00000 -1.50000 H26C 2 0.128799 0.345627 0.448043 11.00000 -1.50000 AFIX 0 C27 1 -0.006845 0.471277 0.493062 11.00000 0.05593 0.07532 = 0.03380 0.01003 -0.01555 -0.00854 AFIX 137 H27A 2 0.038233 0.517251 0.471768 11.00000 -1.50000 H27B 2 -0.065706 0.494355 0.524432 11.00000 -1.50000 H27C 2 -0.060680 0.438713 0.464346 11.00000 -1.50000 AFIX 0 C28 1 0.315604 0.691176 0.736793 11.00000 0.03081 0.03498 = 0.04986 -0.00743 -0.00183 0.00085 AFIX 23 H28A 2 0.329753 0.678167 0.693557 11.00000 -1.20000 H28B 2 0.374600 0.654626 0.761388 11.00000 -1.20000 AFIX 0 C29 1 0.343234 0.782708 0.749572 11.00000 0.04251 0.04018 = 0.08202 -0.01380 -0.01113 -0.01201 AFIX 23 H29A 2 0.308543 0.819223 0.716945 11.00000 -1.20000 H29B 2 0.440540 0.793414 0.755268 11.00000 -1.20000 AFIX 0 C30 1 0.265361 0.794931 0.807814 11.00000 0.07637 0.03878 = 0.05744 -0.01600 -0.02912 0.00283 AFIX 23 H30A 2 0.316375 0.773424 0.842942 11.00000 -1.20000 H30B 2 0.243552 0.854804 0.814501 11.00000 -1.20000 AFIX 0 C31 1 0.140465 0.744174 0.796944 11.00000 0.06268 0.03229 = 0.06023 -0.01405 0.02098 -0.00639 AFIX 23 H31A 2 0.109231 0.718076 0.834999 11.00000 -1.20000 H31B 2 0.067608 0.780219 0.780941 11.00000 -1.20000 AFIX 0 C32 1 -0.148189 0.693876 0.706113 11.00000 0.03338 0.02681 = 0.04901 -0.01071 -0.00283 0.00483 AFIX 23 H32A 2 -0.086468 0.735657 0.688045 11.00000 -1.20000 H32B 2 -0.160327 0.707304 0.749406 11.00000 -1.20000 AFIX 0 C33 1 -0.281839 0.694000 0.673768 11.00000 0.03734 0.02596 = 0.07792 0.00050 -0.01527 0.00220 AFIX 23 H33A 2 -0.306748 0.751017 0.660038 11.00000 -1.20000 H33B 2 -0.354505 0.671260 0.699591 11.00000 -1.20000 AFIX 0 C34 1 -0.251806 0.636073 0.620561 11.00000 0.04801 0.04210 = 0.04728 0.00421 -0.01565 -0.00398 AFIX 23 H34A 2 -0.335339 0.610697 0.604452 11.00000 -1.20000 H34B 2 -0.205261 0.666584 0.587711 11.00000 -1.20000 AFIX 0 C35 1 -0.161950 0.570734 0.648087 11.00000 0.03229 0.03553 = 0.04030 -0.01221 -0.00156 0.00027 AFIX 23 H35A 2 -0.215487 0.521973 0.661832 11.00000 -1.20000 H35B 2 -0.094652 0.551136 0.618306 11.00000 -1.20000 AFIX 0 LI1 3 0.085058 0.579368 0.724184 11.00000 0.02898 0.02639 = 0.02974 0.00015 0.00051 -0.00206 HKLF 4 REM shelxl R = 0.02 REM R1 = 0.0239 for 5250 Fo > 4sig(Fo) and 0.0268 for all 5560 data REM 386 parameters refined using 0 restraints END WGHT 0.0380 0.1967 REM Highest difference peak 0.441, deepest hole -0.505, 1-sigma level 0.057 Q1 1 0.2813 0.5251 0.6422 11.00000 0.05 0.44 Q2 1 0.2841 0.4228 0.6377 11.00000 0.05 0.39 Q3 1 0.1803 0.5313 0.6406 11.00000 0.05 0.37 Q4 1 0.1785 0.4222 0.6380 11.00000 0.05 0.32 Q5 1 0.2629 0.4200 0.7804 11.00000 0.05 0.27 Q6 1 0.0158 0.4787 0.8021 11.00000 0.05 0.24 Q7 1 0.2061 0.7190 0.8612 11.00000 0.05 0.24 Q8 1 0.2428 0.7583 0.8875 11.00000 0.05 0.23 Q9 1 0.3153 0.5602 0.8540 11.00000 0.05 0.23 Q10 1 0.4032 0.5229 0.5527 11.00000 0.05 0.23 Q11 1 0.2841 0.6620 0.5627 11.00000 0.05 0.22 Q12 1 0.3179 0.4590 0.6006 11.00000 0.05 0.22 Q13 1 0.0581 0.7395 0.8111 11.00000 0.05 0.22 Q14 1 -0.2188 0.5968 0.6406 11.00000 0.05 0.22 Q15 1 0.1874 0.7835 0.8247 11.00000 0.05 0.22 Q16 1 0.1346 0.4606 0.6603 11.00000 0.05 0.22 Q17 1 0.1176 0.6807 0.6204 11.00000 0.05 0.21 Q18 1 0.3689 0.5200 0.6089 11.00000 0.05 0.21 Q19 1 0.2183 0.7614 0.8375 11.00000 0.05 0.21 Q20 1 0.3613 0.4749 0.8047 11.00000 0.05 0.21 ; _shelx_res_checksum 77174 _shelx_hkl_file ; 2 0 0 5204276 35391 4 0 0 128672 1829 6 0 0 694417 8707 8 0 0 459139 5228 10 0 0 896 2687 12 0 0 85275 4677 1 1 0 6141679 181745 2 1 0 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21 24976 3881 3 1 21 36518 3582 4 1 21 10149 3284 5 1 21 96718 4975 6 1 21 16518 3980 7 1 21 87365 5075 8 1 21 7662 3582 0 2 21 3881 3085 1 2 21 164083 5373 2 2 21 20100 3582 3 2 21 13035 3582 4 2 21 84678 4577 5 2 21 52936 4478 6 2 21 115027 5174 7 2 21 16219 3582 8 2 21 95624 5174 0 3 21 52638 4080 1 3 21 26070 3582 2 3 21 92937 4876 3 3 21 56419 4080 4 3 21 69454 4577 5 3 21 86270 4776 6 3 21 54926 4378 7 3 21 81196 5075 8 3 21 2786 5672 0 4 21 12140 3383 1 4 21 245776 6169 2 4 21 59006 4577 3 4 21 127565 5075 4 4 21 41692 4080 5 4 21 77812 4776 6 4 21 43483 4378 7 4 21 22388 4080 8 4 21 103783 5473 0 5 21 206173 5970 1 5 21 40896 4080 2 5 21 178511 5871 3 5 21 20896 3781 4 5 21 93236 5075 5 5 21 21493 3781 6 5 21 82390 5373 7 5 21 58210 4876 8 5 21 10647 4279 0 6 21 28856 3881 1 6 21 257716 6965 2 6 21 37414 4080 3 6 21 127664 5572 4 6 21 3781 3781 5 6 21 86270 4975 6 6 21 20498 3682 7 6 21 92440 5373 8 6 21 54528 4975 0 7 21 401699 7960 1 7 21 59603 4378 2 7 21 216920 6368 3 7 21 13035 3582 4 7 21 117216 5572 5 7 21 11543 3781 6 7 21 107365 5672 7 7 21 65573 5075 0 8 21 89852 5174 1 8 21 296921 7164 2 8 21 57812 4378 3 8 21 219308 6567 4 8 21 8358 4080 5 8 21 158311 6269 6 8 21 12637 4478 7 8 21 102788 5871 0 9 21 267866 7164 1 9 21 64180 4876 2 9 21 163088 6169 3 9 21 13732 