# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1530 data_global #============================================================================ # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr P J Brothers Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; _publ_contact_author_phone '64 9 373 7999' _publ_contact_author_fax '64 9 373 7422' _publ_contact_author_email p.brothers@auckland.ac.nz _publ_contact_letter ; The data described in these .cif files has been submited for publication in Dalton transactions. ; #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Tin Complexes of Dibenzotetramethyltetraaza[14]annulene: Organometallic Derivatives. ; loop_ _publ_author_name _publ_author_address 'Belcher, Warwick J.' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Brothers, Penelope J' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Meredith, Anthony P' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Oliver, Allen G.' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Rickard, Clifton E. F.' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Uffing, Christoph' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Ware, David C.' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; #============================================================================ data_apmze _audit_creation_method SHELXL-97 _chemical_name_systematic ; (u-methylene)bis(5,14-dihydro-6,8,15,17-tetramethyldibenzo[b,i][1,4,8,11]- tetraazacyclotetradecinatotin(IV))diiodide.lithium iodide.dihydrate. dichloroform solvate ; _chemical_name_common ? _chemical_formula_moiety 'C45 H46 N8 Sn2 I2, Li I, 3(H2 O), 2(C H Cl3)' _chemical_formula_sum 'C47 H54 Cl6 I3 Li N8 O3 Sn2' _chemical_formula_weight 1610.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P 21/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 14.45100(10) _cell_length_b 16.7506(2) _cell_length_c 24.8794(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.1760(10) _cell_angle_gamma 90.00 _cell_volume 5838.99(12) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 7880 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26.0 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 2.761 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5452 _exptl_absorpt_correction_T_max 0.8518 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33860 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.43 _reflns_number_total 11899 _reflns_number_gt 8591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+37.6328P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11899 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.044 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.80303(3) 0.92216(3) 0.18352(2) 0.02613(12) Uani 1 d . . . Sn2 Sn 1.03642(3) 0.91252(3) 0.285290(19) 0.02277(12) Uani 1 d . . . N1 N 0.7828(4) 1.0376(4) 0.2116(3) 0.0319(14) Uani 1 d . . . N2 N 0.8431(4) 0.9719(4) 0.1151(2) 0.0327(14) Uani 1 d . . . N3 N 0.7423(4) 0.8415(4) 0.1187(2) 0.0306(14) Uani 1 d . . . N4 N 0.6854(4) 0.9061(4) 0.2180(3) 0.0312(14) Uani 1 d . . . N5 N 1.0520(4) 1.0289(3) 0.2577(2) 0.0277(13) Uani 1 d . . . N6 N 0.9939(4) 