data_publication_text _publ_requested_journal 'Chemistry of Materials' _publ_contact_author_name 'Matthias Driess' _publ_contact_author_address ;Technische Universitaet Berlin, Institute of Chemistry Strasse des 17. Juni 136, D-10623 Berlin, Germany ; _publ_contact_author_email matthias.driess@tu-berlin.de _publ_contact_author_phone +49(0)30-314-29731 _publ_contact_author_fax +49(0)30-314-29732 loop_ _publ_author_name _publ_author_address ' Driess, Matthias' ;Technische Universitaet Berlin, Institute of Chemistry Strasse des 17. Juni 136, D-10623 Berlin, Germany ; 'Tsaroucha, Marianna' ;Technische Universitaet Berlin, Institute of Chemistry Strasse des 17. Juni 136, D-10623 Berlin, Germany ; 'Aksu, Yilmaz' ;Technische Universitaet Berlin, Institute of Chemistry Strasse des 17. Juni 136, D-10623 Berlin, Germany ; data_tsar3 _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H64 O4 Sn4 Zn4' _chemical_formula_weight 1189.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.3691(8) _cell_length_b 11.2041(6) _cell_length_c 17.6065(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.148(7) _cell_angle_gamma 90.00 _cell_volume 2200.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9832 _cell_measurement_theta_min 2.9806 _cell_measurement_theta_max 28.8806 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 4.396 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.2537 _exptl_absorpt_correction_T_max 0.6435 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14024 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7005 _reflns_number_gt 6161 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0782P)^2^+24.5649P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(4) _refine_ls_number_reflns 7005 _refine_ls_number_parameters 367 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.55060(9) 0.31633(9) 0.08316(6) 0.0315(3) Uani 1 1 d . . . Sn2 Sn 0.75673(11) 0.73907(9) 0.29708(6) 0.0370(3) Uani 1 1 d . . . Sn3 Sn 0.86489(12) 0.21784(10) 0.38999(6) 0.0411(3) Uani 1 1 d . . . Sn4 Sn 1.07576(11) 0.44726(11) 0.13402(7) 0.0415(3) Uani 1 1 d . . . Zn1 Zn 0.93785(17) 0.48556(15) 0.29778(11) 0.0347(5) Uani 1 1 d . . . Zn2 Zn 0.84314(16) 0.28610(15) 0.19009(10) 0.0302(4) Uani 1 1 d . . . Zn3 Zn 0.77599(16) 0.54020(16) 0.14484(10) 0.0288(4) Uani 1 1 d . . . Zn4 Zn 0.67733(16) 0.42332(16) 0.27221(10) 0.0294(4) Uani 1 1 d . . . O1 O 0.6880(8) 0.3834(9) 0.1594(5) 0.024(2) Uani 1 1 d . . . O2 O 0.7753(9) 0.5709(8) 0.2603(5) 0.025(2) Uani 1 1 d . . . O3 O 0.8390(10) 0.3350(9) 0.3024(5) 0.030(2) Uani 1 1 d . . . O4 O 0.9309(8) 0.4443(10) 0.1825(5) 0.026(2) Uani 1 1 d . . . C1 C 1.074(2) 0.552(2) 0.3699(16) 0.081(9) Uani 1 1 d . . . H1A H 1.1197 0.6006 0.3390 0.097 Uiso 1 1 calc R . . H1B H 1.0405 0.6077 0.4039 0.097 Uiso 1 1 calc R . . C2 C 1.160(3) 0.476(3) 0.4203(15) 0.090(9) Uani 1 1 d . . . H2A H 1.1205 0.4365 0.4582 0.135 Uiso 1 1 calc R . . H2B H 1.2263 0.5253 0.4474 0.135 Uiso 1 1 calc R . . H2C H 1.1912 0.4158 0.3891 0.135 Uiso 1 1 calc R . . C3 C 0.888(2) 0.1281(17) 0.1522(12) 0.066(7) Uani 1 1 d . . . H3A H 0.9410 0.1456 0.1153 0.079 Uiso 1 1 calc R . . H3B H 0.9386 0.0890 0.1974 0.079 Uiso 1 1 calc R . . C4 C 0.809(3) 0.040(3) 0.117(2) 0.114(12) Uani 1 1 d . . . H4A H 0.7426 0.0319 0.1450 0.170 Uiso 1 1 calc R . . H4B H 0.8513 -0.0360 0.1179 0.170 Uiso 1 1 calc R . . H4C H 0.7767 0.0630 0.0632 0.170 Uiso 1 1 calc R . . C5 C 0.7326(18) 0.6555(18) 0.0586(11) 0.051(5) Uani 1 1 d . . . H5A H 0.6440 0.6589 0.0441 0.061 Uiso 1 1 calc R . . H5B H 0.7607 0.7356 0.0778 0.061 Uiso 1 1 calc R . . C6 