# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Francois Ribot' _publ_contact_author_address ; Chimie de la Matiere Condensee (UMR 7574) Universite Pierre et Marie Curie 4 Place Jussieu (case 174) Paris Cedex 05 75252 FRANCE ; _publ_contact_author_email FRI@CCR.JUSSIEU.FR _publ_section_title ; Poly[{(BuSn)12O14(OH)6}(AMPS)2] and poly[Methylacrylate-co-{(BuSn)12O14(OH)6}(AMPS)2] : hybrid polymers cross-linked through electrostatic interactions ; _publ_requested_category FA loop_ _publ_author_name 'Francois Ribot' 'Steven J. Guillaudeu' 'Thierry Lalot' 'Delphine Veautier' data_fran3 _database_code_depnum_ccdc_archive 'CCDC 272683' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H114 O20 Sn12 2+, (C7 H12 N1 O4 S1 1-)2' _chemical_formula_sum 'C62 H138 N2 O28 S2 Sn12' _chemical_formula_weight 2848.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 35.505(8) _cell_length_b 35.505(8) _cell_length_c 15.724(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19822(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.9 _cell_measurement_theta_max 14.1 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_max 0.4 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10992 _exptl_absorpt_coefficient_mu 3.073 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7303 _exptl_absorpt_correction_T_max 0.8002 _exptl_absorpt_process_details ; A.C.T. North, D.C. Philips & F.S. Mathews, Acta Cryst. (1968), A24, 351-359 ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-nonius CAD4 ' _diffrn_measurement_method 2\q/\w _diffrn_standards_number 2 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 17.55 _diffrn_reflns_number 9021 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 24.98 _reflns_number_total 8708 _reflns_number_gt 3850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _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. Poor quality single crystals (decay 17.55 %, theta max. 24.98 deg.) Because of the high degree of disorder, the carbon atoms of the six independent butyl chains were treated in the following manner: - the first carbon atoms in the chains (C11,C21,C31,C41,C51,C61) were refined independently with anisotropic thermal parameters, all others being considered isotropically - the similar C atoms of the different chains were considered with the same isotropic thermal parameter (i.e. C12,C22,C32,C42,C52,C62 then C13,C23,C33,C43,C53,C63 and C14,C24,C34,C44,C54,C64) - the lengths and angles of the carbon-carbon bonds were restrained to normal values. The hydrogen atoms bond to C or N atoms were simply introduced in structure factor calculations. The hydrogen atoms bond to O atoms (O6, O7 and O8) were not introduced in the structure refinement. A data collection at low temperature did not improve the results. ; _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^)+(0.1933P)^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_number_reflns 8708 _refine_ls_number_parameters 381 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 0.03090(4) -0.08115(4) 0.04808(9) 0.1081(4) Uani 1 1 d D . . Sn2 Sn 0.09509(3) -0.01642(4) 0.00975(9) 