# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'M Lappert' 'Peter B Hitchcock' 'Luc J.-M. Pierssens' 'Andrey V Protchenko' 'Patrick G. H. Uiterweerd' _publ_contact_author_name 'Michael F Lappert' _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis and characterisation of twelve crystalline Sn(IV) diaryls and a toluene solution of a Sn(III) triaryl ; _publ_requested_category FM # Attachment 'mfl-nov-2008.cif' data_(2)-jun1399 _database_code_depnum_ccdc_archive 'CCDC 710453' _audit_creation_date 1999-06-28T12:16:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H60 N8 O2 Sn2, 0.5(C4 H10 O)' _chemical_formula_sum 'C42 H65 N8 O2.5 Sn2' _chemical_formula_weight 959.4 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 21.315(4) _cell_length_b 19.714(3) _cell_length_c 21.970(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9232(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3944 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_factor_muR 0.179 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_correction_T_ave 0.8009 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.22408E-1 _diffrn_orient_matrix_ub_12 -0.17649E-1 _diffrn_orient_matrix_ub_13 0.37108E-1 _diffrn_orient_matrix_ub_21 -0.8565E-2 _diffrn_orient_matrix_ub_22 -0.04347 _diffrn_orient_matrix_ub_23 -0.15372E-1 _diffrn_orient_matrix_ub_31 0.44687E-1 _diffrn_orient_matrix_ub_32 0.507E-3 _diffrn_orient_matrix_ub_33 -0.21439E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_standards_decay_corr_max 1.018 _diffrn_standards_decay_corr_min 0.953 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 4 3 7 1 4 _diffrn_reflns_number 5646 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 5646 _reflns_number_gt 4448 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+24.1452P] 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_number_reflns 5646 _refine_ls_number_parameters 503 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.518 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.12 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.22923(2) 0.36400(2) 0.42880(2) 0.02754(18) Uani 1 1 d . . . Sn2 Sn 0.24200(2) 0.31344(2) 0.55834(2) 0.02467(17) Uani 1 1 d . . . O1 O 0.2666(2) 0.3940(2) 0.5080(2) 0.0296(11) Uani 1 1 d . . . O2 O 0.2062(2) 0.2823(2) 0.4781(2) 0.0296(11) Uani 1 1 d . . . O3 O 0.5 0.5 0.5 0.116(4) Uani 1 2 d SD . . N1 N 0.1191(3) 0.5093(3) 0.4574(3) 0.0491(18) Uani 1 1 d . . . N2 N 0.1661(3) 0.3076(3) 0.3403(3) 0.0371(16) Uani 1 1 d . . . N3 N 0.2845(3) 0.4733(3) 0.3888(3) 0.0454(18) Uani 1 1 d . . . N4 N 0.3226(3) 0.2384(3) 0.3443(3) 0.0400(16) Uani 1 1 d . . . N5 N 0.4160(3) 0.3040(4) 0.5819(3) 0.0465(18) Uani 1 1 d . . . N6 N 0.2149(3) 0.1919(3) 0.5916(3) 0.0326(14) Uani 1 1 d . . . N7 N 0.2787(3) 0.3976(3) 0.6436(3) 0.0358(15) Uani 1 1 d . . . N8 N 0.0744(3) 0.2990(4) 0.6080(4) 0.060(2) Uani 1 1 d . . . C1 C 0.1405(3) 0.4064(4) 0.3984(3) 0.0361(19) Uani 1 1 d . . . C2 C 0.1033(4) 0.4638(4) 0.4116(3) 0.041(2) Uani 1 1 d . . . C3 C 0.0490(4) 0.4735(4) 0.3761(3) 0.042(2) Uani 1 1 d . . . H3 H 0.0222 0.5107 0.3847 0.05 Uiso 1 1 calc R . . C4 C 0.0340(4) 0.4304(5) 0.3291(4) 0.048(2) Uani 1 1 d . . . H4 H -0.0023 0.4391 0.3052 0.058 Uiso 1 1 calc R . . C5 C 0.0711(4) 0.3742(5) 0.3159(4) 0.047(2) Uani 1 1 d . . . H5 H 0.0609 0.3443 0.2835 0.056 Uiso 1 1 calc R . . C6 C 0.1231(3) 0.3638(4) 0.3518(3) 0.0357(19) Uani 1 1 d . . . C7 C 0.0790(4) 0.5680(4) 0.4663(4) 0.060(3) Uani 1 1 d . . . H7A H 0.0718 0.5904 0.4271 0.09 Uiso 1 1 calc R . . H7B H 0.0994 0.5998 0.4943 0.09 Uiso 1 1 calc R . . H7C H 0.0388 0.5535 0.4835 0.09 Uiso 1 1 calc R . . C8 C 0.1420(7) 0.4837(6) 0.5153(4) 0.120(6) Uani 1 1 d . . . H8A H 0.1418 0.434 0.5147 0.179 Uiso 1 1 calc R . . H8B H 0.1148 0.4999 0.5482 0.179 Uiso 1 1 calc R . . H8C H 0.1849 0.4999 0.5221 0.179 Uiso 1 1 calc R . . C9 C 0.1401(4) 0.2412(4) 0.3547(4) 0.050(2) Uani 1 1 d . . . H9A H 0.1257 0.2408 0.3971 0.075 Uiso 1 1 calc R . . H9B H 0.1724 0.2065 0.3492 0.075 Uiso 1 1 calc R . . H9C H 0.1047 0.2318 0.3276 0.075 Uiso 1 1 calc R . . C10 C 0.1914(4) 0.3090(4) 0.2782(3) 0.046(2) Uani 1 1 d . . . H10A H 0.1575 0.3007 0.2491 0.07 Uiso 1 1 calc R . . H10B H 0.2235 0.2737 0.2739 0.07 Uiso 1 1 calc R . . H10C H 0.2102 0.3535 0.2702 0.07 Uiso 1 1 calc R . . C11 C 0.3077(3) 0.3582(4) 0.3670(3) 0.0295(17) Uani 1 1 d . . . C12 C 0.3218(4) 0.4245(4) 0.3552(3) 0.039(2) Uani 1 1 d . . . C13 C 0.3665(4) 0.4437(5) 0.3113(4) 0.051(2) Uani 1 1 d . . . H13 H 0.3755 0.49 0.3032 0.062 Uiso 1 1 calc R . . C14 C 0.3964(4) 0.3920(5) 0.2809(4) 0.059(3) Uani 1 1 d . . . H14 H 0.4272 0.403 0.2513 0.07 Uiso 1 1 calc R . . C15 C 0.3832(4) 0.3253(4) 0.2920(3) 0.043(2) Uani 1 1 d . . . H15 H 0.405 0.2912 0.2699 0.052 Uiso 1 1 calc R . . C16 C 0.3388(3) 0.3061(4) 0.3348(3) 0.0348(19) Uani 1 1 d . . . C17 C 0.3216(6) 0.5114(5) 0.4335(4) 0.090(4) Uani 1 1 d . . . H17A H 0.3426 0.4796 0.4611 0.135 Uiso 1 1 calc R . . H17B H 0.2939 0.5413 0.4569 0.135 Uiso 1 1 calc R . . H17C H 0.3532 0.5388 0.4123 0.135 Uiso 1 1 calc R . . C18 C 0.2480(5) 0.5193(5) 0.3491(4) 0.080(3) Uani 1 1 d . . . H18A H 0.2762 0.5523 0.3302 0.12 Uiso 1 1 calc R . . H18B H 0.2164 0.5431 0.3734 0.12 Uiso 1 1 calc R . . H18C H 0.2271 0.4927 0.3173 0.12 Uiso 1 1 calc R . . C19 C 0.3216(5) 0.2129(4) 0.4064(4) 0.057(3) Uani 1 1 d . . . H19A H 0.3638 0.2157 0.4239 0.085 Uiso 1 1 calc R . . H19B H 0.3076 0.1655 0.4063 0.085 Uiso 1 1 calc R . . H19C H 0.2926 0.2402 0.4309 0.085 Uiso 1 1 calc R . . C20 C 0.3481(4) 0.1882(4) 0.3016(4) 0.053(2) Uani 1 1 d . . . H20A H 0.3406 0.2034 0.2598 0.08 Uiso 1 1 calc R . . H20B H 0.3274 0.1444 0.3082 0.08 Uiso 1 1 calc R . . H20C H 0.3933 0.1833 0.3084 0.08 Uiso 1 1 calc R . . C21 C 0.3154(3) 0.2440(3) 0.5850(3) 0.0269(17) Uani 1 1 d . . . C22 C 0.3811(4) 0.2450(4) 0.5926(3) 0.0379(19) Uani 1 1 d . . . C23 C 0.4094(4) 0.1857(4) 0.6152(4) 0.047(2) Uani 1 1 d . . . H23 H 0.4535 0.1849 0.6215 0.057 Uiso 1 1 calc R . . C24 C 0.3744(4) 0.1283(4) 0.6283(4) 0.049(2) Uani 1 1 d . . . H24 H 0.395 0.0887 0.6426 0.058 Uiso 1 1 calc R . . C25 C 0.3113(4) 0.1276(4) 0.6211(3) 0.043(2) Uani 1 1 d . . . H25 H 0.2874 0.0885 0.631 0.052 Uiso 1 1 calc R . . C26 C 0.2828(3) 0.1854(4) 0.5990(3) 0.0285(17) Uani 1 1 d . . . C27 C 0.4087(4) 0.3372(4) 0.5235(4) 0.058(3) Uani 1 1 d . . . H27A H 0.4268 0.3086 0.4915 0.087 Uiso 1 1 calc R . . H27B H 0.4303 0.381 0.5242 0.087 Uiso 1 1 calc R . . H27C H 0.364 0.3443 0.5153 0.087 Uiso 1 1 calc R . . C28 C 0.4816(4) 0.3016(6) 0.6001(5) 0.080(3) Uani 1 1 d . . . H28A H 0.4846 0.2865 0.6425 0.12 Uiso 1 1 calc R . . H28B H 0.5002 0.3468 0.5962 0.12 Uiso 1 1 calc R . . H28C H 0.5043 0.2697 0.5739 0.12 Uiso 1 1 calc R . . C29 C 0.1910(4) 0.1471(4) 0.5436(4) 0.046(2) Uani 1 1 d . . . H29A H 0.194 0.0998 0.5571 0.068 Uiso 1 1 calc R . . H29B H 0.216 0.1533 0.5066 0.068 Uiso 1 1 calc R . . H29C H 0.1471 0.1584 0.5352 0.068 Uiso 1 1 calc R . . C30 C 0.1822(4) 0.1811(4) 0.6494(3) 0.043(2) Uani 1 1 d . . . H30A H 0.1864 0.1335 0.6616 0.064 Uiso 1 1 calc R . . H30B H 0.1377 0.1924 0.6445 0.064 Uiso 1 1 calc R . . H30C H 0.2007 0.2103 0.6808 0.064 Uiso 1 1 calc R . . C31 C 0.1761(4) 0.3561(4) 0.6225(3) 0.0345(19) Uani 1 1 d . . . C32 C 0.2111(4) 0.4030(4) 0.6545(3) 0.0375(19) Uani 1 1 d . . . C33 C 0.1857(5) 0.4489(4) 0.6948(3) 0.052(2) Uani 1 1 d . . . H33 H 0.2114 0.4817 0.7143 0.062 Uiso 1 1 calc R . . C34 C 0.1229(6) 0.4463(5) 0.7061(4) 0.069(3) Uani 1 1 d . . . H34 H 0.1042 0.4779 0.7332 0.083 Uiso 1 1 calc R . . C35 C 0.0868(5) 0.3978(5) 0.6778(4) 0.061(3) Uani 1 1 d . . . H35 H 0.0435 0.3954 0.6878 0.073 Uiso 1 1 calc R . . C36 C 0.1107(4) 0.3510(5) 0.6346(4) 0.047(2) Uani 1 1 d . . . C37 C 0.3092(4) 0.4611(4) 0.6257(4) 0.051(2) Uani 1 1 d . . . H37A H 0.3054 0.4942 0.6588 0.077 Uiso 1 1 calc R . . H37B H 0.2889 0.479 0.589 0.077 Uiso 1 1 calc R . . H37C H 0.3536 0.4526 0.6173 0.077 Uiso 1 1 calc R . . C38 C 0.3106(4) 0.3658(4) 0.6950(3) 0.044(2) Uani 1 1 d . . . H38A H 0.3548 0.3583 0.6847 0.066 Uiso 1 1 calc R . . H38B H 0.2906 0.3222 0.7041 0.066 Uiso 1 1 calc R . . H38C H 0.3078 0.3954 0.7307 0.066 Uiso 1 1 calc R . . C39 C 0.0704(4) 0.2965(6) 0.5430(5) 0.077(3) Uani 1 1 d . . . H39A H 0.0408 0.331 0.5287 0.115 Uiso 1 1 calc R . . H39B H 0.0559 0.2515 0.5303 0.115 Uiso 1 1 calc R . . H39C H 0.1119 0.3052 0.5254 0.115 Uiso 1 1 calc R . . C40 C 0.0137(4) 0.2852(6) 0.6363(5) 0.093(4) Uani 1 1 d . . . H40A H 0.018 0.2871 0.6807 0.139 Uiso 1 1 calc R . . H40B H -0.0008 0.2399 0.6243 0.139 Uiso 1 1 calc R . . H40C H -0.0169 0.3192 0.623 0.139 Uiso 1 1 calc R . . C41 C 0.4907(13) 0.4896(14) 0.4326(9) 0.125(10) Uiso 0.5 1 d PD A 1 H41A H 0.4459 0.4787 0.4256 0.15 Uiso 0.5 1 calc PR A 1 H41B H 0.4992 0.5332 0.4119 0.15 Uiso 0.5 1 calc PR A 1 C42 C 0.5266(7) 0.4397(8) 0.4042(7) 0.137(6) Uiso 0.5 1 d PD A 1 H42A H 0.5156 0.4375 0.361 0.205 Uiso 0.5 1 calc PR A 1 H42B H 0.5182 0.3957 0.4234 0.205 Uiso 0.5 1 calc PR A 1 H42C H 0.5712 0.4508 0.4085 0.205 Uiso 0.5 1 calc PR A 1 C41A C 0.5403(11) 0.4532(12) 0.4663(10) 0.101(8) Uiso 0.5 1 d PD A 2 H41C H 0.5401 0.4093 0.4882 0.122 Uiso 0.5 1 calc PR A 2 H41D H 0.5837 0.471 0.4683 0.122 Uiso 0.5 1 calc PR A 2 C42A C 0.5266(7) 0.4397(8) 0.4042(7) 0.137(6) Uiso 0.5 1 d P A 2 H42D H 0.5579 0.4084 0.3877 0.205 Uiso 0.5 1 calc PR A 2 H42E H 0.5274 0.4822 0.3812 0.205 Uiso 0.5 1 calc PR A 2 H42F H 0.4848 0.4191 0.4011 0.205 Uiso 0.5 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0322(3) 