0.9567(4) 0.3544(2) 0.0297(13) Uani 1 d . . . N7 N 1.0895(4) 0.8245(3) 0.3446(2) 0.0243(12) Uani 1 d . . . N8 N 1.1502(4) 0.8971(3) 0.2495(2) 0.0249(12) Uani 1 d . . . C1 C 0.7490(8) 1.1823(6) 0.2022(4) 0.063(3) Uani 1 d . . . H1A H 0.6956 1.1718 0.2184 0.094 Uiso 1 calc R . . H1B H 0.7292 1.2189 0.1713 0.094 Uiso 1 calc R . . H1C H 0.8008 1.2059 0.2300 0.094 Uiso 1 calc R . . C2 C 0.7820(6) 1.1057(5) 0.1821(4) 0.042(2) Uani 1 d . . . C3 C 0.8084(6) 1.1082(5) 0.1323(4) 0.042(2) Uani 1 d . . . H3A H 0.8095 1.1598 0.1177 0.050 Uiso 1 calc R . . C4 C 0.8338(5) 1.0478(5) 0.0999(3) 0.0366(18) Uani 1 d . . . C5 C 0.8475(7) 1.0733(5) 0.0442(4) 0.052(2) Uani 1 d . . . H5A H 0.8263 1.0310 0.0174 0.079 Uiso 1 calc R . . H5B H 0.9145 1.0842 0.0474 0.079 Uiso 1 calc R . . H5C H 0.8105 1.1212 0.0321 0.079 Uiso 1 calc R . . C6 C 0.6137(6) 0.7636(5) 0.0574(3) 0.0404(19) Uani 1 d . . . H6A H 0.6288 0.7919 0.0266 0.061 Uiso 1 calc R . . H6B H 0.5450 0.7601 0.0516 0.061 Uiso 1 calc R . . H6C H 0.6406 0.7103 0.0598 0.061 Uiso 1 calc R . . C7 C 0.6553(5) 0.8081(4) 0.1106(3) 0.0341(17) Uani 1 d . . . C8 C 0.5983(5) 0.8159(5) 0.1481(3) 0.0319(17) Uani 1 d . . . H8A H 0.5433 0.7837 0.1399 0.038 Uiso 1 calc R . . C9 C 0.6077(5) 0.8625(5) 0.1955(3) 0.0332(17) Uani 1 d . . . C10 C 0.5244(6) 0.8653(5) 0.2208(4) 0.044(2) Uani 1 d . . . H10A H 0.5169 0.9191 0.2335 0.066 Uiso 1 calc R . . H10B H 0.5349 0.8288 0.2520 0.066 Uiso 1 calc R . . H10C H 0.4672 0.8497 0.1934 0.066 Uiso 1 calc R . . C11 C 0.8606(5) 0.9063(5) 0.0821(3) 0.0328(17) Uani 1 d . . . C12 C 0.9349(6) 0.9051(5) 0.0548(3) 0.042(2) Uani 1 d . . . H12A H 0.9729 0.9506 0.0546 0.050 Uiso 1 calc R . . C13 C 0.9512(6) 0.8363(6) 0.0285(3) 0.047(2) Uani 1 d . . . H13A H 1.0003 0.8356 0.0097 0.056 Uiso 1 calc R . . C14 C 0.8979(6) 0.7687(6) 0.0288(3) 0.044(2) Uani 1 d . . . H14A H 0.9097 0.7228 0.0098 0.053 Uiso 1 calc R . . C15 C 0.8259(6) 0.7684(5) 0.0575(3) 0.0360(18) Uani 1 d . . . H15A H 0.7911 0.7214 0.0591 0.043 Uiso 1 calc R . . C16 C 0.8057(5) 0.8367(5) 0.0834(3) 0.0310(16) Uani 1 d . . . C21 C 0.6969(5) 0.9586(5) 0.2641(3) 0.0349(17) Uani 1 d . . . C22 C 0.6696(6) 0.9409(6) 0.3122(4) 0.046(2) Uani 1 d . . . H22A H 0.6390 0.8923 0.3155 0.055 Uiso 1 calc R . . C23 C 0.6876(7) 0.9955(6) 0.3559(4) 0.052(2) Uani 1 d . . . H23A H 0.6662 0.9851 0.3880 0.063 Uiso 1 calc R . . C24 C 0.7373(7) 1.0653(6) 0.3518(4) 0.053(2) Uani 1 d . . . H24A H 0.7487 1.1022 0.3812 0.064 Uiso 1 calc R . . C25 C 0.7705(6) 1.0815(5) 0.3050(4) 0.046(2) Uani 1 d . . . H25A H 0.8072 1.1274 0.3035 0.055 Uiso 1 calc R . . C26 C 0.7485(5) 1.0286(5) 0.2606(3) 0.0358(18) Uani 1 d . . . C30 C 0.9167(5) 0.8569(4) 0.2329(3) 0.0285(15) Uani 1 d . . . H30A H 0.9411 0.8222 0.2078 0.034 Uiso 1 calc R . . H30B H 0.8892 0.8218 0.2564 0.034 Uiso 1 calc R . . C31 C 1.0854(7) 1.1722(5) 0.2708(4) 0.055(2) Uani 1 d . . . H31A H 1.1390 1.1631 0.2546 0.082 Uiso 1 calc R . . H31B H 1.1049 1.2070 0.3028 0.082 Uiso 1 calc R . . H31C H 1.0337 1.1971 0.2437 0.082 Uiso 1 calc R . . C32 C 1.0522(5) 1.0943(5) 0.2885(3) 0.0359(18) Uani 1 d . . . C33 C 1.0263(6) 1.0942(4) 0.3391(3) 