# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jose Goicoechea' _publ_contact_author_email JOSE.GOICOECHEA@CHEM.OX.AC.UK _publ_section_title ; Reductive cleavage of Zn-C bonds by group 14 Zintl anions: Synthesis and characterisation of [E9ZnR]3- (E = Ge, Sn, Pb; R = Mes, iPr) ; _publ_contact_author ; Dr. J. M. Goicoechea Chemistry Research Laboratory University of Oxford Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_phone '+44 1865 275961' loop_ _publ_author_name 'Jose Goicoechea' 'Mark S. Denning' 'Carl Jones' 'Binbin Zhou.' # Attachment 'combined_revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 700660' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)]3[Ge9Zn(C9H11)] ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K-(2,2,2-crypt))3(Ge9Zn(C9H11)) _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), C9 H11 Ge9 Zn' _chemical_formula_sum 'C63 H119 Ge9 K3 N6 O18 Zn' _chemical_formula_weight 2084.62 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' K K 0.2009 0.2494 '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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 17.38970(10) _cell_length_b 22.46850(20) _cell_length_c 22.09430(20) _cell_angle_alpha 90.0000 _cell_angle_beta 98.0425(3) _cell_angle_gamma 90.0000 _cell_volume 8547.789(119) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4232 _exptl_absorpt_coefficient_mu 3.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4787 _exptl_absorpt_correction_T_max 0.7616 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29330 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14916 _reflns_number_gt 11538 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The maximum residual electron density for this structure is rather high (3.77e/A), however upon inspection we found this to be chemically insignificant. The largest Q peak is located at 1.15 Angstrom from Ge3 and is thus too close to be considered as an additional atomic position. The presence of large peaks near heavy cluster atoms is a common phenomenon and frequently observed in other structures of Zintl ion containing species. ; _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^)+(0.0698P)^2^+34.7056P] 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 14916 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _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 Ge1 Ge 0.28709(5) 0.58800(4) 0.62168(3) 0.0542(2) Uani 1 1 d . . . Ge2 Ge 0.21952(4) 0.66347(3) 0.68272(3) 0.04355(18) Uani 1 1 d . . . Ge3 Ge 0.36584(4) 0.61620(3) 0.72372(3) 0.04029(17) Uani 1 1 d . . . Ge4 Ge 0.30609(4) 0.49802(3) 0.69615(3) 0.04519(18) Uani 1 1 d . . . Ge5 Ge 0.16001(4) 0.54902(3) 0.65521(3) 0.04411(18) Uani 1 1 d . . . Ge6 Ge 0.27555(4) 0.65519(3) 0.79578(3) 0.03837(17) Uani 1 1 d . . . Ge7 Ge 0.33987(4) 0.54066(3) 0.80351(3) 0.03858(17) Uani 1 1 d . . . Ge8 Ge 0.19214(4) 0.49396(3) 0.75800(3) 0.04169(17) Uani 1 1 d . . . Ge9 Ge 0.13225(3) 0.60832(3) 0.74901(3) 0.03629(16) Uani 1 1 d . . . Zn1 Zn 0.21545(4) 0.56910(3) 0.84927(4) 0.04436(19) Uani 1 1 d . . . K1 K 0.44834(7) 0.27173(6) 0.98374(6) 0.0408(3) Uani 1 1 d . . . K2 K 0.07137(7) 0.25608(6) 1.01967(6) 0.0355(3) Uani 1 1 d . . . K3 K 0.26112(7) 0.52773(5) 1.31645(6) 0.0356(3) Uani 1 1 d . . . C1 C 0.1970(4) 0.5609(3) 0.9363(3) 0.0474(16) Uani 1 1 d . . . C2 C 0.1241(4) 0.5446(3) 0.9518(3) 0.0511(17) Uani 1 1 d . . . C3 C 0.1145(5) 0.5322(3) 1.0120(4) 0.060(2) Uani 1 1 d . . . H3 H 0.0641 0.5231 1.0214 0.072 Uiso 1 1 calc R . . C4 C 0.1770(5) 0.5329(3) 1.0586(4) 0.062(2) Uani 1 1 d . . . C5 C 0.2495(5) 0.5497(3) 1.0445(3) 0.061(2) Uani 1 1 d . . . H5 H 0.2933 0.5499 1.0754 0.074 Uiso 1 1 calc R . . C6 C 0.2580(4) 0.5663(3) 0.9848(3) 0.0532(17) Uani 1 1 d . . . C7 C 0.0530(5) 0.5401(4) 0.9026(4) 0.065(2) Uani 1 1 d . . . H7A H 0.0683 0.5492 0.8625 0.097 Uiso 1 1 calc R . . H7B H 0.0135 0.5686 0.9115 0.097 Uiso 1 1 calc R . . H7C H 0.0318 0.4997 0.9022 0.097 Uiso 1 1 calc R . . C8 C 0.1664(7) 0.5144(5) 1.1230(4) 0.091(3) Uani 1 1 d . . . H8A H 0.1117 0.5048 1.1243 0.136 Uiso 1 1 calc R . . H8B H 0.1823 0.5471 1.1514 0.136 Uiso 1 1 calc R . . H8C H 0.1984 0.4793 1.1349 0.136 Uiso 1 1 calc R . . C9 C 0.3367(4) 0.5902(4) 0.9734(4) 0.061(2) Uani 1 1 d . . . H9A H 0.3343 0.6013 0.9303 0.091 Uiso 1 1 calc R . . H9B H 0.3763 0.5594 0.9835 0.091 Uiso 1 1 calc R . . H9C H 0.3501 0.6252 0.9991 0.091 Uiso 1 1 calc R . . C101 C 0.4294(6) 0.3429(5) 0.8286(4) 0.085(3) Uani 1 1 d . . . H10A H 0.4592 0.3791 0.8428 0.102 Uiso 1 1 calc R . . H10B H 0.4028 0.3508 0.7867 0.102 Uiso 1 1 calc R . . C102 C 0.4843(7) 0.2923(5) 0.8265(5) 0.099(4) Uani 1 1 d . . . H10C H 0.4547 0.2551 0.8168 0.118 Uiso 1 1 calc R . . H10D H 0.5169 0.2993 0.7938 0.118 Uiso 1 1 calc R . . C103 C 0.5896(7) 0.2392(5) 0.8838(6) 0.101(4) Uani 1 1 d . . . H10E H 0.6235 0.2471 0.8522 0.122 Uiso 1 1 calc R . . H10F H 0.5631 0.2007 0.8741 0.122 Uiso 1 1 calc R . . C104 C 0.6373(6) 0.2356(4) 0.9444(6) 0.096(4) Uani 1 1 d . . . H10G H 0.6809 0.2076 0.9428 0.115 Uiso 1 1 calc R . . H10H H 0.6594 0.2753 0.9562 0.115 Uiso 1 1 calc R . . C105 C 0.6354(5) 0.2035(4) 1.0451(6) 0.091(3) Uani 1 1 d . . . H10I H 0.6572 0.2408 1.0641 0.109 Uiso 1 1 calc R . . H10J H 0.6790 0.1768 1.0391 0.109 Uiso 1 1 calc R . . C106 C 0.5841(5) 0.1738(4) 1.0863(5) 0.076(3) Uani 1 1 d . . . H10K H 0.5635 0.1363 1.0668 0.091 Uiso 1 1 calc R . . H10L H 0.6165 0.1632 1.1253 0.091 Uiso 1 1 calc R . . C107 C 0.3104(5) 0.2934(3) 0.8371(3) 0.058(2) Uani 1 1 d . . . H10M H 0.3354 0.2625 0.8145 0.070 Uiso 1 1 calc R . . H10N H 0.2768 0.3177 0.8067 0.070 Uiso 1 1 calc R . . C108 C 0.2607(4) 0.2634(3) 0.8780(3) 0.0464(16) Uani 1 1 d . . . H10O H 0.2367 0.2936 0.9020 0.056 Uiso 1 1 calc R . . H10P H 0.2186 0.2410 0.8531 0.056 Uiso 1 1 calc R . . C109 C 0.2613(3) 0.1928(3) 0.9564(3) 0.0413(14) Uani 1 1 d . . . H10Q H 0.2176 0.1726 0.9310 0.050 Uiso 1 1 calc R . . H10R H 0.2395 0.2214 0.9836 0.050 Uiso 1 1 calc R . . C110 C 0.3100(4) 0.1483(3) 0.9937(3) 0.0447(15) Uani 1 1 d . . . H11A H 0.2767 0.1221 1.0150 0.054 Uiso 1 1 calc R . . H11B H 0.3378 0.1233 0.9669 0.054 Uiso 1 1 calc R . . C111 C 0.4107(5) 0.1376(3) 1.0765(4) 0.0577(19) Uani 1 1 d . . . H11C H 0.4424 0.1129 1.0523 0.069 Uiso 1 1 calc R . . H11D H 0.3767 0.1108 1.0965 0.069 Uiso 1 1 calc R . . C112 C 0.4628(5) 0.1722(4) 1.1241(3) 0.065(2) Uani 1 1 d . . . H11E H 0.4302 0.1975 1.1469 0.078 Uiso 1 1 calc R . . H11F H 0.4909 0.1438 1.1536 0.078 Uiso 1 1 calc R . . C113 C 0.3344(5) 0.3873(3) 0.8861(3) 0.064(2) Uani 1 1 d . . . H11G H 0.2864 0.3774 0.9034 0.077 Uiso 1 1 calc R . . H11H H 