0.1050(4) Uani 1 1 d D . . Sn3 Sn 0.02298(4) -0.01752(4) 0.19052(8) 0.1101(4) Uani 1 1 d D . . Sn4 Sn 0.02374(4) -0.05745(4) -0.14775(8) 0.1080(4) Uani 1 1 d D . . Sn5 Sn 0.06208(4) 0.06614(4) 0.06901(9) 0.1080(4) Uani 1 1 d D . . Sn6 Sn 0.06242(3) 0.04250(4) -0.13326(8) 0.1054(4) Uani 1 1 d D . . O1 O 0.0605(3) -0.0392(3) 0.1094(7) 0.109(3) Uani 1 1 d . . . O2 O 0.0617(3) -0.0580(3) -0.0512(7) 0.106(3) Uani 1 1 d . . . O3 O 0.0517(3) 0.0217(3) -0.0115(7) 0.093(3) Uani 1 1 d . . . O4 O -0.0060(3) -0.0615(3) 0.1356(8) 0.111(3) Uani 1 1 d . . . O5 O 0.0310(3) 0.0376(3) 0.1646(7) 0.107(3) Uani 1 1 d . . . O6 O 0.1087(3) 0.0312(4) 0.0863(8) 0.111(3) Uani 1 1 d . . . O7 O 0.0785(3) 0.0871(3) -0.0521(8) 0.107(3) Uani 1 1 d . . . O8 O 0.1103(3) 0.0094(4) -0.1081(9) 0.117(4) Uani 1 1 d . . . O9 O -0.0060(3) -0.0838(3) -0.0501(8) 0.107(3) Uani 1 1 d . . . O10 O -0.0319(3) 0.0037(3) 0.1831(8) 0.106(3) Uani 1 1 d . . . C11 C 0.0497(6) -0.1359(5) 0.087(2) 0.157(10) Uani 1 1 d D . . H11A H 0.0457 -0.1534 0.0406 0.188 Uiso 1 1 calc R . . H11B H 0.0765 -0.1348 0.0983 0.188 Uiso 1 1 calc R . . C12 C 0.0306(13) -0.1502(9) 0.162(2) 0.246(7) Uiso 1 1 d D . . H12A H 0.0480 -0.1507 0.2101 0.295 Uiso 1 1 calc R . . H12B H 0.0097 -0.1338 0.1770 0.295 Uiso 1 1 calc R . . C13 C 0.0167(16) -0.1883(13) 0.145(4) 0.380(15) Uiso 1 1 d D . . H13A H -0.0091 -0.1896 0.1651 0.456 Uiso 1 1 calc R . . H13B H 0.0163 -0.1917 0.0842 0.456 Uiso 1 1 calc R . . C14 C 0.037(2) -0.2196(13) 0.181(6) 0.48(2) Uiso 1 1 d D . . H14A H 0.0633 -0.2151 0.1779 0.725 Uiso 1 1 calc R . . H14B H 0.0306 -0.2421 0.1507 0.725 Uiso 1 1 calc R . . H14C H 0.0296 -0.2225 0.2400 0.725 Uiso 1 1 calc R . . C21 C 0.1467(5) -0.0475(6) 0.0267(15) 0.131(7) Uani 1 1 d D . . H21A H 0.1560 -0.0552 -0.0287 0.157 Uiso 1 1 calc R . . H21B H 0.1654 -0.0310 0.0520 0.157 Uiso 1 1 calc R . . C22 C 0.1424(10) -0.0808(9) 0.080(3) 0.246(7) Uiso 1 1 d D . . H22A H 0.1256 -0.0981 0.0511 0.295 Uiso 1 1 calc R . . H22B H 0.1300 -0.0731 0.1323 0.295 Uiso 1 1 calc R . . C23 C 0.1766(13) -0.1014(15) 0.103(5) 0.380(15) Uiso 1 1 d D . . H23A H 0.1929 -0.1031 0.0536 0.456 Uiso 1 1 calc R . . H23B H 0.1900 -0.0875 0.1467 0.456 Uiso 1 1 calc R . . C24 C 0.168(2) -0.1393(13) 0.134(6) 0.48(2) Uiso 1 1 d D . . H24A H 0.1541 -0.1377 0.1856 0.725 Uiso 1 1 calc R . . H24B H 0.1915 -0.1524 0.1446 0.725 Uiso 1 1 calc R . . H24C H 0.1541 -0.1527 0.0918 0.725 Uiso 1 1 calc R . . C31 C 0.0354(8) -0.0293(12) 0.3206(16) 0.224(18) Uani 1 1 d D . . H31A H 0.0214 -0.0119 0.3562 0.268 Uiso 1 1 calc R . . H31B H 0.0268 -0.0545 0.3339 0.268 Uiso 1 1 calc R . . C32 C 0.0753(9) -0.0264(11) 0.342(2) 0.246(7) Uiso 1 1 d D . . H32A H 0.0781 -0.0236 0.4026 0.295 Uiso 1 1 calc R . . H32B H 0.0857 -0.0040 0.3148 0.295 Uiso 1 1 calc R . . C33 C 0.0971(13) -0.0601(14) 0.313(5) 0.380(15) Uiso 1 1 d D . . H33A H 0.1007 -0.0771 0.3606 0.456 Uiso 1 1 calc R . . H33B H 0.0829 -0.0734 0.2695 0.456 Uiso 1 1 calc R . . C34 C 0.1338(17) -0.049(2) 0.279(6) 0.48(2) Uiso 1 1 d D . . H34A H 0.1470 -0.0342 0.3204 0.725 Uiso 1 1 calc R . . H34B H 0.1302 -0.0344 0.2282 0.725 Uiso 1 1 calc R . . H34C H 0.1482 -0.0712 0.2658 0.725 Uiso 1 1 calc R . . C41 C 0.0356(7) -0.0930(6) -0.2441(12) 0.135(7) Uani 1 1 d D . . H41A H 0.0625 -0.0918 -0.2548 0.162 Uiso 1 1 calc R . . H41B H 0.0300 -0.1184 -0.2253 0.162 Uiso 1 1 calc R . . C42 C 0.0161(12) -0.0865(11) -0.3246(18) 0.246(7) Uiso 1 1 d D . . H42A H 0.0213 -0.0611 -0.3441 0.295 Uiso 1 1 calc R . . H42B H -0.0109 -0.0886 -0.3154 0.295 Uiso 1 1 calc R . . C43 C 0.0276(15) -0.1137(18) -0.391(3) 0.380(15) Uiso 1 1 d D . . H43A H 0.0382 -0.1002 -0.4391 0.456 Uiso 1 1 calc R . . H43B H 0.0468 -0.1304 -0.3686 0.456 Uiso 1 1 calc R . . C44 C -0.005(2) -0.136(2) -0.419(5) 0.48(2) Uiso 1 1 d D . . H44A H -0.0216 -0.1197 -0.4496 0.725 Uiso 1 1 calc R . . H44B H -0.0172 -0.1460 -0.3701 0.725 Uiso 1 1 calc R . . H44C H 0.0038 -0.1557 -0.4551 0.725 Uiso 1 1 calc R . . C51 C 0.0837(7) 0.1115(6) 0.1476(15) 0.138(7) Uani 1 1 d D . . H51A H 0.0700 0.1114 0.2009 0.166 Uiso 1 1 calc R . . H51B H 0.1099 0.1061 0.1605 0.166 Uiso 1 1 calc R . . C52 C 0.0817(11) 0.1484(7) 0.112(3) 0.246(7) Uiso 1 1 d D . . H52A H 0.0960 0.1647 0.1498 0.295 Uiso 1 1 calc R . . H52B H 0.0954 0.1475 0.0589 0.295 Uiso 1 1 calc R . . C53 C 0.0476(13) 0.1675(15) 0.095(5) 0.380(15) Uiso 1 1 d D . . H53A H 0.0338 0.1694 0.1480 0.456 Uiso 1 1 calc R . . H53B H 0.0329 0.1516 0.0573 0.456 Uiso 1 1 calc R . . C54 C 0.049(2) 0.2049(17) 0.057(6) 0.48(2) Uiso 1 1 d D . . H54A H 0.0508 0.2235 0.1017 0.725 Uiso 1 1 calc R . . H54B H 0.0269 0.2092 0.0243 0.725 Uiso 1 1 calc R . . H54C H 0.0709 0.2068 0.0213 0.725 Uiso 1 1 calc R . . C61 C 0.0809(7) 0.0644(6) -0.2509(16) 0.145(8) Uani 1 1 d D . . H61A H 0.1083 0.0649 -0.2513 0.173 Uiso 1 1 calc R . . H61B H 0.0728 0.0478 -0.2961 0.173 Uiso 1 1 calc R . . C62 C 0.0666(12) 0.1030(8) -0.268(2) 0.246(7) Uiso 1 1 d D . . H62A H 0.0815 0.1208 -0.2360 0.295 Uiso 1 1 calc R . . H62B H 0.0408 0.1046 -0.2484 0.295 Uiso 1 1 calc R . . C63 C 0.0677(18) 0.1143(16) -0.361(3) 0.380(15) Uiso 1 1 d D . . H63A H 0.0677 0.0918 -0.3966 0.456 Uiso 1 1 calc R . . H63B H 0.0454 0.1287 -0.3751 0.456 Uiso 1 1 calc R . . C64 C 0.102(2) 0.137(2) -0.380(5) 0.48(2) Uiso 1 1 d D . . H64A H 0.1136 0.1286 -0.4320 0.725 Uiso 1 1 calc R . . H64B H 0.1199 0.1349 -0.3343 0.725 Uiso 1 1 calc R . . H64C H 0.0952 0.1633 -0.3865 0.725 Uiso 1 1 calc R . . S1 S 0.18245(15) 0.09633(17) -0.0039(4) 0.1228(15) Uani 1 1 d . . . O11 O 0.1738(4) 0.0695(5) 0.0620(10) 0.135(4) Uani 1 1 d . . . O12 O 0.1494(4) 0.1109(4) -0.0427(10) 0.136(4) Uani 1 1 d . . . O13 O 0.2073(4) 0.1245(5) 0.0233(10) 0.141(5) Uani 1 1 d . . . O14 O 0.2871(6) 0.0484(8) -0.1284(14) 0.200(10) Uani 1 1 d . . . N1 N 0.2413(7) 0.0584(7) -0.2142(11) 0.156(7) Uani 1 1 d . . . H1 H 0.2332 0.0528 -0.2641 0.187 Uiso 1 1 calc R . . C1 C 0.2057(6) 0.0691(6) -0.0818(12) 0.120(6) Uani 1 1 d . . . H1A H 0.2281 0.0587 -0.0556 0.144 Uiso 1 1 calc R . . H1B H 0.1894 0.0481 -0.0957 0.144 Uiso 1 1 calc R . . C2 C 0.2176(7) 0.0871(7) -0.1644(17) 0.137(7) Uani 1 1 d . . . C3 C 0.2457(11) 0.1208(9) -0.149(2) 0.214(16) Uani 1 1 d . . . H3A H 0.2399 0.1328 -0.0960 0.321 Uiso 1 1 calc R . . H3B H 0.2434 0.1387 -0.1945 0.321 Uiso 1 1 calc R . . H3C H 0.2711 0.1114 -0.1474 0.321 Uiso 1 1 calc R . . C4 C 0.1841(7) 0.0956(9) -0.2173(19) 0.170(10) Uani 1 1 d . . . H4A H 0.1689 0.0733 -0.2228 0.255 Uiso 1 1 calc R . . H4B H 0.1921 0.1038 -0.2726 0.255 Uiso 1 1 calc R . . H4C H 0.1696 0.1151 -0.1907 0.255 Uiso 1 1 calc R . . C5 C 0.2715(9) 0.0419(10) -0.191(2) 0.161(11) Uani 1 1 d . . . C6 C 0.2805(12) 0.0166(12) -0.262(3) 0.25(2) Uani 1 1 d . . . H6 H 0.2632 0.0149 -0.3059 0.299 Uiso 1 1 calc R . . C7 C 0.3077(15) -0.0013(15) -0.266(3) 0.28(3) Uani 1 1 d . . . H7A H 0.3254 -0.0001 -0.2222 0.335 Uiso 1 1 calc R . . H7B H 0.3118 -0.0168 -0.3123 0.335 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 0.1045(8) 0.1027(8) 0.1172(9) -0.0045(7) -0.0031(7) 0.0119(6) Sn2 0.0908(7) 0.1141(8) 0.1102(9) -0.0091(7) -0.0063(6) 0.0106(6) Sn3 0.1120(9) 0.1246(9) 0.0935(8) -0.0063(7) -0.0109(6) 0.0097(7) Sn4 0.1090(8) 0.1108(8) 0.1041(8) -0.0246(6) -0.0007(6) 0.0079(6) Sn5 0.1027(8) 0.1105(8) 0.1109(9) -0.0210(7) -0.0074(6) -0.0003(6) Sn6 0.1028(8) 0.1102(8) 0.1032(8) -0.0067(6) 0.0013(6) 0.0033(6) O1 0.115(8) 0.115(8) 0.098(7) -0.016(6) -0.011(6) 0.003(6) O2 0.095(7) 0.111(7) 0.112(8) -0.019(6) -0.004(6) 0.009(6) O3 0.096(6) 0.095(6) 0.089(6) -0.011(5) -0.002(5) 0.001(5) O4 0.105(7) 0.124(8) 0.105(8) 0.003(7) -0.009(6) 0.021(6) O5 0.098(7) 0.116(8) 0.107(8) -0.013(6) 0.004(6) -0.002(6) O6 0.097(7) 0.123(8) 0.113(8) -0.012(7) -0.010(6) 0.013(6) O7 0.110(8) 0.096(7) 0.114(8) -0.006(6) 0.009(6) -0.003(6) O8 0.093(7) 0.129(9) 0.129(9) -0.016(7) -0.004(6) 0.025(6) O9 0.096(7) 0.112(8) 0.113(8) -0.008(6) -0.002(6) 0.018(6) O10 0.090(6) 0.111(7) 0.117(8) -0.004(6) -0.004(6) 0.009(5) C11 0.124(15) 0.085(11) 0.26(3) 0.002(15) -0.010(18) -0.008(10) C21 0.096(11) 0.155(18) 0.140(17) 0.007(14) 0.003(11) 0.003(11) C31 0.24(3) 0.34(5) 0.098(16) -0.02(2) -0.062(19) 0.10(3) C41 0.176(19) 0.124(14) 0.104(13) -0.046(11) 0.011(13) 0.022(13) C51 0.148(17) 0.123(14) 0.143(17) -0.046(13) -0.017(14) -0.032(12) C61 0.148(17) 0.117(14) 0.17(2) 0.024(14) -0.028(16) -0.010(13) S1 0.110(3) 0.145(4) 0.114(4) -0.024(3) -0.006(3) -0.013(3) O11 0.106(8) 0.166(12) 0.133(11) -0.011(10) -0.002(8) -0.017(8) O12 0.111(9) 0.149(11) 0.148(12) -0.027(9) -0.002(8) -0.013(8) O13 0.121(9) 0.162(12) 0.139(11) -0.049(10) -0.011(8) -0.004(9) O14 0.148(14) 0.32(3) 0.130(14) 0.019(17) -0.006(12) 0.054(16) N1 0.187(19) 0.193(19) 0.088(10) -0.024(12) 0.017(12) 0.009(17) C1 0.119(13) 0.146(16) 0.096(12) 0.012(11) -0.007(10) 0.008(11) C2 0.124(15) 0.140(16) 0.146(19) -0.008(15) -0.015(14) 0.001(13) C3 0.25(4) 0.17(2) 0.21(3) -0.04(2) 0.10(3) -0.09(2) C4 0.142(19) 0.20(3) 0.16(2) 0.00(2) 0.000(18) 0.037(18) C5 0.14(2) 0.21(3) 0.14(2) 0.04(2) 0.024(17) 0.07(2) C6 0.20(3) 0.23(4) 0.31(5) 0.00(4) 0.08(4) 0.11(3) C7 0.30(5) 0.32(6) 0.22(4) 0.07(4) 0.10(4) 0.09(5) _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 O4 2.024(12) . ? Sn1 O9 2.027(12) . ? Sn1 O2 2.075(12) . ? Sn1 O1 2.063(11) . ? Sn1 C11 2.14(2) . ? Sn1 Sn3 3.1936(19) . ? Sn1 Sn4 3.202(2) . ? Sn1 Sn2 3.292(2) . ? Sn2 O3 2.078(10) . ? Sn2 O6 2.129(12) . ? Sn2 O2 