0.0376(18) Uani 1 d . . . H33A H 1.0230 1.1454 0.3541 0.045 Uiso 1 calc R . . C34 C 1.0044(5) 1.0325(4) 0.3716(3) 0.0301(16) Uani 1 d . . . C35 C 0.9970(6) 1.0544(5) 0.4290(3) 0.044(2) Uani 1 d . . . H35A H 1.0314 1.0154 0.4553 0.066 Uiso 1 calc R . . H35B H 0.9305 1.0549 0.4302 0.066 Uiso 1 calc R . . H35C H 1.0244 1.1069 0.4385 0.066 Uiso 1 calc R . . C36 C 1.2150(6) 0.7401(5) 0.4027(3) 0.043(2) Uani 1 d . . . H36A H 1.1940 0.7609 0.4341 0.064 Uiso 1 calc R . . H36B H 1.2841 0.7404 0.4110 0.064 Uiso 1 calc R . . H36C H 1.1920 0.6858 0.3951 0.064 Uiso 1 calc R . . C37 C 1.1759(5) 0.7913(4) 0.3527(3) 0.0281(15) Uani 1 d . . . C38 C 1.2356(5) 0.8036(4) 0.3170(3) 0.0334(17) Uani 1 d . . . H38A H 1.2914 0.7724 0.3256 0.040 Uiso 1 calc R . . C39 C 1.2287(5) 0.8529(4) 0.2714(3) 0.0316(17) Uani 1 d . . . C40 C 1.3149(6) 0.8593(5) 0.2487(4) 0.043(2) Uani 1 d . . . H40A H 1.3261 0.9148 0.2412 0.064 Uiso 1 calc R . . H40B H 1.3048 0.8289 0.2145 0.064 Uiso 1 calc R . . H40C H 1.3699 0.8382 0.2754 0.064 Uiso 1 calc R . . C41 C 0.9759(5) 0.8897(4) 0.3860(3) 0.0273(15) Uani 1 d . . . C42 C 0.9057(6) 0.8875(5) 0.4149(3) 0.042(2) Uani 1 d . . . H42A H 0.8706 0.9338 0.4179 0.051 Uiso 1 calc R . . C43 C 0.8870(6) 0.8169(6) 0.4397(4) 0.047(2) Uani 1 d . . . H43A H 0.8418 0.8163 0.4612 0.056 Uiso 1 calc R . . C44 C 0.9340(6) 0.7490(5) 0.4328(3) 0.043(2) Uani 1 d . . . H44A H 0.9198 0.7013 0.4491 0.051 Uiso 1 calc R . . C45 C 1.0022(6) 0.7481(5) 0.4024(3) 0.0343(17) Uani 1 d . . . H45A H 1.0326 0.7000 0.3973 0.041 Uiso 1 calc R . . C46 C 1.0257(5) 0.8192(5) 0.3792(3) 0.0317(16) Uani 1 d . . . C51 C 1.1408(5) 0.9536(4) 0.2048(3) 0.0266(15) Uani 1 d . . . C52 C 1.1722(6) 0.9403(5) 0.1570(3) 0.0381(18) Uani 1 d . . . H52A H 1.2028 0.8922 0.1524 0.046 Uiso 1 calc R . . C53 C 1.1579(6) 0.9982(6) 0.1165(3) 0.047(2) Uani 1 d . . . H53A H 1.1827 0.9908 0.0853 0.056 Uiso 1 calc R . . C54 C 1.1082(6) 1.0662(5) 0.1210(3) 0.040(2) Uani 1 d . . . H54A H 1.0996 1.1052 0.0930 0.048 Uiso 1 calc R . . C55 C 1.0704(6) 1.0783(5) 0.1663(3) 0.0377(18) Uani 1 d . . . H55A H 1.0328 1.1236 0.1679 0.045 Uiso 1 calc R . . C56 C 1.0880(5) 1.0230(4) 0.2099(3) 0.0303(16) Uani 1 d . . . I1 I 0.81853(4) 0.70750(3) 0.57651(2) 0.04206(15) Uani 1 d . . . I2 I 0.75748(5) 1.05374(4) 0.51245(3) 0.0622(2) Uani 1 d . . . I3 I 0.53126(4) 0.78718(3) 0.38860(2) 0.04759(16) Uani 1 d . . . C61 C 0.9437(9) 0.4983(6) 0.5873(5) 0.072(3) Uani 1 d . . . H61A H 0.9323 0.5566 0.5841 0.087 Uiso 1 calc R . . Cl1 Cl 0.9190(3) 0.4660(2) 0.64810(16) 0.1046(12) Uani 1 d . . . Cl2 Cl 0.8657(3) 0.4515(2) 0.53170(15) 0.1007(12) Uani 1 d . . . Cl3 Cl 1.0628(3) 0.4801(2) 0.5880(2) 0.1162(15) Uani 1 d . . . C62 C 0.5803(9) 0.8693(8) 0.6943(6) 0.097(4) Uani 1 d . . . H62A H 0.5596 0.9122 0.6666 0.116 Uiso 1 calc R . . Cl4 Cl 0.6775(3) 0.9038(3) 0.7474(2) 0.1212(15) Uani 1 d . . . Cl5 Cl 0.6115(4) 0.7868(3) 0.66232(18) 0.151(2) Uani 1 d . . . Cl6 Cl 0.4890(3) 0.8498(3) 0.7276(3) 0.180(3) Uani 1 d . . . O1 O 0.6514(6) 0.8604(5) 0.5199(3) 0.081(2) Uani 1 d . . . O2 O 0.4948(6) 0.9296(6) 0.5533(4) 0.097(3) Uani 1 d . . . O3 O 0.7868(12) 1.0120(9) 0.6428(6) 