0.3193 0.4112 0.8487 0.077 Uiso 1 1 calc R . . C114 C 0.3863(6) 0.4247(3) 0.9321(3) 0.067(2) Uani 1 1 d . . . H11I H 0.4354 0.4339 0.9161 0.080 Uiso 1 1 calc R . . H11J H 0.3601 0.4627 0.9391 0.080 Uiso 1 1 calc R . . C115 C 0.4473(4) 0.4266(3) 1.0337(3) 0.0537(18) Uani 1 1 d . . . H11K H 0.4227 0.4660 1.0367 0.064 Uiso 1 1 calc R . . H11L H 0.4997 0.4330 1.0223 0.064 Uiso 1 1 calc R . . C116 C 0.4540(5) 0.3970(3) 1.0922(4) 0.0589(19) Uani 1 1 d . . . H11M H 0.4885 0.4204 1.1228 0.071 Uiso 1 1 calc R . . H11N H 0.4022 0.3949 1.1058 0.071 Uiso 1 1 calc R . . C117 C 0.4916(5) 0.3075(4) 1.1475(4) 0.075(3) Uani 1 1 d . . . H11O H 0.4403 0.2923 1.1549 0.090 Uiso 1 1 calc R . . H11P H 0.5112 0.3348 1.1814 0.090 Uiso 1 1 calc R . . C118 C 0.5472(5) 0.2565(4) 1.1454(4) 0.072(3) Uani 1 1 d . . . H11Q H 0.5972 0.2724 1.1357 0.086 Uiso 1 1 calc R . . H11R H 0.5571 0.2380 1.1864 0.086 Uiso 1 1 calc R . . C201 C 0.1960(5) 0.1602(4) 1.1330(3) 0.066(2) Uani 1 1 d . . . H20A H 0.2153 0.1431 1.1736 0.079 Uiso 1 1 calc R . . H20B H 0.2417 0.1677 1.1119 0.079 Uiso 1 1 calc R . . C202 C 0.1450(5) 0.1150(3) 1.0969(4) 0.066(2) Uani 1 1 d . . . H20C H 0.1736 0.0770 1.0957 0.079 Uiso 1 1 calc R . . H20D H 0.0985 0.1075 1.1170 0.079 Uiso 1 1 calc R . . C203 C 0.0683(4) 0.0972(3) 1.0024(4) 0.066(2) Uani 1 1 d . . . H20E H 0.0173 0.1007 1.0172 0.079 Uiso 1 1 calc R . . H20F H 0.0864 0.0556 1.0088 0.079 Uiso 1 1 calc R . . C204 C 0.0597(5) 0.1112(4) 0.9382(5) 0.076(3) Uani 1 1 d . . . H20G H 0.1095 0.1042 0.9223 0.091 Uiso 1 1 calc R . . H20H H 0.0198 0.0851 0.9155 0.091 Uiso 1 1 calc R . . C205 C 0.0277(4) 0.1931(4) 0.8665(3) 0.072(3) Uani 1 1 d . . . H20I H 0.0089 0.1605 0.8381 0.086 Uiso 1 1 calc R . . H20J H 0.0782 0.2071 0.8561 0.086 Uiso 1 1 calc R . . C206 C -0.0303(4) 0.2439(4) 0.8598(3) 0.069(2) Uani 1 1 d . . . H20K H -0.0396 0.2561 0.8163 0.083 Uiso 1 1 calc R . . H20L H -0.0802 0.2292 0.8709 0.083 Uiso 1 1 calc R . . C207 C 0.2170(4) 0.2612(4) 1.1651(3) 0.064(2) Uani 1 1 d . . . H20M H 0.2559 0.2424 1.1963 0.077 Uiso 1 1 calc R . . H20N H 0.1912 0.2933 1.1854 0.077 Uiso 1 1 calc R . . C208 C 0.2580(4) 0.2881(4) 1.1166(3) 0.0530(18) Uani 1 1 d . . . H20O H 0.2995 0.3153 1.1353 0.064 Uiso 1 1 calc R . . H20P H 0.2819 0.2565 1.0942 0.064 Uiso 1 1 calc R . . C209 C 0.2384(4) 0.3611(3) 1.0409(4) 0.0567(19) Uani 1 1 d . . . H20Q H 0.2749 0.3401 1.0177 0.068 Uiso 1 1 calc R . . H20R H 0.2682 0.3906 1.0680 0.068 Uiso 1 1 calc R . . C210 C 0.1774(4) 0.3921(3) 0.9975(4) 0.062(2) Uani 1 1 d . . . H21A H 0.1385 0.4106 1.0203 0.074 Uiso 1 1 calc R . . H21B H 0.2013 0.4237 0.9751 0.074 Uiso 1 1 calc R . . C211 C 0.0913(4) 0.3779(4) 0.9078(4) 0.073(3) Uani 1 1 d . . . H21C H 0.1224 0.4032 0.8838 0.087 Uiso 1 1 calc R . . H21D H 0.0540 0.4036 0.9256 0.087 Uiso 1 1 calc R . . C212 C 0.0489(4) 0.3325(5) 0.8678(4) 0.073(3) Uani 1 1 d . . . H21E H 0.0873 0.3056 0.8528 0.088 Uiso 1 1 calc R . . H21F H 0.0201 0.3527 0.8318 0.088 Uiso 1 1 calc R . . C213 C 0.1009(5) 0.2116(4) 1.1850(3) 0.064(2) Uani 1 1 d . . . H21G H 0.1285 0.2120 1.2273 0.077 Uiso 1 1 calc R . . H21H H 0.0736 0.1730 1.1784 0.077 Uiso 1 1 calc R . . C214 C 0.0422(5) 0.2605(4) 1.1781(3) 0.063(2) Uani 1 1 d . . . H21I H 0.0117 0.2597 1.2128 0.075 Uiso 1 1 calc R . . H21J H 0.0687 0.2995 1.1782 0.075 Uiso 1 1 calc R . . C215 C -0.0727(5) 0.2927(3) 1.1162(4) 0.066(2) Uani 1 1 d . . . H21K H -0.0535 0.3341 1.1208 0.079 Uiso 1 1 calc R . . H21L H -0.1046 0.2848 1.1491 0.079 Uiso 1 1 calc R . . C216 C -0.1213(4) 0.2860(3) 1.0563(4) 0.062(2) Uani 1 1 d . . . H21M H -0.1389 0.2442 1.0505 0.075 Uiso 1 1 calc R . . H21N H -0.1677 0.3118 1.0542 0.075 Uiso 1 1 calc R . . C217 C -0.1230(4) 0.3042(4) 0.9513(4) 0.063(2) Uani 1 1 d . . . H21O H -0.1699 0.3286 0.9534 0.076 Uiso 1 1 calc R . . H21P H -0.1396 0.2635 0.9383 0.076 Uiso 1 1 calc R . . C218 C -0.0748(4) 0.3314(4) 0.9057(4) 0.062(2) Uani 1 1 d . . . H21Q H -0.1081 0.3359 0.8658 0.075 Uiso 1 1 calc R . . H21R H -0.0575 0.3716 0.9201 0.075 Uiso 1 1 calc R . . C301 C 0.0445(4) 0.5558(3) 1.3185(3) 0.0496(16) Uani 1 1 d . . . H30A H -0.0022 0.5806 1.3066 0.059 Uiso 1 1 calc R . . H30B H 0.0375 0.5344 1.3565 0.059 Uiso 1 1 calc R . . C302 C 0.0512(4) 0.5111(3) 1.2690(4) 0.0512(17) Uani 1 1 d . . . H30C H 0.0031 0.4870 1.2611 0.061 Uiso 1 1 calc R . . H30D H 0.0589 0.5317 1.2307 0.061 Uiso 1 1 calc R . . C303 C 0.1138(4) 0.4188(3) 1.2577(3) 0.0468(16) Uani 1 1 d . . . H30E H 0.1143 0.4259 1.2135 0.056 Uiso 1 1 calc R . . H30F H 0.0656 0.3971 1.2628 0.056 Uiso 1 1 calc R . . C304 C 0.1829(4) 0.3833(3) 1.2834(3) 0.0475(16) Uani 1 1 d . . . H30G H 0.1872 0.3823 1.3285 0.057 Uiso 1 1 calc R . . H30H H 0.1774 0.3419 1.2680 0.057 Uiso 1 1 calc R . . C305 C 0.3182(4) 0.3746(3) 1.2827(3) 0.0443(15) Uani 1 1 d . . . H30I H 0.3122 0.3357 1.2615 0.053 Uiso 1 1 calc R . . H30J H 0.3246 0.3672 1.3273 0.053 Uiso 1 1 calc R . . C306 C 0.3883(4) 0.4058(3) 1.2665(3) 0.0456(15) Uani 1 1 d . . . H30K H 0.4327 0.3778 1.2711 0.055 Uiso 1 1 calc R . . H30L H 0.3783 0.4182 1.2231 0.055 Uiso 1 1 calc R . . C307 C 0.1207(4) 0.6176(3) 1.3934(3) 0.0490(16) Uani 1 1 d . . . H30M H 0.0695 0.6323 1.4017 0.059 Uiso 1 1 calc R . . H30N H 0.1568 0.6519 1.3970 0.059 Uiso 1 1 calc R . . C308 C 0.1499(4) 0.5725(3) 1.4411(3) 0.0523(17) Uani 1 1 d . . . H30O H 0.1495 0.5894 1.4824 0.063 Uiso 1 1 calc R . . H30P H 0.1160 0.5369 1.4369 0.063 Uiso 1 1 calc R . . C309 C 0.2573(4) 0.5124(3) 1.4756(3) 0.0509(17) Uani 1 1 d . . . H30Q H 0.2339 0.4732 1.4638 0.061 Uiso 1 1 calc R . . H30R H 0.2452 0.5226 1.5169 0.061 Uiso 1 1 calc R . . C310 C 0.3440(4) 0.5100(3) 1.4760(3) 0.0492(17) Uani 1 1 d . . . H31A H 0.3661 0.5507 1.4804 0.059 Uiso 1 1 calc R . . H31B H 0.3683 0.4857 1.5109 0.059 Uiso 1 1 calc R . . C311 C 0.4394(4) 0.4815(3) 1.4158(4) 0.0572(19) Uani 1 1 d . . . H31C H 0.4687 0.4677 1.4549 0.069 Uiso 1 1 calc R . . H31D H 0.4590 0.5213 1.4064 0.069 Uiso 1 1 calc R . . C312 C 0.4503(4) 0.4384(3) 1.3653(4) 0.0547(18) Uani 1 1 d . . . H31E H 0.5064 0.4344 1.3626 0.066 Uiso 1 1 calc R . . H31F H 0.4306 0.3988 1.3752 0.066 Uiso 1 1 calc R . . C313 C 0.1060(4) 0.6444(3) 1.2876(3) 0.0481(16) Uani 1 1 d . . . H31G H 0.0700 0.6742 1.3010 0.058 Uiso 1 1 calc R . . H31H H 0.0824 0.6294 1.2470 0.058 Uiso 1 1 calc R . . C314 C 0.1809(4) 0.6747(3) 1.2806(3) 0.0467(16) Uani 1 1 d . . . H31I H 0.1708 0.7105 1.2546 0.056 Uiso 1 1 calc R . . H31J H 0.2077 0.6873 1.3211 0.056 Uiso 1 1 calc R . . C315 C 0.2909(3) 0.6630(3) 1.2292(3) 0.0431(15) Uani 1 1 d . . . H31K H 0.3247 0.6838 1.2624 0.052 Uiso 1 1 calc R . . H31L H 0.2702 0.6928 1.1981 