C 0.782(3) 0.630(2) -0.0141(12) 0.073(7) Uani 1 1 d . . . H6A H 0.8687 0.6422 -0.0033 0.110 Uiso 1 1 calc R . . H6B H 0.7443 0.6842 -0.0555 0.110 Uiso 1 1 calc R . . H6C H 0.7636 0.5473 -0.0303 0.110 Uiso 1 1 calc R . . C7 C 0.5329(15) 0.4083(17) 0.3189(11) 0.042(4) Uani 1 1 d . . . H7A H 0.4828 0.3427 0.2923 0.050 Uiso 1 1 calc R . . H7B H 0.5587 0.3849 0.3738 0.050 Uiso 1 1 calc R . . C8 C 0.457(2) 0.518(3) 0.3157(16) 0.079(8) Uani 1 1 d . . . H8A H 0.5020 0.5811 0.3468 0.119 Uiso 1 1 calc R . . H8B H 0.3845 0.4993 0.3363 0.119 Uiso 1 1 calc R . . H8C H 0.4333 0.5445 0.2619 0.119 Uiso 1 1 calc R . . C9 C 0.5053(18) 0.1551(18) 0.1396(11) 0.049(5) Uani 1 1 d . . . H9A H 0.5482 0.0871 0.1229 0.074 Uiso 1 1 calc R . . H9B H 0.4187 0.1411 0.1256 0.074 Uiso 1 1 calc R . . H9C H 0.5286 0.1643 0.1959 0.074 Uiso 1 1 calc R . . C10 C 0.4159(18) 0.4492(18) 0.0766(12) 0.056(5) Uani 1 1 d . . . H10A H 0.4068 0.4714 0.1290 0.084 Uiso 1 1 calc R . . H10B H 0.3397 0.4180 0.0478 0.084 Uiso 1 1 calc R . . H10C H 0.4391 0.5197 0.0500 0.084 Uiso 1 1 calc R . . C11 C 0.619(2) 0.3006(17) -0.0205(10) 0.050(5) Uani 1 1 d . . . H11A H 0.6956 0.3429 -0.0145 0.075 Uiso 1 1 calc R . . H11B H 0.5617 0.3357 -0.0635 0.075 Uiso 1 1 calc R . . H11C H 0.6308 0.2162 -0.0312 0.075 Uiso 1 1 calc R . . C12 C 0.5995(14) 0.8049(18) 0.2248(10) 0.043(4) Uani 1 1 d . . . H12A H 0.6064 0.7960 0.1704 0.064 Uiso 1 1 calc R . . H12B H 0.5894 0.8895 0.2361 0.064 Uiso 1 1 calc R . . H12C H 0.5299 0.7598 0.2342 0.064 Uiso 1 1 calc R . . C13 C 0.9174(19) 0.827(2) 0.2763(15) 0.066(6) Uani 1 1 d . . . H13A H 0.9879 0.7798 0.2987 0.099 Uiso 1 1 calc R . . H13B H 0.9237 0.9066 0.3004 0.099 Uiso 1 1 calc R . . H13C H 0.9132 0.8357 0.2204 0.099 Uiso 1 1 calc R . . C14 C 0.751(2) 0.719(2) 0.4161(10) 0.073(7) Uani 1 1 d . . . H14A H 0.6860 0.6645 0.4218 0.110 Uiso 1 1 calc R . . H14B H 0.7367 0.7972 0.4380 0.110 Uiso 1 1 calc R . . H14C H 0.8275 0.6870 0.4437 0.110 Uiso 1 1 calc R . . C15 C 0.731(2) 0.0920(19) 0.3581(13) 0.060(6) Uani 1 1 d . . . H15A H 0.6541 0.1252 0.3652 0.090 Uiso 1 1 calc R . . H15B H 0.7495 0.0206 0.3905 0.090 Uiso 1 1 calc R . . H15C H 0.7259 0.0705 0.3037 0.090 Uiso 1 1 calc R . . C16 C 0.852(3) 0.324(2) 0.4871(12) 0.084(9) Uani 1 1 d . . . H16A H 0.8043 0.3955 0.4700 0.126 Uiso 1 1 calc R . . H16B H 0.9323 0.3476 0.5136 0.126 Uiso 1 1 calc R . . H16C H 0.8128 0.2781 0.5226 0.126 Uiso 1 1 calc R . . C17 C 1.040(2) 0.1446(18) 0.3879(14) 0.069(7) Uani 1 1 d . . . H17A H 1.0384 0.1040 0.3385 0.104 Uiso 1 1 calc R . . H17B H 1.0618 0.0875 0.4305 0.104 Uiso 1 1 calc R . . H17C H 1.0992 0.2092 0.3940 0.104 Uiso 1 1 calc R . . C18 C 1.011(2) 0.389(3) 0.0182(13) 0.081(8) Uani 1 1 d . . . H18A H 0.9358 0.3450 0.0158 0.122 Uiso 1 1 calc R . . H18B H 1.0706 0.3369 0.0018 0.122 Uiso 1 1 calc R . . H18C H 0.9966 0.4585 -0.0162 0.122 Uiso 1 1 calc R . . C19 C 1.137(2) 0.626(2) 0.1366(15) 0.068(7) Uani 1 1 d . . . H19A H 1.0777 0.6748 0.1028 0.102 Uiso 1 1 calc R . . H19B H 1.2134 0.6284 0.1184 0.102 Uiso 1 1 calc R . . H19C H 1.1491 0.6560 0.1897 0.102 Uiso 1 1 calc R . . C20 C 1.1907(15) 0.3263(19) 0.2083(13) 0.055(5) Uani 1 1 d . . . H20A H 1.2234 0.3662 0.2574 0.083 Uiso 1 1 calc R . . H20B H 1.2565 0.3015 0.1832 0.083 Uiso 1 1 calc R . . H20C H 1.1446 0.2561 0.2182 0.083 Uiso 1 1 calc R . . C21 C 0.327(3) 0.955(3) 0.3114(17) 0.119(7) Uani 1 1 d DU . . C22 C 0.347(3) 1.069(3) 0.3401(18) 0.118(7) Uani 1 1 d DU . . H22 H 0.3108 1.1362 0.3114 0.142 Uiso 1 1 calc R . . C23 C 0.420(3) 1.084(3) 0.412(2) 0.140(8) Uani 1 1 d DU . . H23 H 