0.187(6) Uani 1 d . . . Li Li 0.5984(10) 1.0340(8) 0.6221(6) 0.038(3) Uiso 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 0.0199(2) 0.0303(3) 0.0266(3) 0.0011(2) 0.00269(19) -0.00521(19) Sn2 0.0207(2) 0.0249(2) 0.0221(2) -0.00032(19) 0.00417(18) 0.00295(18) N1 0.026(3) 0.031(3) 0.038(4) -0.003(3) 0.006(3) -0.002(3) N2 0.031(3) 0.034(3) 0.031(3) 0.001(3) 0.005(3) -0.011(3) N3 0.029(3) 0.032(3) 0.027(3) 0.002(3) -0.002(3) -0.009(3) N4 0.022(3) 0.038(3) 0.033(3) -0.001(3) 0.007(3) -0.006(3) N5 0.023(3) 0.023(3) 0.039(4) -0.003(3) 0.013(3) 0.000(2) N6 0.028(3) 0.032(3) 0.031(3) 0.000(3) 0.010(3) 0.004(3) N7 0.024(3) 0.028(3) 0.022(3) 0.001(2) 0.008(2) 0.003(2) N8 0.024(3) 0.027(3) 0.025(3) 0.000(2) 0.006(2) 0.003(2) C1 0.067(7) 0.045(5) 0.071(7) 0.002(5) 0.007(6) 0.010(5) C2 0.026(4) 0.035(4) 0.062(6) 0.000(4) 0.003(4) -0.005(3) C3 0.037(5) 0.034(4) 0.050(5) 0.014(4) 0.003(4) -0.009(4) C4 0.027(4) 0.041(5) 0.038(4) 0.006(4) 0.002(3) -0.012(3) C5 0.057(6) 0.049(5) 0.050(6) 0.020(4) 0.012(5) -0.007(4) C6 0.034(4) 0.043(5) 0.040(5) -0.001(4) -0.001(4) -0.013(4) C7 0.030(4) 0.027(4) 0.040(4) 0.003(3) -0.002(3) -0.010(3) C8 0.019(4) 0.043(4) 0.032(4) 0.005(3) 0.003(3) -0.014(3) C9 0.023(4) 0.040(4) 0.036(4) 0.013(3) 0.008(3) -0.004(3) C10 0.027(4) 0.053(5) 0.053(5) 0.003(4) 0.011(4) -0.008(4) C11 0.028(4) 0.043(4) 0.025(4) 0.002(3) 0.000(3) -0.007(3) C12 0.034(4) 0.060(5) 0.033(4) -0.002(4) 0.010(4) -0.018(4) C13 0.043(5) 0.065(6) 0.036(5) 0.000(4) 0.017(4) -0.006(4) C14 0.043(5) 0.058(6) 0.032(4) -0.003(4) 0.009(4) 0.001(4) C15 0.035(4) 0.040(4) 0.030(4) -0.002(3) 0.003(3) -0.009(3) C16 0.022(4) 0.043(4) 0.026(4) 0.000(3) 0.002(3) -0.008(3) C21 0.029(4) 0.038(4) 0.039(4) -0.002(3) 0.012(3) -0.001(3) C22 0.032(4) 0.059(6) 0.048(5) 0.000(4) 0.014(4) -0.004(4) C23 0.053(6) 0.068(6) 0.038(5) -0.007(4) 0.014(4) 0.009(5) C24 0.046(5) 0.059(6) 0.050(6) -0.013(5) 0.003(4) 0.008(5) C25 0.035(5) 0.048(5) 0.049(5) -0.005(4) 0.001(4) 0.005(4) C26 0.024(4) 0.042(4) 0.039(5) -0.011(4) 0.004(3) 0.001(3) C30 0.022(4) 0.031(4) 0.030(4) 0.003(3) 0.001(3) -0.006(3) C31 0.066(6) 0.029(4) 0.072(7) -0.005(4) 0.023(5) -0.011(4) C32 0.026(4) 0.032(4) 0.048(5) -0.002(4) 0.005(4) 0.003(3) C33 0.037(4) 0.027(4) 0.048(5) -0.014(3) 0.008(4) 0.003(3) C34 0.021(4) 0.031(4) 0.041(4) -0.008(3) 0.012(3) 0.004(3) C35 0.045(5) 0.053(5) 0.037(5) -0.010(4) 0.015(4) 0.006(4) C36 0.041(5) 0.043(5) 0.039(5) 0.007(4) 0.000(4) 0.012(4) C37 0.033(4) 0.025(3) 0.025(4) -0.003(3) 0.004(3) 0.006(3) C38 0.028(4) 0.025(4) 0.047(5) 0.002(3) 0.010(4) 0.011(3) C39 0.024(4) 0.026(4) 0.045(5) -0.010(3) 0.009(3) 0.002(3) C40 0.032(4) 0.046(5) 0.054(5) 0.002(4) 0.016(4) 0.013(4) C41 0.030(4) 0.032(4) 0.023(4) 0.005(3) 0.011(3) 0.004(3) C42 0.042(5) 0.056(5) 0.033(4) -0.001(4) 0.016(4) 0.010(4) C43 0.040(5) 0.064(6) 0.040(5) 0.010(4) 0.017(4) 0.000(4) C44 0.050(5) 0.048(5) 0.030(4) 0.011(4) 0.011(4) -0.006(4) C45 0.037(4) 0.034(4) 0.030(4) 0.002(3) 0.004(3) 0.000(3) C46 0.028(4) 0.042(4) 0.022(4) 0.000(3) 0.003(3) -0.002(3) C51 0.019(3) 0.036(4) 0.026(4) -0.005(3) 0.007(3) -0.010(3) C52 0.030(4) 0.048(5) 0.038(4) -0.003(4) 