0.052 Uiso 1 1 calc R . . C316 C 0.3359(4) 0.6172(3) 1.2013(3) 0.0524(17) Uani 1 1 d . . . H31M H 0.3009 0.5939 1.1709 0.063 Uiso 1 1 calc R . . H31N H 0.3759 0.6364 1.1801 0.063 Uiso 1 1 calc R . . C317 C 0.4206(5) 0.5349(3) 1.2243(4) 0.066(2) Uani 1 1 d . . . H31O H 0.4593 0.5552 1.2026 0.080 Uiso 1 1 calc R . . H31P H 0.3883 0.5089 1.1947 0.080 Uiso 1 1 calc R . . C318 C 0.4614(4) 0.4981(3) 1.2762(4) 0.065(2) Uani 1 1 d . . . H31Q H 0.5016 0.4735 1.2606 0.078 Uiso 1 1 calc R . . H31R H 0.4881 0.5251 1.3077 0.078 Uiso 1 1 calc R . . N11 N 0.3708(4) 0.3315(2) 0.8692(2) 0.0500(14) Uani 1 1 d . . . N12 N 0.5194(3) 0.2097(3) 1.0997(3) 0.0539(15) Uani 1 1 d . . . N21 N 0.1587(3) 0.2165(3) 1.1418(2) 0.0500(14) Uani 1 1 d . . . N22 N -0.0064(3) 0.2960(3) 0.8969(3) 0.0534(15) Uani 1 1 d . . . N31 N 0.1127(3) 0.5948(2) 1.3308(2) 0.0398(12) Uani 1 1 d . . . N32 N 0.4088(3) 0.4584(2) 1.3050(3) 0.0431(12) Uani 1 1 d . . . O11 O 0.5320(4) 0.2864(3) 0.8830(3) 0.0775(18) Uani 1 1 d . . . O12 O 0.5908(3) 0.2159(2) 0.9885(3) 0.0760(18) Uani 1 1 d . . . O13 O 0.3072(2) 0.22372(18) 0.91828(18) 0.0371(9) Uani 1 1 d . . . O14 O 0.3646(2) 0.17832(18) 1.03733(19) 0.0409(10) Uani 1 1 d . . . O15 O 0.4024(3) 0.39244(19) 0.9881(2) 0.0508(12) Uani 1 1 d . . . O16 O 0.4838(3) 0.3398(2) 1.0889(2) 0.0672(15) Uani 1 1 d . . . O21 O 0.1220(3) 0.1357(2) 1.0365(2) 0.0526(12) Uani 1 1 d . . . O22 O 0.0376(3) 0.1713(3) 0.9296(3) 0.0771(18) Uani 1 1 d . . . O23 O 0.2024(2) 0.3199(2) 1.0762(2) 0.0476(11) Uani 1 1 d . . . O24 O 0.1411(3) 0.34857(19) 0.9555(2) 0.0493(11) Uani 1 1 d . . . O25 O -0.0081(3) 0.2526(2) 1.1221(2) 0.0481(11) Uani 1 1 d . . . O26 O -0.0766(3) 0.3023(2) 1.0096(2) 0.0526(12) Uani 1 1 d . . . O31 O 0.1165(2) 0.47370(19) 1.2894(2) 0.0465(11) Uani 1 1 d . . . O32 O 0.2513(2) 0.40985(18) 1.26540(19) 0.0409(10) Uani 1 1 d . . . O33 O 0.2271(3) 0.5563(2) 1.43296(19) 0.0464(11) Uani 1 1 d . . . O34 O 0.3588(2) 0.4847(2) 1.4206(2) 0.0481(11) Uani 1 1 d . . . O35 O 0.2285(2) 0.63383(18) 1.2531(2) 0.0410(10) Uani 1 1 d . . . O36 O 0.3724(3) 0.5784(2) 1.2486(2) 0.0485(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0543(5) 0.0652(5) 0.0445(4) -0.0124(4) 0.0123(3) -0.0052(4) Ge2 0.0406(4) 0.0389(4) 0.0526(4) 0.0088(3) 0.0113(3) 0.0039(3) Ge3 0.0324(4) 0.0417(4) 0.0481(4) -0.0050(3) 0.0106(3) -0.0042(3) Ge4 0.0330(4) 0.0439(4) 0.0592(4) -0.0189(3) 0.0086(3) 0.0039(3) Ge5 0.0373(4) 0.0447(4) 0.0472(4) -0.0091(3) -0.0053(3) -0.0044(3) Ge6 0.0366(4) 0.0284(3) 0.0506(4) -0.0070(3) 0.0078(3) -0.0030(3) Ge7 0.0328(3) 0.0334(3) 0.0477(4) -0.0014(3) -0.0008(3) 0.0031(3) Ge8 0.0363(4) 0.0318(3) 0.0582(4) -0.0004(3) 0.0107(3) -0.0006(3) Ge9 0.0255(3) 0.0358(3) 0.0487(4) 0.0014(3) 0.0090(3) 0.0049(2) Zn1 0.0404(4) 0.0431(4) 0.0504(4) 0.0045(3) 0.0092(3) 0.0009(3) K1 0.0318(7) 0.0449(8) 0.0463(8) -0.0151(6) 0.0078(6) -0.0034(6) K2 0.0315(7) 0.0395(7) 0.0361(7) -0.0072(5) 0.0070(5) -0.0011(5) K3 0.0326(7) 0.0305(6) 0.0450(7) -0.0011(5) 0.0101(5) 0.0004(5) C1 0.054(4) 0.036(3) 0.054(4) -0.001(3) 0.014(3) 0.000(3) C2 0.057(4) 0.031(3) 0.067(5) 0.000(3) 0.014(4) -0.003(3) C3 0.069(5) 0.040(4) 0.076(5) -0.013(4) 0.031(4) -0.016(3) C4 0.076(6) 0.053(4) 0.061(5) -0.019(4) 0.025(4) -0.022(4) C5 0.076(5) 0.061(5) 0.049(4) -0.011(4) 0.013(4) -0.013(4) C6 0.058(4) 0.038(4) 0.065(5) -0.010(3) 0.014(4) 0.000(3) C7 0.058(5) 0.059(5) 0.079(5) 0.019(4) 0.018(4) -0.005(4) C8 0.110(8) 0.103(8) 0.063(6) -0.009(5) 0.027(5) -0.036(6) C9 0.048(4) 0.072(5) 0.063(5) -0.017(4) 0.008(3) -0.004(4) C101 0.119(8) 0.090(7) 0.052(5) -0.008(5) 0.034(5) -0.056(6) C102 0.106(8) 0.123(9) 0.081(7) -0.050(6) 0.062(6) -0.067(7) C103 0.106(8) 0.082(7) 0.136(10) -0.042(7) 0.087(8) -0.025(6) C104 0.063(6) 0.072(6) 0.167(12) -0.034(7) 0.067(7) -0.001(5) C105 0.041(5) 0.064(6) 0.162(10) -0.031(6) -0.003(6) 0.017(4) C106 0.053(5) 0.045(4) 0.121(8) -0.015(5) -0.019(5) 0.014(4) C107 0.082(5) 0.054(4) 0.035(4) -0.001(3) -0.007(3) -0.020(4) C108 0.045(4) 0.045(4) 0.046(4) -0.006(3) -0.005(3) -0.006(3) C109 0.033(3) 0.049(4) 0.043(3) -0.010(3) 0.007(3) -0.016(3) C110 0.055(4) 0.038(3) 0.042(3) -0.005(3) 0.009(3) -0.015(3) C111 0.064(5) 0.043(4) 0.063(5) 0.007(3) -0.005(4) 0.004(3) C112 0.075(6) 0.058(5) 0.054(4) 0.008(4) -0.017(4) 0.015(4) C113 0.102(6) 0.040(4) 0.046(4) 0.008(3) -0.005(4) -0.012(4) C114 0.108(7) 0.040(4) 0.052(4) 0.002(3) 0.007(4) -0.023(4) C115 0.048(4) 0.048(4) 0.064(5) -0.022(4) 0.005(3) -0.016(3) C116 0.059(5) 0.047(4) 0.068(5) -0.017(4) -0.002(4) -0.012(3) C117 0.088(6) 0.061(5) 0.062(5) -0.032(4) -0.039(4) 0.025(4) C118 0.069(5) 0.055(5) 0.079(6) -0.021(4) -0.037(4) 0.012(4) C201 0.066(5) 0.085(6) 0.047(4) 0.030(4) 0.006(4) 0.003(4) C202 0.079(6) 0.047(4) 0.076(5) 0.023(4) 0.025(4) 0.001(4) C203 0.052(5) 0.046(4) 0.107(7) -0.030(4) 0.037(4) -0.016(3) C204 0.057(5) 0.073(6) 0.103(7) -0.054(5) 0.027(5) -0.029(4) C205 0.045(4) 0.111(7) 0.055(5) -0.047(5) -0.008(3) 0.006(4) C206 0.037(4) 0.120(7) 0.047(4) -0.015(4) -0.006(3) 0.011(4) C207 0.048(4) 0.108(7) 0.035(4) -0.007(4) 0.003(3) -0.025(4) C208 0.044(4) 0.073(5) 0.041(4) -0.013(3) 0.001(3) -0.018(3) C209 0.046(4) 0.046(4) 0.078(5) -0.010(4) 0.010(4) -0.019(3) C210 0.055(5) 0.033(4) 0.099(6) -0.002(4) 0.018(4) -0.008(3) C211 0.041(4) 0.082(6) 0.095(6) 0.047(5) 0.011(4) 0.014(4) C212 0.039(4) 0.116(7) 0.063(5) 0.038(5) 0.002(4) 0.011(4) C213 0.070(5) 0.090(6) 0.036(4) 0.000(4) 0.017(3) -0.031(5) C214 0.066(5) 0.081(6) 0.047(4) -0.019(4) 0.029(4) -0.031(4) C215 0.083(6) 0.046(4) 0.082(6) -0.001(4) 0.060(5) 0.015(4) C216 0.054(5) 0.051(4) 0.090(6) 0.020(4) 0.040(4) 0.018(4) C217 0.037(4) 0.073(5) 0.080(6) 0.001(4) 0.012(4) 0.015(4) C218 0.039(4) 0.091(6) 0.057(4) 0.013(4) 0.007(3) 0.018(4) C301 0.035(4) 0.049(4) 0.068(5) 0.001(3) 0.017(3) 0.002(3) C302 0.031(3) 0.049(4) 0.074(5) 0.002(3) 0.011(3) -0.002(3) C303 0.036(4) 0.049(4) 0.058(4) -0.007(3) 0.014(3) -0.012(3) C304 0.055(4) 0.034(3) 0.057(4) -0.003(3) 0.019(3) -0.011(3) C305 0.053(4) 0.033(3) 0.048(4) -0.005(3) 0.010(3) 0.000(3) C306 0.042(4) 0.045(4) 0.051(4) -0.005(3) 0.013(3) 0.009(3) C307 0.047(4) 0.042(4) 0.061(4) 0.003(3) 0.018(3) 0.015(3) C308 0.053(4) 0.054(4) 0.053(4) 0.008(3) 0.021(3) 0.017(3) C309 0.059(5) 0.050(4) 0.042(4) 0.002(3) 0.005(3) 0.006(3) C310 0.060(4) 0.042(4) 0.042(4) 0.003(3) -0.004(3) 0.012(3) C311 0.042(4) 0.050(4) 0.076(5) -0.013(4) -0.002(3) 0.003(3) C312 0.034(4) 0.050(4) 0.079(5) -0.010(4) 0.005(3) 0.006(3) C313 0.042(4) 0.047(4) 0.056(4) 0.009(3) 0.008(3) 0.012(3) C314 0.044(4) 0.039(4) 0.057(4) 0.009(3) 0.008(3) 0.003(3) C315 0.030(3) 0.045(4) 0.054(4) 0.013(3) 