0.4435 1.1612 0.4304 0.169 Uiso 1 1 calc R . . C24 C 0.459(3) 0.984(3) 0.4554(18) 0.146(9) Uani 1 1 d DU . . H24 H 0.5043 0.9939 0.5062 0.175 Uiso 1 1 calc R . . C25 C 0.432(3) 0.872(3) 0.427(2) 0.145(9) Uani 1 1 d DU . . H25 H 0.4634 0.8045 0.4568 0.174 Uiso 1 1 calc R . . C26 C 0.361(3) 0.855(3) 0.3550(19) 0.132(8) Uani 1 1 d DU . . H26 H 0.3365 0.7770 0.3364 0.159 Uiso 1 1 calc R . . C27 C 0.256(4) 0.936(5) 0.232(2) 0.154(11) Uani 1 1 d U . . H27A H 0.2722 0.8566 0.2133 0.230 Uiso 1 1 calc R . . H27B H 0.2779 0.9967 0.1967 0.230 Uiso 1 1 calc R . . H27C H 0.1700 0.9433 0.2326 0.230 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0264(5) 0.0328(6) 0.0313(5) 0.0005(5) -0.0047(4) -0.0028(5) Sn2 0.0432(7) 0.0235(6) 0.0396(6) -0.0053(5) -0.0038(5) 0.0021(5) Sn3 0.0596(8) 0.0261(6) 0.0328(6) 0.0083(5) -0.0032(5) 0.0014(5) Sn4 0.0304(6) 0.0404(7) 0.0566(7) 0.0076(6) 0.0159(5) 0.0025(5) Zn1 0.0347(10) 0.0247(9) 0.0376(10) -0.0010(8) -0.0107(8) -0.0034(8) Zn2 0.0325(9) 0.0214(9) 0.0347(9) -0.0017(7) 0.0019(7) 0.0011(7) Zn3 0.0325(10) 0.0236(8) 0.0294(9) 0.0052(7) 0.0036(7) -0.0010(8) Zn4 0.0297(9) 0.0281(9) 0.0300(9) 0.0009(7) 0.0052(7) -0.0028(8) O1 0.015(5) 0.028(5) 0.027(5) -0.001(4) -0.001(4) -0.006(4) O2 0.038(6) 0.017(5) 0.021(5) -0.003(4) 0.011(4) 0.008(4) O3 0.049(7) 0.024(5) 0.016(4) 0.001(4) 0.002(4) 0.001(5) O4 0.012(4) 0.037(6) 0.034(5) -0.003(5) 0.014(4) 0.003(5) C1 0.063(15) 0.058(14) 0.097(18) -0.006(13) -0.041(14) -0.006(12) C2 0.084(18) 0.10(2) 0.071(16) 0.006(15) -0.029(14) -0.012(16) C3 0.12(2) 0.027(10) 0.051(12) -0.009(9) 0.005(12) 0.011(11) C4 0.13(3) 0.08(2) 0.15(3) -0.04(2) 0.07(2) -0.04(2) C5 0.051(12) 0.048(11) 0.049(11) 0.031(9) -0.005(9) -0.003(9) C6 0.11(2) 0.066(15) 0.041(11) 0.014(10) 0.005(12) -0.009(15) C7 0.026(9) 0.051(11) 0.058(11) 0.008(9) 0.033(8) -0.005(8) C8 0.048(13) 0.10(2) 0.096(18) -0.024(16) 0.039(13) -0.004(14) C9 0.052(12) 0.051(12) 0.043(10) 0.008(9) 0.001(9) -0.011(9) C10 0.060(12) 0.038(10) 0.065(12) 0.026(10) -0.003(10) -0.001(10) C11 0.075(13) 0.041(11) 0.033(9) -0.013(8) 0.009(9) -0.021(10) C12 0.026(8) 0.050(11) 0.048(10) -0.002(9) -0.003(7) 0.007(8) C13 0.054(12) 0.047(12) 0.097(17) 0.001(12) 0.014(12) -0.019(11) C14 0.11(2) 0.066(15) 0.030(9) -0.014(10) -0.013(11) 0.008(15) C15 0.078(15) 0.046(12) 0.068(13) 0.003(10) 0.044(12) -0.005(11) C16 0.15(3) 0.036(11) 0.052(12) 0.000(10) -0.007(14) 0.017(15) C17 0.069(15) 0.038(11) 0.081(15) -0.004(10) -0.036(12) 0.023(10) C18 0.047(13) 0.13(3) 0.060(14) -0.017(15) 0.003(11) 0.014(14) C19 0.045(12) 0.070(15) 0.092(17) 0.014(13) 0.018(11) -0.030(11) C20 0.019(8) 0.051(12) 0.098(15) 0.004(11) 0.014(9) 0.011(8) C21 0.078(13) 0.163(16) 0.138(14) 0.025(13) 0.073(11) 0.038(15) C22 0.083(14) 0.163(16) 0.129(15) 0.030(14) 0.071(12) 0.025(16) C23 0.106(17) 0.182(18) 0.144(17) 0.030(14) 0.052(13) 0.016(17) C24 0.111(17) 0.20(2) 0.139(17) 0.043(15) 0.059(13) 0.026(18) C25 0.107(17) 0.188(19) 0.158(17) 0.053(16) 0.068(13) 0.037(18) C26 0.096(16) 0.166(17) 0.158(17) 0.034(15) 0.079(13) 0.041(16) C27 0.15(3) 0.18(3) 0.140(19) 0.025(17) 0.059(17) 0.00(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 1.999(9) . ? Sn1 C10 2.12(2) . ? Sn1 C11 2.124(19) . ? Sn1 C9 2.171(19) . ? Sn2 O2 2.017(9) . ? Sn2 C12 2.117(15) . ? Sn2 C14 2.12(2) . ? Sn2 C13 2.17(2) . ? Sn3 O3 2.003(9) . ? Sn3 C15 2.07(2) . ? Sn3 C16 2.11(2) . ? Sn3 C17 2.16(2) . ? Sn4 O4 1.996(9) . ? Sn4 C19 2.11(2) . ? Sn4 C18 2.13(2) . ? Sn4 C20 2.143(19) . ? Zn1 C1 1.946(19) . ? Zn1 O3 2.037(11) . ? Zn1 O4 2.068(10) . ? Zn1 O2 2.072(10) . ? Zn1 Zn4 