0.0317(3) 0.0187(3) -0.0001(2) -0.0019(2) 0.0061(2) Sn2 0.0260(3) 0.0278(3) 0.0202(3) 0.0010(2) -0.0004(2) 0.0055(2) O1 0.035(3) 0.031(3) 0.023(3) 0.003(2) -0.005(2) 0.000(2) O2 0.031(3) 0.033(3) 0.025(3) 0.001(2) -0.002(2) 0.002(2) O3 0.087(8) 0.115(10) 0.146(12) 0.016(9) -0.014(8) -0.013(8) N1 0.056(4) 0.056(5) 0.036(4) -0.002(4) -0.002(3) 0.023(4) N2 0.043(4) 0.047(4) 0.021(3) -0.002(3) -0.002(3) -0.001(3) N3 0.084(5) 0.032(4) 0.020(3) 0.001(3) 0.002(3) 0.007(4) N4 0.044(4) 0.036(4) 0.040(4) -0.012(3) -0.001(3) 0.007(3) N5 0.023(4) 0.066(5) 0.051(4) 0.004(4) -0.003(3) 0.005(3) N6 0.039(4) 0.028(3) 0.031(3) 0.000(3) -0.002(3) -0.003(3) N7 0.059(4) 0.027(3) 0.022(3) -0.001(3) -0.006(3) 0.002(3) N8 0.025(4) 0.083(6) 0.072(6) 0.014(5) 0.006(4) 0.004(4) C1 0.040(5) 0.048(5) 0.020(4) 0.005(4) 0.001(3) 0.015(4) C2 0.044(5) 0.054(5) 0.025(4) 0.002(4) 0.003(4) 0.012(4) C3 0.036(5) 0.054(5) 0.034(5) 0.016(4) 0.002(4) 0.016(4) C4 0.029(5) 0.079(7) 0.036(5) 0.014(5) -0.004(4) 0.004(5) C5 0.035(5) 0.074(6) 0.032(5) 0.004(4) 0.000(4) -0.002(5) C6 0.031(4) 0.050(5) 0.027(4) 0.009(4) -0.002(3) 0.012(4) C7 0.073(7) 0.045(5) 0.062(6) 0.001(5) -0.001(5) 0.025(5) C8 0.192(14) 0.107(10) 0.060(7) -0.048(7) -0.066(8) 0.108(10) C9 0.053(6) 0.047(5) 0.050(5) -0.004(4) -0.002(4) -0.001(4) C10 0.046(5) 0.064(6) 0.030(4) -0.013(4) 0.000(4) 0.004(4) C11 0.030(4) 0.036(5) 0.023(4) 0.002(3) -0.006(3) -0.001(4) C12 0.052(5) 0.043(5) 0.022(4) 0.004(4) -0.009(4) -0.012(4) C13 0.057(6) 0.058(6) 0.039(5) 0.003(4) 0.000(4) -0.018(5) C14 0.043(5) 0.092(8) 0.041(5) 0.004(5) 0.013(4) -0.017(5) C15 0.036(5) 0.062(6) 0.032(5) -0.016(4) 0.003(4) -0.005(4) C16 0.028(4) 0.049(5) 0.027(4) -0.011(4) -0.008(3) 0.004(4) C17 0.179(13) 0.043(6) 0.048(6) -0.015(5) 0.013(7) -0.040(7) C18 0.126(9) 0.063(7) 0.052(6) 0.027(5) 0.026(6) 0.033(7) C19 0.073(7) 0.043(5) 0.054(6) -0.001(4) 0.020(5) 0.011(5) C20 0.062(6) 0.055(6) 0.043(5) -0.021(4) 0.000(4) 0.018(5) C21 0.028(4) 0.027(4) 0.026(4) -0.004(3) 0.002(3) 0.010(3) C22 0.037(5) 0.045(5) 0.033(4) -0.004(4) 0.000(4) 0.009(4) C23 0.037(5) 0.064(6) 0.040(5) -0.004(4) -0.007(4) 0.025(5) C24 0.060(6) 0.038(5) 0.047(5) 0.011(4) 0.001(4) 0.019(5) C25 0.052(6) 0.037(5) 0.040(5) 0.005(4) 0.007(4) 0.006(4) C26 0.036(4) 0.030(4) 0.019(4) -0.002(3) 0.002(3) 0.008(4) C27 0.038(5) 0.058(6) 0.079(7) 0.018(5) 0.004(5) -0.003(4) C28 0.034(6) 0.114(9) 0.093(8) 0.012(7) -0.007(5) -0.019(6) C29 0.068(6) 0.026(4) 0.042(5) -0.004(4) -0.006(4) -0.010(4) C30 0.044(5) 0.045(5) 0.039(5) 0.013(4) 0.007(4) 0.000(4) C31 0.040(5) 0.036(5) 0.028(4) 0.006(4) 0.006(4) 0.015(4) C32 0.054(5) 0.036(5) 0.023(4) 0.007(4) 0.002(4) 0.016(4) C33 0.092(8) 0.036(5) 0.027(4) -0.001(4) 0.001(5) 0.024(5) C34 0.104(9) 0.068(7) 0.034(6) 0.017(5) 0.023(6) 0.060(7) C35 0.059(6) 0.076(7) 0.047(6) 0.028(5) 0.024(5) 0.046(6) C36 0.037(5) 0.067(6) 0.038(5) 0.022(4) 0.010(4) 0.033(5) C37 0.077(6) 0.033(5) 0.043(5) -0.001(4) -0.005(5) -0.013(5) C38 0.063(6) 0.047(5) 0.024(4) 0.005(4) -0.011(4) 0.007(4) C39 0.033(5) 0.115(9) 0.082(8) -0.029(7) 0.004(5) 0.004(6) C40 0.031(5) 0.136(11) 0.112(10) 0.048(8) 0.019(6) 0.014(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 2.003(4) . ? Sn1 O1 2.003(4) . ? Sn1 C11 2.158(7) . ? Sn1 C1 2.173(7) . ? Sn1 N3 2.609(6) . ? Sn1 N2 2.612(6) . ? Sn2 O1 2.005(4) . ? Sn2 O2 2.016(4) . ? Sn2 C21 2.161(7) . ? Sn2 C31 2.159(7) . ? Sn2 N6 2.571(6) . ? Sn2 N7 2.622(6) . ? O3 C41A 1.46(2) 5_666 ? O3 C41A 1.46(2) . ? O3 C41 1.51(2) 5_666 ? O3 C41 1.51(2) . ? N1 C2 1.389(10) . ? N1 C7 1.451(10) . ? N1 C8 1.454(11) . ? N2 C9 1.456(10) . ? N2 C6 1.459(9) . ? N2 C10 1.468(9) . ? N3 C12 1.450(10) . ? N3 C17 1.468(11) . ? N3 C18 1.478(11) . ? N4 C16 1.394(10) . ? N4 C19 1.455(10) . ? N4 C20 1.467(9) . ? N5 C22 1.401(10) . ? N5 C27 1.449(11) . ? N5 C28 1.455(10) . ? N6 C30 1.464(9) . ? N6 C26 1.462(9) . ? N6 C29 1.466(9) . ? N7 C38 1.460(9) . ? N7 C37 1.464(9) . ? N7 C32 1.465(10) . ? N8 C36 1.411(12) . ? N8 C39 1.432(12) . ? N8 C40 1.462(11) . ? C1 C6 1.375(10) . ? C1 C2 1.412(10) . ? C2 C3 1.410(10) . ? C3 C4 1.375(11) . ? C4 C5 1.391(11) . ? C5 C6 1.377(10) . ? C11 C12 1.366(10) . ? C11 C16 1.412(10) . ? C12 C13 1.407(11) . ? C13 C14 1.376(12) . ? C14 C15 1.368(12) . ? C15 C16 1.386(11) . ? C21 C26 1.383(10) . ? C21 C22 1.410(10) . ? C22 C23 1.407(10) . ? C23 C24 1.386(11) . ? C24 C25 1.353(11) . ? C25 C26 1.380(10) . ? C31 C32 1.381(11) . ? C31 C36 1.423(11) . ? C32 C33 1.377(11) . ? C33 C34 1.362(14) . ? C34 C35 1.376(14) . ? C35 C36 1.418(12) . ? C41 C42 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sn1 O1 82.24(18) . . ? O2 Sn1 C11 119.2(2) . . ? O1 Sn1 C11 104.8(2) . . ? O2 Sn1 C1 105.2(2) . . ? O1 Sn1 C1 120.0(2) . . ? C11 Sn1 C1 120.1(3) . . ? O2 Sn1 N3 163.28(19) . . ? O1 Sn1 N3 82.50(18) . . ? C11 Sn1 N3 58.8(2) . . ? C1 Sn1 N3 88.4(3) . . ? O2 Sn1 N2 86.22(19) . . ? O1 Sn1 N2 167.65(18) . . ? C11 Sn1 N2 84.7(2) . . ? C1 Sn1 N2 59.1(2) . . ? N3 Sn1 N2 109.46(19) . . ? O1 Sn2 O2 81.87(18) . . ? O1 Sn2 C21 117.5(2) . . ? O2 Sn2 C21 108.5(2) . . ? O1 Sn2 C31 102.8(2) . . ? O2 Sn2 C31 116.3(2) . . ? C21 Sn2 C31 122.8(3) . . ? O1 Sn2 N6 162.54(18) . . ? O2 Sn2 N6 83.08(18) . . ? C21 Sn2 N6 59.6(2) . . ? C31 Sn2 N6 91.8(2) . . ? O1 Sn2 N7 79.30(18) . . ? O2 Sn2 N7 158.48(18) . . ? C21 Sn2 N7 89.5(2) . . ? C31 Sn2 N7 58.8(3) . . ? N6 Sn2 N7 116.98(18) . . ? Sn1 O1 Sn2 98.11(19) . . ? Sn1 O2 Sn2 97.75(19) . . ? C41A O3 C41A 179.997(6) 5_666 . ? C41A O3 C41 59.7(15) 5_666 5_666 ? C41A O3 C41 120.3(15) . 5_666 ? C41A O3 C41 120.3(15) 5_666 . ? C41A O3 C41 59.7(15) . . ? C41 O3 C41 179.998(6) 5_666 . ? C2 N1 C7 118.1(7) . . ? C2 N1 C8 119.3(7) . . ? C7 N1 C8 110.9(7) . . ? C9 N2 C6 113.9(6) . . ? C9 N2 C10 111.0(6) . . ? C6 N2 C10 112.2(6) . . ? C9 N2 Sn1 114.6(5) . . ? C6 N2 Sn1 82.6(4) . . ? C10 N2 Sn1 119.7(5) . . ? C12 N3 C17 112.6(8) . . ? C12 N3 C18 113.3(6) . . ? C17 N3 C18 111.4(7) . . ? C12 N3 Sn1 82.5(4) . . ? C17 N3 Sn1 116.1(5) . . ? C18 N3 Sn1 117.9(6) . . ? C16 N4 C19 118.4(6) . . ? C16 N4 C20 117.3(7) . . ? C19 N4 C20 111.8(6) . . ? C22 N5 C27 117.7(7) . . ? C22 N5 C28 115.9(7) . . ? C27 N5 C28 111.3(7) . . ? C30 N6 C26 111.2(6) . . ? C30 N6 C29 111.8(6) . . ? C26 N6 C29 111.8(6) . . ? C30 N6 Sn2 119.2(4) . . ? C26 N6 Sn2 83.7(4) . . ? C29 N6 Sn2 115.7(4) . . ? C38 N7 C37 111.7(6) . . ? C38 N7 C32 111.2(6) . . ? C37 N7 C32 114.7(6) . . ? C38 N7 Sn2 114.8(4) . . ? C37 N7 Sn2 118.8(4) . . ? C32 N7 Sn2 82.5(4) . . ? C36 N8 C39 118.1(8) . . ? C36 N8 C40 116.5(9) . . ? C39 N8 C40 111.5(8) . . ? C6 C1 C2 119.5(7) . . ? C6 C1 Sn1 103.2(5) . . ? C2 C1 Sn1 137.2(6) . . ? N1 C2 C3 120.8(7) . . ? N1 C2 C1 122.1(7) . . ? C3 C2 C1 117.1(7) . . ? C4 C3 C2 121.6(8) . . ? C3 C4 C5 121.1(7) . . ? C6 C5 C4 117.3(8) . . ? C1 C6 C5 123.5(8) . . ? C1 C6 N2 115.0(6) . . ? C5 C6 N2 121.4(7) . . ? C1 C6 Sn1 48.5(4) . . ? C5 C6 Sn1 171.2(6) . . ? N2 C6 Sn1 66.5(3) . . ? C12 C11 C16 119.9(7) . . ? C12 C11 Sn1 103.8(5) . . ? C16 C11 Sn1 135.8(5) . . ? C11 C12 C13 122.4(8) . . ? C11 C12 N3 114.8(7) . . ? C13 C12 N3 122.8(7) . . ? C11 C12 Sn1 48.1(4) . . ? C13 C12 Sn1 169.0(6) . . ? N3 C12 Sn1 66.7(4) . . ? C14 C13 C12 116.6(8) . . ? C15 C14 C13 122.0(8) . . ? C14 C15 C16 121.6(8) . . ? C15 C16 N4 122.1(7) . . ? C15 C16 C11 117.5(7) . . ? N4 C16 C11 120.4(7) . . ? C26 C21 C22 119.0(6) . . ? C26 C21 Sn2 103.0(5) . . ? C22 C21 Sn2 137.9(6) . . ? N5 C22 C23 121.5(7) . . ? N5 C22 C21 121.3(7) . . ? C23 C22 C21 117.0(7) . . ? C24 C23 C22 121.5(8) . . ? C25 C24 C23 121.2(8) . . ? C24 C25 C26 118.1(8) . . ? C25 C26 C21 123.1(7) . . ? C25 C26 N6 123.2(7) . . ? C21 C26 N6 113.6(6) . . ? C25 C26 Sn2 171.2(6) . . ? C21 C26 Sn2 48.4(3) . . ? N6 C26 Sn2 65.2(3) . . ? C32 C31 C36 118.7(7) . . ? C32 C31 Sn2 104.0(5) . . ? C36 C31 Sn2 137.0(6) . . ? C33 C32 C31 123.8(8) . . ? C33 C32 N7 122.7(8) . . ? C31 C32 N7 113.5(6) . . ? C33 C32 Sn2 168.8(6) . . ? C31 C32 Sn2 47.7(4) . . ? N7 C32 Sn2 66.6(3) . . ? C34 C33 C32 118.6(9) . . ? C33 C34 C35 119.5(9) . . ? C34 C35 C36 123.6(9) . . ? N8 C36 C35 123.5(8) . . ? N8 C36 C31 120.8(7) . . ? C35 C36 C31 115.6(9) . . ? C42 C41 O3 117.5(17) . . ? #===END data_(5)-sep1999 _database_code_depnum_ccdc_archive 'CCDC 710454' _audit_creation_date 1999-09-21T08:32:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H60 N8 Sn2 Te2' _chemical_formula_sum 'C40 H60 N8 Sn2 Te2' _chemical_formula_weight 1145.