2.123(11) . ? Sn2 O1 2.149(12) . ? Sn2 O8 2.136(14) . ? Sn2 C21 2.155(19) . ? Sn2 Sn6 3.283(2) . ? Sn2 Sn5 3.2916(19) . ? Sn3 O5 2.021(12) . ? Sn3 O1 1.998(12) . ? Sn3 O4 2.062(13) . ? Sn3 O10 2.093(11) . ? Sn3 C31 2.13(2) . ? Sn3 Sn4 3.208(2) 9 ? Sn3 Sn6 3.2851(19) 9 ? Sn4 O10 2.007(12) 9 ? Sn4 O2 2.030(11) . ? Sn4 C41 2.016(16) . ? Sn4 O5 2.085(11) 9 ? Sn4 O9 2.084(13) . ? Sn4 Sn3 3.208(2) 9 ? Sn5 O3 2.057(10) . ? Sn5 O6 2.086(11) . ? Sn5 O9 2.110(11) 9 ? Sn5 O7 2.126(12) . ? Sn5 O5 2.121(12) . ? Sn5 C51 2.169(17) . ? Sn5 Sn6 3.289(2) . ? Sn6 O3 2.088(11) . ? Sn6 C61 2.11(2) . ? Sn6 O7 2.112(11) . ? Sn6 O8 2.107(11) . ? Sn6 O4 2.113(11) 9 ? Sn6 O10 2.117(12) 9 ? Sn6 Sn3 3.2851(19) 9 ? O4 Sn6 2.113(11) 9 ? O5 Sn4 2.085(11) 9 ? O9 Sn5 2.110(11) 9 ? O10 Sn4 2.007(12) 9 ? O10 Sn6 2.117(12) 9 ? C11 C12 1.45(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.47(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.44(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9500 . ? C14 H14B 0.9600 . ? C14 H14C 0.9700 . ? C21 C22 1.46(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.46(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.46(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9500 . ? C24 H24B 0.9765 . ? C24 H24C 0.9500 . ? C31 C32 1.46(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.50(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.46(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C41 C42 1.46(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.48(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.47(9) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9500 . ? C44 H44C 0.9500 . ? C51 C52 1.43(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.41(6) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.46(9) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9500 . ? C54 H54C 0.9600 . ? C61 C62 1.49(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.52(6) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.49(9) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9601 . ? C64 H64B 0.9601 . ? C64 H64C 0.9601 . ? S1 O13 1.403(15) . ? S1 O12 1.419(16) . ? S1 O11 1.441(16) . ? S1 C1 1.76(2) . ? O14 C5 1.15(3) . ? N1 C5 1.28(3) . ? N1 C2 1.53(3) . ? N1 H1 0.8600 . ? C1 C2 1.51(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.48(3) . ? C2 C3 1.58(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9603 . ? C4 H4B 0.9603 . ? C4 H4C 0.9603 . ? C5 C6 1.47(5) . ? C6 C7 1.16(5) . ? C6 H6 0.9300 . ? C7 H7A 0.9300 . ? C7 H7B 0.9300 . ? 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 O4 Sn1 O9 96.6(5) . . ? O4 Sn1 O2 135.8(5) . . ? O9 Sn1 O2 77.6(5) . . ? O4 Sn1 O1 76.3(5) . . ? O9 Sn1 O1 136.0(5) . . ? O2 Sn1 O1 78.3(5) . . ? O4 Sn1 C11 108.6(8) . . ? O9 Sn1 C11 112.1(8) . . ? O2 Sn1 C11 114.2(8) . . ? O1 Sn1 C11 111.3(8) . . ? O4 Sn1 Sn3 39.0(4) . . ? O9 Sn1 Sn3 120.7(3) . . ? O2 Sn1 Sn3 107.1(3) . . ? O1 Sn1 Sn3 37.4(3) . . ? C11 Sn1 Sn3 117.9(8) . . ? O4 Sn1 Sn4 120.8(3) . . ? O9 Sn1 Sn4 39.5(4) . . ? O2 Sn1 Sn4 38.2(3) . . ? O1 Sn1 Sn4 107.5(3) . . ? C11 Sn1 Sn4 122.5(8) . . ? Sn3 Sn1 Sn4 118.78(5) . . ? O4 