2.991(3) . ? Zn1 Zn2 2.993(2) . ? Zn1 Zn3 3.016(2) . ? Zn2 C3 1.992(19) . ? Zn2 O4 2.051(11) . ? Zn2 O1 2.055(10) . ? Zn2 O3 2.061(9) . ? Zn2 Zn4 3.010(3) . ? Zn2 Zn3 3.015(2) . ? Zn3 C5 1.982(16) . ? Zn3 O4 2.061(10) . ? Zn3 O1 2.062(10) . ? Zn3 O2 2.063(9) . ? Zn3 Zn4 2.996(3) . ? Zn4 C7 1.981(15) . ? Zn4 O2 2.027(10) . ? Zn4 O1 2.063(10) . ? Zn4 O3 2.065(11) . ? C1 C2 1.46(3) . ? C3 C4 1.39(4) . ? C5 C6 1.52(3) . ? C7 C8 1.50(3) . ? C21 C26 1.37(2) . ? C21 C22 1.38(2) . ? C21 C27 1.49(5) . ? C22 C23 1.38(2) . ? C23 C24 1.38(2) . ? C24 C25 1.37(2) . ? C25 C26 1.38(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 O1 Sn1 C10 103.6(6) . . ? O1 Sn1 C11 103.9(6) . . ? C10 Sn1 C11 113.0(8) . . ? O1 Sn1 C9 103.2(6) . . ? C10 Sn1 C9 112.1(8) . . ? C11 Sn1 C9 118.9(8) . . ? O2 Sn2 C12 105.1(6) . . ? O2 Sn2 C14 104.2(7) . . ? C12 Sn2 C14 116.6(9) . . ? O2 Sn2 C13 103.2(7) . . ? C12 Sn2 C13 112.3(8) . . ? C14 Sn2 C13 113.7(10) . . ? O3 Sn3 C15 104.3(7) . . ? O3 Sn3 C16 103.4(7) . . ? C15 Sn3 C16 116.1(11) . . ? O3 Sn3 C17 103.6(8) . . ? C15 Sn3 C17 111.6(9) . . ? C16 Sn3 C17 115.9(10) . . ? O4 Sn4 C19 107.7(8) . . ? O4 Sn4 C18 104.0(8) . . ? C19 Sn4 C18 111.2(11) . . ? O4 Sn4 C20 100.6(6) . . ? C19 Sn4 C20 115.1(9) . . ? C18 Sn4 C20 116.6(10) . . ? C1 Zn1 O3 131.6(9) . . ? C1 Zn1 O4 126.9(10) . . ? O3 Zn1 O4 86.4(4) . . ? C1 Zn1 O2 125.3(8) . . ? O3 Zn1 O2 86.0(4) . . ? O4 Zn1 O2 85.9(4) . . ? C1 Zn1 Zn4 145.5(10) . . ? O3 Zn1 Zn4 43.6(3) . . ? O4 Zn1 Zn4 87.2(3) . . ? O2 Zn1 Zn4 42.6(3) . . ? C1 Zn1 Zn2 147.2(8) . . ? O3 Zn1 Zn2 43.4(3) . . ? O4 Zn1 Zn2 43.2(3) . . ? O2 Zn1 Zn2 87.3(3) . . ? Zn4 Zn1 Zn2 60.40(6) . . ? C1 Zn1 Zn3 140.8(8) . . ? O3 Zn1 Zn3 87.6(3) . . ? O4 Zn1 Zn3 43.0(3) . . ? O2 Zn1 Zn3 43.0(3) . . ? Zn4 Zn1 Zn3 59.83(6) . . ? Zn2 Zn1 Zn3 60.22(6) . . ? C3 Zn2 O4 126.0(9) . . ? C3 Zn2 O1 130.1(8) . . ? O4 Zn2 O1 85.9(4) . . ? C3 Zn2 O3 127.7(7) . . ? O4 Zn2 O3 86.2(4) . . ? O1 Zn2 O3 86.2(4) . . ? C3 Zn2 Zn1 142.4(7) . . ? O4 Zn2 Zn1 43.6(3) . . ? O1 Zn2 Zn1 87.5(3) . . ? O3 Zn2 Zn1 42.8(3) . . ? C3 Zn2 Zn4 147.0(8) . . ? O4 Zn2 Zn4 87.0(3) . . ? O1 Zn2 Zn4 43.1(3) . . ? O3 Zn2 Zn4 43.2(3) . . ? Zn1 Zn2 Zn4 59.76(6) . . ? C3 Zn2 Zn3 145.0(7) . . ? O4 Zn2 Zn3 43.0(3) . . ? O1 Zn2 Zn3 43.0(3) . . ? O3 Zn2 Zn3 87.2(3) . . ? Zn1 Zn2 Zn3 60.26(6) . . ? Zn4 Zn2 Zn3 59.63(6) . . ? C5 Zn3 O4 131.1(7) . . ? C5 Zn3 O1 126.5(6) . . ? O4 Zn3 O1 85.5(4) . . ? C5 Zn3 O2 126.8(7) . . ? O4 Zn3 O2 86.3(4) . . ? O1 Zn3 O2 85.7(4) . . ? C5 Zn3 Zn4 141.7(7) . . ? O4 Zn3 Zn4 87.2(3) . . ? O1 Zn3 Zn4 43.4(3) . . ? O2 Zn3 Zn4 42.4(3) . . ? C5 Zn3 Zn2 146.2(7) . . ? O4 Zn3 Zn2 42.7(3) . . ? O1 Zn3 Zn2 42.8(3) . . ? O2 Zn3 Zn2 86.9(3) . . ? Zn4 Zn3 Zn2 60.11(6) . . ? C5 Zn3 Zn1 146.6(6) . . ? O4 Zn3 Zn1 43.2(3) . . ? O1 Zn3 Zn1 86.7(3) . . ? O2 Zn3 Zn1 43.3(3) . . ? Zn4 Zn3 Zn1 59.67(6) . . ? Zn2 Zn3 Zn1 59.52(5) . . ? C7 Zn4 O2 128.9(6) . . ? C7 Zn4 O1 126.1(7) . . ? O2 Zn4 O1 86.6(4) . . ? C7 Zn4 O3 128.4(6) . . ? O2 Zn4 O3 86.5(4) . . ? O1 Zn4 O3 85.9(4) . . ? C7 Zn4 Zn1 146.5(6) . . ? O2 Zn4 Zn1 43.7(3) . . ? O1 Zn4 Zn1 87.4(3) . . ? O3 Zn4 Zn1 42.8(3) . . ? C7 Zn4 Zn3 143.9(6) . . ? O2 Zn4 Zn3 43.4(3) . . ? O1 Zn4 Zn3 43.4(3) . . ? O3 Zn4 Zn3 87.6(3) . . ? Zn1 Zn4 Zn3 60.50(6) . . ? C7 Zn4 Zn2 143.4(6) . . ? O2 Zn4 Zn2 87.7(3) . . ? O1 Zn4 Zn2 42.9(3) . . ? O3 Zn4 Zn2 43.1(3) . . ? Zn1 Zn4 Zn2 59.83(6) . . ? Zn3 Zn4 Zn2 60.25(6) . . ? Sn1 O1 Zn2 119.8(5) . . ? Sn1 O1 Zn3 124.9(5) . . ? Zn2 O1 Zn3 94.1(4) . . ? Sn1 O1 Zn4 123.0(5) . . ? Zn2 O1 Zn4 93.9(4) . . ? Zn3 O1 Zn4 93.1(4) . . ? Sn2 O2 Zn4 