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2557(2) _cell_length_b 18.2574(5) _cell_length_c 9.6048(2) _cell_angle_alpha 90 _cell_angle_beta 108.154(1) _cell_angle_gamma 90 _cell_volume 2208.79(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18869 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.777 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 21504 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 6385 _reflns_number_gt 5825 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+4.8777P] 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_number_reflns 6385 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.89 _refine_ls_restrained_S_all 0.89 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.975 _refine_diff_density_min -1.322 _refine_diff_density_rms 0.269 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te Te 0.050235(13) -0.019966(10) -0.172184(18) 0.02136(6) Uani 1 1 d . . . Sn Sn 0.143178(13) -0.010002(9) 0.129098(18) 0.01658(6) Uani 1 1 d . . . N1 N 0.32772(16) -0.05546(12) 0.0747(2) 0.0202(4) Uani 1 1 d . . . N2 N 0.09663(19) -0.18060(14) 0.3075(3) 0.0291(5) Uani 1 1 d . . . N3 N 0.2397(2) 0.14109(15) -0.0034(3) 0.0311(5) Uani 1 1 d . . . N4 N 0.2512(2) 0.01932(15) 0.4481(3) 0.0285(5) Uani 1 1 d . . . C1 C 0.21671(19) -0.11620(14) 0.1961(3) 0.0196(4) Uani 1 1 d . . . C2 C 0.3043(2) -0.12077(15) 0.1452(3) 0.0219(5) Uani 1 1 d . . . C3 C 0.3657(3) -0.18364(18) 0.1585(4) 0.0349(7) Uani 1 1 d . . . H3 H 0.4255 -0.1848 0.1241 0.042 Uiso 1 1 calc R . . C4 C 0.3371(3) -0.24448(19) 0.2233(4) 0.0422(8) Uani 1 1 d . . . H4 H 0.3772 -0.2883 0.2322 0.051 Uiso 1 1 calc R . . C5 C 0.2508(3) -0.24232(18) 0.2754(4) 0.0358(7) Uani 1 1 d . . . H5 H 0.2335 -0.2846 0.3211 0.043 Uiso 1 1 calc R . . C6 C 0.1882(2) -0.17902(15) 0.2623(3) 0.0242(5) Uani 1 1 d . . . C7 C 0.4301(2) -0.02320(18) 0.1588(4) 0.0296(6) Uani 1 1 d . . . H7A H 0.4435 0.0205 0.1082 0.044 Uiso 1 1 calc R . . H7B H 0.4869 -0.059 0.1677 0.044 Uiso 1 1 calc R . . H7C H 0.4282 -0.0096 0.2567 0.044 Uiso 1 1 calc R . . C8 C 0.3262(2) -0.06778(18) -0.0768(3) 0.0286(6) Uani 1 1 d . . . H8A H 0.3429 -0.0219 -0.1179 0.043 Uiso 1 1 calc R . . H8B H 0.2556 -0.0847 -0.1354 0.043 Uiso 1 1 calc R . . H8C H 0.3792 -0.105 -0.0784 0.043 Uiso 1 1 calc R . . C9 C 0.0909(3) -0.12843(19) 0.4192(4) 0.0345(7) Uani 1 1 d . . . H9A H 0.0237 -0.1349 0.4403 0.052 Uiso 1 1 calc R . . H9B H 0.0948 -0.0785 0.3838 0.052 Uiso 1 1 calc R . . H9C H 0.1503 -0.1367 0.5087 0.052 Uiso 1 1 calc R . . C10 C 0.0588(3) -0.2529(2) 0.3345(5) 0.0442(8) Uani 1 1 d . . . H10A H -0.0051 -0.2473 0.3643 0.066 Uiso 1 1 calc R . . H10B H 0.1141 -0.2775 0.4125 0.066 Uiso 1 1 calc R . . H10C H 0.0419 -0.2822 0.2447 0.066 Uiso 1 1 calc R . . C11 C 0.2517(2) 0.07881(14) 0.2238(3) 0.0209(5) Uani 1 1 d . . . C12 C 0.2919(2) 0.13111(15) 0.1473(3) 0.0239(5) Uani 1 1 d . . . C13 C 0.3850(2) 0.16974(17) 0.2226(4) 0.0307(6) Uani 1 1 d . . . H13 H 0.4143 0.204 0.1715 0.037 Uiso 1 1 calc R . . C14 C 0.4339(2) 0.15804(17) 0.3709(4) 0.0341(7) Uani 1 1 d . . . H14 H 0.4979 0.1832 0.4196 0.041 Uiso 1 1 calc R . . C15 C 0.3912(2) 0.11035(18) 0.4491(4) 0.0321(6) Uani 1 1 d . . . H15 H 0.4233 0.1043 0.5517 0.038 Uiso 1 1 calc R . . C16 C 0.2994(2) 0.07106(16) 0.3741(3) 0.0235(5) Uani 1 1 d . . . C17 C 0.1320(3) 0.17021(19) -0.0349(4) 0.0422(8) Uani 1 1 d . . . H17A H 0.0999 0.176 -0.141 0.063 Uiso 1 1 calc R . . H17B H 0.1348 0.2179 0.013 0.063 Uiso 1 1 calc R . . H17C H 0.0891 0.1362 0.0022 0.063 Uiso 1 1 calc R . . C18 C 0.2971(4) 0.1799(3) -0.0865(4) 0.0557(11) Uani 1 1 d . . . H18A H 0.2528 0.1835 -0.1891 0.084 Uiso 1 1 calc R . . H18B H 0.3625 0.1533 -0.0806 0.084 Uiso 1 1 calc R . . H18C H 0.3149 0.2292 -0.0459 0.084 Uiso 1 1 calc R . . C19 C 0.3275(3) -0.0319(3) 0.5440(4) 0.0476(9) Uani 1 1 d . . . H19A H 0.2899 -0.0653 0.5905 0.071 Uiso 1 1 calc R . . H19B H 0.3807 -0.0042 0.6197 0.071 Uiso 1 1 calc R . . H19C H 0.3628 -0.0601 0.4857 0.071 Uiso 1 1 calc R . . C20 C 0.1879(3) 0.0578(3) 0.5258(4) 0.0501(10) Uani 1 1 d . . . H20A H 0.156 0.0221 0.5758 0.075 Uiso 1 1 calc R . . H20B H 0.1317 0.0859 0.4555 0.075 Uiso 1 1 calc R . . H20C H 0.2337 0.0913 0.5981 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te 0.01804(9) 0.03003(10) 0.01761(9) 0.00082(6) 0.00789(7) 0.00273(6) Sn 0.01549(9) 0.01726(9) 0.01759(9) 0.00109(5) 0.00602(7) -0.00030(5) N1 0.0175(9) 0.0248(10) 0.0195(10) -0.0019(8) 0.0076(8) -0.0014(8) N2 0.0273(11) 0.0287(12) 0.0336(13) 0.0105(10) 0.0128(10) -0.0005(9) N3 0.0397(13) 0.0292(12) 0.0264(12) 0.0000(10) 0.0132(11) -0.0096(10) N4 0.0275(12) 0.0396(14) 0.0197(11) -0.0001(9) 0.0091(9) -0.0036(10) C1 0.0177(10) 0.0217(11) 0.0177(11) 0.0016(9) 0.0033(9) 0.0016(9) C2 0.0201(11) 0.0233(12) 0.0222(12) -0.0004(9) 0.0065(9) 0.0013(9) C3 0.0317(14) 0.0322(15) 0.0458(18) 0.0058(13) 0.0194(14) 0.0109(12) C4 0.0446(18) 0.0279(15) 0.060(2) 0.0127(15) 0.0243(17) 0.0171(13) C5 0.0420(17) 0.0262(14) 0.0426(17) 0.0138(13) 0.0181(14) 0.0094(12) C6 0.0231(12) 0.0242(12) 0.0232(12) 0.0061(10) 0.0040(10) 0.0029(10) C7 0.0184(11) 0.0359(15) 0.0349(15) -0.0090(12) 0.0086(11) -0.0026(10) C8 0.0278(13) 0.0355(15) 0.0262(13) -0.0023(11) 0.0137(11) 0.0001(11) C9 0.0347(15) 0.0415(17) 0.0324(15) 0.0100(13) 0.0177(13) 0.0036(13) C10 0.0413(18) 0.0361(18) 0.058(2) 0.0189(16) 0.0195(17) -0.0054(14) C11 0.0196(11) 0.0218(11) 0.0236(12) -0.0032(9) 0.0101(9) -0.0016(9) C12 0.0237(12) 0.0217(12) 0.0284(13) -0.0036(10) 0.0112(10) -0.0027(9) C13 0.0267(13) 0.0244(13) 0.0437(17) -0.0044(12) 0.0148(12) -0.0062(11) C14 0.0235(12) 0.0292(14) 0.0471(18) -0.0108(13) 0.0072(12) -0.0060(11) C15 0.0248(13) 0.0358(16) 0.0307(15) -0.0093(12) 0.0014(11) -0.0038(11) C16 0.0213(11) 0.0271(13) 0.0220(12) -0.0045(10) 0.0067(9) -0.0016(10) C17 0.0472(19) 0.0285(15) 0.0421(18) 0.0094(14) 0.0009(15) -0.0020(14) C18 0.076(3) 0.061(3) 0.0366(19) 0.0021(17) 0.026(2) -0.027(2) C19 0.0373(18) 0.061(2) 0.0359(18) 0.0176(17) -0.0008(15) -0.0077(17) C20 0.058(2) 0.064(3) 0.0417(19) -0.0221(18) 0.0344(18) -0.0163(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Te Sn 2.7755(2) . ? Te Sn 2.7758(2) 3 ? Sn C11 2.171(3) . ? Sn C1 2.175(3) . ? Sn Te 2.7758(2) 3 ? N1 C2 1.452(3) . ? N1 C8 1.467(3) . ? N1 C7 1.469(3) . ? N2 C6 1.411(4) . ? N2 C9 1.454(4) . ? N2 C10 1.463(4) . ? N3 C12 1.408(4) . ? N3 C18 1.448(4) . ? N3 C17 1.464(5) . ? N4 C16 1.445(4) . ? N4 C20 1.464(4) . ? N4 C19 1.471(5) . ? C1 C2 1.395(3) . ? C1 C6 1.419(4) . ? C2 C3 1.390(4) . ? C3 C4 1.382(5) . ? C4 C5 1.385(5) . ? C5 C6 1.406(4) . ? C11 C16 1.391(4) . ? C11 C12 1.407(4) . ? C12 C13 1.409(4) . ? C13 C14 1.385(5) . ? C14 C15 1.382(5) . ? C15 C16 1.403(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sn Te Sn 87.835(7) . 3 ? C11 Sn C1 111.37(9) . . ? C11 Sn Te 120.44(7) . . ? C1 Sn Te 105.22(7) . . ? C11 Sn Te 108.24(6) . 3 ? C1 Sn Te 118.76(6) . 3 ? Te Sn Te 92.165(7) . 3 ? C2 N1 C8 113.5(2) . . ? C2 N1 C7 111.6(2) . . ? C8 N1 C7 109.4(2) . . ? C6 N2 C9 117.5(2) . . ? C6 N2 C10 116.6(3) . . ? C9 N2 C10 111.1(3) . . ? C12 N3 C18 117.1(3) . . ? C12 N3 C17 113.3(3) . . ? C18 N3 C17 110.7(3) . . ? C16 N4 C20 110.3(3) . . ? C16 N4 C19 113.6(2) . . ? C20 N4 C19 112.2(3) . . ? C2 C1 C6 118.4(2) . . ? C2 C1 Sn 107.13(18) . . ? C6 C1 Sn 134.08(19) . . ? C3 C2 C1 123.0(3) . . ? C3 C2 N1 121.1(2) . . ? C1 C2 N1 115.9(2) . . ? C4 C3 C2 118.1(3) . . ? C3 C4 C5 120.9(3) . . ? C4 C5 C6 121.5(3) . . ? C5 C6 N2 119.7(3) . . ? C5 C6 C1 118.2(3) . . ? N2 C6 C1 122.0(2) . . ? C16 C11 C12 119.2(2) . . ? C16 C11 Sn 112.71(19) . . ? C12 C11 Sn 126.71(19) . . ? C11 C12 N3 118.6(2) . . ? C11 C12 C13 119.0(3) . . ? N3 C12 C13 122.3(3) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 121.1(3) . . ? C14 C15 C16 118.7(3) . . ? C11 C16 C15 121.5(3) . . ? C11 C16 N4 116.7(2) . . ? C15 C16 N4 121.8(3) . . ? #===END data_(6)-feb601 _database_code_depnum_ccdc_archive 'CCDC 710455' _audit_creation_date 2001-02-05T13:50:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H44 N4 S2 Sn1' _chemical_formula_sum 'C34 H44 N4 S2 Sn' _chemical_formula_weight 691.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.3987(3) _cell_length_b 18.6282(7) _cell_length_c 19.6314(8) _cell_angle_alpha 90 _cell_angle_beta 94.126(2) _cell_angle_gamma 90 _cell_volume 3428.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8534 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7995 _exptl_absorpt_correction_T_max 0.8177 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 11724 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_unetI/netI 0.053 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5438 _reflns_number_gt 4996 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+3.7036P] 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_number_reflns 5438 _refine_ls_number_parameters 370 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.065 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(19) _refine_diff_density_max 0.322 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn 0.495153(19) 0.528632(12) 0.166164(16) 0.02930(8) Uani 1 1 d . . . S1 S 0.50966(14) 0.65426(6) 0.13396(6) 0.0423(3) Uani 1 1 d . . . S2 S 0.30448(12) 0.49340(7) 0.08297(7) 0.0453(3) Uani 1 1 d . . . N1 N 0.3798(5) 0.6516(3) 0.2821(3) 0.0434(13) Uani 1 1 d . . . N2 N 0.4273(4) 0.3978(2) 0.2365(2) 0.0396(10) Uani 1 1 d . . . N3 N 0.7780(4) 0.5459(2) 0.2409(2) 0.0406(11) Uani 1 1 d . . . N4 N 0.5742(4) 0.3939(2) 0.0607(2) 0.0423(12) Uani 1 1 d . . . C1 C 0.4015(4) 0.5229(2) 0.2623(2) 0.0303(10) Uani 1 1 d . . . C2 C 0.3494(4) 0.5796(2) 0.3008(2) 0.0330(10) Uani 1 1 d . . . C3 C 0.2672(5) 0.5634(3) 0.3550(2) 0.0445(12) Uani 1 1 d . . . H3 H 0.2316 0.6012 0.3815 0.053 Uiso 1 1 calc R . . C4 C 0.2368(5) 0.4929(3) 0.3706(3) 0.0514(13) Uani 1 1 d . . . H4 H 0.1791 0.4828 0.4072 0.062 Uiso 1 1 calc R . . C5 C 0.2891(5) 0.4367(3) 0.3335(2) 0.0421(11) Uani 1 1 d . . . H5 H 0.2693 0.3884 0.3449 0.05 Uiso 1 1 calc R . . C6 C 0.3711(4) 0.4524(2) 0.2796(2) 0.0340(10) Uani 1 1 d . . . C7 C 0.5233(6) 0.6743(3) 0.3043(3) 0.0546(13) Uani 1 1 d . . . H7A H 0.5375 0.7241 0.2902 0.082 Uiso 1 1 calc R . . H7B H 0.5924 0.6433 0.2836 0.082 Uiso 1 1 calc R . . H7C H 0.5369 0.6709 0.3542 0.082 Uiso 1 1 calc R . . C8 C 0.2785(6) 0.7050(3) 0.2991(4) 0.087(2) Uani 1 1 d . . . H8A H 0.3106 0.7523 0.2846 0.13 Uiso 1 1 calc R . . H8B H 0.2703 0.7052 0.3486 0.13 Uiso 1 1 calc R . . H8C H 0.1854 0.6941 0.2757 0.13 Uiso 1 1 calc R . . C9 C 0.3178(6) 0.3482(3) 0.2067(3) 0.0664(17) Uani 