0.004(3) -0.007(3) C316 0.048(4) 0.056(4) 0.056(4) 0.008(3) 0.015(3) -0.008(3) C317 0.060(5) 0.049(4) 0.102(6) 0.008(4) 0.052(5) 0.006(4) C318 0.044(4) 0.048(4) 0.109(7) 0.001(4) 0.032(4) -0.001(3) N11 0.069(4) 0.045(3) 0.036(3) -0.001(2) 0.009(3) -0.020(3) N12 0.044(3) 0.044(3) 0.069(4) -0.012(3) -0.013(3) 0.010(3) N21 0.050(3) 0.069(4) 0.032(3) 0.000(3) 0.009(2) -0.019(3) N22 0.033(3) 0.080(4) 0.047(3) 0.001(3) 0.002(2) 0.009(3) N31 0.037(3) 0.035(3) 0.048(3) 0.006(2) 0.012(2) 0.005(2) N32 0.031(3) 0.038(3) 0.062(3) -0.002(2) 0.013(2) 0.002(2) O11 0.077(4) 0.077(4) 0.090(4) -0.038(3) 0.051(4) -0.019(3) O12 0.041(3) 0.063(3) 0.129(5) -0.034(3) 0.030(3) -0.001(3) O13 0.031(2) 0.041(2) 0.039(2) -0.0034(18) 0.0036(17) -0.0061(17) O14 0.042(2) 0.032(2) 0.046(2) -0.0025(18) -0.0039(19) -0.0061(18) O15 0.071(3) 0.041(2) 0.040(2) -0.004(2) 0.007(2) -0.023(2) O16 0.081(4) 0.058(3) 0.053(3) -0.018(2) -0.024(3) 0.026(3) O21 0.059(3) 0.039(2) 0.062(3) -0.001(2) 0.014(2) -0.015(2) O22 0.080(4) 0.078(4) 0.064(3) -0.045(3) -0.023(3) 0.028(3) O23 0.038(2) 0.053(3) 0.053(3) -0.010(2) 0.009(2) -0.015(2) O24 0.044(3) 0.041(3) 0.063(3) 0.011(2) 0.005(2) 0.004(2) O25 0.053(3) 0.045(3) 0.052(3) -0.009(2) 0.024(2) -0.003(2) O26 0.044(3) 0.049(3) 0.070(3) 0.005(2) 0.026(2) 0.010(2) O31 0.033(2) 0.040(2) 0.065(3) -0.011(2) 0.006(2) -0.0043(19) O32 0.039(2) 0.033(2) 0.053(3) 0.0016(19) 0.0138(19) -0.0018(18) O33 0.051(3) 0.048(3) 0.042(2) 0.010(2) 0.013(2) 0.017(2) O34 0.038(2) 0.048(3) 0.056(3) -0.006(2) 0.000(2) 0.011(2) O35 0.034(2) 0.036(2) 0.054(3) 0.0057(19) 0.0094(19) -0.0022(18) O36 0.044(3) 0.041(2) 0.063(3) 0.007(2) 0.017(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 Ge3 2.5486(12) . ? Ge1 Ge2 2.5529(11) . ? Ge1 Ge5 2.5801(12) . ? Ge1 Ge4 2.5984(12) . ? Ge2 Ge6 2.5579(12) . ? Ge2 Ge9 2.5703(11) . ? Ge2 Ge3 2.7889(11) . ? Ge2 Ge5 2.8066(11) . ? Ge3 Ge7 2.5327(10) . ? Ge3 Ge6 2.5431(11) . ? Ge3 Ge4 2.8852(11) . ? Ge4 Ge7 2.5495(11) . ? Ge4 Ge8 2.5613(12) . ? Ge4 Ge5 2.8181(11) . ? Ge5 Ge9 2.5659(10) . ? Ge5 Ge8 2.5780(11) . ? Ge6 Zn1 2.5644(11) . ? Ge6 Ge9 2.7687(11) . ? Ge6 Ge7 2.8015(10) . ? Ge7 Zn1 2.5930(12) . ? Ge7 Ge8 2.8264(11) . ? Ge8 Zn1 2.6177(11) . ? Ge8 Ge9 2.7693(10) . ? Ge9 Zn1 2.6230(12) . ? Zn1 C1 2.001(7) . ? K1 O12 2.765(5) . ? K1 O16 2.777(5) . ? K1 O15 2.833(5) . ? K1 O11 2.844(6) . ? K1 O13 2.878(4) . ? K1 O14 2.900(4) . ? K1 N11 3.013(6) . ? K1 N12 3.025(6) . ? K2 O26 2.755(5) . ? K2 O22 2.759(5) . ? K2 O25 2.813(4) . ? K2 O23 2.830(4) . ? K2 O21 2.852(5) . ? K2 O24 2.877(5) . ? K2 N22 2.993(6) . ? K2 N21 3.038(6) . ? K3 O31 2.782(4) . ? K3 O35 2.783(4) . ? K3 O33 2.796(4) . ? K3 O34 2.832(5) . ? K3 O36 2.845(5) . ? K3 O32 2.874(4) . ? K3 N31 3.043(5) . ? K3 N32 3.044(5) . ? C1 C6 1.403(10) . ? C1 C2 1.408(10) . ? C2 C3 1.392(11) . ? C2 C7 1.531(11) . ? C3 C4 1.389(12) . ? C3 H3 0.9500 . ? C4 C5 1.393(11) . ? C4 C8 1.518(12) . ? C5 C6 1.397(11) . ? C5 H5 0.9500 . ? C6 C9 1.524(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C101 N11 1.471(10) . ? C101 C102 1.490(15) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 O11 1.405(13) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 O11 1.458(12) . ? C103 C104 1.475(16) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 O12 1.421(11) . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 O12 1.405(12) . ? C105 C106 1.515(14) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 N12 1.448(10) . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 N11 1.460(8) . ? C107 C108 1.495(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 O13 1.429(8) . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 O13 1.421(7) . ? C109 C110 1.483(9) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 O14 1.424(7) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 O14 1.427(8) . ? C111 C112 1.505(10) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 N12 1.456(10) . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 N11 1.476(10) . ? C113 C114 1.514(10) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 O15 1.429(8) . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 O15 1.412(7) . ? C115 C116 1.443(11) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 O16 1.394(9) . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 O16 1.475(10) . ? C117 C118 1.505(10) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 N12 1.490(9) . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 N21 1.448(10) . ? C201 C202 1.502(12) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 O21 1.418(9) . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 O21 1.410(9) . ? C203 C204 1.441(13) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 O22 1.410(11) . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 O22 1.465(10) . ? C205 C206 1.516(12) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 N22 1.455(10) . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 N21 1.468(9) . ? C207 C208 1.494(10) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 O23 1.415(9) . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 O23 1.413(8) . ? C209 C210 1.497(11) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 O24 1.433(9) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 O24 1.427(9) . ? C211 C212 1.478(13) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 N22 1.478(10) . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 N21 1.484(9) . ? C213 C214 1.492(12) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 O25 1.423(9) . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 O25 1.433(9) . ? C215 C216 1.475(12) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 O26 1.424(8) . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 O26 1.420(9) . ? C217 C218 1.526(11) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 N22 1.466(9) . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? C301 N31 1.470(8) . ? C301 C302 1.502(10) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 O31 1.434(8) . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 O31 1.416(8) . ? C303 C304 1.487(10) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 O32 1.435(7) . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 O32 1.417(8) . ? C305 C306 1.492(9) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 N32 1.472(8) . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 N31 1.464(9) . ? C307 C308 1.499(9) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 O33 1.425(8) . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 O33 1.415(8) . ? C309 C310 1.506(10) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 O34 1.408(8) . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 O34 1.422(8) . ? C311 C312 1.508(10) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 N32 1.494(9) . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 N31 1.461(8) . ? C313 C314 1.498(9) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 O35 1.428(8) . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 O35 1.431(7) . ? C315 C316 1.478(10) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 O36 1.439(8) . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 O36 1.439(8) . ? C317 C318 1.509(12) . ? C317 H31O 0.9900 . ? C317 H31P 0.9900 . ? C318 N32 1.482(9) . ? C318 H31Q 0.9900 . ? C318 H31R 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ge3 Ge1 Ge2 66.28(3) . . ? Ge3 Ge1 Ge5 101.90(4) . . ? Ge2 Ge1 Ge5 66.29(3) . . ? Ge3 Ge1 Ge4 68.18(3) . . ? Ge2 Ge1 Ge4 102.09(4) . . ? Ge5 Ge1 Ge4 65.94(3) . . ? Ge1 Ge2 Ge6 109.09(4) . . ? Ge1 Ge2 Ge9 109.45(4) . . ? Ge6 Ge2 Ge9 65.35(3) . . ? Ge1 Ge2 Ge3 56.79(3) . . ? Ge6 Ge2 Ge3 56.60(3) . . ? Ge9 Ge2 Ge3 102.47(3) . . ? Ge1 Ge2 Ge5 57.32(3) . . ? Ge6 Ge2 Ge5 102.91(3) . . ? Ge9 Ge2 Ge5 56.80(3) . . ? Ge3 Ge2 Ge5 90.77(3) . . ? Ge7 Ge3 Ge6 67.00(3) . . ? Ge7 Ge3 Ge1 108.85(4) . . ? Ge6 Ge3 Ge1 109.69(4) . . ? Ge7 Ge3 Ge2 103.76(3) . . ? Ge6 Ge3 Ge2 57.11(3) . . ? Ge1 Ge3 Ge2 56.93(3) . . ? Ge7 Ge3 Ge4 55.68(3) . . ? Ge6 Ge3 Ge4 102.33(3) . . ? Ge1 Ge3 Ge4 56.73(3) . . ? Ge2 Ge3 Ge4 89.81(3) . . ? Ge7 Ge4 Ge8 67.15(3) . . ? Ge7 Ge4 Ge1 106.80(3) . . ? Ge8 Ge4 Ge1 109.04(3) . . ? Ge7 Ge4 Ge5 103.05(4) . . ? Ge8 Ge4 Ge5 57.03(3) . . ? Ge1 Ge4 Ge5 56.72(3) . . ? Ge7 Ge4 Ge3 55.14(3) . . ? Ge8 Ge4 Ge3 101.70(3) . . ? Ge1 Ge4 Ge3 55.09(3) . . ? Ge5 Ge4 Ge3 88.59(3) . . ? Ge9 Ge5 Ge8 65.15(3) . . ? Ge9 Ge5 Ge1 108.73(4) . . ? Ge8 Ge5 Ge1 109.09(4) . . ? Ge9 Ge5 Ge2 56.95(3) . . ? Ge8 Ge5 Ge2 102.77(3) . . ? Ge1 Ge5 Ge2 56.39(3) . . ? Ge9 Ge5 Ge4 102.41(4) . . ? Ge8 Ge5 Ge4 56.46(3) . . ? Ge1 Ge5 Ge4 57.34(3) . . ? Ge2 Ge5 Ge4 90.84(3) . . ? Ge3 Ge6 Ge2 66.29(3) . . ? Ge3 Ge6 Zn1 110.84(4) . . ? Ge2 Ge6 Zn1 112.39(3) . . ? Ge3 Ge6 Ge9 103.75(3) . . ? Ge2 Ge6 Ge9 57.54(3) . . ? Zn1 Ge6 Ge9 58.77(3) . . ? Ge3 Ge6 Ge7 56.32(2) . . ? Ge2 Ge6 Ge7 102.74(3) . . ? Zn1 Ge6 Ge7 57.59(3) . . ? Ge9 Ge6 Ge7 90.24(3) . . ? Ge3 Ge7 Ge4 69.18(3) . . ? Ge3 Ge7 Zn1 110.25(4) . . ? Ge4 Ge7 Zn1 111.05(4) . . ? Ge3 Ge7 Ge6 56.68(3) . . ? Ge4 Ge7 Ge6 104.51(3) . . ? Zn1 Ge7 Ge6 56.61(2) . . ? Ge3 Ge7 Ge8 104.06(4) . . ? Ge4 Ge7 Ge8 56.62(3) . . ? Zn1 Ge7 Ge8 57.57(3) . . ? Ge6 Ge7 Ge8 89.09(3) . . ? Ge4 Ge8 Ge5 66.51(3) . . ? Ge4 Ge8 Zn1 109.88(4) . . ? Ge5 Ge8 Zn1 111.12(4) . . ? Ge4 Ge8 Ge9 103.89(3) . . ? Ge5 Ge8 Ge9 57.22(3) . . ? Zn1 Ge8 Ge9 58.19(3) . . ? Ge4 Ge8 Ge7 56.23(3) . . ? Ge5 Ge8 Ge7 102.09(4) . . ? Zn1 Ge8 Ge7 56.73(3) . . ? Ge9 Ge8 Ge7 89.71(3) . . ? Ge5 Ge9 Ge2 66.24(3) . . ? Ge5 Ge9 Zn1 111.33(3) . . ? Ge2 Ge9 Zn1 110.08(3) . . ? Ge5 Ge9 Ge6 103.75(3) . . ? Ge2 Ge9 Ge6 57.11(3) . . ? Zn1 Ge9 Ge6 56.72(3) . . ? Ge5 Ge9 Ge8 57.64(3) . . ? Ge2 Ge9 Ge8 104.01(3) . . ? Zn1 Ge9 Ge8 58.01(3) . . ? Ge6 Ge9 Ge8 90.93(3) . . ? C1 Zn1 Ge6 129.98(19) . . ? C1 Zn1 Ge7 127.3(2) . . ? Ge6 Zn1 Ge7 65.80(3) . . ? C1 Zn1 Ge8 130.72(19) . . ? Ge6 Zn1 Ge8 99.24(4) . . ? Ge7 Zn1 Ge8 65.69(3) . . ? C1 Zn1 Ge9 134.3(2) . . ? Ge6 Zn1 Ge9 64.50(3) . . ? Ge7 Zn1 Ge9 98.35(4) . . ? Ge8 Zn1 Ge9 63.80(3) . . ? O12 K1 O16 97.19(17) . . ? O12 K1 O15 133.49(15) . . ? O16 K1 O15 58.33(14) . . ? O12 K1 O11 61.9(2) . . ? O16 K1 O11 120.84(19) . . ? O15 K1 O11 95.34(16) . . ? O12 K1 O13 123.03(15) . . ? O16 K1 O13 134.48(15) . . ? O15 K1 O13 98.72(13) . . ? O11 K1 O13 98.26(16) . . ? O12 K1 O14 98.91(16) . . ? O16 K1 O14 97.03(16) . . ? O15 K1 O14 121.25(13) . . ? O11 K1 O14 138.14(15) . . ? O13 K1 O14 59.49(12) . . ? O12 K1 N11 121.8(2) . . ? O16 K1 N11 118.57(15) . . ? O15 K1 N11 60.43(14) . . ? O11 K1 N11 60.54(19) . . ? O13 K1 N11 59.67(13) . . ? O14 K1 N11 118.32(14) . . ? O12 K1 N12 60.09(19) . . ? O16 K1 N12 61.86(15) . . ? O15 K1 N12 119.73(14) . . ? O11 K1 N12 121.56(19) . . ? O13 K1 N12 118.14(15) . . ? O14 K1 N12 59.33(14) . . ? N11 K1 N12 177.54(17) . . ? O26 K2 O22 95.74(16) . . ? O26 K2 O25 61.16(15) . . ? O22 K2 O25 118.83(18) . . ? O26 K2 O23 121.98(15) . . ? O22 K2 O23 138.19(16) . . ? O25 K2 O23 96.57(14) . . ? O26 K2 O21 129.48(14) . . ? O22 K2 O21 57.97(16) . . ? O25 K2 O21 92.62(14) . . ? O23 K2 O21 102.02(14) . . ? O26 K2 O24 98.09(14) . . ? O22 K2 O24 101.84(18) . . ? O25 K2 O24 134.82(14) . . ? O23 K2 O24 58.88(14) . . ? O21 K2 O24 127.27(14) . . ? O26 K2 N22 61.02(15) . . ? O22 K2 N22 61.93(18) . . ? O25 K2 N22 121.82(15) . . ? O23 K2 N22 118.82(16) . . ? O21 K2 N22 119.59(16) . . ? O24 K2 N22 60.36(15) . . ? O26 K2 N21 121.83(16) . . ? O22 K2 N21 117.92(18) . . ? O25 K2 N21 61.17(15) . . ? O23 K2 N21 58.97(15) . . ? O21 K2 N21 60.01(15) . . ? O24 K2 N21 117.14(14) . . ? N22 K2 N21 176.90(16) . . ? O31 K3 O35 98.69(13) . . ? O31 K3 O33 89.79(14) . . ? O35 K3 O33 102.23(13) . . ? O31 K3 O34 116.55(15) . . ? O35 K3 O34 139.33(14) . . ? O33 K3 O34 60.72(13) . . ? O31 K3 O36 136.27(15) . . ? O35 K3 O36 59.89(13) . . ? O33 K3 O36 129.82(15) . . ? O34 K3 O36 100.93(14) . . ? O31 K3 O32 60.73(12) . . ? O35 K3 O32 126.52(13) . . ? O33 K3 O32 124.36(13) . . ? O34 K3 O32 90.00(13) . . ? O36 K3 O32 99.75(13) . . ? O31 K3 N31 58.94(13) . . ? O35 K3 N31 60.77(13) . . ? O33 K3 N31 59.89(14) . . ? O34 K3 N31 120.38(14) . . ? O36 K3 N31 120.38(14) . . ? O32 K3 N31 119.50(14) . . ? O31 K3 N32 120.48(14) . . ? O35 K3 N32 120.75(14) . . ? O33 K3 N32 118.95(15) . . ? O34 K3 N32 58.38(14) . . ? O36 K3 N32 61.09(14) . . ? O32 K3 N32 60.06(13) . . ? N31 K3 N32 178.46(15) . . ? C6 C1 C2 116.5(6) . . ? C6 C1 Zn1 121.4(5) . . ? C2 C1 Zn1 121.9(5) . . ? C3 C2 C1 121.2(7) . . ? C3 C2 C7 118.2(7) . . ? C1 C2 C7 120.6(7) . . ? C4 C3 C2 121.3(7) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.4(7) . . ? C3 C4 C8 120.4(8) . . ? C5 C4 C8 121.1(8) . . ? C4 C5 C6 120.1(8) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 122.0(7) . . ? C5 C6 C9 117.7(7) . . ? C1 C6 C9 120.3(7) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N11 C101 C102 112.8(7) . . ? N11 C101 H10A 109.0 . . ? C102 C101 H10A 109.0 . . ? N11 C101 H10B 109.0 . . ? C102 C101 H10B 109.0 . . ? H10A C101 H10B 107.8 . . ? O11 C102 C101 110.2(7) . . ? O11 C102 H10C 109.6 . . ? C101 C102 H10C 109.6 . . ? O11 C102 H10D 109.6 . . ? C101 C102 H10D 109.6 . . ? H10C C102 H10D 108.1 . . ? O11 C103 C104 110.4(8) . . ? O11 C103 H10E 109.6 . . ? C104 C103 H10E 109.6 . . ? O11 C103 H10F 109.6 . . ? C104 C103 H10F 109.6 . . ? H10E