129.4(5) . . ? Sn2 O2 Zn3 119.5(5) . . ? Zn4 O2 Zn3 94.2(4) . . ? Sn2 O2 Zn1 118.1(5) . . ? Zn4 O2 Zn1 93.7(4) . . ? Zn3 O2 Zn1 93.7(4) . . ? Sn3 O3 Zn1 125.0(5) . . ? Sn3 O3 Zn2 122.5(5) . . ? Zn1 O3 Zn2 93.8(4) . . ? Sn3 O3 Zn4 120.2(6) . . ? Zn1 O3 Zn4 93.6(4) . . ? Zn2 O3 Zn4 93.7(4) . . ? Sn4 O4 Zn2 119.6(5) . . ? Sn4 O4 Zn3 125.3(5) . . ? Zn2 O4 Zn3 94.3(4) . . ? Sn4 O4 Zn1 122.5(5) . . ? Zn2 O4 Zn1 93.2(4) . . ? Zn3 O4 Zn1 93.8(4) . . ? C2 C1 Zn1 122.0(18) . . ? C4 C3 Zn2 126(2) . . ? C6 C5 Zn3 116.4(15) . . ? C8 C7 Zn4 115.8(14) . . ? C26 C21 C22 123(2) . . ? C26 C21 C27 117(3) . . ? C22 C21 C27 120(3) . . ? C23 C22 C21 118(2) . . ? C22 C23 C24 119.3(17) . . ? C25 C24 C23 120.8(18) . . ? C24 C25 C26 121.1(17) . . ? C21 C26 C25 117(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.767 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.245 data_tsar2 _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H56 O4 Sn4 Zn4' _chemical_formula_weight 1132.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.2398(2) _cell_length_b 11.0673(2) _cell_length_c 16.6253(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.927(2) _cell_angle_gamma 90.00 _cell_volume 2043.04(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7873 _cell_measurement_theta_min 3.0796 _cell_measurement_theta_max 28.7641 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 4.729 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3844 _exptl_absorpt_correction_T_max 0.6007 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9053 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5139 _reflns_number_gt 4862 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.060(12) _refine_ls_number_reflns 5139 _refine_ls_number_parameters 333 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0405 _refine_ls_wR_factor_gt 0.0401 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.54259(3) 0.32138(3) 0.07791(2) 0.02607(8) Uani 1 1 d . . . Sn2 Sn 0.76380(3) 0.74234(3) 0.30250(2) 0.02936(9) Uani 1 1 d . . . Sn3 Sn 0.86739(3) 0.21999(3) 0.39833(2) 0.03013(9) Uani 1 1 d . . . Sn4 Sn 1.06776(3) 0.43454(3) 0.11765(2) 0.03278(9) Uani 1 1 d . . . Zn1 Zn 0.93418(5) 0.47817(5) 0.29660(3) 0.02603(14) Uani 1 1 d . . . Zn2 Zn 0.82678(5) 0.28094(5) 0.18617(3) 0.02573(14) Uani 1 1 d . . . Zn3 Zn 0.77637(5) 0.54006(5) 0.13999(3) 0.02532(13) Uani 1 1 d . . . Zn4 Zn 0.66775(5) 0.43070(5) 0.27601(3) 0.02652(13) Uani 1 1 d . . . O1 O 0.6779(3) 0.3897(3) 0.15682(18) 0.0242(8) Uani 1 1 d . . . O2 O 0.7789(3) 0.5737(3) 0.26201(19) 0.0260(8) Uani 1 1 d . . . O3 O 0.8226(3) 0.3319(3) 0.30359(17) 0.0263(8) Uani 1 1 d . . . O4 O 0.9252(3) 0.4353(3) 0.17634(18) 0.0254(7) Uani 1 1 d . . . C1 C 1.0768(6) 0.5204(5) 0.3751(4) 0.0492(17) Uani 1 1 d . . . H1A H 1.1264 0.5779 0.3501 0.074 Uiso 1 1 calc R . . H1B H 1.1237 0.4472 0.3910 0.074 Uiso 1 1 calc R . . H1C H 1.0515 0.5571 0.4234 0.074 Uiso 1 1 calc R . . C2 C 0.8506(6) 0.1215(5) 0.1392(4) 0.0480(17) Uani 1 1 d . . . H2A H 0.9363 0.1005 0.1496 0.072 Uiso 1 1 calc R . . H2B H 0.8229 0.1237 0.0803 0.072 Uiso 1 1 calc R . . H2C H 0.8044 0.0608 0.1641 0.072 Uiso 1 1 calc R . . C3 C 0.7475(6) 0.6611(6) 0.0524(3) 0.0508(17) Uani 1 1 d . . . H3A H 0.7835 0.6334 0.0057 0.076 Uiso 1 1 calc R . . H3B H 0.7840 0.7381 0.0721 0.076 Uiso 1 1 calc R . . H3C H 0.6606 0.6720 0.0360 0.076 Uiso 1 1 calc R . . C4 C 0.5170(5) 0.4313(7) 0.3212(4) 0.0547(17) Uani 1 1 d . . . H4A H 0.5303 0.4694 0.3750 0.082 Uiso 1 1 calc R . . H4B H 0.4894 0.3480 0.3262 0.082 Uiso 1 1 calc R . . H4C H 0.4557 0.4767 0.2850 0.082 Uiso 1 1 calc