4080 4 9 21 232542 7065 5 9 21 7264 3781 6 9 21 114331 6468 0 10 21 8458 3881 1 10 21 209556 6667 2 10 21 10448 4080 3 10 21 156620 6368 4 10 21 13334 4080 5 10 21 155426 6468 6 10 21 7662 4179 0 11 21 318613 8259 1 11 21 2786 4080 2 11 21 223288 6866 3 11 21 3085 6070 4 11 21 246174 7562 5 11 21 2985 5473 0 12 21 49752 4876 1 12 21 171745 6965 2 12 21 3085 6169 3 12 21 193934 7065 4 12 21 6766 4279 0 13 21 156719 6965 1 13 21 21791 4577 2 13 21 112937 5871 3 13 21 13931 4577 0 14 21 3085 6468 1 14 21 158809 6965 0 0 22 109355 4975 1 0 22 132838 5174 2 0 22 212243 6269 3 0 22 123883 5174 4 0 22 281398 6866 5 0 22 75723 4776 6 0 22 77414 4975 7 0 22 3682 3881 8 0 22 86768 5274 0 1 22 39802 3881 1 1 22 252741 6269 2 1 22 210054 6169 3 1 22 326573 7463 4 1 22 115027 5075 5 1 22 116321 5572 6 1 22 37812 4179 7 1 22 73235 5373 8 1 22 6468 3582 0 2 22 315926 6965 1 2 22 170550 5672 2 2 22 277020 6965 3 2 22 151744 5672 4 2 22 188859 6070 5 2 22 114132 5274 6 2 22 41991 4478 7 2 22 52837 4378 8 2 22 41195 4776 0 3 22 79205 4677 1 3 22 163884 5672 2 3 22 339210 7463 3 3 22 269159 6965 4 3 22 173436 6070 5 3 22 80400 4776 6 3 22 66568 4975 7 3 22 20299 3881 8 3 22 12040 3980 0 4 22 252144 6766 1 4 22 121296 5174 2 4 22 185078 6169 3 4 22 117714 5373 4 4 22 151844 5572 5 4 22 91445 4975 6 4 22 74728 4677 7 4 22 40697 4577 0 5 22 14727 3582 1 5 22 152441 5672 2 5 22 77116 4677 3 5 22 184979 6169 4 5 22 131246 5572 5 5 22 40100 4478 6 5 22 80002 5174 7 5 22 61096 4876 0 6 22 158510 5672 1 6 22 46071 4378 2 6 22 67762 4876 3 6 22 66867 4577 4 6 22 79504 4776 5 6 22 98907 5274 6 6 22 56917 4975 7 6 22 27065 4378 0 7 22 9851 3582 1 7 22 54528 4677 2 7 22 30846 3881 3 7 22 135525 5672 4 7 22 54827 4776 5 7 22 58011 4776 6 7 22 58011 4975 7 7 22 39603 4876 0 8 22 28757 4179 1 8 22 7264 3881 2 8 22 20597 4080 3 8 22 31941 4577 4 8 22 47165 4776 5 8 22 53732 4975 6 8 22 18906 4478 0 9 22 17612 3881 1 9 22 3085 5672 2 9 22 15125 3881 3 9 22 31841 4378 4 9 22 25374 4279 5 9 22 12339 4478 6 9 22 64180 5174 0 10 22 5473 3881 1 10 22 2786 5970 2 10 22 30249 4577 3 10 22 27762 4577 4 10 22 10149 4080 5 10 22 16518 4776 0 11 22 4876 3881 1 11 22 2289 5672 2 11 22 11045 4378 3 11 22 25672 4577 4 11 22 13433 4577 0 12 22 2587 5473 1 12 22 2289 6169 2 12 22 35324 5075 3 12 22 28956 4876 0 13 22 995 4378 1 13 22 22090 4876 1 0 23 30946 3980 2 0 23 22687 4179 3 0 23 28757 4179 4 0 23 7662 3881 5 0 23 59902 4776 6 0 23 8259 3980 7 0 23 73235 5373 0 1 23 10746 3682 1 1 23 10746 3881 2 1 23 32040 4179 3 1 23 2587 5174 4 1 23 14627 4080 5 1 23 2786 5572 6 1 23 95126 5174 7 1 23 3383 5373 0 2 23 98609 5274 1 2 23 17513 3682 2 2 23 58011 4378 3 2 23 60996 4677 4 2 23 27364 4080 5 2 23 38508 4279 6 2 23 14627 3980 7 2 23 55722 4876 0 3 23 20896 3881 1 3 23 70250 4677 2 3 23 4179 3682 3 3 23 56717 4378 4 3 23 29652 4080 5 3 23 37513 4279 6 3 23 64678 4677 7 3 23 14130 3682 0 4 23 39105 4179 1 4 23 34429 4179 2 4 23 93236 5174 3 4 23 45075 4378 4 4 23 71245 4876 5 4 23 24976 3980 6 4 23 44578 4677 7 4 23 56618 4577 0 5 23 10647 3881 1 5 23 169257 5970 2 5 23 12140 3582 3 5 23 100698 5373 4 5 23 44876 4577 5 5 23 59006 5075 6 5 23 52140 4975 7 5 23 67464 4876 0 6 23 105475 5174 1 6 23 11443 3682 2 6 23 186969 6468 3 6 23 19005 4378 4 6 23 70947 5075 5 6 23 25672 4577 6 6 23 67563 5174 0 7 23 1791 3682 1 7 23 220104 6965 2 7 23 2886 3881 3 7 23 165476 6468 4 7 23 20896 4378 5 7 23 100897 5771 6 7 23 44777 4975 0 8 23 231845 7065 1 8 23 9851 4378 2 8 23 299409 7960 3 8 23 22587 4378 4 8 23 163983 6667 5 8 23 29752 4577 0 9 23 3085 3881 1 9 23 220502 6965 2 9 23 12339 4378 3 9 23 199307 7164 4 9 23 17513 4279 5 9 23 120201 6269 0 10 23 210452 7264 1 10 23 2886 5970 2 10 23 231248 7761 3 10 23 13035 4378 4 10 23 147266 6567 0 11 23 3383 5970 1 11 23 179207 7264 2 11 23 5174 4378 3 11 23 246174 7960 0 12 23 197019 7264 1 12 23 1791 6667 2 12 23 184979 7662 0 0 24 111743 5274 1 0 24 143983 5771 2 0 24 133833 5771 3 0 24 40598 4378 4 0 24 121495 5672 5 0 24 78409 5075 6 0 24 85872 5274 7 0 24 65971 5174 0 1 24 31344 4179 1 1 24 162789 6070 2 1 24 153834 5771 3 1 24 138610 5970 4 1 24 103584 5373 5 1 24 102589 5572 6 1 24 56021 5274 7 1 24 40100 4677 0 2 24 248064 6866 1 2 24 148063 5771 2 2 24 248960 6766 3 2 24 92937 5174 4 2 24 62688 4876 5 2 24 69852 5075 6 2 24 58210 4975 7 2 24 38110 4677 0 3 24 59205 4478 1 3 24 170949 6269 2 3 24 140102 5771 3 3 24 204680 6766 4 3 24 84479 5373 5 3 24 72638 5075 6 3 24 54230 4975 0 4 24 109753 5274 1 4 24 105674 5274 2 4 24 162192 6269 3 4 24 88957 5174 4 4 24 143684 6169 5 4 24 50847 4577 6 4 24 102290 5771 0 5 24 117813 5771 1 5 24 57315 4677 2 5 24 69056 4975 3 5 24 107465 5473 4 5 24 51842 4876 5 5 24 46071 5075 6 5 24 40100 4975 0 6 24 30946 4677 1 6 24 77912 5274 2 6 24 48459 4975 3 6 24 50648 4677 4 6 24 67364 4876 5 6 24 52638 4776 6 6 24 30448 4776 0 