Sn1 Sn2 109.4(4) . . ? O9 Sn1 Sn2 109.9(4) . . ? O2 Sn1 Sn2 38.9(3) . . ? O1 Sn1 Sn2 39.5(3) . . ? C11 Sn1 Sn2 118.0(6) . . ? Sn3 Sn1 Sn2 72.27(4) . . ? Sn4 Sn1 Sn2 72.27(4) . . ? O3 Sn2 O6 75.1(4) . . ? O3 Sn2 O2 88.1(4) . . ? O6 Sn2 O2 159.0(4) . . ? O3 Sn2 O1 86.4(4) . . ? O6 Sn2 O1 90.9(5) . . ? O2 Sn2 O1 75.4(4) . . ? O3 Sn2 O8 76.7(4) . . ? O6 Sn2 O8 95.3(5) . . ? O2 Sn2 O8 92.8(5) . . ? O1 Sn2 O8 159.8(4) . . ? O3 Sn2 C21 169.7(7) . . ? O6 Sn2 C21 98.3(7) . . ? O2 Sn2 C21 100.0(7) . . ? O1 Sn2 C21 101.7(7) . . ? O8 Sn2 C21 96.4(7) . . ? O3 Sn2 Sn6 38.1(3) . . ? O6 Sn2 Sn6 87.8(3) . . ? O2 Sn2 Sn6 86.4(3) . . ? O1 Sn2 Sn6 122.5(3) . . ? O8 Sn2 Sn6 39.0(3) . . ? C21 Sn2 Sn6 135.3(6) . . ? O3 Sn2 Sn5 37.0(3) . . ? O6 Sn2 Sn5 38.2(3) . . ? O2 Sn2 Sn5 123.3(3) . . ? O1 Sn2 Sn5 85.7(3) . . ? O8 Sn2 Sn5 87.4(3) . . ? C21 Sn2 Sn5 136.4(7) . . ? Sn6 Sn2 Sn5 60.05(4) . . ? O3 Sn2 Sn1 88.3(3) . . ? O6 Sn2 Sn1 127.4(4) . . ? O2 Sn2 Sn1 37.8(3) . . ? O1 Sn2 Sn1 37.7(3) . . ? O8 Sn2 Sn1 129.3(3) . . ? C21 Sn2 Sn1 102.0(6) . . ? Sn6 Sn2 Sn1 109.01(5) . . ? Sn5 Sn2 Sn1 108.87(5) . . ? O5 Sn3 O1 98.6(5) . . ? O5 Sn3 O4 136.1(5) . . ? O1 Sn3 O4 76.9(5) . . ? O5 Sn3 O10 76.7(5) . . ? O1 Sn3 O10 136.4(5) . . ? O4 Sn3 O10 77.6(5) . . ? O5 Sn3 C31 110.7(12) . . ? O1 Sn3 C31 113.5(9) . . ? O4 Sn3 C31 110.9(12) . . ? O10 Sn3 C31 108.4(9) . . ? O5 Sn3 Sn1 122.1(3) . . ? O1 Sn3 Sn1 38.9(3) . . ? O4 Sn3 Sn1 38.2(3) . . ? O10 Sn3 Sn1 107.3(3) . . ? C31 Sn3 Sn1 121.0(11) . . ? O5 Sn3 Sn4 39.3(3) . 9 ? O1 Sn3 Sn4 122.0(4) . 9 ? O4 Sn3 Sn4 106.4(3) . 9 ? O10 Sn3 Sn4 37.6(3) . 9 ? C31 Sn3 Sn4 118.0(10) . 9 ? Sn1 Sn3 Sn4 119.05(5) . 9 ? O5 Sn3 Sn6 109.7(3) . 9 ? O1 Sn3 Sn6 109.7(3) . 9 ? O4 Sn3 Sn6 38.7(3) . 9 ? O10 Sn3 Sn6 39.0(3) . 9 ? C31 Sn3 Sn6 113.6(9) . 9 ? Sn1 Sn3 Sn6 72.43(4) . 9 ? Sn4 Sn3 Sn6 71.89(4) 9 9 ? O10 Sn4 O2 97.0(5) 9 . ? O10 Sn4 C41 110.9(8) 9 . ? O2 Sn4 C41 114.6(7) . . ? O10 Sn4 O5 77.2(5) 9 9 ? O2 Sn4 O5 135.8(4) . 9 ? C41 Sn4 O5 108.1(7) . 9 ? O10 Sn4 O9 134.7(5) 9 . ? O2 Sn4 O9 77.3(5) . . ? C41 Sn4 O9 112.3(8) . . ? O5 Sn4 O9 76.9(4) 9 . ? O10 Sn4 Sn1 120.3(3) 9 . ? O2 Sn4 Sn1 39.2(3) . . ? C41 Sn4 Sn1 122.8(6) . . ? O5 Sn4 Sn1 106.5(3) 9 . ? O9 Sn4 Sn1 38.2(3) . . ? O10 Sn4 Sn3 39.5(3) 9 9 ? O2 Sn4 Sn3 120.6(3) . 9 ? C41 Sn4 Sn3 118.0(6) . 9 ? O5 Sn4 Sn3 37.9(3) 9 9 ? O9 Sn4 Sn3 105.4(3) . 9 ? Sn1 Sn4 Sn3 117.43(5) . 9 ? O3 Sn5 O6 76.4(4) . . ? O3 Sn5 O9 88.4(4) . 9 ? O6 Sn5 O9 160.7(5) . 9 ? O3 Sn5 O7 76.5(4) . . ? O6 Sn5 O7 96.1(5) . . ? O9 Sn5 O7 91.7(5) 9 . ? O3 Sn5 O5 88.6(4) . . ? O6 Sn5 O5 92.1(5) . . ? O9 Sn5 O5 75.5(5) 9 . ? O7 Sn5 O5 160.8(5) . . ? O3 Sn5 C51 169.5(7) . . ? O6 Sn5 C51 95.0(7) . . ? O9 Sn5 C51 101.2(7) 9 . ? O7 Sn5 C51 98.8(7) . . ? O5 Sn5 C51 97.7(7) . . ? O3 Sn5 Sn6 37.8(3) . . ? O6 Sn5 Sn6 88.3(3) . . ? O9 Sn5 Sn6 86.7(3) 9 . ? O7 Sn5 Sn6 38.9(3) . . ? O5 Sn5 Sn6 124.4(3) . . ? C51 Sn5 Sn6 137.6(7) . . ? O3 Sn5 Sn2 37.5(3) . . ? O6 Sn5 Sn2 39.1(3) . . ? O9 Sn5 Sn2 124.1(3) 9 . ? O7 Sn5 Sn2 87.7(3) . . ? O5 Sn5 Sn2 87.7(3) . . ? C51 Sn5 Sn2 134.1(6) . . ? Sn6 Sn5 Sn2 59.85(4) . . ? O3 Sn6 C61 172.2(7) . . ? O3 Sn6 O7 76.1(4) . . ? C61 Sn6 O7 99.7(7) . . ? O3 Sn6 O8 77.2(5) . . ? C61 Sn6 O8 96.9(7) . . ? O7 Sn6 O8 94.9(5) . . ? O3 Sn6 O4 87.4(4) . 