R . . C5 C 0.5021(5) 0.1587(5) 0.1351(4) 0.0451(15) Uani 1 1 d . . . H5A H 0.5739 0.1073 0.1441 0.068 Uiso 1 1 calc R . . H5B H 0.4371 0.1163 0.1001 0.068 Uiso 1 1 calc R . . H5C H 0.4766 0.1773 0.1875 0.068 Uiso 1 1 calc R . . C6 C 0.4059(5) 0.4540(5) 0.0677(4) 0.0464(15) Uani 1 1 d . . . H6A H 0.3887 0.4747 0.1220 0.070 Uiso 1 1 calc R . . H6B H 0.3328 0.4224 0.0346 0.070 Uiso 1 1 calc R . . H6C H 0.4328 0.5264 0.0417 0.070 Uiso 1 1 calc R . . C7 C 0.6218(5) 0.3058(6) -0.0304(3) 0.0402(14) Uani 1 1 d . . . H7A H 0.6521 0.3849 -0.0444 0.060 Uiso 1 1 calc R . . H7B H 0.5611 0.2774 -0.0751 0.060 Uiso 1 1 calc R . . H7C H 0.6886 0.2481 -0.0214 0.060 Uiso 1 1 calc R . . C8 C 0.6028(5) 0.8125(6) 0.2353(3) 0.0460(15) Uani 1 1 d . . . H8A H 0.6212 0.8531 0.1863 0.069 Uiso 1 1 calc R . . H8B H 0.5668 0.8705 0.2690 0.069 Uiso 1 1 calc R . . H8C H 0.5461 0.7462 0.2196 0.069 Uiso 1 1 calc R . . C9 C 0.9224(6) 0.8282(6) 0.2747(4) 0.0498(16) Uani 1 1 d . . . H9A H 0.9936 0.7849 0.3016 0.075 Uiso 1 1 calc R . . H9B H 0.9249 0.9120 0.2940 0.075 Uiso 1 1 calc R . . H9C H 0.9214 0.8273 0.2156 0.075 Uiso 1 1 calc R . . C10 C 0.7598(6) 0.7183(6) 0.4286(3) 0.0554(18) Uani 1 1 d . . . H10A H 0.7017 0.6549 0.4361 0.083 Uiso 1 1 calc R . . H10B H 0.7358 0.7941 0.4519 0.083 Uiso 1 1 calc R . . H10C H 0.8400 0.6948 0.4560 0.083 Uiso 1 1 calc R . . C11 C 0.7267(6) 0.0920(6) 0.3884(4) 0.062(2) Uani 1 1 d . . . H11A H 0.6511 0.1328 0.3940 0.092 Uiso 1 1 calc R . . H11B H 0.7450 0.0313 0.4314 0.092 Uiso 1 1 calc R . . H11C H 0.7187 0.0524 0.3351 0.092 Uiso 1 1 calc R . . C12 C 0.8808(6) 0.3352(5) 0.5019(3) 0.0433(15) Uani 1 1 d . . . H12A H 0.9636 0.3648 0.5156 0.065 Uiso 1 1 calc R . . H12B H 0.8589 0.2899 0.5482 0.065 Uiso 1 1 calc R . . H12C H 0.8260 0.4039 0.4897 0.065 Uiso 1 1 calc R . . C13 C 1.0341(6) 0.1471(5) 0.3747(3) 0.0443(16) Uani 1 1 d . . . H13A H 1.0248 0.1182 0.3183 0.066 Uiso 1 1 calc R . . H13B H 1.0579 0.0797 0.4119 0.066 Uiso 1 1 calc R . . H13C H 1.0962 0.2100 0.3829 0.066 Uiso 1 1 calc R . . C14 C 0.9936(7) 0.3973(7) -0.0059(4) 0.066(2) Uani 1 1 d . . . H14A H 0.9554 0.3175 -0.0094 0.100 Uiso 1 1 calc R . . H14B H 1.0580 0.3984 -0.0395 0.100 Uiso 1 1 calc R . . H14C H 0.9334 0.4588 -0.0256 0.100 Uiso 1 1 calc R . . C15 C 1.1383(6) 0.6134(6) 0.1365(4) 0.0550(17) Uani 1 1 d . . . H15A H 1.0820 0.6711 0.1064 0.083 Uiso 1 1 calc R . . H15B H 1.2161 0.6183 0.1171 0.083 Uiso 1 1 calc R . . H15C H 1.1491 0.6327 0.1947 0.083 Uiso 1 1 calc R . . C16 C 1.1793(6) 0.2952(6) 0.1758(5) 0.0631(19) Uani 1 1 d . . . H16A H 1.2222 0.3249 0.2279 0.095 Uiso 1 1 calc R . . H16B H 1.2377 0.2707 0.1408 0.095 Uiso 1 1 calc R . . H16C H 1.1294 0.2256 0.1855 0.095 Uiso 1 1 calc R . . C17 C 0.3055(7) 0.9138(8) 0.3053(5) 0.072(2) Uani 1 1 d . . . C18 C 0.3594(9) 0.9999(10) 0.3588(7) 0.104(4) Uani 1 1 d . . . H18 H 0.3516 1.0835 0.3461 0.156 Uiso 1 1 calc R . . C19 C 0.4268(10) 0.9605(14) 0.4336(8) 0.115(5) Uani 1 1 d . . . H19 H 0.4627 1.0193 0.4714 0.173 Uiso 1 1 calc R . . C20 C 0.4414(10) 0.8444(15) 0.4524(7) 0.123(5) Uani 1 1 d . . . H20 H 0.4872 0.8214 0.5030 0.185 Uiso 1 1 calc R . . C21 C 0.3918(9) 0.7589(11) 0.4002(6) 0.109(4) Uani 1 1 d . . . H21 H 0.4054 0.6760 0.4133 0.163 Uiso 1 1 calc R . . C22 C 0.3211(7) 0.7905(8) 0.3275(5) 0.075(2) Uani 1 1 d . . . H22 H 0.2831 0.7294 0.2924 0.112 Uiso 1 1 calc R . . C23 C 0.2340(9) 0.9457(9) 0.2268(6) 0.101(3) Uani 1 1 d . . . H23A H 0.1676 0.9989 0.2359 0.151 Uiso 1 1 calc R . . H23B H 0.2013 0.8721 0.1990 0.151 Uiso 1 1 calc R . . H23C H 0.2852 0.9875 0.1931 0.151 