7 24 111942 5771 1 7 24 56917 4975 2 7 24 18209 4378 3 7 24 94529 5473 4 7 24 56817 5075 5 7 24 45573 4776 0 8 24 50150 4677 1 8 24 39304 4478 2 8 24 24677 4975 3 8 24 16219 4080 4 8 24 32438 4577 5 8 24 49852 5075 0 9 24 23782 4478 1 9 24 26767 4677 2 9 24 995 4378 3 9 24 23185 4677 4 9 24 26269 4876 0 10 24 1791 6269 1 10 24 2090 4179 2 10 24 12936 4677 3 10 24 2587 6965 0 11 24 3085 6269 1 11 24 15324 4677 1 0 25 25971 4478 2 0 25 84181 5274 3 0 25 16219 4179 4 0 25 45274 4677 5 0 25 2786 5871 6 0 25 86171 5473 0 1 25 18806 3980 1 1 25 25672 4279 2 1 25 3980 3980 3 1 25 51543 4677 4 1 25 7463 4179 5 1 25 45075 4876 6 1 25 5771 4279 0 2 25 31244 4478 1 2 25 23583 4279 2 2 25 5771 3980 3 2 25 17712 4478 4 2 25 7463 4179 5 2 25 22090 4577 6 2 25 45971 4776 0 3 25 106669 5572 1 3 25 1592 5572 2 3 25 53434 4776 3 3 25 15622 4179 4 3 25 27861 4378 5 3 25 3085 6070 6 3 25 41692 4975 0 4 25 2687 5572 1 4 25 54926 5274 2 4 25 2587 5473 3 4 25 36220 4478 4 4 25 46469 4876 5 4 25 68957 5075 0 5 25 63583 4975 1 5 25 3383 3980 2 5 25 88658 5274 3 5 25 47663 4975 4 5 25 51842 4876 5 5 25 26170 4876 0 6 25 2587 5572 1 6 25 143087 6269 2 6 25 18806 4179 3 6 25 83484 5473 4 6 25 52837 5174 5 6 25 99703 5871 0 7 25 133634 6269 1 7 25 8358 3980 2 7 25 140301 6269 3 7 25 14528 4378 4 7 25 90350 5871 0 8 25 3184 6269 1 8 25 188362 7363 2 8 25 10149 4478 3 8 25 109554 6169 4 8 25 3085 6169 0 9 25 188063 7363 1 9 25 10149 4478 2 9 25 179804 7065 3 9 25 11941 4378 0 10 25 8657 4478 1 10 25 171944 7264 0 0 26 48956 5075 1 0 26 173337 6965 2 0 26 34827 4478 3 0 26 113435 5771 4 0 26 48558 4677 5 0 26 161396 6667 0 1 26 374833 8557 1 1 26 92539 5871 2 1 26 73733 5075 3 1 26 43384 4975 4 1 26 118410 6269 5 1 26 43682 5075 0 2 26 46966 5075 1 2 26 196024 6965 2 2 26 66270 5274 3 2 26 127664 5771 4 2 26 78907 5473 5 2 26 110151 6169 0 3 26 412048 9353 1 3 26 26866 4478 2 3 26 114331 5871 3 3 26 41991 4975 4 3 26 103286 5970 5 3 26 23483 4577 0 4 26 17612 4279 1 4 26 112042 6070 2 4 26 39901 4975 3 4 26 111644 6269 4 4 26 65872 5473 0 5 26 107863 6070 1 5 26 16916 4478 2 5 26 74131 5274 3 5 26 25971 4975 4 5 26 57315 5473 0 6 26 17811 4478 1 6 26 84678 5572 2 6 26 16020 4776 3 6 26 84479 5771 4 6 26 51046 5174 0 7 26 38906 5274 1 7 26 11841 4478 2 7 26 66469 5473 3 7 26 23782 4677 0 8 26 3184 6368 1 8 26 55822 5274 2 8 26 7363 4478 1 0 27 4080 5871 2 0 27 10149 4279 3 0 27 32239 4776 4 0 27 2587 4677 0 1 27 3184 6766 1 1 27 2687 6468 2 1 27 12538 4577 3 1 27 2886 6070 4 1 27 23483 4677 0 2 27 27662 4876 1 2 27 10945 4577 2 2 27 3781 6368 3 2 27 22488 4478 4 2 27 21891 4677 0 3 27 5672 4279 1 3 27 29752 4776 2 3 27 2886 5871 3 3 27 18508 4179 4 3 27 20896 4478 0 4 27 81992 5871 1 4 27 25075 4776 2 4 27 48658 5274 3 4 27 30050 4776 0 5 27 35822 5075 1 5 27 85872 6169 2 5 27 6368 5075 3 5 27 68160 5572 0 6 27 137714 6368 1 6 27 21791 4776 2 6 27 79504 5871 0 7 27 38906 5373 1 7 27 142291 6866 0 0 28 219308 8159 1 0 28 4876 4279 2 0 28 144779 6965 3 0 28 49951 5274 0 1 28 27364 4577 1 1 28 215626 7861 2 1 28 15821 4577 0 2 28 301996 8657 1 2 28 8358 5174 2 2 28 146669 6667 0 3 28 7562 4279 1 3 28 200999 7562 2 3 28 13433 4776 0 4 28 184680 7264 1 4 28 2985 6169 ; _shelx_hkl_checksum 44986 #===END data_3b _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ; tris-(2-((dimethylamino)methyl)phenyl)-(tetrahydrofuran)-tin-lithium ; _chemical_formula_moiety 'C31 H44 Li N3 O Sn' _chemical_formula_sum 'C31 H44 Li N3 O Sn' _chemical_formula_weight 600.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 10.0617(6) _cell_length_b 15.8787(7) _cell_length_c 20.0617(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3205.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.244 _exptl_crystal_F_000 1248 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 0.822 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.650 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'Zr-filter' _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method 'omega/2theta-scan' _diffrn_standards_number 3 _diffrn_standards_decay_% 35 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 3 0 0 -2 -5 0 4 2 _diffrn_reflns_number 6072 _diffrn_reflns_av_unetI/netI 0.1499 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.636 _diffrn_reflns_theta_max 27.477 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 6072 _reflns_number_gt 2297 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.787 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 0.999 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Locally modified CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.04(9) _chemical_absolute_configuration ad _refine_ls_number_reflns 6072 _refine_ls_number_parameters 340 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1520 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max 0.006 