0.011(4) -0.004(4) C53 0.038(5) 0.074(6) 0.029(4) -0.001(4) 0.010(4) -0.014(5) C54 0.034(4) 0.048(5) 0.037(4) 0.016(4) 0.004(4) -0.010(4) C55 0.033(4) 0.037(4) 0.039(5) 0.007(3) 0.000(4) -0.008(3) C56 0.020(4) 0.034(4) 0.035(4) -0.003(3) 0.004(3) -0.005(3) I1 0.0358(3) 0.0451(3) 0.0414(3) 0.0036(2) 0.0022(2) -0.0001(2) I2 0.0496(4) 0.0501(4) 0.0777(5) -0.0070(3) -0.0018(3) 0.0034(3) I3 0.0473(4) 0.0432(3) 0.0495(3) -0.0003(3) 0.0065(3) 0.0044(3) C61 0.103(9) 0.041(5) 0.076(8) -0.012(5) 0.026(7) 0.005(6) Cl1 0.148(4) 0.082(2) 0.096(3) -0.0190(19) 0.054(3) -0.018(2) Cl2 0.125(3) 0.079(2) 0.080(2) -0.0009(17) -0.009(2) 0.018(2) Cl3 0.085(2) 0.087(2) 0.187(4) -0.048(3) 0.055(3) -0.010(2) C62 0.079(9) 0.076(9) 0.121(12) 0.012(8) -0.004(8) 0.020(7) Cl4 0.064(2) 0.114(3) 0.179(4) -0.041(3) 0.017(2) -0.009(2) Cl5 0.226(6) 0.109(3) 0.093(3) -0.007(2) -0.009(3) 0.074(4) Cl6 0.086(3) 0.121(4) 0.334(8) -0.039(5) 0.054(4) -0.042(3) O1 0.083(6) 0.066(5) 0.086(6) -0.001(4) 0.007(5) 0.008(4) O2 0.055(5) 0.108(7) 0.121(7) -0.042(6) 0.005(5) 0.013(5) O3 0.221(16) 0.174(14) 0.173(13) 0.020(11) 0.064(12) 0.053(12) _geom_special_details ; ? ; 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 2.100(6) . ? Sn1 N1 2.101(6) . ? Sn1 C30 2.101(7) . ? Sn1 N4 2.101(6) . ? Sn1 N3 2.122(6) . ? Sn2 N8 2.069(6) . ? Sn2 N7 2.095(5) . ? Sn2 N5 2.097(6) . ? Sn2 N6 2.098(6) . ? Sn2 C30 2.110(7) . ? N1 C2 1.355(10) . ? N1 C26 1.431(10) . ? N2 C4 1.325(10) . ? N2 C11 1.429(10) . ? N3 C7 1.345(9) . ? N3 C16 1.420(9) . ? N4 C9 1.341(9) . ? N4 C21 1.422(10) . ? N5 C32 1.337(9) . ? N5 C56 1.413(9) . ? N6 C34 1.336(9) . ? N6 C41 1.431(9) . ? N7 C37 1.335(9) . ? N7 C46 1.410(9) . ? N8 C39 1.352(9) . ? N8 C51 1.440(9) . ? C1 C2 1.498(12) . ? C2 C3 1.382(12) . ? C3 C4 1.398(12) . ? C4 C5 1.508(11) . ? C6 C7 1.510(10) . ? C7 C8 1.393(11) . ? C8 C9 1.393(11) . ? C9 C10 1.489(10) . ? C11 C12 1.403(11) . ? C11 C16 1.415(10) . ? C12 C13 1.374(12) . ? C13 C14 1.370(12) . ? C14 C15 1.399(11) . ? C15 C16 1.379(11) . ? C21 C22 1.382(11) . ? C21 C26 1.404(11) . ? C22 C23 1.395(12) . ? C23 C24 1.389(14) . ? C24 C25 1.390(13) . ? C25 C26 1.392(11) . ? C31 C32 1.493(11) . ? C32 C33 1.398(11) . ? C33 C34 1.395(11) . ? C34 C35 1.503(10) . ? C36 C37 1.502(10) . ? C37 C38 1.397(10) . ? C38 C39 1.388(11) . ? C39 C40 1.493(10) . ? C41 C42 1.379(10) . ? C41 C46 1.415(10) . ? C42 C43 1.390(12) . ? C43 C44 1.358(12) . ? C44 C45 1.380(11) . ? C45 C46 1.402(10) . ? C51 C52 1.391(10) . ? C51 C56 1.413(10) . ? C52 C53 1.378(12) . ? C53 C54 1.365(12) . ? C54 C55 1.384(11) . ? C55 C56 1.401(10) . ? C61 Cl1 1.723(12) . ? C61 Cl2 1.743(12) . ? C61 Cl3 1.745(13) . ? C62 Cl5 1.710(14) . ? C62 Cl6 1.751(16) . ? C62 Cl4 1.774(14) . ? O2 Li 2.643(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sn1 N1 89.6(2) . . ? N2 Sn1 C30 110.4(3) . . ? N1 Sn1 C30 115.9(3) . . ? N2 Sn1 N4 142.5(2) . . ? N1 Sn1 N4 77.8(2) . . ? C30 Sn1 N4 106.8(3) . . ? N2 Sn1 N3 77.4(2) . . ? N1 Sn1 N3 140.7(2) . . ? C30 Sn1 N3 103.4(3) . . ? N4 Sn1 N3 90.2(2) . . ? N8 Sn2 N7 91.3(2) . . ? N8 Sn2 N5 79.3(2) . . ? N7 Sn2 N5 146.6(2) . . ? N8 Sn2 N6 145.1(2) . . ? N7 