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02329(19) 0.02573(18) 0.02717(18) -0.00201(15) -0.00245(14) -0.00081(15) Sn2 0.0366(2) 0.02061(18) 0.02864(18) -0.00300(15) -0.00190(16) 0.00268(16) Sn3 0.0408(2) 0.02240(18) 0.02536(18) 0.00515(15) -0.00079(16) -0.00331(17) Sn4 0.0287(2) 0.0325(2) 0.0396(2) 0.00348(17) 0.01320(16) 0.00108(18) Zn1 0.0271(3) 0.0224(3) 0.0264(3) 0.0014(2) -0.0027(3) -0.0030(2) Zn2 0.0277(3) 0.0215(3) 0.0269(3) -0.0016(2) 0.0009(3) 0.0007(2) Zn3 0.0278(3) 0.0237(3) 0.0236(3) 0.0037(2) 0.0014(3) -0.0002(3) Zn4 0.0274(3) 0.0268(3) 0.0256(3) -0.0010(3) 0.0050(2) -0.0021(3) O1 0.026(2) 0.0230(17) 0.0218(17) -0.0026(14) -0.0005(15) 0.0000(15) O2 0.031(2) 0.0222(17) 0.0243(18) -0.0004(14) 0.0035(15) 0.0018(15) O3 0.0299(19) 0.0244(17) 0.0226(17) 0.0005(14) -0.0023(15) 0.0007(16) O4 0.0203(18) 0.0280(17) 0.0292(18) 0.0021(16) 0.0083(14) 0.0007(17) C1 0.041(4) 0.046(4) 0.053(4) 0.011(3) -0.017(3) -0.016(3) C2 0.056(4) 0.032(3) 0.054(4) -0.007(3) 0.000(3) 0.012(3) C3 0.061(5) 0.047(4) 0.043(4) 0.012(3) 0.001(3) 0.002(3) C4 0.042(4) 0.075(5) 0.052(4) -0.004(4) 0.020(3) -0.002(4) C5 0.035(4) 0.039(3) 0.059(4) 0.001(3) -0.001(3) -0.008(3) C6 0.035(3) 0.042(3) 0.061(4) 0.008(3) 0.005(3) 0.012(3) C7 0.041(3) 0.048(3) 0.031(3) -0.006(3) 0.003(3) 0.000(3) C8 0.039(4) 0.046(3) 0.050(4) -0.005(3) -0.003(3) 0.012(3) C9 0.056(4) 0.034(3) 0.056(4) 0.001(3) -0.001(3) -0.010(3) C10 0.085(5) 0.052(4) 0.027(3) -0.002(3) 0.006(3) 0.011(4) C11 0.062(5) 0.045(4) 0.078(5) 0.013(4) 0.014(4) -0.019(4) C12 0.055(4) 0.041(3) 0.033(3) 0.000(3) 0.004(3) -0.001(3) C13 0.053(4) 0.033(3) 0.042(3) 0.008(3) -0.007(3) 0.009(3) C14 0.073(5) 0.092(6) 0.037(4) -0.012(4) 0.022(3) -0.013(4) C15 0.054(4) 0.045(4) 0.072(4) 0.000(3) 0.026(4) -0.009(3) C16 0.040(4) 0.058(4) 0.096(5) 0.022(4) 0.023(4) 0.016(3) C17 0.055(5) 0.092(6) 0.075(6) -0.016(5) 0.029(4) -0.002(5) C18 0.079(7) 0.111(8) 0.137(9) -0.055(7) 0.064(7) -0.036(6) C19 0.077(8) 0.157(12) 0.118(10) -0.073(10) 0.038(7) -0.041(8) C20 0.076(7) 0.202(15) 0.097(8) -0.044(10) 0.030(6) 0.021(10) C21 0.103(8) 0.149(10) 0.078(6) -0.017(7) 0.026(6) 0.032(8) C22 0.065(5) 0.093(7) 0.069(5) -0.024(5) 0.020(4) -0.006(5) C23 0.109(8) 0.096(7) 0.112(7) 0.015(6) 0.059(6) 0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 1.997(3) . ? Sn1 C6 2.112(5) . ? Sn1 C5 2.118(6) . ? Sn1 C7 2.136(5) . ? Sn2 O2 2.001(3) . ? Sn2 C10 2.120(5) . ? Sn2 C8 2.121(5) . ? Sn2 C9 2.133(6) . ? Sn3 O3 2.006(3) . ? Sn3 C11 2.110(6) . ? Sn3 C12 2.129(5) . ? Sn3 C13 2.132(6) . ? Sn4 O4 2.001(3) . ? Sn4 C16 2.124(6) . ? Sn4 C14 2.134(6) . ? Sn4 C15 2.137(6) . ? Zn1 C1 1.960(5) . ? Zn1 O4 2.042(3) . ? Zn1 O2 2.045(3) . ? Zn1 O3 2.062(3) . ? Zn1 Zn2 2.9841(7) . ? Zn1 Zn3 2.9935(8) . ? Zn1 Zn4 3.0071(8) . ? Zn2 C2 1.965(5) . ? Zn2 O3 2.040(3) . ? Zn2 O4 2.055(3) . ? Zn2 O1 2.057(3) . ? Zn2 Zn3 2.9999(8) . ? Zn2 Zn4 3.0002(8) . ? Zn3 C3 1.967(5) . ? Zn3 O1 2.041(3) . ? Zn3 O4 2.048(3) . ? Zn3 O2 2.058(3) . ? Zn3 Zn4 2.9876(8) . ? Zn4 C4 1.957(6) . ? Zn4 O3 2.046(3) . ? Zn4 O2 2.052(3) . ? Zn4 O1 2.053(3) . ? C17 C18 1.379(11) . ? C17 C22 1.417(12) . ? C17 C23 1.465(11) . ? C18 C19 1.420(16) . ? C19 C20 1.327(17) . ? C20 C21 1.345(14) . ? C21 C22 1.384(11) . ? 