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.63185(7) 0.05371(4) 0.35021(3) 0.0673(2) Uani 1 1 d . . . . . O1 O 0.3713(9) 0.2110(5) 0.2609(4) 0.096(2) Uani 1 1 d . . . . . N1 N 0.6790(8) 0.2595(5) 0.2892(4) 0.069(2) Uani 1 1 d . . . . . N2 N 0.5763(11) 0.0854(6) 0.1697(4) 0.086(3) Uani 1 1 d . . . . . N3 N 0.2688(17) -0.0292(11) 0.4796(7) 0.176(6) Uani 1 1 d D U . . . C1 C 0.7591(10) 0.1356(5) 0.4120(5) 0.059(2) Uani 1 1 d . . . . . C2 C 0.7817(14) 0.1184(7) 0.4783(6) 0.093(4) Uani 1 1 d . . . . . H21 H 0.7454 0.0695 0.4962 0.112 Uiso 1 1 calc R U . . . C3 C 0.8548(18) 0.1694(8) 0.5191(6) 0.123(5) Uani 1 1 d . . . . . H31 H 0.8656 0.1560 0.5639 0.148 Uiso 1 1 calc R U . . . C4 C 0.9121(15) 0.2407(9) 0.4933(8) 0.113(5) Uani 1 1 d . . . . . H41 H 0.9652 0.2748 0.5200 0.135 Uiso 1 1 calc R U . . . C5 C 0.8909(14) 0.2607(7) 0.4295(6) 0.095(4) Uani 1 1 d . . . . . H51 H 0.9271 0.3101 0.4123 0.115 Uiso 1 1 calc R U . . . C6 C 0.8169(11) 0.2097(7) 0.3893(6) 0.073(3) Uani 1 1 d . . . . . C7 C 0.8134(11) 0.2343(6) 0.3150(5) 0.070(3) Uani 1 1 d . . . . . H71 H 0.8745 0.2806 0.3080 0.084 Uiso 1 1 calc R U . . . H72 H 0.8452 0.1869 0.2890 0.084 Uiso 1 1 calc R U . . . C8 C 0.6964(16) 0.3000(9) 0.2246(7) 0.128(6) Uani 1 1 d . . . . . H81 H 0.7405 0.2619 0.1947 0.192 Uiso 1 1 calc R U . . . H82 H 0.7491 0.3499 0.2299 0.192 Uiso 1 1 calc R U . . . H83 H 0.6110 0.3147 0.2067 0.192 Uiso 1 1 calc R U . . . C9 C 0.6158(14) 0.3165(7) 0.3359(6) 0.106(4) Uani 1 1 d . . . . . H91 H 0.6112 0.2904 0.3790 0.159 Uiso 1 1 calc R U . . . H92 H 0.5276 0.3293 0.3207 0.159 Uiso 1 1 calc R U . . . H93 H 0.6666 0.3675 0.3389 0.159 Uiso 1 1 calc R U . . . C10 C 0.7980(11) 0.0163(7) 0.2823(6) 0.079(3) Uani 1 1 d . U . . . C11 C 0.9314(14) 0.0144(8) 0.3014(8) 0.104(5) Uani 1 1 d . U . . . H111 H 0.9510 0.0238 0.3461 0.125 Uiso 1 1 calc R U . . . C12 C 1.0334(17) 0.0000(10) 0.2597(10) 0.138(6) Uani 1 1 d . . . . . H121 H 1.1200 -0.0004 0.2759 0.165 Uiso 1 1 calc R U . . . C13 C 1.0095(19) -0.0143(11) 0.1925(10) 0.140(6) Uani 1 1 d . U . . . H131 H 1.0782 -0.0254 0.1628 0.168 Uiso 1 1 calc R U . . . C14 C 0.8817(17) -0.0112(9) 0.1727(8) 0.119(4) Uani 1 1 d . U . . . H141 H 0.8641 -0.0195 0.1276 0.143 Uiso 1 1 calc R U . . . C15 C 0.7723(14) 0.0038(7) 0.2153(6) 0.082(3) Uani 1 1 d . U . . . C16 C 0.6326(15) 0.0013(7) 0.1865(5) 0.092(3) Uani 1 1 d . U . . . H161 H 0.6336 -0.0330 0.1465 0.110 Uiso 1 1 calc R U . . . H162 H 0.5744 -0.0260 0.2185 0.110 Uiso 1 1 calc R U . . . C17 C 0.4399(16) 0.0704(9) 0.1480(8) 0.139(6) Uani 1 1 d . . . . . H171 H 0.3922 0.0413 0.1824 0.208 Uiso 1 1 calc R U . . . H172 H 0.4405 0.0368 0.1082 0.208 Uiso 1 1 calc R U . . . H173 H 0.3973 0.1233 0.1390 0.208 Uiso 1 1 calc R U . . . C18 C 0.648(2) 0.1240(8) 0.1146(6) 0.146(7) Uani 1 1 d . . . . . H181 H 0.7382 0.1348 0.1278 0.219 Uiso 1 1 calc R U . . . H182 H 0.6059 0.1761 0.1026 0.219 Uiso 1 1 calc R U . . . H183 H 0.6475 0.0867 0.0769 0.219 Uiso 1 1 calc R U . . . C19 C 0.6309(18) -0.0584(7) 0.4177(6) 0.108(4) Uani 1 1 d . U . . . C20 C 0.734(2) -0.1112(7) 0.4212(7) 0.135(6) Uani 1 1 d . U . . . H201 H 0.8118 -0.0973 0.3984 0.162 Uiso 1 1 calc R U . . . C21 C 0.731(3) -0.1856(11) 0.4574(9) 0.194(10) Uani 1 1 d . U . . . H211 H 0.8031 -0.2226 0.4587 0.232 Uiso 1 1 calc R U . . . C22 C 0.616(4) -0.2004(15) 0.4908(16) 0.265(16) Uani 1 1 d . U . . . H221 H 0.6030 -0.2552 0.5057 0.318 Uiso 1 1 calc R U . . . C23 C 0.505(3) -0.1359(14) 0.5068(14) 0.241(11) Uani 1 1 d . U . . . H231 H 0.4421 -0.1398 0.5408 0.289 Uiso 1 1 calc R U . . . C24 C 0.516(2) -0.0705(12) 0.4600(11) 0.189(8) Uani 1 1 d D U . . . C25 C 0.4069(17) -0.0033(12) 0.4706(11) 0.199(8) Uani 1 1 d D U . . . H251 H 0.4040 0.0349 0.4322 0.239 Uiso 1 1 d R U . . . H252 H 0.4239 0.0292 0.5112 0.239 Uiso 1 1 d R U . . . C26 C 0.182(2) 0.0433(15) 0.4869(14) 0.278(14) Uani 1 1 d D U . . . H261 H 0.0970 0.0253 0.5032 0.417 Uiso 1 1 calc R U . . . H262 H 0.1711 0.0702 0.4444 0.417 Uiso 1 1 calc R U . . . H263 H 0.2207 0.0824 0.5178 0.417 Uiso 1 1 calc R U . . . C27 C 0.259(4) -0.0777(12) 0.4201(10) 0.35(2) Uani 1 1 d D U . . . H271 H 0.3235 -0.1220 0.4212 0.521 Uiso 1 1 d R U . . . H272 H 0.2763 -0.0412 0.3830 0.521 Uiso 1 1 d R U . . . H273 H 0.1715 -0.1017 0.4154 0.521 Uiso 1 1 d R U . . . C28 C 0.2867(17) 0.1871(13) 0.3153(9) 0.154(7) Uani 1 1 d . . . . . H281 H 0.2744 0.1265 0.3157 0.184 Uiso 1 1 calc R U . . . H282 H 0.3264 0.2038 0.3573 0.184 Uiso 1 1 calc R U . . . C29 C 0.1625(19) 0.2283(15) 0.3064(12) 0.204(11) Uani 1 1 d . . . . . H291 H 0.1529 0.2743 0.3379 0.245 Uiso 1 1 calc R U . . . H292 H 0.0897 0.1891 0.3129 0.245 Uiso 1 1 calc R U . . . C30 C 0.1632(15) 0.2606(12) 0.2372(10) 0.155(7) Uani 1 1 d . U . . . H301 H 0.1210 0.2209 0.2072 0.186 Uiso 1 1 calc R U . . . H302 H 0.1173 0.3142 0.2344 0.186 Uiso 1 1 calc R U . . . C31 C 0.3021(13) 0.2702(11) 