Sn2 N6 78.5(2) . . ? N5 Sn2 N6 90.9(2) . . ? N8 Sn2 C30 107.3(3) . . ? N7 Sn2 C30 103.2(2) . . ? N5 Sn2 C30 110.2(3) . . ? N6 Sn2 C30 107.6(3) . . ? C2 N1 C26 126.2(7) . . ? C2 N1 Sn1 125.3(5) . . ? C26 N1 Sn1 107.0(5) . . ? C4 N2 C11 126.4(7) . . ? C4 N2 Sn1 125.7(5) . . ? C11 N2 Sn1 106.5(4) . . ? C7 N3 C16 127.3(6) . . ? C7 N3 Sn1 125.2(5) . . ? C16 N3 Sn1 107.2(4) . . ? C9 N4 C21 126.4(6) . . ? C9 N4 Sn1 125.3(5) . . ? C21 N4 Sn1 107.7(4) . . ? C32 N5 C56 126.2(6) . . ? C32 N5 Sn2 124.0(5) . . ? C56 N5 Sn2 107.5(4) . . ? C34 N6 C41 126.2(6) . . ? C34 N6 Sn2 124.4(5) . . ? C41 N6 Sn2 107.6(4) . . ? C37 N7 C46 127.5(6) . . ? C37 N7 Sn2 124.5(5) . . ? C46 N7 Sn2 107.0(4) . . ? C39 N8 C51 125.5(6) . . ? C39 N8 Sn2 124.9(5) . . ? C51 N8 Sn2 108.4(4) . . ? N1 C2 C3 122.9(8) . . ? N1 C2 C1 120.1(8) . . ? C3 C2 C1 117.0(8) . . ? C2 C3 C4 131.6(8) . . ? N2 C4 C3 123.6(7) . . ? N2 C4 C5 120.5(8) . . ? C3 C4 C5 115.9(7) . . ? N3 C7 C8 123.0(7) . . ? N3 C7 C6 119.5(7) . . ? C8 C7 C6 117.4(7) . . ? C7 C8 C9 131.9(7) . . ? N4 C9 C8 123.8(7) . . ? N4 C9 C10 119.2(7) . . ? C8 C9 C10 117.0(7) . . ? C12 C11 C16 119.8(7) . . ? C12 C11 N2 123.6(7) . . ? C16 C11 N2 116.2(6) . . ? C13 C12 C11 118.9(8) . . ? C14 C13 C12 121.9(8) . . ? C13 C14 C15 119.7(8) . . ? C16 C15 C14 120.3(8) . . ? C15 C16 C11 119.3(7) . . ? C15 C16 N3 125.4(7) . . ? C11 C16 N3 114.7(7) . . ? C22 C21 C26 120.2(8) . . ? C22 C21 N4 124.3(7) . . ? C26 C21 N4 115.2(7) . . ? C21 C22 C23 119.7(9) . . ? C24 C23 C22 119.7(9) . . ? C23 C24 C25 121.1(9) . . ? C24 C25 C26 118.9(9) . . ? C25 C26 C21 120.2(8) . . ? C25 C26 N1 123.4(7) . . ? C21 C26 N1 116.1(7) . . ? Sn1 C30 Sn2 122.5(3) . . ? N5 C32 C33 123.5(7) . . ? N5 C32 C31 120.1(7) . . ? C33 C32 C31 116.3(7) . . ? C34 C33 C32 132.2(7) . . ? N6 C34 C33 122.8(7) . . ? N6 C34 C35 120.4(7) . . ? C33 C34 C35 116.7(7) . . ? N7 C37 C38 122.9(6) . . ? N7 C37 C36 120.7(7) . . ? C38 C37 C36 116.4(7) . . ? C39 C38 C37 132.5(7) . . ? N8 C39 C38 122.7(7) . . ? N8 C39 C40 120.3(7) . . ? C38 C39 C40 116.9(7) . . ? C42 C41 C46 120.0(7) . . ? C42 C41 N6 124.3(7) . . ? C46 C41 N6 115.0(6) . . ? C41 C42 C43 120.1(8) . . ? C44 C43 C42 119.9(8) . . ? C43 C44 C45 121.7(8) . . ? C44 C45 C46 119.6(8) . . ? C45 C46 N7 124.4(7) . . ? C45 C46 C41 118.6(7) . . ? N7 C46 C41 116.7(6) . . ? C52 C51 C56 120.3(7) . . ? C52 C51 N8 124.5(7) . . ? C56 C51 N8 115.0(6) . . ? C53 C52 C51 119.4(8) . . ? C54 C53 C52 121.0(8) . . ? C53 C54 C55 120.6(8) . . ? C54 C55 C56 120.1(8) . . ? C55 C56 N5 124.8(7) . . ? C55 C56 C51 118.3(7) . . ? N5 C56 C51 116.8(6) . . ? Cl1 C61 Cl2 108.8(7) . . ? Cl1 C61 Cl3 110.6(7) . . ? Cl2 C61 Cl3 111.9(6) . . ? Cl5 C62 Cl6 112.6(8) . . ? Cl5 C62 Cl4 111.0(7) . . ? Cl6 C62 Cl4 105.1(8) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.622 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.153 #===END data_zzcam _audit_creation_method SHELXL-97 _chemical_name_systematic ; (5,14-dihydro-6,8,15,17-tetramethyldibenzo[b,i][1,4,8,11]- tetraazacyclotetradecinato)methyltin(IV).dichloroform solvate ; _chemical_name_common ? _chemical_formula_moiety 'C23 H18 N4 Sn, 2(C H Cl3), I' _chemical_formula_sum 'C25 H20 Cl6 I N4 Sn' _chemical_formula_weight 834.