9 ? C61 Sn6 O4 99.3(7) . 9 ? O7 Sn6 O4 91.6(5) . 9 ? O8 Sn6 O4 161.3(5) . 9 ? O3 Sn6 O10 88.4(4) . 9 ? C61 Sn6 O10 97.0(7) . 9 ? O7 Sn6 O10 160.6(5) . 9 ? O8 Sn6 O10 92.9(5) . 9 ? O4 Sn6 O10 75.9(5) 9 9 ? O3 Sn6 Sn2 37.9(3) . . ? C61 Sn6 Sn2 136.5(6) . . ? O7 Sn6 Sn2 88.1(3) . . ? O8 Sn6 Sn2 39.6(4) . . ? O4 Sn6 Sn2 123.4(3) 9 . ? O10 Sn6 Sn2 86.6(3) 9 . ? O3 Sn6 Sn3 89.2(3) . 9 ? C61 Sn6 Sn3 98.5(7) . 9 ? O7 Sn6 Sn3 128.2(3) . 9 ? O8 Sn6 Sn3 130.3(4) . 9 ? O4 Sn6 Sn3 37.6(3) 9 9 ? O10 Sn6 Sn3 38.4(3) 9 9 ? Sn2 Sn6 Sn3 109.99(5) . 9 ? O3 Sn6 Sn5 37.1(3) . . ? C61 Sn6 Sn5 138.9(7) . . ? O7 Sn6 Sn5 39.2(3) . . ? O8 Sn6 Sn5 87.9(4) . . ? O4 Sn6 Sn5 86.1(3) 9 . ? O10 Sn6 Sn5 123.6(3) 9 . ? Sn2 Sn6 Sn5 60.11(4) . . ? Sn3 Sn6 Sn5 109.30(5) 9 . ? Sn3 O1 Sn1 103.7(5) . . ? Sn3 O1 Sn2 134.6(6) . . ? Sn1 O1 Sn2 102.8(5) . . ? Sn4 O2 Sn1 102.6(5) . . ? Sn4 O2 Sn2 134.5(6) . . ? Sn1 O2 Sn2 103.3(5) . . ? Sn5 O3 Sn2 105.5(5) . . ? Sn5 O3 Sn6 105.0(5) . . ? Sn2 O3 Sn6 104.0(4) . . ? Sn1 O4 Sn3 102.8(5) . . ? Sn1 O4 Sn6 135.4(6) . 9 ? Sn3 O4 Sn6 103.8(5) . 9 ? Sn3 O5 Sn4 102.8(5) . 9 ? Sn3 O5 Sn5 132.8(6) . . ? Sn4 O5 Sn5 103.5(5) 9 . ? Sn5 O6 Sn2 102.7(5) . . ? Sn6 O7 Sn5 101.8(5) . . ? Sn6 O8 Sn2 101.4(5) . . ? Sn1 O9 Sn4 102.3(5) . . ? Sn1 O9 Sn5 134.7(6) . 9 ? Sn4 O9 Sn5 104.0(5) . 9 ? Sn4 O10 Sn3 102.9(5) 9 . ? Sn4 O10 Sn6 135.1(6) 9 9 ? Sn3 O10 Sn6 102.6(5) . 9 ? C12 C11 Sn1 113.9(19) . . ? C12 C11 H11A 108.0 . . ? Sn1 C11 H11A 108.3 . . ? C12 C11 H11B 109.0 . . ? Sn1 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 109(3) . . ? C13 C12 H12A 109.9 . . ? C11 C12 H12A 110.0 . . ? C13 C12 H12B 111.0 . . ? C11 C12 H12B 110.3 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 118(3) . . ? C14 C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C14 C13 H13B 107.0 . . ? C12 C13 H13B 108.0 . . ? H13A C13 H13B 107.0 . . ? C13 C14 H14A 110.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 110.0 . . ? C13 C14 H14C 109.0 . . ? H14A C14 H14C 109.0 . . ? H14B C14 H14C 109.0 . . ? C22 C21 Sn2 113.4(17) . . ? C22 C21 H21A 108.9 . . ? Sn2 C21 H21A 109.0 . . ? C22 C21 H21B 108.6 . . ? Sn2 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 117(3) . . ? C21 C22 H22A 107.6 . . ? C23 C22 H22A 108.0 . . ? C21 C22 H22B 107.8 . . ? C23 C22 H22B 108.0 . . ? H22A C22 H22B 107.2 . . ? C24 C23 C22 112(3) . . ? C24 C23 H23A 110.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 110.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 110.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 108.3 . . ? C23 C24 H24C 110.0 . . ? H24A C24 H24C 111.0 . . ? H24B C24 H24C 109.0 . . ? C32 C31 Sn3 114(2) . . ? C32 C31 H31A 109.0 . . ? Sn3 C31 H31A 108.8 . . ? C32 C31 H31B 108.1 . . ? Sn3 C31 H31B 108.3 . . ? H31A C31 H31B 107.6 . . ? C31 C32 C33 112(3) . . ? C31 C32 H32A 110.0 . . ? C33 C32 H32A 108.0 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 111(3) . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33B 110.0 . . ? C32 C33 H33B 110.0 . . ? H33A C33 H33B 108.1 . . ? C33 C34 H34A 110.