0.2214(9) 0.138(6) Uani 1 1 d . U . . . H311 H 0.3174 0.2594 0.1745 0.166 Uiso 1 1 calc R U . . . H312 H 0.3316 0.3269 0.2316 0.166 Uiso 1 1 calc R U . . . Li Li 0.5462(19) 0.1639(10) 0.2556(8) 0.067(4) 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 0.0690(4) 0.0635(3) 0.0694(4) 0.0076(4) -0.0099(5) -0.0012(4) O1 0.065(5) 0.121(6) 0.103(6) 0.032(5) 0.003(6) 0.011(6) N1 0.060(6) 0.070(5) 0.076(5) 0.020(4) -0.001(4) 0.006(4) N2 0.099(8) 0.093(6) 0.066(6) 0.002(5) -0.007(5) 0.004(6) N3 0.204(13) 0.209(18) 0.115(9) 0.005(10) 0.064(12) -0.027(11) C1 0.060(6) 0.050(5) 0.066(6) 0.001(4) -0.013(5) -0.004(5) C2 0.130(11) 0.072(7) 0.078(8) 0.008(6) -0.029(8) -0.018(8) C3 0.185(16) 0.106(9) 0.079(8) 0.005(7) -0.070(11) -0.033(12) C4 0.136(15) 0.091(8) 0.111(10) -0.021(7) -0.042(10) -0.025(9) C5 0.110(11) 0.091(7) 0.085(8) -0.003(6) -0.023(9) -0.030(8) C6 0.074(8) 0.068(6) 0.077(7) 0.000(5) -0.015(6) 0.002(6) C7 0.066(8) 0.063(6) 0.080(7) -0.004(5) 0.002(6) 0.001(5) C8 0.140(14) 0.134(12) 0.111(10) 0.035(9) -0.015(10) -0.049(10) C9 0.095(9) 0.101(8) 0.122(10) -0.025(8) -0.019(10) 0.023(8) C10 0.069(7) 0.072(6) 0.095(7) -0.012(6) -0.014(6) 0.014(6) C11 0.081(8) 0.097(9) 0.135(11) -0.032(8) -0.024(8) 0.041(8) C12 0.086(12) 0.136(13) 0.192(18) -0.041(13) -0.025(13) 0.035(10) C13 0.116(10) 0.125(12) 0.178(17) -0.048(12) 0.018(13) 0.025(12) C14 0.125(9) 0.117(9) 0.116(10) -0.040(8) 0.026(10) 0.017(11) C15 0.096(8) 0.068(6) 0.082(7) -0.016(6) -0.003(6) 0.002(7) C16 0.111(8) 0.094(8) 0.070(6) -0.020(6) -0.006(7) 0.006(10) C17 0.139(13) 0.125(11) 0.153(13) -0.024(12) -0.064(12) 0.018(10) C18 0.25(2) 0.116(10) 0.075(7) 0.005(7) 0.049(13) 0.017(14) C19 0.157(10) 0.069(5) 0.097(8) 0.019(7) -0.058(9) -0.008(10) C20 0.244(15) 0.077(8) 0.084(8) -0.008(7) -0.071(10) 0.053(10) C21 0.38(3) 0.085(11) 0.111(13) 0.000(10) -0.136(17) 0.017(17) C22 0.40(4) 0.093(11) 0.30(4) 0.078(17) -0.12(3) -0.069(14) C23 0.27(2) 0.169(16) 0.28(3) 0.134(19) -0.08(2) -0.111(14) C24 0.160(13) 0.177(17) 0.23(2) 0.130(17) -0.043(12) -0.047(11) C25 0.171(15) 0.214(17) 0.213(19) 0.124(15) 0.033(17) -0.036(11) C26 0.23(2) 0.29(3) 0.31(3) 0.02(3) 0.03(3) 0.04(2) C27 0.71(6) 0.146(17) 0.192(19) -0.018(14) -0.16(3) -0.05(2) C28 0.098(12) 0.212(18) 0.151(15) 0.036(14) 0.036(12) 0.038(13) C29 0.103(16) 0.28(3) 0.23(2) 0.10(2) 0.058(16) 0.052(17) C30 0.070(9) 0.173(16) 0.22(2) 0.033(16) -0.022(12) 0.011(11) C31 0.058(8) 0.161(14) 0.196(16) 0.065(13) -0.008(10) 0.047(9) Li 0.080(12) 0.059(8) 0.063(10) 0.006(8) -0.003(10) 0.001(9) _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 C1 2.206(9) . ? Sn1 C10 2.236(12) . ? Sn1 C19 2.237(11) . ? Sn1 Li 2.721(16) . ? O1 C31 1.413(14) . ? O1 C28 1.435(16) . ? O1 Li 1.92(2) . ? N1 C9 1.450(13) . ? N1 C8 1.456(15) . ? N1 C7 1.502(13) . ? N1 Li 2.133(19) . ? N2 C18 1.457(15) . ? N2 C17 1.459(16) . ? N2 C16 1.490(14) . ? N2 Li 2.148(19) . ? N3 C27 1.424(11) . ? N3 C26 1.453(11) . ? N3 C25 1.461(11) . ? C1 C2 1.377(13) . ? C1 C6 1.389(13) . ? C2 C3 1.367(15) . ? C2 H21 0.9300 . ? C3 C4 1.371(19) . ? C3 H31 0.9300 . ? C4 C5 1.337(17) . ? C4 H41 0.9300 . ? C5 C6 1.365(14) . ? C5 H51 0.9300 . ? C6 C7 1.539(14) . ? C7 H71 0.9700 . ? C7 H72 0.9700 . ? C8 Li 2.71(2) . ? C8 H81 0.9600 . ? C8 H82 0.9600 . ? C8 H83 0.9600 . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? C10 C15 1.384(16) . ? C10 C11 1.396(16) . ? C11 C12 1.34(2) . ? C11 H111 0.9300 . ? C12 C13 1.39(2) . ? C12 H121 0.9300 . ? C13 C14 1.35(2) . ? C13 H131 0.9300 . ? C14 C15 1.414(17) . ? C14 H141 0.9300 . ? C15 C16 1.520(18) . ? C16 H161 0.9700 . ? C16 H162 0.9700 . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? C18 H181 0.9600 . ? C18 H182 0.9600 . ? C18 H183 0.9600 . ? C19 C20 1.34(2) . ? C19 C24 1.44(2) . ? C20 C21 1.39(2) . ? C20 H201 0.9300 . ? C21 C22 1.36(4) . ? C21 H211 0.9300 . ? C22 C23 1.56(4) . ? C22 H221 0.9300 . ? C23 C24 1.40(2) . ? C23 H231 0.9300 . ? C24 C25 1.547(12) . ? C25 H251 0.9801 . ? C25 H252 0.9799 . ? C26 H261 0.9600 . ? C26 H262 0.9600 . ? C26 H263 0.9600 . ? C27 H271 0.9600 . ? C27 H272 0.9600 . ? C27 H273 0.9600 . ? C28 C29 1.42(2) . ? C28 H281 0.9700 . ? C28 H282 0.9700 . ? C29 C30 1.48(2) . ? C29 H291 0.9700 . ? C29 H292 0.9700 . ? C30 C31 1.441(19) . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 H311 0.9700 . ? C31 H312 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 C1 Sn1 C10 93.7(4) . . ? C1 Sn1 C19 97.6(4) . . ? C10 Sn1 C19 99.2(5) . . ? C1 Sn1 Li 101.3(4) . . ? C10 Sn1 Li 89.0(5) . . ? C19 Sn1 Li 158.8(5) . . ? C31 O1 C28 108.1(11) . . ? C31 O1 Li 133.0(10) . . ? C28 O1 Li 118.9(10) . . ? C9 N1 C8 110.6(9) . . ? C9 N1 C7 109.8(9) . . ? C8 N1 C7 108.5(10) . . ? C9 N1 Li 111.9(9) . . ? C8 N1 Li 96.2(8) . . ? C7 N1 Li 118.9(8) . . ? C18 N2 C17 107.9(12) . . ? C18 N2 C16 111.2(10) . . ? C17 N2 C16 106.2(10) . . ? C18 N2 Li 115.8(9) . . ? C17 N2 Li 101.7(10) . . ? C16 N2 Li 113.1(8) . . ? C27 N3 C26 118(2) . . ? C27 N3 C25 97(2) . . ? C26 N3 C25 111.1(18) . . ? C2 C1 C6 114.6(10) . . ? C2 C1 Sn1 121.4(8) . . ? C6 C1 Sn1 123.9(7) . . ? C3 C2 C1 123.3(11) . . ? C3 C2 H21 118.3 . . ? C1 C2 H21 118.3 . . ? C2 C3 C4 119.3(12) . . ? C2 C3 H31 120.3 . . ? C4 C3 H31 120.3 . . ? C5 C4 C3 119.4(13) . . ? C5 C4 H41 120.3 . . ? C3 C4 H41 120.3 . . ? C4 C5 C6 120.8(12) . . ? C4 C5 H51 119.6 . . ? C6 C5 H51 119.6 . . ? C5 C6 C1 122.5(11) . . ? C5 C6 C7 115.8(10) . . ? C1 C6 C7 121.4(10) . . ? N1 C7 C6 115.0(9) . . ? N1 C7 H71 108.5 . . ? C6 C7 H71 108.5 . . ? N1 C7 H72 108.5 . . ? C6 C7 H72 108.5 . . ? H71 C7 H72 107.5 . . ? N1 C8 Li 51.5(6) . . ? N1 C8 H81 109.5 . . ? Li C8 H81 84.2 . . ? N1 C8 H82 109.5 . . ? Li C8 H82 160.4 . . ? H81 C8 H82 109.5 . . ? N1 C8 H83 109.5 . . ? Li C8 H83 77.4 . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? N1 C9 H91 109.5 . . ? N1 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? N1 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? C15 C10 C11 116.3(13) . . ? C15 C10 Sn1 119.4(9) . . ? C11 C10 Sn1 123.9(10) . . ? C12 C11 C10 124.6(15) . . ? C12 C11 H111 117.7 . . ? C10 C11 H111 117.7 . . ? C11 C12 C13 120.0(16) . . ? C11 C12 H121 120.0 . . ? C13 C12 H121 120.0 . . ? C14 C13 C12 116.5(18) . . ? C14 C13 H131 121.7 . . ? C12 C13 H131 121.7 . . ? C13 C14 C15 124.8(16) . . ? C13 C14 H141 117.6 . . ? C15 C14 H141 117.6 . . ? C10 C15 C14 117.9(13) . . ? C10 C15 C16 123.0(12) . . ? C14 C15 C16 119.1(11) . . ? N2 C16 C15 114.5(10) . . ? N2 C16 H161 108.6 . . ? C15 C16 H161 108.6 . . ? N2 C16 H162 108.6 . . ? C15 C16 H162 108.6 . . ? H161 C16 H162 107.6 . . ? N2 C17 H171 109.5 . . ? N2 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? N2 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? N2 C18 H181 109.5 . . ? N2 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? N2 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? C20 C19 C24 120.5(13) . . ? C20 C19 Sn1 121.8(13) . . ? C24 C19 Sn1 117.7(11) . . ? C19 C20 C21 123(2) . . ? C19 C20 H201 118.5 . . ? C21 C20 H201 118.5 . . ? C22 C21 C20 115(3) . . ? C22 C21 H211 122.5 . . ? C20 C21 H211 122.5 . . ? C21 C22 C23 127(2) . . ? C21 C22 H221 116.4 . . ? C23 C22 H221 116.4 . . ? C24 C23 C22 107(2) . . ? C24 C23 H231 126.6 . . ? C22 C23 H231 126.6 . . ? C23 C24 C19 124(2) . . ? C23 C24 C25 111(2) . . ? C19 C24 C25 123.8(14) . . ? N3 C25 C24 119.9(17) . . ? N3 C25 H251 104.1 . . ? C24 C25 H251 109.9 . . ? N3 C25 H252 102.2 . . ? C24 C25 H252 110.7 . . ? H251 C25 H252 109.5 . . ? N3 C26 H261 109.5 . . ? N3 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? N3 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? N3 C27 H271 109.1 . . ? N3 C27 H272 108.0 . . ? H271 C27 H272 109.5 . . ? N3 C27 H273 111.3 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C29 C28 O1 107.7(15) . . ? C29 C28 H281 110.2 . . ? O1 C28 H281 110.2 . . ? C29 C28 H282 110.2 . . ? O1 C28 H282 110.2 . . ? H281 C28 H282 108.5 . . ? C28 C29 C30 105.9(16) . . ? C28 C29 H291 110.6 . . ? C30 C29 H291 110.6 . . ? C28 C29 H292 110.6 . . ? C30 C29 H292 110.6 . . ? H291 C29 H292 108.7 . . ? C31 C30 C29 104.3(15) . . ? C31 C30 H301 110.9 . . ? C29 C30 H301 110.9 . . ? C31 C30 H302 110.9 . . ? C29 C30 H302 110.9 . . ? H301 C30 H302 108.9 . . ? O1 C31 C30 106.5(14) . . ? O1 C31 H311 110.4 . . ? C30 C31 H311 110.4 . . ? O1 C31 H312 110.4 . . ? C30 C31 H312 110.4 . . ? H311 C31 H312 108.6 . . ? O1 Li N1 106.2(8) . . ? O1 Li N2 113.6(9) . . ? N1 Li N2 125.4(10) . . ? O1 Li C8 102.3(8) . . ? N1 Li C8 32.3(4) . . ? N2 Li C8 101.6(8) . . ? O1 Li Sn1 120.2(8) . . ? N1 Li Sn1 92.2(6) . . ? N2 Li Sn1 98.2(6) . . ? C8 Li Sn1 119.8(7) . . ? 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 C6 C1 C2 C3 0.0(19) . . . . ? Sn1 C1 C2 C3 -176.9(11) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? C2 C3 C4 C5 3(3) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C4 C5 C6 C1 1(2) . . . . ? C4 C5 C6 C7 -173.1(13) . . . . ? C2 C1 C6 C5 0.5(17) . . . . ? Sn1 C1 C6 C5 177.4(9) . . . . ? C2 C1 C6 C7 173.9(11) . . . . ? Sn1 C1 C6 C7 -9.3(15) . . . . ? C9 N1 C7 C6 45.3(11) . . . . ? C8 N1 C7 C6 166.3(10) . . . . ? Li N1 C7 C6 -85.4(11) . . . . ? C5 C6 C7 N1 -115.7(12) . . . . ? C1 C6 C7 N1 70.6(13) . . . . ? C9 N1 C8 Li -116.3(10) . . . . ? C7 N1 C8 Li 123.2(10) . . . . ? C15 C10 C11 C12 -1(2) . . . . ? Sn1 C10 C11 C12 -173.3(12) . . . . ? C10 C11 C12 C13 0(3) . . . . ? C11 C12 C13 C14 1(3) . . . . ? C12 C13 C14 C15 -1(3) . . . . ? C11 C10 C15 C14 1.2(18) . . . . ? Sn1 C10 C15 C14 173.6(9) . . . . ? C11 C10 C15 C16 178.1(12) . . . . ? Sn1 C10 C15 C16 -9.5(16) . . . . ? C13 C14 C15 C10 0(2) . . . . ? C13 C14 C15 C16 -177.0(15) . . . . ? C18 N2 C16 C15 67.0(13) . . . . ? C17 N2 C16 C15 -175.8(11) . . . . ? Li N2 C16 C15 -65.1(13) . . . . ? C10 C15 C16 N2 85.3(14) . . . . ? C14 