C103 H10F 108.1 . . ? O12 C104 C103 109.7(8) . . ? O12 C104 H10G 109.7 . . ? C103 C104 H10G 109.7 . . ? O12 C104 H10H 109.7 . . ? C103 C104 H10H 109.7 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 109.0(7) . . ? O12 C105 H10I 109.9 . . ? C106 C105 H10I 109.9 . . ? O12 C105 H10J 109.9 . . ? C106 C105 H10J 109.9 . . ? H10I C105 H10J 108.3 . . ? N12 C106 C105 114.6(7) . . ? N12 C106 H10K 108.6 . . ? C105 C106 H10K 108.6 . . ? N12 C106 H10L 108.6 . . ? C105 C106 H10L 108.6 . . ? H10K C106 H10L 107.6 . . ? N11 C107 C108 114.1(5) . . ? N11 C107 H10M 108.7 . . ? C108 C107 H10M 108.7 . . ? N11 C107 H10N 108.7 . . ? C108 C107 H10N 108.7 . . ? H10M C107 H10N 107.6 . . ? O13 C108 C107 109.4(6) . . ? O13 C108 H10O 109.8 . . ? C107 C108 H10O 109.8 . . ? O13 C108 H10P 109.8 . . ? C107 C108 H10P 109.8 . . ? H10O C108 H10P 108.2 . . ? O13 C109 C110 109.5(5) . . ? O13 C109 H10Q 109.8 . . ? C110 C109 H10Q 109.8 . . ? O13 C109 H10R 109.8 . . ? C110 C109 H10R 109.8 . . ? H10Q C109 H10R 108.2 . . ? O14 C110 C109 109.3(5) . . ? O14 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O14 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.3 . . ? O14 C111 C112 109.0(6) . . ? O14 C111 H11C 109.9 . . ? C112 C111 H11C 109.9 . . ? O14 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? H11C C111 H11D 108.3 . . ? N12 C112 C111 114.4(7) . . ? N12 C112 H11E 108.7 . . ? C111 C112 H11E 108.7 . . ? N12 C112 H11F 108.7 . . ? C111 C112 H11F 108.7 . . ? H11E C112 H11F 107.6 . . ? N11 C113 C114 113.9(7) . . ? N11 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? N11 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? O15 C114 C113 109.0(5) . . ? O15 C114 H11I 109.9 . . ? C113 C114 H11I 109.9 . . ? O15 C114 H11J 109.9 . . ? C113 C114 H11J 109.9 . . ? H11I C114 H11J 108.3 . . ? O15 C115 C116 110.8(6) . . ? O15 C115 H11K 109.5 . . ? C116 C115 H11K 109.5 . . ? O15 C115 H11L 109.5 . . ? C116 C115 H11L 109.5 . . ? H11K C115 H11L 108.1 . . ? O16 C116 C115 111.2(6) . . ? O16 C116 H11M 109.4 . . ? C115 C116 H11M 109.4 . . ? O16 C116 H11N 109.4 . . ? C115 C116 H11N 109.4 . . ? H11M C116 H11N 108.0 . . ? O16 C117 C118 109.0(7) . . ? O16 C117 H11O 109.9 . . ? C118 C117 H11O 109.9 . . ? O16 C117 H11P 109.9 . . ? C118 C117 H11P 109.9 . . ? H11O C117 H11P 108.3 . . ? N12 C118 C117 114.2(6) . . ? N12 C118 H11Q 108.7 . . ? C117 C118 H11Q 108.7 . . ? N12 C118 H11R 108.7 . . ? C117 C118 H11R 108.7 . . ? H11Q C118 H11R 107.6 . . ? N21 C201 C202 114.9(7) . . ? N21 C201 H20A 108.6 . . ? C202 C201 H20A 108.6 . . ? N21 C201 H20B 108.6 . . ? C202 C201 H20B 108.6 . . ? H20A C201 H20B 107.5 . . ? O21 C202 C201 110.2(6) . . ? O21 C202 H20C 109.6 . . ? C201 C202 H20C 109.6 . . ? O21 C202 H20D 109.6 . . ? C201 C202 H20D 109.6 . . ? H20C C202 H20D 108.1 . . ? O21 C203 C204 111.2(6) . . ? O21 C203 H20E 109.4 . . ? C204 C203 H20E 109.4 . . ? O21 C203 H20F 109.4 . . ? C204 C203 H20F 109.4 . . ? H20E C203 H20F 108.0 . . ? O22 C204 C203 109.3(6) . . ? O22 C204 H20G 109.8 . . ? C203 C204 H20G 109.8 . . ? O22 C204 H20H 109.8 . . ? C203 C204 H20H 109.8 . . ? H20G C204 H20H 108.3 . . ? O22 C205 C206 109.5(6) . . ? O22 C205 H20I 109.8 . . ? C206 C205 H20I 109.8 . . ? O22 C205 H20J 109.8 . . ? C206 C205 H20J 109.8 . . ? H20I C205 H20J 108.2 . . ? N22 C206 C205 114.5(6) . . ? N22 C206 H20K 108.6 . . ? C205 C206 H20K 108.6 . . ? N22 C206 H20L 108.6 . . ? C205 C206 H20L 108.6 . . ? H20K C206 H20L 107.6 . . ? N21 C207 C208 113.6(5) . . ? N21 C207 H20M 108.8 . . ? C208 C207 H20M 108.8 . . ? N21 C207 H20N 108.8 . . ? C208 C207 H20N 108.8 . . ? H20M C207 H20N 107.7 . . ? O23 C208 C207 107.7(6) . . ? O23 C208 H20O 110.2 . . ? C207 C208 H20O 110.2 . . ? O23 C208 H20P 110.2 . . ? C207 C208 H20P 110.2 . . ? H20O C208 H20P 108.5 . . ? O23 C209 C210 109.2(6) . . ? O23 C209 H20Q 109.8 . . ? C210 C209 H20Q 109.8 . . ? O23 C209 H20R 109.8 . . ? C210 C209 H20R 109.8 . . ? H20Q C209 H20R 108.3 . . ? O24 C210 C209 107.8(6) . . ? O24 C210 H21A 110.1 . . ? C209 C210 H21A 110.1 . . ? O24 C210 H21B 110.1 . . ? C209 C210 H21B 110.1 . . ? H21A C210 H21B 108.5 . . ? O24 C211 C212 108.9(7) . . ? O24 C211 H21C 109.9 . . ? C212 C211 H21C 109.9 . . ? O24 C211 H21D 109.9 . . ? C212 C211 H21D 109.9 . . ? H21C C211 H21D 108.3 . . ? C211 C212 N22 115.0(7) . . ? C211 C212 H21E 108.5 . . ? N22 C212 H21E 108.5 . . ? C211 C212 H21F 108.5 . . ? N22 C212 H21F 108.5 . . ? H21E C212 H21F 107.5 . . ? N21 C213 C214 113.3(6) . . ? N21 C213 H21G 108.9 . . ? C214 C213 H21G 108.9 . . ? N21 C213 H21H 108.9 . . ? C214 C213 H21H 108.9 . . ? H21G C213 H21H 107.7 . . ? O25 C214 C213 108.9(6) . . ? O25 C214 H21I 109.9 . . ? C213 C214 H21I 109.9 . . ? O25 C214 H21J 109.9 . . ? C213 C214 H21J 109.9 . . ? H21I C214 H21J 108.3 . . ? O25 C215 C216 111.2(6) . . ? O25 C215 H21K 109.4 . . ? C216 C215 H21K 109.4 . . ? O25 C215 H21L 109.4 . . ? C216 C215 H21L 109.4 . . ? H21K C215 H21L 108.0 . . ? O26 C216 C215 108.7(6) . . ? O26 C216 H21M 109.9 . . ? C215 C216 H21M 109.9 . . ? O26 C216 H21N 109.9 . . ? C215 C216 H21N 109.9 . . ? H21M C216 H21N 108.3 . . ? O26 C217 C218 108.4(6) . . ? O26 C217 H21O 110.0 . . ? C218 C217 H21O 110.0 . . ? O26 C217 H21P 110.0 . . ? C218 C217 H21P 110.0 . . ? H21O C217 H21P 108.4 . . ? N22 C218 C217 113.7(6) . . ? N22 C218 H21Q 108.8 . . ? C217 C218 H21Q 108.8 . . ? N22 C218 H21R 108.8 . . ? C217 C218 H21R 108.8 . . ? H21Q C218 H21R 107.7 . . ? N31 C301 C302 113.0(5) . . ? N31 C301 H30A 109.0 . . ? C302 C301 H30A 109.0 . . ? N31 C301 H30B 109.0 . . ? C302 C301 H30B 109.0 . . ? H30A C301 H30B 107.8 . . ? O31 C302 C301 107.5(6) . . ? O31 C302 H30C 110.2 . . ? C301 C302 H30C 110.2 . . ? O31 C302 H30D 110.2 . . ? C301 C302 H30D 110.2 . . ? H30C C302 H30D 108.5 . . ? O31 C303 C304 108.1(5) . . ? O31 C303 H30E 110.1 . . ? C304 C303 H30E 110.1 . . ? O31 C303 H30F 110.1 . . ? C304 C303 H30F 110.1 . . ? H30E C303 H30F 108.4 . . ? O32 C304 C303 109.2(5) . . ? O32 C304 H30G 109.8 . . ? C303 C304 H30G 109.8 . . ? O32 C304 H30H 109.8 . . ? C303 C304 H30H 109.8 . . ? H30G C304 H30H 108.3 . . ? O32 C305 C306 109.9(5) . . ? O32 C305 H30I 109.7 . . ? C306 C305 H30I 109.7 . . ? O32 C305 H30J 109.7 . . ? C306 C305 H30J 109.7 . . ? H30I C305 H30J 108.2 . . ? N32 C306 C305 112.3(5) . . ? N32 C306 H30K 109.1 . . ? C305 C306 H30K 109.1 . . ? N32 C306 H30L 109.1 . . ? C305 C306 H30L 109.1 . . ? H30K C306 H30L 107.9 . . ? N31 C307 C308 113.9(5) . . ? N31 C307 H30M 108.8 . . ? C308 C307 H30M 108.8 . . ? N31 C307 H30N 108.8 . . ? C308 C307 H30N 108.8 . . ? H30M C307 H30N 107.7 . . ? O33 C308 C307 108.5(5) . . ? O33 C308 H30O 110.0 . . ? C307 C308 H30O 110.0 . . ? O33 C308 H30P 110.0 . . ? C307 C308 H30P 110.0 . . ? H30O C308 H30P 108.4 . . ? O33 C309 C310 107.8(6) . . ? O33 C309 H30Q 110.1 . . ? C310 C309 H30Q 110.1 . . ? O33 C309 H30R 110.1 . . ? C310 C309 H30R 110.1 . . ? H30Q C309 H30R 108.5 . . ? O34 C310 C309 108.3(5) . . ? O34 C310 H31A 110.0 . . ? C309 C310 H31A 110.0 . . ? O34 C310 H31B 110.0 . . ? C309 C310 H31B 110.0 . . ? H31A C310 H31B 108.4 . . ? O34 C311 C312 108.3(6) . . ? O34 C311 H31C 110.0 . . ? C312 C311 H31C 110.0 . . ? O34 C311 H31D 110.0 . . ? C312 C311 H31D 110.0 . . ? H31C C311 H31D 108.4 . . ? N32 C312 C311 111.8(6) . . ? N32 C312 H31E 109.3 . . ? C311 C312 H31E 109.3 . . ? N32 C312 H31F 109.3 . . ? C311 C312 H31F 109.3 . . ? H31E C312 H31F 107.9 . . ? N31 C313 C314 114.9(5) . . ? N31 C313 H31G 108.5 . . ? C314 C313 H31G 108.5 . . ? N31 C313 H31H 108.5 . . ? C314 C313 H31H 108.5 . . ? H31G C313 H31H 107.5 . . ? O35 C314 C313 108.4(5) . . ? O35 C314 H31I 110.0 . . ? C313 C314 H31I 110.0 . . ? O35 C314 H31J 110.0 . . ? C313 C314 H31J 110.0 . . ? H31I C314 H31J 108.4 . . ? O35 C315 C316 107.9(5) . . ? O35 C315 H31K 110.1 . . ? C316 C315 H31K 110.1 . . ? O35 C315 H31L 110.1 . . ? C316 C315 H31L 110.1 . . ? H31K C315 H31L 108.4 . . ? O36 C316 C315 108.9(6) . . ? O36 C316 H31M 109.9 . . ? C315 C316 H31M 109.9 . . ? O36 C316 H31N 109.9 . . ? C315 C316 H31N 109.9 . . ? H31M C316 H31N 108.3 . . ? O36 C317 C318 109.0(7) . . ? O36 C317 H31O 109.9 . . ? C318 C317 H31O 109.9 . . ? O36 C317 H31P 109.9 . . ? C318 C317 H31P 109.9 . . ? H31O C317 H31P 108.3 . . ? N32 C318 C317 113.8(6) . . ? N32 C318 H31Q 108.8 . . ? C317 C318 H31Q 108.8 . . ? N32 C318 H31R 108.8 . . ? C317 C318 H31R 108.8 . . ? H31Q C318 H31R 107.7 . . ? C107 N11 C101 108.6(6) . . ? C107 N11 C113 108.5(6) . . ? C101 N11 C113 111.5(6) . . ? C107 N11 K1 110.6(4) . . ? C101 N11 K1 108.8(5) . . ? C113 N11 K1 108.8(4) . . ? C106 N12 C112 109.7(6) . . ? C106 N12 C118 110.1(6) . . ? C112 N12 C118 109.3(7) . . ? C106 N12 K1 108.7(5) . . ? C112 N12 K1 111.3(4) . . ? C118 N12 K1 107.6(4) . . ? C201 N21 C207 110.2(6) . . ? C201 N21 C213 112.2(6) . . ? C207 N21 C213 108.8(5) . . ? C201 N21 K2 108.3(4) . . ? C207 N21 K2 110.3(4) . . ? C213 N21 K2 107.1(4) . . ? C206 N22 C218 109.7(6) . . ? C206 N22 C212 110.6(6) . . ? C218 N22 C212 110.2(6) . . ? C206 N22 K2 109.1(5) . . ? C218 N22 K2 108.3(4) . . ? C212 N22 K2 108.8(4) . . ? C313 N31 C307 109.9(5) . . ? C313 N31 C301 110.2(5) . . ? C307 N31 C301 110.5(5) . . ? C313 N31 K3 107.6(4) . . ? C307 N31 K3 107.6(4) . . ? C301 N31 K3 111.1(4) . . ? C306 N32 C318 110.4(6) . . ? C306 N32 C312 108.8(5) . . ? C318 N32 C312 108.3(6) . . ? C306 N32 K3 108.6(4) . . ? C318 N32 K3 107.9(4) . . ? C312 N32 K3 112.8(4) . . ? C102 O11 C103 113.5(8) . . ? C102 O11 K1 113.8(5) . . ? C103 O11 K1 109.4(6) . . ? C105 O12 C104 112.0(8) . . ? C105 O12 K1 120.3(5) . . ? C104 O12 K1 115.2(6) . . ? C109 O13 C108 111.0(5) . . ? C109 O13 K1 113.3(3) . . ? C108 O13 K1 116.6(3) . . ? C110 O14 C111 111.8(5) . . ? C110 O14 K1 113.0(3) . . ? C111 O14 K1 116.1(4) . . ? C115 O15 C114 111.4(5) . . ? C115 O15 K1 114.5(4) . . ? C114 O15 K1 118.6(4) . . ? C116 O16 C117 113.3(6) . . ? C116 O16 K1 120.8(4) . . ? C117 O16 K1 116.6(4) . . ? C203 O21 C202 112.3(6) . . ? C203 O21 K2 110.1(4) . . ? C202 O21 K2 118.4(4) . . ? C204 O22 C205 116.3(6) . . ? C204 O22 K2 122.5(5) . . ? C205 O22 K2 116.1(5) . . ? C209 O23 C208 111.3(5) . . ? C209 O23 K2 118.6(4) . . ? C208 O23 K2 117.4(4) . . ? C211 O24 C210 109.3(6) . . ? C211 O24 K2 116.3(4) . . ? C210 O24 K2 110.6(4) . . ? C214 O25 C215 112.3(6) . . ? C214 O25 K2 112.7(4) . . ? C215 O25 K2 112.1(4) . . ? C217 O26 C216 111.4(6) . . ? C217 O26 K2 119.4(4) . . ? C216 O26 K2 116.3(4) . . ? C303 O31 C302 112.7(5) . . ? C303 O31 K3 116.9(3) . . ? C302 O31 K3 117.7(4) . . ? C305 O32 C304 112.0(5) . . ? C305 O32 K3 114.1(3) . . ? C304 O32 K3 106.3(3) . . ? C309 O33 C308 111.3(5) . . ? C309 O33 K3 110.3(4) . . ? C308 O33 K3 119.9(4) . . ? C310 O34 C311 112.8(5) . . ? C310 O34 K3 114.0(3) . . ? C311 O34 K3 116.2(4) . . ? C314 O35 C315 112.2(5) . . ? C314 O35 K3 115.2(3) . . ? C315 O35 K3 117.8(3) . . ? C317 O36 C316 111.1(6) . . ? C317 O36 K3 113.6(4) . . ? C316 O36 K3 111.2(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.774 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.111 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 700661' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)]3[Sn9Zn(C9H11)]*tol ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K-(2,2,2-crypt))3(Sn9Zn(C9H11))*tol _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), C9 H11 Sn9 Zn, C7 H8' _chemical_formula_sum 'C70 H127 K3 N6 O18 Sn9 Zn' _chemical_formula_weight 2590.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6540 1.4250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2840 1.4300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 14.7470(1) _cell_length_b 24.6645(2) _cell_length_c 27.0957(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.4626(3) _cell_angle_gamma 90.00 _cell_volume 9658.86(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5079 _exptl_absorpt_coefficient_mu 2.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4769 _exptl_absorpt_correction_T_max 0.8540 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31887 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16791 _reflns_number_gt 13034 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0579P)^2^+97.3469P] 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 16791 _refine_ls_number_parameters 993 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _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 1.00349(6) 0.34040(4) 0.22163(3) 0.0870(3) Uani 1 1 d . . . Sn2 Sn 1.02075(6) 0.24420(4) 0.16237(3) 0.0899(3) Uani 1 1 d . A . Sn5 Sn 0.89302(6) 0.24555(3) 0.23533(3) 0.0792(3) Uani 1 1 d . A . Sn8 Sn 0.69886(6) 0.24927(4) 0.15999(4) 0.0865(3) Uani 1 1 d . . . Sn9 Sn 0.85776(6) 0.17070(4) 0.14996(3) 0.0831(3) Uani 1 1 d . A . Sn3 Sn 0.9251(3) 0.3575(3) 0.11427(18) 0.0747(11) Uani 0.682(13) 1 d P A . Sn4 Sn 0.7963(3) 0.3593(2) 0.1848(2) 0.0796(11) Uani 0.682(13) 1 d P A . Sn6 Sn 0.8745(3) 0.2503(3) 0.06424(14) 0.0992(11) Uani 0.682(13) 1 d P . . Sn7 Sn 0.7183(2) 0.3261(3) 0.0784(2) 0.0948(12) Uani 0.682(13) 1 d P A . Sn3A Sn 0.9203(6) 0.3424(3) 0.1051(3) 0.0552(15) Uani 0.318(13) 1 d P A 2 Sn4A Sn 0.7836(8) 0.3471(4) 0.1736(4) 0.086(3) Uani 0.318(13) 1 d P A 2 Sn6A Sn 0.8796(5) 0.2357(2) 0.0598(3) 0.0601(13) Uani 0.318(13) 1 d P A 2 Sn7A Sn 0.7169(5) 0.3136(3) 0.0679(3) 0.0624(16) Uani 0.318(13) 1 d P A 2 Zn1 Zn 