1 1 d . . . H9A H 0.3626 0.3126 0.1784 0.1 Uiso 1 1 calc R . . H9B H 0.2462 0.3753 0.1785 0.1 Uiso 1 1 calc R . . H9C H 0.2717 0.3238 0.2435 0.1 Uiso 1 1 calc R . . C10 C 0.5466(6) 0.3580(3) 0.2714(3) 0.0645(16) Uani 1 1 d . . . H10A H 0.5815 0.3219 0.2404 0.097 Uiso 1 1 calc R . . H10B H 0.5139 0.3342 0.312 0.097 Uiso 1 1 calc R . . H10C H 0.6239 0.3915 0.2852 0.097 Uiso 1 1 calc R . . C11 C 0.6835(4) 0.4680(2) 0.1522(2) 0.0305(9) Uani 1 1 d . . . C12 C 0.7942(4) 0.4824(2) 0.2002(2) 0.0350(10) Uani 1 1 d . . . C13 C 0.9106(4) 0.4360(3) 0.2098(3) 0.0462(12) Uani 1 1 d . . . H13 H 0.987 0.4464 0.2426 0.055 Uiso 1 1 calc R . . C14 C 0.9122(5) 0.3749(3) 0.1706(3) 0.0518(13) Uani 1 1 d . . . H14 H 0.989 0.342 0.1782 0.062 Uiso 1 1 calc R . . C15 C 0.8049(5) 0.3598(2) 0.1205(3) 0.0477(13) Uani 1 1 d . . . H15 H 0.8103 0.318 0.0931 0.057 Uiso 1 1 calc R . . C16 C 0.6901(4) 0.4060(2) 0.1105(2) 0.0357(10) Uani 1 1 d . . . C17 C 0.8617(6) 0.6064(3) 0.2167(4) 0.0680(18) Uani 1 1 d . . . H17A H 0.8479 0.6485 0.2454 0.102 Uiso 1 1 calc R . . H17B H 0.8298 0.6174 0.1693 0.102 Uiso 1 1 calc R . . H17C H 0.963 0.5934 0.2195 0.102 Uiso 1 1 calc R . . C18 C 0.8105(7) 0.5331(3) 0.3141(3) 0.0739(19) Uani 1 1 d . . . H18A H 0.7982 0.5777 0.3394 0.111 Uiso 1 1 calc R . . H18B H 0.9092 0.5164 0.322 0.111 Uiso 1 1 calc R . . H18C H 0.7456 0.4964 0.3299 0.111 Uiso 1 1 calc R . . C19 C 0.5523(6) 0.3180(3) 0.0406(3) 0.0671(17) Uani 1 1 d . . . H19A H 0.4719 0.3145 0.0061 0.101 Uiso 1 1 calc R . . H19B H 0.5318 0.2896 0.0808 0.101 Uiso 1 1 calc R . . H19C H 0.6387 0.2995 0.0216 0.101 Uiso 1 1 calc R . . C20 C 0.5825(6) 0.4379(3) -0.0008(3) 0.0533(13) Uani 1 1 d . . . H20A H 0.5009 0.4272 -0.0331 0.08 Uiso 1 1 calc R . . H20B H 0.6712 0.4271 -0.0221 0.08 Uiso 1 1 calc R . . H20C H 0.5811 0.4888 0.0117 0.08 Uiso 1 1 calc R . . C21 C 0.1621(6) 0.5541(3) 0.1085(3) 0.0467(14) Uani 1 1 d . . . H21A H 0.1009 0.5286 0.1396 0.056 Uiso 1 1 calc R . . H21B H 0.2049 0.5962 0.1329 0.056 Uiso 1 1 calc R . . C22 C 0.0739(4) 0.5784(2) 0.0459(2) 0.0399(11) Uani 1 1 d . . . C23 C -0.0493(5) 0.5435(3) 0.0234(3) 0.0444(12) Uani 1 1 d . . . H23 H -0.0816 0.5036 0.0483 0.053 Uiso 1 1 calc R . . C24 C -0.1264(5) 0.5663(3) -0.0354(3) 0.0543(14) Uani 1 1 d . . . H24 H -0.2108 0.5413 -0.0509 0.065 Uiso 1 1 calc R . . C25 C -0.0830(6) 0.6243(3) -0.0719(3) 0.0585(15) Uani 1 1 d . . . H25 H -0.1368 0.6397 -0.1121 0.07 Uiso 1 1 calc R . . C26 C 0.0396(6) 0.6597(3) -0.0491(3) 0.0593(15) Uani 1 1 d . . . H26 H 0.0707 0.7001 -0.0737 0.071 Uiso 1 1 calc R . . C27 C 0.1185(5) 0.6369(3) 0.0093(3) 0.0507(13) Uani 1 1 d . . . H27 H 0.2035 0.6616 0.0244 0.061 Uiso 1 1 calc R . . C28 C 0.5695(8) 0.6451(3) 0.0479(3) 0.0519(18) Uani 1 1 d . . . H28A H 0.672 0.6321 0.0504 0.062 Uiso 1 1 calc R . . H28B H 0.5151 0.6065 0.0231 0.062 Uiso 1 1 calc R . . C29 C 0.5467(5) 0.7149(2) 0.0106(2) 0.0390(11) Uani 1 1 d . . . C30 C 0.4443(6) 0.7229(3) -0.0428(3) 0.0550(14) Uani 1 1 d . . . H30 H 0.3907 0.6823 -0.0588 0.066 Uiso 1 1 calc R . . C31 C 0.4182(6) 0.7889(3) -0.0736(3) 0.0627(16) Uani 1 1 d . . . H31 H 0.3469 0.7933 -0.1102 0.075 Uiso 1 1 calc R . . C32 C 0.4944(6) 0.8474(3) -0.0513(3) 0.0556(14) Uani 1 1 d . . . H32 H 0.4757 0.8929 -0.072 0.067 Uiso 1 1 calc R . . C33 C 0.5968(6) 0.8409(3) 0.0001(3) 0.0567(14) Uani 1 1 d . . . H33 H 0.6509 0.8818 0.0152 0.068 Uiso 1 1 calc R . . C34 C 0.6231(5) 0.7760(3) 0.0306(3) 0.0488(13) Uani 1 1 d . . . H34 H 0.6958 0.7725 0.0667 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn 0.03144(12) 0.02784(12) 0.02883(14) 0.00034(17) 0.00364(9) 0.00550(18) S1 0.0671(8) 0.0280(6) 0.0333(7) 0.0037(5) 0.0143(6) 0.0073(5) S2 0.0373(6) 0.0509(7) 0.0463(8) -0.0140(6) -0.0066(5) 0.0136(6) N1 0.047(3) 0.035(3) 0.050(3) -0.004(2) 0.011(2) 0.006(2) N2 0.038(2) 0.030(2) 0.052(3) 0.000(2) 0.006(2) 0.0083(17) N3 0.038(2) 0.050(2) 0.034(3) -0.008(2) -0.0019(19) -0.002(2) N4 0.036(2) 0.039(2) 0.051(3) -0.021(2) 0.001(2) -0.0022(19) C1 0.0246(19) 0.033(2) 0.033(3) 0.001(2) -0.0006(18) 0.0025(18) C2 0.030(2) 0.038(2) 0.031(3) -0.004(2) 0.0013(18) 0.0064(19) C3 0.046(3) 0.049(3) 0.039(3) -0.004(2) 0.005(2) 0.010(2) C4 0.056(3) 0.062(3) 0.037(3) 0.007(3) 0.013(2) -0.002(3) C5 0.048(3) 0.040(3) 0.039(3) 0.010(2) 0.008(2) 0.005(2) C6 0.026(2) 0.040(3) 0.035(3) 0.009(2) -0.0022(19) 0.0032(19) C7 0.060(3) 0.047(3) 0.057(4) -0.002(3) 0.002(3) -0.007(3) C8 0.064(4) 0.050(3) 0.149(7) 0.013(4) 0.028(4) 0.023(3) C9 0.061(3) 0.047(3) 0.093(5) -0.019(3) 0.015(3) -0.017(3) C10 0.064(3) 0.063(4) 0.069(4) 0.019(3) 0.018(3) 0.030(3) C11 0.028(2) 0.031(2) 0.033(3) -0.0007(19) 0.0062(18) 0.0004(18) C12 0.032(2) 0.037(2) 0.037(3) -0.002(2) 0.0053(19) 0.0034(19) C13 0.029(2) 0.055(3) 0.054(3) -0.003(3) -0.001(2) 0.003(2) C14 0.039(3) 0.049(3) 0.068(4) 0.000(3) 0.002(3) 0.017(2) C15 0.038(3) 0.037(3) 0.069(4) -0.009(2) 0.011(2) 0.007(2) C16 0.031(2) 0.035(2) 0.042(3) -0.005(2) 0.0114(19) 0.001(2) C17 0.057(3) 0.047(3) 0.102(5) -0.029(3) 0.021(3) -0.012(3) C18 0.087(4) 0.088(5) 0.043(4) -0.017(3) -0.019(3) 0.022(4) C19 0.063(3) 0.056(3) 0.084(5) -0.037(3) 0.013(3) -0.012(3) C20 0.057(3) 0.055(3) 0.047(4) -0.011(3) -0.002(3) 0.011(3) C21 0.041(3) 0.061(3) 0.038(3) -0.003(3) -0.002(2) 0.014(3) C22 0.030(2) 0.045(3) 0.044(3) -0.006(2) -0.001(2) 0.011(2) C23 0.041(3) 0.054(3) 0.040(3) -0.003(2) 0.012(2) 0.002(2) C24 0.041(3) 0.073(4) 0.048(3) -0.015(3) 0.000(2) -0.003(3) C25 0.062(3) 0.062(4) 0.048(4) -0.008(3) -0.016(3) 0.020(3) C26 0.076(4) 0.037(3) 0.063(4) -0.002(3) -0.008(3) 0.009(3) C27 0.050(3) 0.039(3) 0.062(4) -0.005(3) -0.003(3) -0.001(2) C28 0.083(5) 0.036(3) 0.040(4) 0.008(3) 0.023(3) 0.018(3) C29 0.051(3) 0.038(3) 0.030(3) 0.003(2) 0.018(2) 0.003(2) C30 0.066(3) 0.060(3) 0.040(3) -0.005(3) 0.006(3) -0.024(3) C31 0.055(3) 0.084(4) 0.047(4) 0.021(3) -0.009(3) -0.004(3) C32 0.067(3) 0.052(3) 0.050(4) 0.016(3) 0.020(3) 0.006(3) C33 0.072(4) 0.038(3) 0.061(4) -0.001(3) 0.014(3) -0.019(3) C34 0.048(3) 0.055(3) 0.044(3) 0.002(3) -0.001(2) -0.011(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn C11 2.135(4) . ? Sn C1 2.141(4) . ? Sn S2 2.4266(12) . ? Sn S1 2.4305(11) . ? S1 C28 1.827(6) . ? S2 C21 1.848(5) . ? N1 C2 1.424(7) . ? N1 C8 1.433(7) . ? N1 C7 1.450(7) . ? N2 C6 1.448(6) . ? N2 C10 1.472(6) . ? N2 C9 1.471(6) . ? N3 C12 1.441(6) . ? N3 C18 1.468(7) . ? N3 C17 1.471(7) . ? N4 C16 1.428(6) . ? N4 C20 1.466(7) . ? N4 C19 1.478(7) . ? C1 C6 1.390(6) . ? C1 C2 1.407(6) . ? C2 C3 1.393(6) . ? C3 C4 1.384(7) . ? C4 C5 1.384(7) . ? C5 C6 1.385(6) . ? C11 C12 1.378(6) . ? C11 C16 1.420(6) . ? C12 C13 1.397(6) . ? C13 C14 1.374(7) . ? C14 C15 1.387(7) . ? C15 C16 1.383(6) . ? C21 C22 1.502(7) . ? C22 C23 1.373(6) . ? C22 C27 1.386(7) . ? C23 C24 1.386(7) . ? C24 C25 1.375(8) . ? C25 C26 1.374(8) . ? C26 C27 1.388(7) . ? C28 C29 1.500(7) . ? C29 C30 1.379(7) . ? C29 C34 1.387(7) . ? C30 C31 1.383(8) . ? C31 C32 1.360(8) . ? C32 C33 1.350(8) . ? C33 C34 1.364(7) . ? 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 C11 Sn C1 118.90(16) . . ? C11 Sn S2 110.48(12) . . ? C1 Sn S2 104.43(11) . . ? C11 Sn S1 114.45(11) . . ? C1 Sn S1 108.17(12) . . ? S2 Sn S1 97.92(5) . . ? C28 S1 Sn 100.21(19) . . ? C21 S2 Sn 99.58(18) . . ? C2 N1 C8 116.5(4) . . ? C2 N1 C7 113.4(4) . . ? C8 N1 C7 110.3(5) . . ? C6 N2 C10 112.3(4) . . ? C6 N2 C9 113.5(4) . . ? C10 N2 C9 110.9(4) . . ? C12 N3 C18 112.7(4) . . ? C12 N3 C17 111.7(4) . . ? C18 N3 C17 111.2(5) . . ? C16 N4 C20 113.0(4) . . ? C16 N4 C19 114.7(4) . . ? C20 N4 C19 109.3(4) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 Sn 111.6(3) . . ? C2 C1 Sn 128.0(3) . . ? C3 C2 C1 118.8(4) . . ? C3 C2 N1 122.2(4) . . ? C1 C2 N1 119.0(4) . . ? C4 C3 C2 120.6(4) . . ? C3 C4 C5 121.0(5) . . ? C4 C5 C6 118.7(4) . . ? C5 C6 C1 121.5(4) . . ? C5 C6 N2 123.0(4) . . ? C1 C6 N2 115.5(4) . . ? C12 C11 C16 119.5(4) . . ? C12 C11 Sn 113.6(3) . . ? C16 C11 Sn 125.1(3) . . ? C11 C12 C13 121.0(4) . . ? C11 C12 N3 115.8(4) . . ? C13 C12 N3 123.2(4) . . ? C14 C13 C12 118.6(4) . . ? C13 C14 C15 121.9(4) . . ? C16 C15 C14 119.7(4) . . ? C15 C16 C11 119.3(4) . . ? C15 C16 N4 123.2(4) . . ? C11 C16 N4 117.5(4) . . ? C22 C21 S2 109.3(4) . . ? C23 C22 C27 119.1(5) . . ? C23 C22 C21 121.4(5) . . ? C27 C22 C21 119.4(4) . . ? C22 C23 C24 120.0(5) . . ? C25 C24 C23 121.2(5) . . ? C26 C25 C24 118.8(5) . . ? C25 C26 C27 120.5(5) . . ? C22 C27 C26 120.3(5) . . ? C29 C28 S1 109.1(4) . . ? C30 C29 C34 116.4(4) . . ? C30 C29 C28 122.2(5) . . ? C34 C29 C28 121.3(5) . . ? C29 C30 C31 121.4(5) . . ? C32 C31 C30 120.0(5) . . ? C33 C32 C31 119.9(5) . . ? C32 C33 C34 120.3(5) . . ? C33 C34 C29 122.0(5) . . ? #===END data_(8)-nov2700 _database_code_depnum_ccdc_archive 'CCDC 710456' _audit_creation_date 2000-11-29T12:19:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C32 H40 N4 Sn1 Te2).0.25(C5 H12 O1)' _chemical_formula_sum 'C33.25 H43 N4 O0.25 Sn Te2' _chemical_formula_weight 876.61 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.1879(10) _cell_length_b 10.2940(2) _cell_length_c 36.4313(9) _cell_angle_alpha 90 _cell_angle_beta 111.8160(10) _cell_angle_gamma 90 _cell_volume 13992.0(6) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 41274 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6824 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.413 _exptl_absorpt_correction_T_max 0.481 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 33834 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_unetI/netI 0.0798 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 16590 _reflns_number_gt 10994 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two independent molecules of the complex in general positions and a molecule of tBuOMe disordered about a 2-fold axis. The solvate H atoms were omitted. The disordered solvate molecule is poorly defined with resultant low accuracy of the solvate dimensions. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+4.4720P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.000024(14) _refine_ls_number_reflns 16590 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.153 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.132 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.084039(11) 0.35931(3) 0.403883(11) 0.04101(11) Uani 1 1 d . . . Te2 Te 0.131958(11) 0.57383(4) 0.511506(11) 0.04234(11) Uani 1 1 d . . . Sn Sn 0.117099(9) 0.59126(3) 0.431711(10) 0.03027(10) Uani 1 1 d . . . N1 N 0.09005(12) 0.6871(4) 0.34747(13) 0.0380(10) Uani 1 1 d . . . N2 N 0.07914(13) 0.8166(4) 0.47065(14) 0.0445(12) Uani 1 1 d . . . N3 N 0.15544(13) 0.3881(4) 0.38917(13) 0.0414(11) Uani 1 1 d . . . N4 N 0.17399(12) 0.8102(4) 0.45416(13) 0.0384(11) Uani 1 1 d . . . C1 C 0.03994(15) 0.3930(5) 0.42227(17) 0.0400(13) Uani 1 1 d . . . C2 C 0.04006(17) 0.3453(6) 0.45705(17) 0.0482(15) Uani 1 1 d . . . H2 H 0.0599 0.2955 0.4734 0.058 Uiso 1 1 calc R . . C3 C 0.01118(18) 0.3685(7) 0.4692(2) 0.0604(18) Uani 1 1 d . . . H3 H 0.0115 0.3344 0.4936 0.072 Uiso 1 1 calc R . . C4 C -0.01744(18) 0.4411(6) 0.4454(2) 0.0629(19) Uani 1 1 d . . . H4 H -0.0368 0.46 0.4536 0.075 Uiso 1 1 calc R . . C5 C -0.01777(19) 0.4855(7) 0.4103(2) 0.077(2) Uani 1 1 d . . . H5 H -0.0379 0.5331 0.3934 0.092 Uiso 1 1 calc R . . C6 C 0.01064(17) 0.4625(6) 0.3985(2) 0.0617(19) Uani 1 1 d . . . H6 H 0.0099 0.4949 0.3738 0.074 Uiso 1 1 calc R . . C7 C 0.16753(16) 0.4134(5) 0.51948(16) 0.0425(14) Uani 1 1 d . . . C8 C 0.15617(19) 0.2870(6) 0.52046(17) 0.0535(16) Uani 1 1 d . . . H8 H 0.1317 0.2701 0.5158 0.064 Uiso 1 1 calc R . . C9 C 0.1804(2) 0.1843(6) 0.5282(2) 0.068(2) Uani 1 1 d . . . H9 H 0.1724 0.098 0.5293 0.082 Uiso 1 1 calc R . . C10 C 0.2157(2) 0.2068(8) 0.5342(2) 0.073(2) Uani 1 1 d . . . H10 H 0.232 0.1363 0.5393 0.088 Uiso 1 1 calc R . . C11 C 0.2270(2) 0.3288(7) 0.5328(2) 0.075(2) Uani 1 1 d . . . H11 H 0.2513 0.3439 0.5364 0.09 Uiso 1 1 calc R . . C12 C 0.20346(18) 0.4335(6) 0.5260(2) 0.0612(18) Uani 1 1 d . . . H12 H 0.2121 0.5194 0.5258 0.073 Uiso 1 1 calc R . . C13 C 0.08456(13) 0.7579(5) 0.40795(15) 0.0319(11) Uani 1 1 d . . . C14 C 0.07914(14) 0.7854(5) 0.36868(16) 0.0357(12) Uani 1 1 d . . . C15 C 0.06411(17) 0.9037(5) 0.35199(19) 0.0498(15) Uani 1 1 d . . . H15 H 0.0603 0.9221 0.3252 0.06 Uiso 1 1 calc R . . C16 C 0.05477(18) 0.9937(6) 0.3744(2) 0.0578(18) Uani 1 1 d . . . H16 H 0.0451 1.0751 0.3631 0.069 Uiso 1 1 calc R . . C17 C 0.05932(16) 0.9669(5) 0.41319(18) 0.0465(15) Uani 1 1 d . . . H17 H 0.0524 1.0293 0.4282 0.056 Uiso 1 1 calc R . . C18 C 0.07395(14) 0.8489(5) 0.43034(17) 0.0381(13) Uani 1 1 d . . . C19 C 0.11408(16) 0.7372(6) 0.32852(18) 0.0523(16) Uani 1 1 d . . . H19A H 0.1207 0.6665 0.3145 0.078 Uiso 1 1 calc R . . H19B H 0.1358 0.7729 0.3488 0.078 Uiso 1 1 calc R . . H19C H 0.1018 0.8057 0.3097 0.078 Uiso 1 1 calc R . . C20 C 0.05909(15) 0.6211(5) 0.31858(16) 0.0459(14) Uani 1 1 d . . . H20A H 0.0674 0.5547 0.3047 0.069 Uiso 1 1 calc R . . H20B H 0.0442 0.6846 0.2995 0.069 Uiso 1 1 calc R . . H20C H 0.045 0.5799 0.3323 0.069 Uiso 1 1 calc R . . C21 C 0.0936(3) 0.9236(7) 0.4983(2) 0.109(4) Uani 1 1 d . . . H21A H 0.115 0.9583 0.4949 0.164 Uiso 1 1 calc R . . H21B H 0.1 0.892 0.5254 0.164 Uiso 1 1 calc R . . H21C H 0.0755 0.9923 0.493 0.164 Uiso 1 1 calc R . . C22 C 0.0478(2) 0.7620(9) 0.4742(2) 0.097(3) Uani 1 1 d . . . H22A H 0.0527 0.7415 0.502 0.146 Uiso 1 1 calc R . . H22B H 0.0411 0.6824 0.4584 0.146 Uiso 1 1 calc R . . H22C H 0.0281 0.8246 0.4646 0.146 Uiso 1 1 calc R . . C23 C 0.16591(13) 0.6019(5) 0.42106(15) 0.0315(11) Uani 1 1 d . . . C24 C 0.18558(14) 0.7152(5) 0.43210(15) 0.0397(13) Uani 1 1 d . . . C25 C 0.21543(16) 0.7351(6) 0.42228(17) 0.0505(15) Uani 1 1 d . . . H25 H 0.2288 0.8132 0.4298 0.061 Uiso 1 1 calc R . . C26 C 0.22562(17) 0.6404(7) 0.40133(19) 0.0599(18) Uani 1 1 d . . . H26 H 0.246 0.654 0.3944 0.072 Uiso 1 1 calc R . . C27 C 0.20654(16) 0.5286(7) 0.39070(17) 0.0529(16) Uani 1 1 d . . . H27 H 0.2139 0.4638 0.3767 0.063 Uiso 1 1 calc R . . C28 C 0.17612(15) 0.5073(5) 0.40012(15) 0.0388(13) Uani 1 1 d . . . C29 C 0.14478(19) 0.3554(6) 0.34762(18) 0.0610(18) Uani 1 1 d . . . H29A H 0.131 0.2745 0.3422 0.092 Uiso 1 1 calc R . . H29B H 0.1662 0.3442 0.3411 0.092 Uiso 1 1 calc R . . H29C H 0.13 0.4255 0.3315 0.092 Uiso 1 1 calc R . . C30 C 0.17389(19) 0.2804(6) 0.4147(2) 0.0644(19) Uani 1 1 d . . . H30A H 0.1594 0.2015 0.4067 0.097 Uiso 1 1 calc R . . H30B H 0.1775 0.3012 0.4422 0.097 Uiso 1 1 calc R . . H30C H 0.1972 0.2663 0.4125 0.097 Uiso 1 1 calc R . . C31 C 0.16495(16) 0.9368(5) 0.43479(18) 0.0498(15) Uani 1 1 d . . . H31A H 0.1574 0.9958 0.4514 0.075 Uiso 1 1 calc R . . H31B H 0.1454 0.9266 0.4091 0.075 Uiso 1 1 calc R . . H31C H 0.186 0.9728 0.431 0.075 Uiso 1 1 calc R . . C32 C 0.20038(17) 0.8248(6) 0.49505(17) 0.0541(16) Uani 1 1 d . . . H32A H 0.1917 0.8895 0.5091 0.081 Uiso 1 1 calc R . . H32B H 0.2234 0.8534 0.4943 0.081 Uiso 1 1 calc R . . H32C H 0.2035 0.7412 0.5088 0.081 Uiso 1 1 calc R . . O O 0.0279(2) 0.1593(7) 0.2709(2) 0.111(2) Uiso 0.5 1 d P B . C33 C 0.0574(4) 0.2024(14) 0.2860(4) 0.068(4) Uiso 0.5 1 d P . . C34 C 0 0.2531(9) 0.25 0.055(2) Uiso 1 2 d S . . C35 C 0.0069(4) 0.3671(14) 0.2300(4) 0.068(4) Uiso 0.5 1 d P . . C36 C -0.0096(4) 0.2869(15) 0.2919(5) 0.080(4) Uiso 0.5 1 d P . . Te1B Te 0.123442(12) 1.13709(4) 0.225685(15) 0.05807(14) Uani 1 1 d . A 1 Te2B Te 0.204431(10) 0.91277(4) 0.206048(13) 0.04520(11) Uani 1 1 d . A 1 Sn1B Sn 0.133037(9) 0.90509(3) 0.193950(11) 0.03274(10) Uani 1 1 d . A 1 N1B N 0.05846(11) 0.8221(4) 0.18988(13) 0.0381(10) Uani 1 1 d . A 1 N2B N 0.18061(12) 0.6649(4) 0.25029(13) 0.0397(11) Uani 1 1 d . A 1 N3B N 0.07582(13) 1.1109(4) 0.13280(16) 0.0488(13) Uani 1 1 d . A 1 N4B N 0.13093(11) 0.6897(4) 0.13496(13) 0.0361(10) Uani 1 1 d . A 1 C1B C 0.16700(17) 1.1132(5) 0.28122(18) 0.0476(15) Uani 1 1 d . A 1 C2B C 0.19790(19) 1.1837(6) 0.2896(2) 0.0600(18) Uani 1 1 d . A 1 H2B H 0.1997 1.2429 0.2704 0.072 Uiso 1 1 calc R A 1 C3B C 0.2263(2) 1.1710(7) 0.3249(2) 0.069(2) Uani 1 1 d . A 1 H3B H 0.2475 1.2213 0.3307 0.083 Uiso 1 1 calc R A 1 C4B C 0.2229(3) 1.0819(8) 0.3521(2) 0.079(2) Uani 1 1 d . A 1 H4B H 0.2424 1.0682 0.3764 0.095 Uiso 1 1 calc R A 1 C5B C 0.1924(3) 1.0153(8) 0.3442(3) 0.098(3) Uani 1 1 d . A 1 H5B H 0.1903 0.9557 0.3632 0.118 Uiso 1 1 calc R A 1 C6B C 0.1641(2) 1.0321(8) 0.3091(2) 0.083(3) Uani 1 1 d . A 1 H6B H 0.1423 0.9865 0.3043 0.099 Uiso 1 1 calc R A 1 C7B C 0.19842(14) 1.0798(5) 0.16878(19) 0.0438(14) Uani 1 1 d . A 1 C8B C 0.20681(16) 1.2012(6) 0.18512(19) 0.0506(15) Uani 1 1 d . A 1 H8B H 0.2146 1.2118 0.213 0.061 Uiso 1 1 calc R A 1 C9B C 0.20390(18) 1.3094(6) 0.1610(2) 0.0582(17) Uani 1 1 d . A 1 H9B H 0.2102 1.393 0.1726 0.07 Uiso 1 1 calc R A 1 C10B C 0.19196(18) 1.2959(7) 0.1207(2) 0.0591(18) Uani 1 1 d . A 1 H10B H 0.1899 1.3696 0.1043 0.071 Uiso 1 1 calc R A 1 C11B C 0.18312(17) 1.1756(7) 0.1045(2) 0.0593(17) Uani 1 1 d . A 1 H11B H 0.1744 1.1654 0.0766 0.071 Uiso 1 1 calc R A 1 C12B C 0.18685(17) 1.0680(6) 0.1286(2) 0.0550(17) Uani 1 1 d . A 1 H12B H 0.1813 0.9843 0.1169 0.066 Uiso 1 1 calc R A 1 C13B C 0.11870(14) 0.7366(5) 0.21985(15) 0.0331(12) Uani 1 1 d . A 1 C14B C 0.08239(15) 0.7167(5) 0.20954(16) 0.0359(12) Uani 1 1 d . A 1 C15B C 0.06947(16) 0.5993(5) 0.21713(19) 0.0473(15) Uani 1 1 d . A 1 H15B H 0.0445 0.586 0.2101 0.057 Uiso 1 1 calc R A 1 C16B C 0.09380(18) 0.5010(6) 0.23531(19) 0.0538(17) Uani 1 1 d . A 1 H16B H 0.0854 0.4188 0.2399 0.065 Uiso 1 1 calc R A 1 C17B C 0.12996(17) 0.5226(5) 0.24658(17) 0.0462(15) Uani 1 1 d . A 1 H17B H 0.1463 0.4556 0.2598 0.055 Uiso 1 1 calc R A 1 C18B C 0.14325(15) 0.6403(5) 0.23912(16) 0.0364(12) Uani 1 1 d . A 1 C19B C 0.02956(15) 0.7833(6) 0.15352(18) 0.0515(15) Uani 1 1 d . A 1 H19D H 0.0144 0.8586 0.1419 0.077 Uiso 1 1 calc R A 1 H19E H 0.0151 0.7156 0.1594 0.077 Uiso 1 1 calc R A 1 H19F H 0.0397 0.7494 0.1348 0.077 Uiso 1 1 calc R A 1 C20B C 0.04423(17) 0.8864(5) 0.21698(19) 0.0500(15) Uani 1 1 d . A 1 H20D H 0.0282 0.9573 0.2031 0.075 Uiso 1 1 calc R A 1 H20E H 0.0641 0.9214 0.2397 0.075 Uiso 1 1 calc R A 1 H20F H 0.0309 0.8232 0.2263 0.075 Uiso 1 1 calc R A 1 C21B C 0.2014(2) 0.5615(7) 0.2444(3) 0.089(3) Uani 1 1 d . A 1 H21D H 0.2265 0.5886 0.2529 0.134 Uiso 1 1 calc R A 1 H21E H 0.1925 0.5382 0.2164 0.134 Uiso 1 1 calc R A 1 H21F H 0.1995 0.486 0.26 0.134 Uiso 1 1 calc R A 1 C22B C 0.1961(2) 0.7197(12) 0.2894(2) 0.127(4) Uani 1 1 d . A 1 H22D H 0.1811 0.7915 0.292 0.191 Uiso 1 1 calc R A 1 H22E H 0.2202 0.7522 0.2939 0.191 Uiso 1 1 calc R A 1 H22F H 0.1975 0.6527 0.3091 0.191 Uiso 1 1 calc R A 1 C23B C 0.10203(13) 0.8992(5) 0.13172(16) 0.0348(12) Uani 1 1 d . A 1 C24B C 0.10444(15) 0.7847(5) 0.11231(16) 0.0392(13) Uani 1 1 d . A 1 C25B C 0.08215(16) 0.7669(6) 0.07302(17) 0.0471(15) Uani 1 1 d . A 1 H25B H 0.0842 0.6905 0.0594 0.057 Uiso 1 1 calc R A 1 C26B C 0.05728(18) 0.8592(6) 0.0540(2) 0.0569(17) Uani 1 1 d . A 1 