C15 C16 N2 -97.9(13) . . . . ? C24 C19 C20 C21 9(2) . . . . ? Sn1 C19 C20 C21 -173.3(10) . . . . ? C19 C20 C21 C22 -2(3) . . . . ? C20 C21 C22 C23 -16(5) . . . . ? C21 C22 C23 C24 23(4) . . . . ? C22 C23 C24 C19 -14(3) . . . . ? C22 C23 C24 C25 179(2) . . . . ? C20 C19 C24 C23 0(3) . . . . ? Sn1 C19 C24 C23 -177.1(17) . . . . ? C20 C19 C24 C25 166.2(17) . . . . ? Sn1 C19 C24 C25 -11(3) . . . . ? C27 N3 C25 C24 -55(2) . . . . ? C26 N3 C25 C24 -178(2) . . . . ? C23 C24 C25 N3 -47(3) . . . . ? C19 C24 C25 N3 145.4(18) . . . . ? C31 O1 C28 C29 3(2) . . . . ? Li O1 C28 C29 -178.1(15) . . . . ? O1 C28 C29 C30 14(2) . . . . ? C28 C29 C30 C31 -25(2) . . . . ? C28 O1 C31 C30 -20(2) . . . . ? Li O1 C31 C30 162.2(14) . . . . ? C29 C30 C31 O1 27(2) . . . . ? _refine_diff_density_max 0.483 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.069 _shelx_res_file ; h.res created by SHELXL-2014/7 TITL S787A MOKA 50KV 30MA 22C ZR 191192 (Spek, 1997)' CELL 0.71073 10.0617 15.8787 20.0617 90.000 90.000 90.000 ZERR 4 0.0006 0.0007 0.0010 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H Li N O Sn UNIT 124 176 4 12 4 4 MERG 2 OMIT -2 55 L.S. 10 FMAP 2 PLAN -20 ACTA BOND $H CONF DFIX 1.52 0.01 C24 C25 DFIX 1.45 0.01 N3 C26 N3 C27 DFIX 1.50 0.01 N3 C25 ISOR N3 C21 C22 C23 C24 C27 DELU N3 C25 N3 C27 N3 C26 C21 C22 C22 C23 C24 C25 DELU C19 C24 C10 C11 C13 C14 C15 C16 C19 C20 C30 C31 TWIN WGHT 0.060600 BASF 0.04116 FVAR 15.18365 SN1 6 0.631853 0.053714 0.350205 11.00000 0.06897 0.06350 = 0.06943 0.00760 -0.00985 -0.00120 O1 5 0.371314 0.211023 0.260935 11.00000 0.06531 0.12138 = 0.10275 0.03182 0.00255 0.01086 N1 4 0.679047 0.259531 0.289191 11.00000 0.05952 0.06981 = 0.07641 0.02044 -0.00072 0.00554 N2 4 0.576253 0.085368 0.169715 11.00000 0.09945 0.09336 = 0.06627 0.00242 -0.00682 0.00386 N3 4 0.268837 -0.029242 0.479626 11.00000 0.20424 0.20885 = 0.11545 0.00466 0.06379 -0.02736 C1 1 0.759112 0.135625 0.411962 11.00000 0.06028 0.04962 = 0.06597 0.00106 -0.01310 -0.00351 C2 1 0.781724 0.118368 0.478287 11.00000 0.12979 0.07166 = 0.07778 0.00809 -0.02908 -0.01754 AFIX 43 H21 2 0.745426 0.069492 0.496204 11.00000 -1.20000 AFIX 0 C3 1 0.854817 0.169433 0.519125 11.00000 0.18510 0.10579 = 0.07910 0.00488 -0.06975 -0.03323 AFIX 43 H31 2 0.865575 0.155971 0.563917 11.00000 -1.20000 AFIX 0 C4 1 0.912088 0.240703 0.493342 11.00000 0.13577 0.09130 = 0.11102 -0.02075 -0.04180 -0.02492 AFIX 43 H41 2 0.965171 0.274789 0.520031 11.00000 -1.20000 AFIX 0 C5 1 0.890944 0.260746 0.429512 11.00000 0.10980 0.09127 = 0.08531 -0.00294 -0.02273 -0.02957 AFIX 43 H51 2 0.927146 0.310056 0.412305 11.00000 -1.20000 AFIX 0 C6 1 0.816873 0.209742 0.389261 11.00000 0.07398 0.06772 = 0.07722 0.00030 -0.01459 0.00219 C7 1 0.813352 0.234259 0.315045 11.00000 0.06623 0.06298 = 0.07995 -0.00421 0.00212 0.00057 AFIX 23 H71 2 0.874504 0.280646 0.308032 11.00000 -1.20000 H72 2 0.845154 0.186913 0.288985 11.00000 -1.20000 AFIX 0 C8 1 0.696398 0.299967 0.224625 11.00000 0.14028 0.13351 = 0.11088 0.03483 -0.01464 -0.04946 AFIX 137 H81 2 0.740530 0.261913 0.194746 11.00000 -1.50000 H82 2 0.749063 0.349945 0.229861 11.00000 -1.50000 H83 2 0.611042 0.314701 0.206703 11.00000 -1.50000 AFIX 0 C9 1 0.615757 0.316516 0.335914 11.00000 0.09532 0.10057 = 0.12175 -0.02457 -0.01949 0.02306 AFIX 137 H91 2 0.611227 0.290392 0.379009 11.00000 -1.50000 H92 2 0.527561 0.329342 0.320741 11.00000 -1.50000 H93 2 0.666583 0.367541 0.338924 11.00000 -1.50000 AFIX 0 C10 1 0.797951 0.016333 0.282340 11.00000 0.06874 0.07200 = 0.09537 -0.01212 -0.01431 0.01435 C11 1 0.931384 0.014439 0.301423 11.00000 0.08082 0.09721 = 0.13526 -0.03225 -0.02435 0.04121 AFIX 43 H111 2 0.951030 0.023812 0.346109 11.00000 -1.20000 AFIX 0 C12 1 1.033371 0.000017 0.259718 11.00000 0.08558 0.13589 = 0.19172 -0.04119 -0.02484 0.03523 AFIX 43 H121 2 1.119990 -0.000400 0.275892 11.00000 -1.20000 AFIX 0 C13 1 1.009539 -0.014256 0.192520 11.00000 0.11626 0.12499 = 0.17795 -0.04757 0.01832 0.02535 AFIX 43 H131 2 1.078207 -0.025364 0.162762 11.00000 -1.20000 AFIX 0 C14 1 0.881706 -0.011179 0.172653 11.00000 0.12520 0.11700 = 0.11629 -0.04042 0.02638 0.01720 AFIX 43 H141 2 0.864135 -0.019532 0.127624 11.00000 -1.20000 AFIX 0 C15 1 0.772336 0.003827 0.215284 11.00000 0.09597 0.06846 = 0.08170 -0.01566 -0.00324 0.00178 C16 1 0.632611 0.001269 0.186546 11.00000 0.11050 0.09419 = 0.07032 -0.01976 -0.00561 0.00598 AFIX 23 H161 2 0.633560 -0.033039 0.146543 11.00000 -1.20000 H162 2 0.574405 -0.025971 0.218495 11.00000 -1.20000 AFIX 0 C17 1 0.439915 0.070400 0.147954 11.00000 0.13890 0.12505 = 0.15296 -0.02388 -0.06413 0.01838 AFIX 137 H171 2 0.392188 0.041300 0.182398 11.00000 -1.50000 H172 2 0.440514 0.036756 0.108197 11.00000 -1.50000 H173 2 0.397339 0.123295 0.138950 11.00000 -1.50000 AFIX 0 C18 1 0.648089 0.124035 0.114555 11.00000 0.24700 0.11586 = 