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 109.0 . . ? C33 C34 H34C 109.0 . . ? H34A C34 H34C 110.0 . . ? H34B C34 H34C 109.0 . . ? C42 C41 Sn4 116.9(18) . . ? C42 C41 H41A 108.1 . . ? Sn4 C41 H41A 108.1 . . ? C42 C41 H41B 108.5 . . ? Sn4 C41 H41B 107.7 . . ? H41A C41 H41B 107.2 . . ? C41 C42 C43 112(3) . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42B 109.2 . . ? C43 C42 H42B 109.1 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 110(3) . . ? C44 C43 H43A 110.5 . . ? C42 C43 H43A 109.8 . . ? C44 C43 H43B 109.1 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.1 . . ? C43 C44 H44A 108.0 . . ? C43 C44 H44B 109.0 . . ? H44A C44 H44B 111.0 . . ? C43 C44 H44C 108.0 . . ? H44A C44 H44C 110.0 . . ? H44B C44 H44C 111.0 . . ? C52 C51 Sn5 116.2(19) . . ? C52 C51 H51A 109.0 . . ? Sn5 C51 H51A 108.5 . . ? C52 C51 H51B 108.3 . . ? Sn5 C51 H51B 108.1 . . ? H51A C51 H51B 107.4 . . ? C53 C52 C51 124(3) . . ? C53 C52 H52A 106.9 . . ? C51 C52 H52A 106.9 . . ? C53 C52 H52B 105.4 . . ? C51 C52 H52B 106.1 . . ? H52A C52 H52B 106.5 . . ? C52 C53 C54 119(3) . . ? C52 C53 H53A 108.0 . . ? C54 C53 H53A 108.0 . . ? C52 C53 H53B 107.0 . . ? C54 C53 H53B 107.0 . . ? H53A C53 H53B 107.1 . . ? C53 C54 H54A 109.0 . . ? C53 C54 H54B 110.0 . . ? H54A C54 H54B 110.0 . . ? C53 C54 H54C 109.0 . . ? H54A C54 H54C 109.0 . . ? H54B C54 H54C 110.0 . . ? C62 C61 Sn6 113.3(19) . . ? C62 C61 H61A 109.2 . . ? Sn6 C61 H61A 108.7 . . ? C62 C61 H61B 109.0 . . ? Sn6 C61 H61B 108.8 . . ? H61A C61 H61B 107.6 . . ? C61 C62 C63 114(3) . . ? C61 C62 H62A 108.7 . . ? C63 C62 H62A 108.6 . . ? C61 C62 H62B 109.2 . . ? C63 C62 H62B 108.1 . . ? H62A C62 H62B 107.6 . . ? C64 C63 C62 111(3) . . ? C64 C63 H63A 109.0 . . ? C62 C63 H63A 109.2 . . ? C64 C63 H63B 110.0 . . ? C62 C63 H63B 110.0 . . ? H63A C63 H63B 108.1 . . ? C63 C64 H64A 111.0 . . ? C63 C64 H64B 109.0 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 110.3 . . ? H64A C64 H64C 108.0 . . ? H64B C64 H64C 109.5 . . ? O13 S1 O12 113.0(10) . . ? O13 S1 O11 112.8(10) . . ? O12 S1 O11 112.0(9) . . ? O13 S1 C1 107.9(10) . . ? O12 S1 C1 106.7(9) . . ? O11 S1 C1 103.7(10) . . ? C5 N1 C2 128(2) . . ? C5 N1 H1 116.0 . . ? C2 N1 H1 115.9 . . ? C2 C1 S1 119.9(16) . . ? C2 C1 H1A 107.4 . . ? S1 C1 H1A 107.4 . . ? C2 C1 H1B 107.3 . . ? S1 C1 H1B 107.3 . . ? H1A C1 H1B 106.9 . . ? C1 C2 N1 108.2(19) . . ? C1 C2 C4 110(2) . . ? N1 C2 C4 107(2) . . ? C1 C2 C3 111(2) . . ? N1 C2 C3 104(2) . . ? C4 C2 C3 116(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 110.0 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 110.0 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.4 . . ? C2 C4 H4B 109.4 . . ? H4A C4 H4B 109.4 . . ? C2 C4 H4C 109.7 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.4 . . ? O14 C5 N1 124(3) . . ? O14 C5 C6 132(3) . . ? N1 C5 C6 104(3) . . ? C7 C6 C5 124(6) . . ? C7 C6 H6 118.2 . . ? C5 C6 H6 117.7 . . ? C6 C7 H7A 120.7 . . ? C6 C7 H7B 119.3 . . ? H7A C7 H7B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.037 _refine_diff_density_min -1.332 _refine_diff_density_rms 0.380