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.4459(3) _cell_length_b 10.6470(2) _cell_length_c 28.3609(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3154.23(13) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 7193 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.0 _exptl_crystal_description tablet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 2.319 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4573 _exptl_absorpt_correction_T_max 0.8545 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Seimens SMART CCD' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18687 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3734 _reflns_number_gt 3167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+8.7801P] 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 3734 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn 0.23314(3) 0.2500 0.340922(10) 0.02055(10) Uani 1 d S . . N1 N 0.1576(3) 0.1258(3) 0.39199(9) 0.0248(6) Uani 1 d . . . N2 N 0.1703(3) 0.1256(3) 0.28764(9) 0.0238(6) Uani 1 d . . . C1 C 0.0210(4) -0.0444(4) 0.42337(14) 0.0400(9) Uani 1 d . . . H1A H 0.0799 -0.1040 0.4375 0.048 Uiso 1 calc R . . H1B H -0.0531 -0.0889 0.4113 0.048 Uiso 1 calc R . . H1C H -0.0062 0.0158 0.4470 0.048 Uiso 1 calc R . . C2 C 0.0869(3) 0.0237(3) 0.38346(12) 0.0266(7) Uani 1 d . . . C3 C 0.0638(3) -0.0234(3) 0.33817(12) 0.0276(7) Uani 1 d . . . H3 H 0.0184 -0.0996 0.3375 0.033 Uiso 1 calc R . . C4 C 0.0970(3) 0.0240(3) 0.29364(12) 0.0252(7) Uani 1 d . . . C5 C 0.0400(4) -0.0435(4) 0.25180(13) 0.0354(8) Uani 1 d . . . H5A H 0.0160 0.0173 0.2279 0.042 Uiso 1 calc R . . H5B H -0.0352 -0.0899 0.2617 0.042 Uiso 1 calc R . . H5C H 0.1026 -0.1013 0.2389 0.042 Uiso 1 calc R . . C7 C 0.1792(3) 0.1837(3) 0.43680(11) 0.0249(7) Uani 1 d . . . C8 C 0.2150(4) 0.1188(4) 0.47769(12) 0.0334(8) Uani 1 d . . . H8 H 0.2180 0.0305 0.4777 0.040 Uiso 1 calc R . . C9 C 0.2462(4) 0.1857(4) 0.51834(13) 0.0365(8) Uani 1 d . . . H9 H 0.2675 0.1421 0.5461 0.044 Uiso 1 calc R . . C11 C 0.2030(3) 0.1830(3) 0.24385(11) 0.0242(6) Uani 1 d . . . C12 C 0.2472(3) 0.1171(4) 0.20423(12) 0.0313(8) Uani 1 d . . . C13 C 0.2876(4) 0.1844(4) 0.16433(12) 0.0354(8) Uani 1 d . . . C14 C 0.4359(5) 0.2500 0.3426(2) 0.0402(13) Uani 1 d S . . I I -0.23931(3) -0.2500 0.337877(11) 0.03088(11) Uani 1 d S . . C15 C 0.5837(5) 0.2500 0.6366(2) 0.0427(13) Uani 1 d S . . H15 H 0.4929 0.2500 0.6466 0.051 Uiso 1 calc SR . . Cl1 Cl 0.68107(17) 0.2500 0.68767(6) 0.0564(4) Uani 1 d S . . Cl2 Cl 0.61190(15) 0.11405(13) 0.60274(6) 0.0717(4) Uani 1 d . . . C16 C 0.6463(9) 0.2500 0.4784(3) 0.075(2) Uani 1 d S . . H16 H 0.6237 0.2500 0.5123 0.090 Uiso 1 calc SR . . Cl3 Cl 0.8155(2) 0.2500 0.47476(8) 0.0712(5) Uani 1 d S . . Cl4 Cl 0.58374(16) 0.11426(14) 0.45418(6) 0.0833(5) Uani 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 Sn 0.02027(16) 0.02184(17) 0.01955(16) 0.000 0.00100(11) 0.000 N1 0.0266(14) 0.0265(14) 0.0212(12) 0.0007(11) 0.0019(10) -0.0010(11) N2 0.0262(14) 0.0242(13) 0.0209(12) -0.0023(11) -0.0015(10) -0.0012(11) C1 