0.07501 0.00471 0.04926 0.01687 AFIX 137 H181 2 0.738183 0.134816 0.127797 11.00000 -1.50000 H182 2 0.605882 0.176105 0.102588 11.00000 -1.50000 H183 2 0.647523 0.086654 0.076947 11.00000 -1.50000 AFIX 0 C19 1 0.630886 -0.058398 0.417713 11.00000 0.15717 0.06944 = 0.09699 0.01939 -0.05769 -0.00837 C20 1 0.734409 -0.111150 0.421210 11.00000 0.24376 0.07727 = 0.08359 -0.00827 -0.07078 0.05258 AFIX 43 H201 2 0.811788 -0.097283 0.398354 11.00000 -1.20000 AFIX 0 C21 1 0.731480 -0.185601 0.457404 11.00000 0.38373 0.08544 = 0.11136 -0.00047 -0.13581 0.01737 AFIX 43 H211 2 0.803069 -0.222610 0.458717 11.00000 -1.20000 AFIX 0 C22 1 0.616426 -0.200448 0.490758 11.00000 0.40479 0.09302 = 0.29722 0.07789 -0.11701 -0.06901 AFIX 43 H221 2 0.602979 -0.255249 0.505663 11.00000 -1.20000 AFIX 0 C23 1 0.504629 -0.135889 0.506784 11.00000 0.26953 0.16893 = 0.28371 0.13353 -0.07920 -0.11145 AFIX 43 H231 2 0.442130 -0.139828 0.540794 11.00000 -1.20000 AFIX 0 C24 1 0.516251 -0.070522 0.460013 11.00000 0.15969 0.17684 = 0.22906 0.13019 -0.04318 -0.04693 C25 1 0.406928 -0.003309 0.470571 11.00000 0.17117 0.21374 = 0.21264 0.12391 0.03270 -0.03640 AFIX 3 H251 2 0.404008 0.034851 0.432201 11.00000 -1.20000 H252 2 0.423928 0.029181 0.511212 11.00000 -1.20000 AFIX 0 C26 1 0.182071 0.043295 0.486852 11.00000 0.22677 0.29266 = 0.31418 0.01537 0.02933 0.04127 AFIX 137 H261 2 0.097023 0.025265 0.503186 11.00000 -1.50000 H262 2 0.171097 0.070197 0.444352 11.00000 -1.50000 H263 2 0.220746 0.082365 0.517793 11.00000 -1.50000 AFIX 0 C27 1 0.258569 -0.077716 0.420107 11.00000 0.70506 0.14564 = 0.19188 -0.01786 -0.16136 -0.05439 AFIX 3 H271 2 0.323529 -0.121977 0.421168 11.00000 -1.50000 H272 2 0.276285 -0.041167 0.383039 11.00000 -1.50000 H273 2 0.171479 -0.101690 0.415420 11.00000 -1.50000 AFIX 0 C28 1 0.286716 0.187113 0.315304 11.00000 0.09773 0.21181 = 0.15131 0.03575 0.03632 0.03766 AFIX 23 H281 2 0.274362 0.126531 0.315705 11.00000 -1.20000 H282 2 0.326351 0.203826 0.357348 11.00000 -1.20000 AFIX 0 C29 1 0.162499 0.228322 0.306393 11.00000 0.10342 0.27737 = 0.23175 0.10159 0.05850 0.05170 AFIX 23 H291 2 0.152938 0.274261 0.337901 11.00000 -1.20000 H292 2 0.089719 0.189101 0.312854 11.00000 -1.20000 AFIX 0 C30 1 0.163189 0.260587 0.237232 11.00000 0.07015 0.17282 = 0.22214 0.03261 -0.02220 0.01109 AFIX 23 H301 2 0.120961 0.220935 0.207161 11.00000 -1.20000 H302 2 0.117252 0.314175 0.234402 11.00000 -1.20000 AFIX 0 C31 1 0.302102 0.270177 0.221428 11.00000 0.05805 0.16078 = 0.19601 0.06547 -0.00786 0.04673 AFIX 23 H311 2 0.317409 0.259358 0.174464 11.00000 -1.20000 H312 2 0.331621 0.326904 0.231560 11.00000 -1.20000 AFIX 0 LI 3 0.546232 0.163854 0.255613 11.00000 0.07989 0.05896 = 0.06340 0.00585 -0.00300 0.00146 HKLF 4 REM S787A MOKA 50KV 30MA 22C ZR 191192 REM R1 = 0.0628 for 2297 Fo > 4sig(Fo) and 0.1520 for all 6072 data REM 340 parameters refined using 68 restraints END WGHT 0.0608 0.0000 REM Highest difference peak 0.483, deepest hole -0.482, 1-sigma level 0.069 Q1 1 0.3689 -0.0395 0.5390 11.00000 0.05 0.48 Q2 1 0.3788 0.0053 0.4762 11.00000 0.05 0.46 Q3 1 0.4050 -0.0556 0.4183 11.00000 0.05 0.45 Q4 1 0.6247 0.1374 0.3472 11.00000 0.05 0.38 Q5 1 0.5385 -0.1939 0.4618 11.00000 0.05 0.33 Q6 1 0.3727 -0.0998 0.4652 11.00000 0.05 0.31 Q7 1 0.5757 -0.1151 0.4221 11.00000 0.05 0.29 Q8 1 0.6565 -0.0805 0.3761 11.00000 0.05 0.28 Q9 1 0.5827 -0.2032 0.5200 11.00000 0.05 0.27 Q10 1 0.6384 0.4003 0.2734 11.00000 0.05 0.26 Q11 1 0.8767 0.0773 0.2720 11.00000 0.05 0.26 Q12 1 0.5930 -0.0218 0.3803 11.00000 0.05 0.25 Q13 1 0.2520 0.1409 0.2636 11.00000 0.05 0.25 Q14 1 0.2584 0.0412 0.2527 11.00000 0.05 0.25 Q15 1 0.8760 0.2458 0.2490 11.00000 0.05 0.25 Q16 1 0.6276 0.0568 0.3814 11.00000 0.05 0.25 Q17 1 0.3690 0.0031 0.2282 11.00000 0.05 0.25 Q18 1 0.2025 -0.0420 0.4248 11.00000 0.05 0.24 Q19 1 0.5740 0.1361 0.3863 11.00000 0.05 0.24 Q20 1 0.1415 0.1669 0.2359 11.00000 0.05 0.24 ; _shelx_res_checksum 26119 _shelx_hkl_file ; 2 0 0 5463737 65828 4 0 0 6640118 89327 6 0 0 166751 13553 8 0 0 343131 18330 10 0 0 44612 21866 12 0 0 23127 13612 1 1 0 9080320 97344 2 1 0 1467 3114 3 1 0 1392392 29146 4 1 0 6374 12770 5 1 0 1542449 35885 6 1 0 256968 13032 7 1 0 262710 15301 8 1 0 79311 14728 9 1 0 174899 20502 10 1 0 21446 29920 11 1 0 22701 32543 12 1 0 21860 16208 13 1 0 20629 7933 0 2 0 3830921 46586 1 2 0 301580 6782 2 2 0 1542449 27651 3 2 0 292372 8026 4 2 0 481912 11104 5 2 0 895390 19863 6 2 0 60031 11049 7 2 0 312503 15743 8 2 0 495694 20132 9 2 0 22278 18259 10 2 0 21446 29920 11 2 0 18965 18489 12 2 0 16600 23925 1 3 0 487795 10667 2 3 0 6640118 81647 3 3 0 1013645 23151 4 3 0 21035 6715 5 3 0 1209416 26175 6 3 0 1250013 28743 7 3 0 178450 15359 8 3 0 27142 14672 9 3 0 53981 19728 10 3 0 84141 15721 11 3 0 20226 28321 12 3 0 14024 24858 0 4 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