H26B H 0.0417 0.8447 0.0274 0.068 Uiso 1 1 calc R A 1 C27B C 0.05433(16) 0.9741(6) 0.07282(18) 0.0518(16) Uani 1 1 d . A 1 H27B H 0.0371 1.0379 0.0591 0.062 Uiso 1 1 calc R A 1 C28B C 0.07705(15) 0.9944(5) 0.11210(17) 0.0394(13) Uani 1 1 d . A 1 C29B C 0.03971(17) 1.1536(6) 0.1283(2) 0.069(2) Uani 1 1 d . A 1 H29D H 0.0413 1.2339 0.1433 0.104 Uiso 1 1 calc R A 1 H29E H 0.0281 1.086 0.1383 0.104 Uiso 1 1 calc R A 1 H29F H 0.0256 1.1694 0.1002 0.104 Uiso 1 1 calc R A 1 C30B C 0.09547(18) 1.2173(6) 0.1225(2) 0.068(2) Uani 1 1 d . A 1 H30D H 0.0941 1.296 0.137 0.102 Uiso 1 1 calc R A 1 H30E H 0.0847 1.2341 0.094 0.102 Uiso 1 1 calc R A 1 H30F H 0.1206 1.1922 0.1296 0.102 Uiso 1 1 calc R A 1 C31B C 0.11558(16) 0.5640(5) 0.13758(18) 0.0451(14) Uani 1 1 d . A 1 H31D H 0.1347 0.5046 0.1531 0.068 Uiso 1 1 calc R A 1 H31E H 0.1034 0.5287 0.1109 0.068 Uiso 1 1 calc R A 1 H31F H 0.0983 0.574 0.1505 0.068 Uiso 1 1 calc R A 1 C32B C 0.15991(17) 0.6740(6) 0.11930(19) 0.0530(16) Uani 1 1 d . A 1 H32D H 0.17 0.7593 0.1174 0.079 Uiso 1 1 calc R A 1 H32E H 0.1501 0.6342 0.093 0.079 Uiso 1 1 calc R A 1 H32F H 0.1788 0.6181 0.1371 0.079 Uiso 1 1 calc R A 1 C37 C 0.0279(2) 0.1593(7) 0.2709(2) 0.111(2) Uiso 0.5 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0462(2) 0.0317(2) 0.0436(2) -0.00207(17) 0.01500(18) -0.00660(16) Te2 0.0479(2) 0.0439(2) 0.0353(2) -0.00020(17) 0.01551(17) 0.00231(18) Sn 0.02834(19) 0.02801(18) 0.0346(2) 0.00217(15) 0.01183(15) 0.00032(14) N1 0.036(3) 0.037(2) 0.040(3) 0.000(2) 0.014(2) -0.004(2) N2 0.044(3) 0.044(3) 0.053(3) -0.003(2) 0.027(2) 0.002(2) N3 0.044(3) 0.039(3) 0.040(3) 0.003(2) 0.014(2) 0.014(2) N4 0.035(3) 0.035(2) 0.038(3) 0.005(2) 0.005(2) -0.001(2) C1 0.036(3) 0.034(3) 0.045(3) 0.006(3) 0.009(3) -0.010(2) C2 0.047(4) 0.048(4) 0.047(4) 0.007(3) 0.014(3) 0.001(3) C3 0.049(4) 0.073(5) 0.060(4) 0.012(4) 0.021(3) 0.001(4) C4 0.041(4) 0.059(4) 0.090(6) 0.003(4) 0.026(4) -0.004(3) C5 0.041(4) 0.081(5) 0.102(6) 0.050(5) 0.020(4) 0.008(4) C6 0.044(4) 0.068(4) 0.073(5) 0.039(4) 0.023(3) 0.005(3) C7 0.049(4) 0.042(3) 0.034(3) 0.010(3) 0.013(3) 0.006(3) C8 0.064(4) 0.052(4) 0.047(4) -0.006(3) 0.023(3) -0.004(3) C9 0.093(6) 0.041(4) 0.062(5) 0.000(3) 0.019(4) 0.013(4) C10 0.071(6) 0.066(5) 0.062(5) 0.001(4) 0.000(4) 0.025(4) C11 0.047(4) 0.070(5) 0.088(6) 0.004(5) 0.003(4) 0.011(4) C12 0.045(4) 0.053(4) 0.075(5) 0.015(4) 0.010(4) 0.005(3) C13 0.023(3) 0.026(3) 0.045(3) 0.001(2) 0.009(2) -0.003(2) C14 0.029(3) 0.030(3) 0.045(3) 0.005(3) 0.010(2) 0.000(2) C15 0.053(4) 0.037(3) 0.054(4) 0.007(3) 0.015(3) 0.002(3) C16 0.064(5) 0.028(3) 0.067(4) 0.005(3) 0.008(4) 0.004(3) C17 0.044(4) 0.031(3) 0.061(4) -0.008(3) 0.014(3) 0.003(3) C18 0.025(3) 0.036(3) 0.056(4) 0.001(3) 0.018(3) -0.001(2) C19 0.050(4) 0.056(4) 0.057(4) 0.011(3) 0.027(3) 0.000(3) C20 0.042(4) 0.051(3) 0.040(3) -0.003(3) 0.010(3) -0.007(3) C21 0.193(12) 0.070(5) 0.069(6) -0.024(5) 0.053(7) -0.001(6) C22 0.065(6) 0.137(8) 0.107(7) 0.045(6) 0.051(5) 0.002(5) C23 0.022(2) 0.036(3) 0.036(3) 0.007(2) 0.010(2) 0.006(2) C24 0.031(3) 0.049(3) 0.036(3) 0.009(3) 0.008(2) 0.002(3) C25 0.037(3) 0.060(4) 0.052(4) 0.000(3) 0.014(3) -0.012(3) C26 0.035(4) 0.086(5) 0.065(4) 0.002(4) 0.026(3) -0.007(3) C27 0.040(4) 0.077(5) 0.047(4) 0.001(3) 0.022(3) 0.013(3) C28 0.035(3) 0.046(3) 0.032(3) 0.008(3) 0.010(2) 0.008(3) C29 0.073(5) 0.062(4) 0.049(4) -0.010(3) 0.023(4) 0.004(4) C30 0.066(5) 0.054(4) 0.067(5) 0.015(4) 0.018(4) 0.024(3) C31 0.046(4) 0.041(3) 0.053(4) 0.006(3) 0.008(3) -0.006(3) C32 0.055(4) 0.047(4) 0.051(4) 0.001(3) 0.009(3) -0.006(3) Te1B 0.0476(3) 0.0382(2) 0.0876(3) -0.0221(2) 0.0242(2) 0.00156(19) Te2B 0.0272(2) 0.0416(2) 0.0659(3) 0.00183(19) 0.01630(18) 0.00021(16) Sn1B 0.02745(19) 0.02717(18) 0.0438(2) -0.00351(16) 0.01344(16) -0.00124(14) N1B 0.029(2) 0.034(2) 0.052(3) -0.001(2) 0.016(2) 0.0041(19) N2B 0.033(3) 0.039(3) 0.043(3) -0.002(2) 0.010(2) 0.011(2) N3B 0.039(3) 0.033(3) 0.079(4) 0.006(3) 0.027(3) 0.002(2) N4B 0.031(2) 0.035(2) 0.045(3) -0.008(2) 0.017(2) -0.002(2) C1B 0.059(4) 0.036(3) 0.059(4) -0.019(3) 0.035(3) -0.011(3) C2B 0.066(5) 0.060(4) 0.063(4) -0.009(4) 0.035(4) -0.016(4) C3B 0.059(5) 0.085(5) 0.068(5) -0.017(4) 0.031(4) -0.018(4) C4B 0.106(7) 0.079(6) 0.046(4) -0.008(4) 0.022(4) 0.007(5) C5B 0.156(10) 0.082(6) 0.068(6) -0.012(5) 0.054(6) -0.045(6) C6B 0.112(7) 0.086(6) 0.058(5) -0.018(4) 0.041(5) -0.056(5) C7B 0.024(3) 0.050(4) 0.063(4) -0.005(3) 0.021(3) 0.003(2) C8B 0.048(4) 0.045(4) 0.060(4) -0.001(3) 0.021(3) 0.009(3) C9B 0.066(5) 0.038(3) 0.076(5) 0.004(4) 0.033(4) 0.007(3) C10B 0.052(4) 0.057(4) 0.076(5) 0.009(4) 0.033(4) 0.009(3) C11B 0.048(4) 0.070(5) 0.066(4) 0.008(4) 0.029(3) -0.001(3) C12B 0.051(4) 0.050(4) 0.065(4) -0.006(3) 0.023(3) -0.017(3) C13B 0.034(3) 0.035(3) 0.032(3) -0.001(2) 0.015(2) 0.000(2) C14B 0.037(3) 0.028(3) 0.048(3) -0.005(2) 0.022(3) -0.001(2) C15B 0.036(3) 0.040(3) 0.071(4) -0.006(3) 0.025(3) -0.007(3) C16B 0.056(4) 0.035(3) 0.081(5) 0.007(3) 0.037(4) -0.001(3) C17B 0.058(4) 0.033(3) 0.051(4) 0.012(3) 0.023(3) 0.017(3) C18B 0.036(3) 0.032(3) 0.045(3) -0.005(3) 0.019(3) 0.004(2) C19B 0.037(3) 0.054(4) 0.061(4) -0.002(3) 0.014(3) -0.004(3) C20B 0.051(4) 0.039(3) 0.066(4) 0.003(3) 0.029(3) 0.012(3) C21B 0.052(5) 0.073(5) 0.147(8) -0.032(5) 0.042(5) 0.011(4) C22B 0.054(5) 0.246(13) 0.077(6) -0.073(7) 0.018(5) -0.018(7) C23B 0.026(3) 0.034(3) 0.047(3) 0.000(3) 0.017(2) -0.004(2) C24B 0.038(3) 0.035(3) 0.046(3) 0.000(3) 0.017(3) -0.008(2) C25B 0.047(4) 0.047(3) 0.046(4) 0.001(3) 0.015(3) -0.009(3) C26B 0.053(4) 0.059(4) 0.050(4) 0.004(3) 0.010(3) -0.015(3) C27B 0.036(4) 0.055(4) 0.058(4) 0.019(3) 0.010(3) 0.002(3) C28B 0.035(3) 0.032(3) 0.055(4) 0.006(3) 0.021(3) -0.005(2) C29B 0.045(4) 0.060(4) 0.110(6) 0.005(4) 0.036(4) 0.006(3) C30B 0.054(4) 0.045(4) 0.102(6) 0.007(4) 0.025(4) -0.010(3) C31B 0.048(4) 0.029(3) 0.056(4) -0.005(3) 0.016(3) -0.006(3) C32B 0.055(4) 0.048(4) 0.064(4) -0.006(3) 0.031(3) -0.004(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Te1 C1 2.143(6) . ? Te1 Sn 2.7374(5) . ? Te2 C7 2.132(6) . ? Te2 Sn 2.7476(5) . ? Sn C13 2.135(5) . ? Sn C23 2.139(5) . ? N1 C14 1.438(7) . ? N1 C20 1.464(6) . ? N1 C19 1.473(6) . ? N2 C22 1.428(8) . ? N2 C18 1.443(7) . ? N2 C21 1.459(8) . ? N3 C29 1.452(7) . ? N3 C28 1.452(7) . ? N3 C30 1.461(7) . ? N4 C24 1.448(7) . ? N4 C31 1.462(7) . ? N4 C32 1.481(7) . ? C1 C2 1.358(8) . ? C1 C6 1.374(8) . ? C2 C3 1.409(8) . ? C3 C4 1.375(9) . ? C4 C5 1.356(9) . ? C5 C6 1.381(9) . ? C7 C8 1.384(8) . ? C7 C12 1.389(8) . ? C8 C9 1.392(9) . ? C9 C10 1.373(10) . ? C10 C11 1.343(10) . ? C11 C12 1.394(9) . ? C13 C14 1.394(7) . ? C13 C18 1.408(7) . ? C14 C15 1.394(7) . ? C15 C16 1.375(8) . ? C16 C17 1.385(8) . ? C17 C18 1.392(7) . ? C23 C24 1.383(7) . ? C23 C28 1.389(7) . ? C24 C25 1.388(7) . ? C25 C26 1.390(8) . ? C26 C27 1.357(9) . ? C27 C28 1.404(8) . ? O C33 1.191(15) . ? O C34 1.460(9) . ? C34 C37 1.460(9) 2 ? C34 O 1.460(9) 2 ? C34 C35 1.460(15) 2 ? C34 C35 1.460(15) . ? C35 C36 1.184(18) 2 ? C36 C35 1.184(18) 2 ? Te1B C1B 2.141(7) . ? Te1B Sn1B 2.7423(5) . ? Te2B C7B 2.148(6) . ? Te2B Sn1B 2.7373(5) . ? Sn1B C23B 2.144(6) . ? Sn1B C13B 2.153(5) . ? N1B C14B 1.451(6) . ? N1B C19B 1.456(7) . ? N1B C20B 1.469(7) . ? N2B C21B 1.417(7) . ? N2B C18B 1.425(7) . ? N2B C22B 1.442(8) . ? N3B C28B 1.427(7) . ? N3B C29B 1.466(7) . ? N3B C30B 1.478(7) . ? N4B C31B 1.452(6) . ? N4B C24B 1.455(7) . ? N4B C32B 1.484(6) . ? C1B C6B 1.352(9) . ? C1B C2B 1.372(8) . ? C2B C3B 1.374(9) . ? C3B C4B 1.391(10) . ? C4B C5B 1.341(11) . ? C5B C6B 1.371(11) . ? C7B C12B 1.367(8) . ? C7B C8B 1.372(8) . ? C8B C9B 1.396(8) . ? C9B C10B 1.372(9) . ? C10B C11B 1.360(9) . ? C11B C12B 1.385(8) . ? C13B C14B 1.380(7) . ? C13B C18B 1.390(7) . ? C14B C15B 1.383(7) . ? C15B C16B 1.392(8) . ? C16B C17B 1.373(8) . ? C17B C18B 1.392(7) . ? C23B C28B 1.395(7) . ? C23B C24B 1.397(7) . ? C24B C25B 1.390(8) . ? C25B C26B 1.366(8) . ? C26B C27B 1.394(9) . ? C27B C28B 1.398(8) . ? 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 Te1 Sn 94.98(14) . . ? C7 Te2 Sn 93.77(15) . . ? C13 Sn C23 110.50(18) . . ? C13 Sn Te1 114.24(13) . . ? C23 Sn Te1 109.20(14) . . ? C13 Sn Te2 109.94(14) . . ? C23 Sn Te2 109.99(14) . . ? Te1 Sn Te2 102.685(15) . . ? C14 N1 C20 111.4(4) . . ? C14 N1 C19 112.9(4) . . ? C20 N1 C19 110.8(4) . . ? C22 N2 C18 112.6(5) . . ? C22 N2 C21 112.0(6) . . ? C18 N2 C21 113.4(5) . . ? C29 N3 C28 113.5(5) . . ? C29 N3 C30 111.8(5) . . ? C28 N3 C30 111.3(5) . . ? C24 N4 C31 114.0(4) . . ? C24 N4 C32 111.7(4) . . ? C31 N4 C32 110.6(4) . . ? C2 C1 C6 118.7(6) . . ? C2 C1 Te1 121.1(4) . . ? C6 C1 Te1 120.1(4) . . ? C1 C2 C3 121.0(6) . . ? C4 C3 C2 119.2(6) . . ? C5 C4 C3 119.4(7) . . ? C4 C5 C6 121.1(7) . . ? C1 C6 C5 120.5(6) . . ? C8 C7 C12 117.9(6) . . ? C8 C7 Te2 121.4(5) . . ? C12 C7 Te2 120.6(4) . . ? C7 C8 C9 120.5(7) . . ? C10 C9 C8 120.4(7) . . ? C11 C10 C9 119.8(7) . . ? C10 C11 C12 120.8(7) . . ? C7 C12 C11 120.6(6) . . ? C14 C13 C18 119.6(5) . . ? C14 C13 Sn 114.7(4) . . ? C18 C13 Sn 124.8(4) . . ? C15 C14 C13 120.2(5) . . ? C15 C14 N1 123.4(5) . . ? C13 C14 N1 116.5(4) . . ? C16 C15 C14 119.9(6) . . ? C15 C16 C17 120.6(5) . . ? C16 C17 C18 120.4(5) . . ? C17 C18 C13 119.3(5) . . ? C17 C18 N2 122.3(5) . . ? C13 C18 N2 118.4(5) . . ? C24 C23 C28 119.8(5) . . ? C24 C23 Sn 117.0(4) . . ? C28 C23 Sn 122.8(4) . . ? C23 C24 C25 120.3(5) . . ? C23 C24 N4 117.6(5) . . ? C25 C24 N4 122.0(5) . . ? C24 C25 C26 119.8(6) . . ? C27 C26 C25 120.0(6) . . ? C26 C27 C28 120.9(6) . . ? C23 C28 C27 119.1(5) . . ? C23 C28 N3 119.1(5) . . ? C27 C28 N3 121.7(5) . . ? C33 O C34 115.7(10) . . ? C37 C34 O 97.2(8) 2 . ? O C34 O 97.2(8) 2 . ? C37 C34 C35 122.7(7) 2 2 ? O C34 C35 122.7(7) 2 2 ? O C34 C35 121.5(7) . 