0.044(2) 0.042(2) 0.0347(19) 0.0069(18) 0.0029(16) -0.0161(18) C2 0.0239(15) 0.0268(17) 0.0292(16) 0.0044(13) 0.0014(13) 0.0008(13) C3 0.0268(17) 0.0221(16) 0.0338(18) -0.0007(13) 0.0012(13) -0.0043(13) C4 0.0240(15) 0.0238(16) 0.0278(16) -0.0058(13) -0.0001(12) 0.0025(13) C5 0.0365(19) 0.037(2) 0.0325(18) -0.0086(16) -0.0009(15) -0.0076(17) C7 0.0247(15) 0.0300(17) 0.0200(14) 0.0001(13) 0.0018(12) -0.0007(14) C8 0.0384(19) 0.0337(19) 0.0280(17) 0.0044(15) 0.0015(15) 0.0007(16) C9 0.039(2) 0.048(2) 0.0222(16) 0.0047(16) 0.0008(14) 0.0015(17) C11 0.0229(15) 0.0305(17) 0.0191(14) 0.0005(12) 0.0002(12) 0.0002(13) C12 0.0292(17) 0.0383(19) 0.0265(16) -0.0044(15) -0.0015(13) 0.0034(15) C13 0.0324(18) 0.050(2) 0.0234(16) -0.0005(15) 0.0009(13) 0.0036(17) C14 0.022(2) 0.054(4) 0.045(3) 0.000 0.000(2) 0.000 I 0.02463(17) 0.03117(19) 0.03683(19) 0.000 -0.00423(12) 0.000 C15 0.029(3) 0.042(3) 0.057(4) 0.000 0.010(3) 0.000 Cl1 0.0509(9) 0.0596(10) 0.0586(9) 0.000 0.0050(8) 0.000 Cl2 0.0717(9) 0.0570(8) 0.0866(10) -0.0236(7) -0.0023(7) 0.0068(7) C16 0.085(6) 0.063(5) 0.077(5) 0.000 -0.015(5) 0.000 Cl3 0.0649(12) 0.0647(11) 0.0839(14) 0.000 -0.0262(11) 0.000 Cl4 0.0918(11) 0.0499(7) 0.1082(12) 0.0181(8) -0.0354(9) -0.0189(7) _geom_special_details ; ? ; 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 Sn N2 2.114(3) . ? Sn N2 2.114(3) 7_565 ? Sn N1 2.114(3) 7_565 ? Sn N1 2.114(3) . ? Sn C14 2.118(5) . ? N1 C2 1.337(4) . ? N1 C7 1.430(4) . ? N2 C4 1.336(4) . ? N2 C11 1.425(4) . ? C1 C2 1.511(5) . ? C2 C3 1.400(5) . ? C3 C4 1.404(5) . ? C4 C5 1.510(5) . ? C7 C8 1.401(5) . ? C7 C7 1.412(7) 7_565 ? C8 C9 1.394(6) . ? C9 C9 1.369(9) 7_565 ? C11 C12 1.403(5) . ? C11 C11 1.428(7) 7_565 ? C12 C13 1.405(5) . ? C13 C13 1.397(9) 7_565 ? C15 Cl2 1.762(4) 7_565 ? C15 Cl2 1.762(4) . ? C15 Cl1 1.770(7) . ? C16 Cl4 1.729(5) . ? C16 Cl4 1.729(5) 7_565 ? C16 Cl3 1.770(10) . ? 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 Sn N2 77.58(15) . 7_565 ? N2 Sn N1 139.98(11) . 7_565 ? N2 Sn N1 88.97(11) 7_565 7_565 ? N2 Sn N1 88.97(11) . . ? N2 Sn N1 139.98(11) 7_565 . ? N1 Sn N1 77.43(15) 7_565 . ? N2 Sn C14 109.07(14) . . ? N2 Sn C14 109.07(14) 7_565 . ? N1 Sn C14 110.95(14) 7_565 . ? N1 Sn C14 110.95(14) . . ? C2 N1 C7 126.8(3) . . ? C2 N1 Sn 126.2(2) . . ? C7 N1 Sn 106.3(2) . . ? C4 N2 C11 126.5(3) . . ? C4 N2 Sn 126.5(2) . . ? C11 N2 Sn 106.3(2) . . ? N1 C2 C3 123.6(3) . . ? N1 C2 C1 120.5(3) . . ? C3 C2 C1 115.9(3) . . ? C2 C3 C4 130.9(3) . . ? N2 C4 C3 123.2(3) . . ? N2 C4 C5 120.8(3) . . ? C3 C4 C5 116.0(3) . . ? C8 C7 C7 119.6(2) . 7_565 ? C8 C7 N1 124.4(3) . . ? C7 C7 N1 115.52(17) 7_565 . ? C9 C8 C7 119.6(4) . . ? C9 C9 C8 120.7(2) 7_565 . ? C12 C11 N2 124.2(3) . . ? C12 C11 C11 120.0(2) . 7_565 ? N2 C11 C11 115.35(17) . 7_565 ? C11 C12 C13 119.3(4) . . ? C13 C13 C12 120.7(2) 7_565 . ? Cl2 C15 Cl2 110.5(3) 7_565 . ? Cl2 C15 Cl1 110.5(2) 7_565 . ? Cl2 C15 Cl1 110.5(2) . . ? Cl4 C16 Cl4 113.4(5) . 7_565 ? Cl4 C16 Cl3 110.7(4) . . ? Cl4 C16 Cl3 110.7(4) 7_565 . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.184 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.106 #===END