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 O1 Sn1 C6 105.07(19) . . ? O1 Sn1 C5 102.82(18) . . ? C6 Sn1 C5 115.0(2) . . ? O1 Sn1 C7 102.09(18) . . ? C6 Sn1 C7 112.4(2) . . ? C5 Sn1 C7 117.2(2) . . ? O2 Sn2 C10 103.4(2) . . ? O2 Sn2 C8 105.92(19) . . ? C10 Sn2 C8 114.8(3) . . ? O2 Sn2 C9 103.0(2) . . ? C10 Sn2 C9 114.7(3) . . ? C8 Sn2 C9 113.3(2) . . ? O3 Sn3 C11 105.0(2) . . ? O3 Sn3 C12 104.06(18) . . ? C11 Sn3 C12 115.0(3) . . ? O3 Sn3 C13 102.10(18) . . ? C11 Sn3 C13 113.6(3) . . ? C12 Sn3 C13 115.0(2) . . ? O4 Sn4 C16 104.0(2) . . ? O4 Sn4 C14 104.3(2) . . ? C16 Sn4 C14 114.4(3) . . ? O4 Sn4 C15 103.4(2) . . ? C16 Sn4 C15 115.3(3) . . ? C14 Sn4 C15 113.6(3) . . ? C1 Zn1 O4 128.2(2) . . ? C1 Zn1 O2 129.7(2) . . ? O4 Zn1 O2 86.24(13) . . ? C1 Zn1 O3 126.24(19) . . ? O4 Zn1 O3 86.25(12) . . ? O2 Zn1 O3 85.50(13) . . ? C1 Zn1 Zn2 142.65(19) . . ? O4 Zn1 Zn2 43.43(9) . . ? O2 Zn1 Zn2 87.65(9) . . ? O3 Zn1 Zn2 43.03(9) . . ? C1 Zn1 Zn3 146.90(17) . . ? O4 Zn1 Zn3 43.04(9) . . ? O2 Zn1 Zn3 43.32(9) . . ? O3 Zn1 Zn3 86.85(8) . . ? Zn2 Zn1 Zn3 60.245(18) . . ? C1 Zn1 Zn4 144.5(2) . . ? O4 Zn1 Zn4 87.19(9) . . ? O2 Zn1 Zn4 42.87(9) . . ? O3 Zn1 Zn4 42.74(9) . . ? Zn2 Zn1 Zn4 60.100(19) . . ? Zn3 Zn1 Zn4 59.721(19) . . ? C2 Zn2 O3 130.8(2) . . ? C2 Zn2 O4 127.3(2) . . ? O3 Zn2 O4 86.49(13) . . ? C2 Zn2 O1 125.9(2) . . ? O3 Zn2 O1 85.78(12) . . ? O4 Zn2 O1 85.57(13) . . ? C2 Zn2 Zn1 146.57(19) . . ? O3 Zn2 Zn1 43.61(9) . . ? O4 Zn2 Zn1 43.09(9) . . ? O1 Zn2 Zn1 87.38(9) . . ? C2 Zn2 Zn3 142.05(18) . . ? O3 Zn2 Zn3 87.07(9) . . ? O4 Zn2 Zn3 42.93(9) . . ? O1 Zn2 Zn3 42.74(9) . . ? Zn1 Zn2 Zn3 60.032(17) . . ? C2 Zn2 Zn4 145.3(2) . . ? O3 Zn2 Zn4 42.83(9) . . ? O4 Zn2 Zn4 87.14(9) . . ? O1 Zn2 Zn4 43.07(9) . . ? Zn1 Zn2 Zn4 60.329(19) . . ? Zn3 Zn2 Zn4 59.726(19) . . ? C3 Zn3 O1 128.7(2) . . ? C3 Zn3 O4 129.6(2) . . ? O1 Zn3 O4 86.17(13) . . ? C3 Zn3 O2 125.6(2) . . ? O1 Zn3 O2 86.40(12) . . ? O4 Zn3 O2 85.74(13) . . ? C3 Zn3 Zn4 142.7(2) . . ? O1 Zn3 Zn4 43.30(9) . . ? O4 Zn3 Zn4 87.61(9) . . ? O2 Zn3 Zn4 43.29(9) . . ? C3 Zn3 Zn1 143.76(19) . . ? O1 Zn3 Zn1 87.41(9) . . ? O4 Zn3 Zn1 42.88(9) . . ? O2 Zn3 Zn1 42.97(9) . . ? Zn4 Zn3 Zn1 60.366(19) . . ? C3 Zn3 Zn2 147.45(19) . . ? O1 Zn3 Zn2 43.16(9) . . ? O4 Zn3 Zn2 43.12(9) . . ? O2 Zn3 Zn2 86.98(9) . . ? Zn4 Zn3 Zn2 60.143(19) . . ? Zn1 Zn3 Zn2 59.723(17) . . ? C4 Zn4 O3 132.3(2) . . ? C4 Zn4 O2 128.3(2) . . ? O3 Zn4 O2 85.73(13) . . ? C4 Zn4 O1 123.5(2) . . ? O3 Zn4 O1 85.72(13) . . ? O2 Zn4 O1 86.25(13) . . ? C4 Zn4 Zn3 140.3(2) . . ? O3 Zn4 Zn3 87.29(9) . . ? O2 Zn4 Zn3 43.45(9) . . ? O1 Zn4 Zn3 42.98(9) . . ? C4 Zn4 Zn2 144.2(2) . . ? O3 Zn4 Zn2 42.67(8) . . ? O2 Zn4 Zn2 87.08(10) . . ? O1 Zn4 Zn2 43.18(9) . . ? Zn3 Zn4 Zn2 60.131(18) . . ? C4 Zn4 Zn1 149.53(19) . . ? O3 Zn4 Zn1 43.15(9) . . ? O2 Zn4 Zn1 42.68(9) . . ? O1 Zn4 Zn1 86.83(10) . . ? Zn3 Zn4 Zn1 59.913(18) . . ? Zn2 Zn4 Zn1 59.570(18) . . ? Sn1 O1 Zn3 126.34(15) . . ? Sn1 O1 Zn4 124.52(18) . . ? Zn3 O1 Zn4 93.72(13) . . ? Sn1 O1 Zn2 116.27(15) . . ? Zn3 O1 Zn2 94.10(14) . . ? Zn4 O1 Zn2 93.75(12) . . ? Sn2 O2 Zn1 120.07(16) . . ? Sn2 O2 Zn4 126.60(18) . . ? Zn1 O2 Zn4 94.45(13) . . ? Sn2 O2 Zn3 120.76(15) . . ? Zn1 O2 Zn3 93.71(14) . . ? Zn4 O2 Zn3 93.26(13) . . ? Sn3 O3 Zn2 122.71(16) . . ? Sn3 O3 Zn4 127.39(17) . . ? Zn2 O3 Zn4 94.50(12) . . ? Sn3 O3 Zn1 116.64(14) . . ? Zn2 O3 Zn1 93.36(13) . . ? Zn4 O3 Zn1 94.12(13) . . ? Sn4 O4 Zn1 123.83(16) . . ? Sn4 O4 Zn3 122.52(15) . . ? Zn1 O4 Zn3 94.08(13) . . ? Sn4 O4 Zn2 121.13(16) . . ? Zn1 O4 Zn2 93.48(13) . . ? Zn3 O4 Zn2 93.95(13) . . ? C18 C17 C22 118.2(9) . . ? C18 C17 C23 122.2(10) . . ? C22 C17 C23 119.5(8) . . ? C17 C18 C19 118.3(11) . . ? C20 C19 C18 122.2(11) . . ? C19 C20 C21 120.4(13) . . ? C20 C21 C22 120.7(12) . . ? C21 C22 C17 120.1(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.469 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.075