2 ? C37 C34 C35 121.5(7) 2 . ? O C34 C35 121.5(7) 2 . ? O C34 C35 122.7(7) . . ? C35 C34 C35 73.0(12) 2 . ? C36 C35 C34 81.9(11) 2 . ? C1B Te1B Sn1B 96.00(14) . . ? C7B Te2B Sn1B 93.23(14) . . ? C23B Sn1B C13B 107.21(19) . . ? C23B Sn1B Te2B 109.48(13) . . ? C13B Sn1B Te2B 112.82(14) . . ? C23B Sn1B Te1B 110.66(14) . . ? C13B Sn1B Te1B 114.49(13) . . ? Te2B Sn1B Te1B 102.133(16) . . ? C14B N1B C19B 113.7(4) . . ? C14B N1B C20B 110.9(4) . . ? C19B N1B C20B 110.9(5) . . ? C21B N2B C18B 116.1(5) . . ? C21B N2B C22B 112.4(6) . . ? C18B N2B C22B 112.0(5) . . ? C28B N3B C29B 114.8(5) . . ? C28B N3B C30B 111.2(5) . . ? C29B N3B C30B 110.5(5) . . ? C31B N4B C24B 113.4(4) . . ? C31B N4B C32B 110.0(4) . . ? C24B N4B C32B 111.6(4) . . ? C6B C1B C2B 118.9(7) . . ? C6B C1B Te1B 120.8(5) . . ? C2B C1B Te1B 120.2(5) . . ? C1B C2B C3B 121.7(7) . . ? C2B C3B C4B 117.5(7) . . ? C5B C4B C3B 120.6(8) . . ? C4B C5B C6B 120.7(8) . . ? C1B C6B C5B 120.4(7) . . ? C12B C7B C8B 118.5(6) . . ? C12B C7B Te2B 121.3(4) . . ? C8B C7B Te2B 120.2(5) . . ? C7B C8B C9B 120.3(6) . . ? C10B C9B C8B 120.4(6) . . ? C11B C10B C9B 119.2(7) . . ? C10B C11B C12B 120.3(7) . . ? C7B C12B C11B 121.3(6) . . ? C14B C13B C18B 120.8(5) . . ? C14B C13B Sn1B 115.4(4) . . ? C18B C13B Sn1B 122.7(4) . . ? C13B C14B C15B 120.8(5) . . ? C13B C14B N1B 117.6(4) . . ? C15B C14B N1B 121.5(5) . . ? C14B C15B C16B 118.7(5) . . ? C17B C16B C15B 120.2(5) . . ? C16B C17B C18B 121.5(5) . . ? C13B C18B C17B 117.9(5) . . ? C13B C18B N2B 119.5(5) . . ? C17B C18B N2B 122.6(5) . . ? C28B C23B C24B 120.4(5) . . ? C28B C23B Sn1B 123.2(4) . . ? C24B C23B Sn1B 115.9(4) . . ? C25B C24B C23B 119.6(5) . . ? C25B C24B N4B 123.4(5) . . ? C23B C24B N4B 117.0(5) . . ? C26B C25B C24B 120.0(6) . . ? C25B C26B C27B 121.4(6) . . ? C26B C27B C28B 119.1(6) . . ? C23B C28B C27B 119.5(5) . . ? C23B C28B N3B 118.6(5) . . ? C27B C28B N3B 121.9(5) . . ? #===END data_(11)-sep1696 _database_code_depnum_ccdc_archive 'CCDC 710457' _audit_creation_date 2008-08-11T15:36:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C51 H69 B N4 Si2 Sn' _chemical_formula_moiety 'C27 H49 N4 Si2 Sn, C24 H20 B' _chemical_formula_weight 923.78 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.935(4) _cell_length_b 12.961(6) _cell_length_c 17.538(4) _cell_angle_alpha 99.51(3) _cell_angle_beta 96.56(2) _cell_angle_gamma 95.89(4) _cell_volume 2416.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.27 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 1.00 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_number 8478 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8478 _reflns_number_gt 7625 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+1.9024P] 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_number_reflns 8478 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.878 _refine_diff_density_min -1.572 _refine_diff_density_rms 0.103 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn 0.078450(19) 0.260414(16) 0.241330(13) 0.02185(10) Uani 1 1 d . . . Si1 Si 0.32282(9) 0.11445(7) 0.23241(6) 0.0263(2) Uani 1 1 d . . . Si2 Si 0.31041(10) 0.26379(8) 0.39682(6) 0.0313(2) Uani 1 1 d . . . B B -0.3757(3) 0.7055(3) 0.2343(2) 0.0224(8) Uani 1 1 d . . . N1 N -0.1275(3) 0.1213(2) 0.36542(19) 0.0334(7) Uani 1 1 d . . . N2 N 0.0344(3) 0.4378(2) 0.28220(18) 0.0287(6) Uani 1 1 d . . . N3 N -0.0672(3) 0.1201(2) 0.15567(18) 0.0276(6) Uani 1 1 d . . . N4 N 0.1675(3) 0.4191(3) 0.0868(2) 0.0404(8) Uani 1 1 d . . . C1 C 0.2620(3) 0.2347(3) 0.2869(2) 0.0243(7) Uani 1 1 d . . . H1 H 0.3136 0.2933 0.2705 0.029 Uiso 1 1 calc R . . C2 C 0.2472(3) -0.0134(3) 0.2499(2) 0.0337(8) Uani 1 1 d . . . H2A H 0.2565 -0.014 0.3061 0.051 Uiso 1 1 calc R . . H2B H 0.2865 -0.0713 0.2235 0.051 Uiso 1 1 calc R . . H2C H 0.1588 -0.022 0.2295 0.051 Uiso 1 1 calc R . . C3 C 0.4933(3) 0.1194(3) 0.2617(3) 0.0396(9) Uani 1 1 d . . . H3A H 0.5359 0.1858 0.2529 0.059 Uiso 1 1 calc R . . H3B H 0.5242 0.0601 0.2305 0.059 Uiso 1 1 calc R . . H3C H 0.5094 0.1148 0.3171 0.059 Uiso 1 1 calc R . . C4 C 0.3042(4) 0.1144(3) 0.1254(2) 0.0363(9) Uani 1 1 d . . . H4A H 0.3435 0.1816 0.1156 0.054 Uiso 1 1 calc R . . H4B H 0.2157 0.1053 0.1051 0.054 Uiso 1 1 calc R . . H4C H 0.3436 0.0564 0.0991 0.054 Uiso 1 1 calc R . . C5 C 0.3276(5) 0.1428(4) 0.4381(2) 0.0470(11) Uani 1 1 d . . . H5A H 0.3834 0.1011 0.4096 0.071 Uiso 1 1 calc R . . H5B H 0.2463 0.101 0.4332 0.071 Uiso 1 1 calc R . . H5C H 0.3624 0.1621 0.4933 0.071 Uiso 1 1 calc R . . C6 C 0.2042(5) 0.3329(4) 0.4576(2) 0.0466(11) Uani 1 1 d . . . H6A H 0.1896 0.3989 0.4398 0.07 Uiso 1 1 calc R . . H6B H 0.242 0.3484 0.5123 0.07 Uiso 1 1 calc R . . H6C H 0.1251 0.2878 0.4527 0.07 Uiso 1 1 calc R . . C7 C 0.4610(5) 0.3519(5) 0.4137(3) 0.0651(15) Uani 1 1 d . . . H7A H 0.5203 0.3183 0.383 0.098 Uiso 1 1 calc R . . H7B H 0.4941 0.3642 0.4692 0.098 Uiso 1 1 calc R . . H7C H 0.4476 0.4193 0.3979 0.098 Uiso 1 1 calc R . . C8 C -0.0469(3) 0.2854(3) 0.3258(2) 0.0247(7) Uani 1 1 d . . . C9 C -0.1180(3) 0.2304(3) 0.3720(2) 0.0288(7) Uani 1 1 d . . . C10 C -0.1853(4) 0.2900(3) 0.4235(2) 0.0357(9) Uani 1 1 d . . . H10 H -0.2362 0.2552 0.4542 0.043 Uiso 1 1 calc R . . C11 C -0.1783(4) 0.3984(3) 0.4299(2) 0.0419(10) Uani 1 1 d . . . H11 H -0.2244 0.4363 0.4654 0.05 Uiso 1 1 calc R . . C12 C -0.1065(4) 0.4533(3) 0.3865(2) 0.0375(9) Uani 1 1 d . . . H12 H -0.101 0.5278 0.3916 0.045 Uiso 1 1 calc R . . C13 C -0.0426(3) 0.3939(3) 0.3348(2) 0.0288(8) Uani 1 1 d . . . C14 C -0.0210(5) 0.0679(3) 0.3514(3) 0.0523(12) Uani 1 1 d . . . H14A H -0.0429 -0.0081 0.3483 0.079 Uiso 1 1 calc R . . H14B H 0.0464 0.0942 0.3942 0.079 Uiso 1 1 calc R . . H14C H 0.0061 0.0811 0.3022 0.079 Uiso 1 1 calc R . . C15 C -0.2052(4) 0.0713(3) 0.4146(2) 0.0407(9) Uani 1 1 d . . . H15A H -0.2031 -0.0051 0.4039 0.061 Uiso 1 1 calc R . . H15B H -0.2907 0.0865 0.4033 0.061 Uiso 1 1 calc R . . H15C H -0.174 0.099 0.4696 0.061 Uiso 1 1 calc R . . C16 C -0.0445(4) 0.4752(3) 0.2196(2) 0.0371(9) Uani 1 1 d . . . H16A H 0.0084 0.5047 0.1849 0.056 Uiso 1 1 calc R . . H16B H -0.0914 0.5297 0.2433 0.056 Uiso 1 1 calc R . . H16C H -0.1023 0.4159 0.1894 0.056 Uiso 1 1 calc R . . C17 C 0.1294(4) 0.5250(3) 0.3233(3) 0.0448(10) Uani 1 1 d . . . H17A H 0.1778 0.5519 0.2855 0.067 Uiso 1 1 calc R . . H17B H 0.1847 0.499 0.3618 0.067 Uiso 1 1 calc R . . H17C H 0.0885 0.5819 0.3498 0.067 Uiso 1 1 calc R . . C18 C 0.0464(3) 0.2665(3) 0.1193(2) 0.0269(7) Uani 1 1 d . . . C19 C -0.0404(3) 0.1777(3) 0.0931(2) 0.0277(7) Uani 1 1 d . . . C20 C -0.0969(4) 0.1480(3) 0.0174(2) 0.0382(9) Uani 1 1 d . . . H20 H -0.1562 0.087 0.0017 0.046 Uiso 1 1 calc R . . C21 C -0.0629(4) 0.2113(4) -0.0347(2) 0.0448(10) Uani 1 1 d . . . H21 H -0.1003 0.1939 -0.0875 0.054 Uiso 1 1 calc R . . C22 C 0.0237(4) 0.2990(3) -0.0118(2) 0.0401(9) Uani 1 1 d . . . H22 H 0.0449 0.34 -0.0496 0.048 Uiso 1 1 calc R . . C23 C 0.0818(4) 0.3299(3) 0.0651(2) 0.0344(8) Uani 1 1 d . . . C24 C -0.1962(3) 0.1280(3) 0.1728(2) 0.0324(8) Uani 1 1 d . . . H24A H -0.2125 0.0889 0.2146 0.049 Uiso 1 1 calc R . . H24B H -0.2546 0.098 0.1258 0.049 Uiso 1 1 calc R . . H24C H -0.2067 0.2022 0.1892 0.049 Uiso 1 1 calc R . . C25 C -0.0480(4) 0.0077(3) 0.1359(3) 0.0366(9) Uani 1 1 d . . . H25A H -0.067 -0.0284 0.1788 0.055 Uiso 1 1 calc R . . H25B H 0.0385 0.0029 0.1277 0.055 Uiso 1 1 calc R . . H25C H -0.1029 -0.0257 0.0882 0.055 Uiso 1 1 calc R . . C26 C 0.2049(6) 0.4755(5) 0.0260(3) 0.0735(17) Uani 1 1 d . . . H26A H 0.2661 0.5362 0.0496 0.11 Uiso 1 1 calc R . . H26B H 0.1321 0.4999 -0.0001 0.11 Uiso 1 1 calc R . . H26C H 0.2414 0.4281 -0.0121 0.11 Uiso 1 1 calc R . . C27 C 0.2652(4) 0.4243(4) 0.1516(3) 0.0564(13) Uani 1 1 d . . . H27A H 0.3185 0.4918 0.1592 0.085 Uiso 1 1 calc R . . H27B H 0.3149 0.3663 0.1401 0.085 Uiso 1 1 calc R . . H27C H 0.228 0.4185 0.1992 0.085 Uiso 1 1 calc R . . C28 C -0.3895(3) 0.5777(3) 0.2037(2) 0.0236(7) Uani 1 1 d . . . C29 C -0.4146(3) 0.5296(3) 0.1254(2) 0.0294(8) Uani 1 1 d . . . H29 H -0.4291 0.5727 0.0873 0.035 Uiso 1 1 calc R . . C30 C -0.4194(4) 0.4217(3) 0.1006(2) 0.0356(9) Uani 1 1 d . . . H30 H -0.4371 0.3927 0.0465 0.043 Uiso 1 1 calc R . . C31 C -0.3984(4) 0.3565(3) 0.1542(2) 0.0359(9) Uani 1 1 d . . . H31 H -0.4021 0.2825 0.1376 0.043 Uiso 1 1 calc R . . C32 C -0.3716(4) 0.4011(3) 0.2327(2) 0.0342(8) Uani 1 1 d . . . H32 H -0.3566 0.3576 0.2705 0.041 Uiso 1 1 calc R . . C33 C -0.3668(3) 0.5087(3) 0.2557(2) 0.0308(8) Uani 1 1 d . . . H33 H -0.347 0.5373 0.3097 0.037 Uiso 1 1 calc R . . C34 C -0.2281(3) 0.7403(2) 0.2677(2) 0.0226(7) Uani 1 1 d . . . C35 C -0.1834(3) 0.7650(3) 0.3471(2) 0.0296(8) Uani 1 1 d . . . H35 H -0.2414 0.7678 0.3836 0.035 Uiso 1 1 calc R . . C36 C -0.0572(4) 0.7857(3) 0.3751(3) 0.0397(9) Uani 1 1 d . . . H36 H -0.0309 0.8 0.4298 0.048 Uiso 1 1 calc R . . C37 C 0.0298(3) 0.7855(3) 0.3242(3) 0.0375(9) Uani 1 1 d . . . H37 H 0.1157 0.8019 0.343 0.045 Uiso 1 1 calc R . . C38 C -0.0112(4) 0.7610(3) 0.2451(3) 0.0374(9) Uani 1 1 d . . . H38 H 0.0474 0.76 0.209 0.045 Uiso 1 1 calc R . . C39 C -0.1364(3) 0.7378(3) 0.2178(2) 0.0319(8) Uani 1 1 d . . . H39 H -0.1613 0.7196 0.1631 0.038 Uiso 1 1 calc R . . C40 C -0.4609(3) 0.7403(3) 0.30314(19) 0.0251(7) Uani 1 1 d . . . C41 C -0.5428(3) 0.6748(3) 0.3338(2) 0.0357(9) Uani 1 1 d . . . H41 H -0.5504 0.6008 0.3158 0.043 Uiso 1 1 calc R . . C42 C -0.6144(4) 0.7141(4) 0.3902(2) 0.0473(11) Uani 1 1 d . . . H42 H -0.6701 0.6666 0.4096 0.057 Uiso 1 1 calc R . . C43 C -0.6057(4) 0.8200(4) 0.4182(2) 0.0434(10) Uani 1 1 d . . . H43 H -0.6548 0.8464 0.4565 0.052 Uiso 1 1 calc R . . C44 C -0.5241(4) 0.8876(3) 0.3896(2) 0.0408(10) Uani 1 1 d . . . H44 H -0.5156 0.9613 0.4088 0.049 Uiso 1 1 calc R . . C45 C -0.4551(4) 0.8482(3) 0.3332(2) 0.0319(8) Uani 1 1 d . . . H45 H -0.4007 0.8964 0.3136 0.038 Uiso 1 1 calc R . . C46 C -0.4268(3) 0.7645(3) 0.1630(2) 0.0247(7) Uani 1 1 d . . . C47 C -0.5515(3) 0.7409(3) 0.1303(2) 0.0345(8) Uani 1 1 d . . . H47 H -0.6035 0.6922 0.151 0.041 Uiso 1 1 calc R . . C48 C -0.6029(4) 0.7851(3) 0.0692(2) 0.0420(10) Uani 1 1 d . . . H48 H -0.688 0.7662 0.0489 0.05 Uiso 1 1 calc R . . C49 C -0.5310(4) 0.8555(3) 0.0383(2) 0.0415(10) Uani 1 1 d . . . H49 H -0.5649 0.8851 -0.0043 0.05 Uiso 1 1 calc R . . C50 C -0.4096(5) 0.8829(3) 0.0695(2) 0.0466(11) Uani 1 1 d . . . H50 H -0.3591 0.9331 0.0492 0.056 Uiso 1 1 calc R . . C51 C -0.3592(4) 0.8382(3) 0.1305(2) 0.0379(9) Uani 1 1 d . . . H51 H -0.2744 0.859 0.1509 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn 0.01697(14) 0.01852(14) 0.03138(15) 0.00750(9) 0.00462(9) 0.00199(9) Si1 0.0193(5) 0.0250(5) 0.0360(5) 0.0063(4) 0.0062(4) 0.0047(4) Si2 0.0310(5) 0.0301(5) 0.0316(5) 0.0058(4) -0.0023(4) 0.0047(4) B 0.0235(19) 0.0190(18) 0.0249(18) 0.0043(14) 0.0058(15) 0.0006(14) N1 0.0357(17) 0.0228(15) 0.0449(18) 0.0079(13) 0.0178(14) 0.0023(13) N2 0.0249(15) 0.0193(14) 0.0423(17) 0.0089(12) 0.0011(13) 0.0022(12) N3 0.0173(14) 0.0261(15) 0.0410(17) 0.0077(13) 0.0087(12) 0.0019(11) N4 0.0387(19) 0.0416(19) 0.047(2) 0.0228(16) 0.0148(16) -0.0007(15) C1 0.0209(16) 0.0230(17) 0.0295(17) 0.0061(14) 0.0034(13) 0.0026(13) C2 0.0270(19) 0.0300(19) 0.045(2) 0.0086(16) 0.0072(16) 0.0043(15) C3 0.0242(19) 0.037(2) 0.060(3) 0.0122(19) 0.0090(18) 0.0065(16) C4 0.031(2) 0.041(2) 0.037(2) 0.0035(17) 0.0095(16) 0.0064(17) C5 0.061(3) 0.045(2) 0.040(2) 0.0126(19) 0.004(2) 0.026(2) C6 0.061(3) 0.043(2) 0.033(2) -0.0030(18) -0.0040(19) 0.022(2) C7 0.050(3) 0.073(4) 0.058(3) 0.005(3) -0.016(2) -0.022(3) C8 0.0229(17) 0.0190(16) 0.0324(18) 0.0020(13) 0.0047(14) 0.0062(13) C9 0.0254(18) 0.0243(18) 0.0351(19) 0.0008(15) 0.0054(15) 0.0019(14) C10 0.040(2) 0.036(2) 0.0326(19) 0.0028(16) 0.0147(17) 0.0051(17) C11 0.048(2) 0.035(2) 0.042(2) -0.0050(17) 0.0151(19) 0.0137(18) C12 0.044(2) 0.0234(18) 0.043(2) -0.0033(16) 0.0027(18) 0.0120(16) C13 0.0263(18) 0.0227(17) 0.0361(19) 0.0050(15) -0.0005(15) 0.0028(14) C14 0.056(3) 0.033(2) 0.084(3) 0.024(2) 0.043(3) 0.016(2) C15 0.040(2) 0.034(2) 0.050(2) 0.0089(18) 0.0208(19) -0.0021(17) C16 0.031(2) 0.032(2) 0.055(2) 0.0207(18) 0.0058(18) 0.0107(16) C17 0.042(2) 0.025(2) 0.064(3) 0.0091(19) -0.001(2) -0.0037(17) C18 0.0173(16) 0.0303(18) 0.0361(19) 0.0108(15) 0.0065(14) 0.0057(14) C19 0.0202(17) 0.0309(18) 0.0337(19) 0.0058(15) 0.0064(14) 0.0078(14) C20 0.032(2) 0.040(2) 0.041(2) 0.0017(17) 0.0047(17) 0.0050(17) C21 0.045(2) 0.056(3) 0.034(2) 0.0048(19) 0.0047(18) 0.016(2) C22 0.045(2) 0.045(2) 0.038(2) 0.0161(18) 0.0158(18) 0.0170(19) C23 0.0299(19) 0.036(2) 0.043(2) 0.0141(17) 0.0137(16) 0.0091(16) C24 0.0154(17) 0.039(2) 0.042(2) 0.0057(17) 0.0070(15) -0.0005(15) C25 0.030(2) 0.0240(18) 0.056(2) 0.0047(17) 0.0091(17) 0.0031(15) C26 0.099(5) 0.065(3) 0.058(3) 0.032(3) 0.018(3) -0.025(3) C27 0.036(2) 0.056(3) 0.081(3) 0.033(3) 0.004(2) -0.010(2) C28 0.0177(16) 0.0207(16) 0.0335(18) 0.0058(14) 0.0081(13) 0.0003(12) C29 0.0325(19) 0.0264(18) 0.0316(18) 0.0071(15) 0.0100(15) 0.0048(15) C30 0.035(2) 0.034(2) 0.036(2) -0.0018(16) 0.0079(16) 0.0029(16) C31 0.032(2) 0.0211(18) 0.052(2) 0.0011(16) 0.0062(17) 0.0008(15) C32 0.040(2) 0.0243(18) 0.039(2) 0.0131(16) 0.0029(17) -0.0002(16) C33 0.034(2) 0.0288(19) 0.0293(18) 0.0088(15) 0.0014(15) -0.0002(15) C34 0.0239(17) 0.0129(15) 0.0326(18) 0.0077(13) 0.0070(14) 0.0012(12) C35 0.0242(18) 0.0292(18) 0.0366(19) 0.0112(15) 0.0020(15) 0.0033(14) C36 0.031(2) 0.035(2) 0.050(2) 0.0116(18) -0.0081(18) 0.0022(16) C37 0.0198(18) 0.0247(19) 0.068(3) 0.0147(18) -0.0011(18) 0.0000(14) C38 0.0261(19) 0.0293(19) 0.063(3) 0.0169(18) 0.0183(18) 0.0030(15) C39 0.0293(19) 0.0284(19) 0.039(2) 0.0066(16) 0.0106(16) 0.0026(15) C40 0.0185(16) 0.0314(18) 0.0258(17) 0.0069(14) 0.0006(13) 0.0047(13) C41 0.029(2) 0.042(2) 0.033(2) 0.0021(17) 0.0069(16) -0.0066(16) C42 0.027(2) 0.076(3) 0.033(2) 0.001(2) 0.0127(17) -0.013(2) C43 0.026(2) 0.073(3) 0.030(2) -0.002(2) 0.0070(16) 0.014(2) C44 0.044(2) 0.044(2) 0.038(2) 0.0045(18) 0.0057(18) 0.0247(19) C45 0.034(2) 0.0309(19) 0.0346(19) 0.0096(15) 0.0069(16) 0.0133(16) C46 0.0249(17) 0.0198(16) 0.0288(17) 0.0015(13) 0.0042(14) 0.0038(13) C47 0.0266(19) 0.036(2) 0.044(2) 0.0140(17) 0.0067(16) 0.0067(16) C48 0.035(2) 0.044(2) 0.046(2) 0.0068(19) -0.0047(18) 0.0142(18) C49 0.060(3) 0.030(2) 0.034(2) 0.0075(16) -0.0080(19) 0.0152(19) C50 0.064(3) 0.036(2) 0.038(2) 0.0172(18) -0.005(2) -0.010(2) C51 0.038(2) 0.036(2) 0.037(2) 0.0134(17) -0.0063(17) -0.0103(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn C8 2.140(3) . ? Sn C18 2.144(4) . ? Sn C1 2.153(3) . ? Sn N2 2.407(3) . ? Sn N3 2.462(3) . ? Si1 C2 1.862(4) . ? Si1 C4 1.865(4) . ? Si1 C3 1.868(4) . ? Si1 C1 1.911(4) . ? Si2 C5 1.850(4) . ? Si2 C6 1.863(4) . ? Si2 C7 1.869(5) . ? Si2 C1 1.903(4) . ? B C40 1.641(5) . ? B C28 1.641(5) . ? B C34 1.643(5) . ? B C46 1.645(5) . ? N1 C9 1.392(5) . ? N1 C14 1.439(5) . ? N1 C15 1.457(5) . ? N2 C13 1.462(5) . ? N2 C17 1.481(5) . ? N2 C16 1.494(5) . ? N3 C19 1.466(5) . ? N3 C25 1.482(5) . ? N3 C24 1.485(4) . ? N4 C23 1.382(5) . ? N4 C27 1.457(6) . ? N4 C26 1.460(5) . ? C8 C13 1.384(5) . ? C8 C9 1.411(5) . ? C9 C10 1.411(5) . ? C10 C11 1.385(6) . ? C11 C12 1.380(6) . ? C12 C13 1.388(5) . ? C18 C19 1.392(5) . ? C18 C23 1.416(5) . ? C19 C20 1.374(5) . ? C20 C21 1.382(6) . ? C21 C22 1.375(6) . ? C22 C23 1.399(6) . ? C28 C29 1.395(5) . ? C28 C33 1.399(5) . ? C29 C30 1.388(5) . ? C30 C31 1.380(6) . ? C31 C32 1.387(6) . ? C32 C33 1.380(5) . ? C34 C35 1.394(5) . ? C34 C39 1.405(5) . ? C35 C36 1.395(5) . ? C36 C37 1.376(6) . ? C37 C38 1.383(6) . ? C38 C39 1.383(5) . ? C40 C41 1.385(5) . ? C40 C45 1.402(5) . ? C41 C42 1.395(6) . ? C42 C43 1.369(7) . ? C43 C44 1.378(6) . ? C44 C45 1.376(5) . ? C46 C51 1.383(5) . ? C46 C47 1.401(5) . ? C47 C48 1.386(5) . ? C48 C49 1.363(6) . ? C49 C50 1.364(6) . ? C50 C51 1.386(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Sn C18 127.95(13) . . ? C8 Sn C1 115.23(13) . . ? C18 Sn C1 116.73(13) . . ? C8 Sn N2 62.23(12) . . ? C18 Sn N2 94.23(12) . . ? C1 Sn N2 113.11(12) . . ? C8 Sn N3 92.98(11) . . ? C18 Sn N3 61.69(12) . . ? C1 Sn N3 122.19(11) . . ? N2 Sn N3 124.70(10) . . ? C2 Si1 C4 108.94(19) . . ? C2 Si1 C3 107.52(18) . . ? C4 Si1 C3 105.15(19) . . ? C2 Si1 C1 113.54(16) . . ? C4 Si1 C1 110.79(17) . . ? C3 Si1 C1 110.51(18) . . ? C5 Si2 C6 103.7(2) . . ? C5 Si2 C7 110.7(2) . . ? C6 Si2 C7 106.6(3) . . ? C5 Si2 C1 112.53(18) . . ? C6 Si2 C1 117.07(17) . . ? C7 Si2 C1 106.1(2) . . ? C40 B C28 113.5(3) . . ? C40 B C34 109.9(3) . . ? C28 B C34 105.4(3) . . ? C40 B C46 104.1(3) . . ? C28 B C46 110.1(3) . . ? C34 B C46 114.1(3) . . ? C9 N1 C14 119.6(3) . . ? C9 N1 C15 118.3(3) . . ? C14 N1 C15 112.5(3) . . ? C13 N2 C17 112.8(3) . . ? C13 N2 C16 110.4(3) . . ? C17 N2 C16 109.6(3) . . ? C13 N2 Sn 86.16(19) . . ? C17 N2 Sn 123.6(2) . . ? C16 N2 Sn 111.9(2) . . ? C19 N3 C25 111.7(3) . . ? C19 N3 C24 110.6(3) . . ? C25 N3 C24 109.8(3) . . ? C19 N3 Sn 85.29(19) . . ? C25 N3 Sn 126.0(2) . . ? C24 N3 Sn 110.7(2) . . ? C23 N4 C27 119.4(3) . . ? C23 N4 C26 118.4(4) . . ? C27 N4 C26 113.7(4) . . ? Si2 C1 Si1 115.27(17) . . ? Si2 C1 Sn 118.98(17) . . ? Si1 C1 Sn 115.10(17) . . ? C13 C8 C9 119.4(3) . . ? C13 C8 Sn 99.4(2) . . ? C9 C8 Sn 141.1(2) . . ? N1 C9 C8 122.3(3) . . ? N1 C9 C10 120.4(3) . . ? C8 C9 C10 117.2(3) . . ? C11 C10 C9 121.1(4) . . ? C12 C11 C10 122.1(4) . . ? C11 C12 C13 116.5(3) . . ? C8 C13 C12 123.7(4) . . ? C8 C13 N2 112.1(3) . . ? C12 C13 N2 124.2(3) . . ? C19 C18 C23 118.8(3) . . ? C19 C18 Sn 100.4(2) . . ? C23 C18 Sn 140.7(3) . . ? C20 C19 C18 124.1(4) . . ? C20 C19 N3 123.3(3) . . ? C18 C19 N3 112.5(3) . . ? C19 C20 C21 116.5(4) . . ? C22 C21 C20 121.5(4) . . ? C21 C22 C23 122.4(4) . . ? N4 C23 C22 121.2(4) . . ? N4 C23 C18 122.2(4) . . ? C22 C23 C18 116.6(4) . . ? C29 C28 C33 114.6(3) . . ? C29 C28 B 124.1(3) . . ? C33 C28 B 121.1(3) . . ? C30 C29 C28 123.1(3) . . ? C31 C30 C29 120.2(4) . . ? C30 C31 C32 118.7(3) . . ? C33 C32 C31 119.9(3) . . ? C32 C33 C28 123.5(3) . . ? C35 C34 C39 115.1(3) . . ? C35 C34 B 123.0(3) . . ? C39 C34 B 121.7(3) . . ? C36 C35 C34 122.7(4) . . ? C37 C36 C35 120.5(4) . . ? C36 C37 C38 118.3(3) . . ? C37 C38 C39 120.8(4) . . ? C38 C39 C34 122.5(4) . . ? C41 C40 C45 115.2(3) . . ? C41 C40 B 127.1(3) . . ? C45 C40 B 117.7(3) . . ? C40 C41 C42 121.9(4) . . ? C43 C42 C41 120.9(4) . . ? C42 C43 C44 118.7(4) . . ? C45 C44 C43 119.9(4) . . ? C44 C45 C40 123.2(4) . . ? C51 C46 C47 114.2(3) . . ? C51 C46 B 126.9(3) . . ? C47 C46 B 118.9(3) . . ? C48 C47 C46 123.2(4) . . ? C49 C48 C47 119.9(4) . . ? C48 C49 C50 119.0(4) . . ? C49 C50 C51 120.6(4) . . ? C46 C51 C50 123.0(4) . . ? #===END