0.70350(10) 0.20552(7) 0.06843(6) 0.0963(5) Uani 1 1 d . A . C1 C 0.6119(10) 0.1563(5) 0.0194(5) 0.096(4) Uani 1 1 d . . . C2 C 0.5650(13) 0.1151(6) 0.0360(6) 0.113(5) Uani 1 1 d . A . C3 C 0.4998(17) 0.0815(7) 0.0014(7) 0.146(8) Uani 1 1 d . . . H3 H 0.4703 0.0531 0.0159 0.176 Uiso 1 1 calc R A . C4 C 0.4772(13) 0.0869(6) -0.0495(7) 0.119(5) Uani 1 1 d . A . C5 C 0.5278(12) 0.1255(6) -0.0663(6) 0.112(5) Uani 1 1 d . . . H5 H 0.5204 0.1313 -0.1016 0.135 Uiso 1 1 calc R A . C6 C 0.5931(11) 0.1581(6) -0.0322(6) 0.103(4) Uani 1 1 d . A . C9 C 0.6397(19) 0.2021(11) -0.0543(7) 0.219(14) Uani 1 1 d . . . H9C H 0.6192 0.2019 -0.0910 0.328 Uiso 1 1 calc R A . H9B H 0.7068 0.1966 -0.0457 0.328 Uiso 1 1 calc R . . H9A H 0.6242 0.2370 -0.0408 0.328 Uiso 1 1 calc R . . C7 C 0.5838(17) 0.1060(7) 0.0915(7) 0.164(9) Uani 1 1 d . . . H7A H 0.5465 0.0754 0.0993 0.246 Uiso 1 1 calc R A . H7B H 0.5678 0.1387 0.1084 0.246 Uiso 1 1 calc R . . H7C H 0.6496 0.0977 0.1032 0.246 Uiso 1 1 calc R . . C8 C 0.394(2) 0.0529(8) -0.0883(8) 0.195(11) Uani 1 1 d . . . H8C H 0.3980 0.0608 -0.1233 0.293 Uiso 1 1 calc R A . H8A H 0.3335 0.0641 -0.0823 0.293 Uiso 1 1 calc R . . H8B H 0.4023 0.0139 -0.0820 0.293 Uiso 1 1 calc R . . K1 K 0.65872(13) 0.03517(9) 0.34993(7) 0.0556(5) Uani 1 1 d . . . O11 O 0.5283(5) -0.0502(3) 0.3440(3) 0.0702(18) Uani 1 1 d . . . O12 O 0.4703(4) 0.0569(3) 0.3549(3) 0.0715(19) Uani 1 1 d . . . O13 O 0.8019(5) 0.0029(3) 0.4430(3) 0.075(2) Uani 1 1 d . . . O14 O 0.7541(5) 0.1122(3) 0.4234(3) 0.081(2) Uani 1 1 d . . . O15 O 0.7506(5) -0.0001(4) 0.2815(3) 0.084(2) Uani 1 1 d . . . O16 O 0.6477(5) 0.0968(3) 0.2643(3) 0.081(2) Uani 1 1 d . . . N11 N 0.7336(6) -0.0752(4) 0.3607(4) 0.076(2) Uani 1 1 d . . . N12 N 0.5825(7) 0.1468(4) 0.3403(4) 0.081(3) Uani 1 1 d . . . C101 C 0.6497(9) -0.1124(5) 0.3427(5) 0.087(3) Uani 1 1 d . . . H10A H 0.6308 -0.1095 0.3057 0.104 Uiso 1 1 calc R . . H10B H 0.6682 -0.1504 0.3509 0.104 Uiso 1 1 calc R . . C102 C 0.5725(8) -0.0996(5) 0.3649(5) 0.082(3) Uani 1 1 d . . . H10C H 0.5935 -0.0953 0.4017 0.098 Uiso 1 1 calc R . . H10D H 0.5273 -0.1297 0.3589 0.098 Uiso 1 1 calc R . . C103 C 0.4507(7) -0.0373(5) 0.3614(5) 0.079(3) Uani 1 1 d . . . H10E H 0.4672 -0.0332 0.3985 0.095 Uiso 1 1 calc R . . H10F H 0.4062 -0.0677 0.3540 0.095 Uiso 1 1 calc R . . C104 C 0.4045(7) 0.0134(5) 0.3393(4) 0.077(3) Uani 1 1 d . . . H10G H 0.3888 0.0108 0.3021 0.092 Uiso 1 1 calc R . . H10H H 0.3469 0.0198 0.3520 0.092 Uiso 1 1 calc R . . C105 C 0.4255(9) 0.1065(6) 0.3385(5) 0.098(4) Uani 1 1 d . . . H10I H 0.3695 0.1116 0.3531 0.117 Uiso 1 1 calc R . . H10J H 0.4074 0.1077 0.3013 0.117 Uiso 1 1 calc R . . C106 C 0.4989(9) 0.1504(5) 0.3581(5) 0.090(4) Uani 1 1 d . . . H10K H 0.4712 0.1864 0.3488 0.107 Uiso 1 1 calc R . . H10L H 0.5138 0.1485 0.3954 0.107 Uiso 1 1 calc R . . C107 C 0.7905(8) -0.0873(5) 0.4132(5) 0.092(4) Uani 1 1 d . . . H10M H 0.8266 -0.1207 0.4109 0.110 Uiso 1 1 calc R . . H10N H 0.7468 -0.0953 0.4357 0.110 Uiso 1 1 calc R . . C108 C 0.8587(8) -0.0427(5) 0.4388(5) 0.090(4) Uani 1 1 d . . . H10O H 0.8917 -0.0547 0.4725 0.108 Uiso 1 1 calc R . . H10P H 0.9047 -0.0339 0.4180 0.108 Uiso 1 1 calc R . . C109 C 0.8594(8) 0.0439(5) 0.4712(4) 0.078(3) Uani 1 1 d . . . H10Q H 0.9111 0.0536 0.4546 0.093 Uiso 1 1 calc R . . H10R H 0.8853 0.0310 0.5058 0.093 Uiso 1 1 calc R . . C110 C 0.7974(9) 0.0908(6) 0.4724(4) 0.098(4) Uani 1 1 d . . . H11A H 0.7481 0.0800 0.4905 0.117 Uiso 1 1 calc R . . H11B H 0.8335 0.1202 0.4921 0.117 Uiso 1 1 calc R . . C111 C 0.7057(10) 0.1626(6) 0.4232(6) 0.102(4) Uani 1 1 d . . . H11C H 0.7497 0.1908 0.4391 0.122 Uiso 1 1 calc R . . H11D H 0.6575 0.1587 0.4437 0.122 Uiso 1 1 calc R . . C112 C 0.6608(12) 0.1808(6) 0.3707(8) 0.117(6) Uani 1 1 d . . . H11E H 0.7100 0.1836 0.3508 0.140 Uiso 1 1 calc R . . H11F H 0.6365 0.2179 0.3735 0.140 Uiso 1 1 calc R . . C113 C 0.7946(10) -0.0842(6) 0.3294(6) 0.109(5) Uani 1 1 d . . . H11G H 0.8028 -0.1237 0.3253 0.130 Uiso 1 1 calc R . . H11H H 0.8555 -0.0683 0.3442 0.130 Uiso 1 1 calc R . . C114 C 0.7564(10) -0.0580(7) 0.2775(6) 0.108(5) Uani 1 1 d . . . H11I H 0.7973 -0.0672 0.2539 0.129 Uiso 1 1 calc R . . H11J H 0.6941 -0.0728 0.2636 0.129 Uiso 1 1 calc R . . C115 C 0.7239(9) 0.0262(7) 0.2351(5) 0.101(5) Uani 1 1 d . . . H11K H 0.6634 0.0117 0.2177 0.122 Uiso 1 1 calc R . . H11L H 0.7697 0.0183 0.2139 0.122 Uiso 1 1 calc R . . C116 C 0.7161(9) 0.0874(7) 0.2407(4) 0.096(4) Uani 1 1 d . . . H11M H 0.7746 0.1022 0.2603 0.116 Uiso 1 1 calc R . . H11N H 0.7033 0.1048 0.2071 0.116 Uiso 1 1 calc R . . C117 C 0.6297(16) 0.1517(7) 0.2653(7) 0.149(8) Uani 1 1 d . . . H11O H 0.6159 0.1659 0.2304 0.179 Uiso 1 1 calc R . . H11P H 0.6855 0.1707 0.2838 0.179 Uiso 1 1 calc R . . C118 C 0.5550(16) 0.1628(8) 0.2886(6) 0.154(9) Uani 1 1 d . . . H11Q H 0.4997 0.1422 0.2721 0.185 Uiso 1 1 calc R . . H11R H 0.5400 0.2020 0.2863 0.185 Uiso 1 1 calc R . . K2 K 0.8273(2) 0.45364(10) 0.38842(9) 0.0814(7) Uani 1 1 d U . . O21 O 0.9010(9) 0.4091(4) 0.4845(3) 0.114(3) Uani 1 1 d . . . O22 O 0.7780(10) 0.4969(5) 0.4693(4) 0.127(4) Uani 1 1 d . . . O23 O 1.0030(8) 0.4770(5) 0.3717(4) 0.124(3) Uani 1 1 d . . . O24 O 0.8394(12) 0.5477(6) 0.3355(5) 0.162(5) Uani 1 1 d . . . O25 O 0.7914(14) 0.3567(6) 0.3341(5) 0.163(6) Uani 1 1 d . . . O26 O 0.6373(12) 0.4252(8) 0.3224(5) 0.194(8) Uani 1 1 d U . . N21 N 0.9893(13) 0.3709(6) 0.4103(6) 0.140(5) Uani 1 1 d . . . N22 N 0.6678(13) 0.5350(8) 0.3659(8) 0.159(6) Uani 1 1 d . . . C201 C 0.996(2) 0.3438(8) 0.4595(8) 0.170(10) Uani 1 1 d . . . H20A H 0.9424 0.3194 0.4584 0.205 Uiso 1 1 calc R . . H20B H 1.0531 0.3215 0.4669 0.205 Uiso 1 1 calc R . . C202 C 0.998(2) 0.3846(10) 0.4990(8) 0.171(9) Uani 1 1 d . . . H20C H 1.0466 0.4122 0.4982 0.206 Uiso 1 1 calc R . . H20D H 1.0085 0.3678 0.5328 0.206 Uiso 1 1 calc R . . C203 C 0.8850(19) 0.4390(8) 0.5242(6) 0.149(8) Uani 1 1 d . . . H20E H 0.9267 0.4708 0.5303 0.179 Uiso 1 1 calc R . . H20F H 0.8933 0.4169 0.5553 0.179 Uiso 1 1 calc R . . C204 C 0.7872(15) 0.4560(9) 0.5076(6) 0.140(7) Uani 1 1 d . . . H20G H 0.7492 0.4241 0.4944 0.167 Uiso 1 1 calc R . . H20H H 0.7638 0.4703 0.5369 0.167 Uiso 1 1 calc R . . C205 C 0.6928(18) 0.5241(12) 0.4576(9) 0.171(9) Uani 1 1 d . . . H20I H 0.6836 0.5435 0.4883 0.206 Uiso 1 1 calc R . . H20J H 0.6433 0.4966 0.4496 0.206 Uiso 1 1 calc R . . C206 C 0.679(2) 0.5659(11) 0.4134(10) 0.187(10) Uani 1 1 d . . . H20K H 0.6239 0.5885 0.4136 0.225 Uiso 1 1 calc R . . H20L H 0.7339 0.5900 0.4169 0.225 Uiso 1 1 calc R . . C207 C 1.0737(16) 0.3962(9) 0.4083(10) 0.176(10) Uani 1 1 d . . . H20M H 1.1202 0.3691 0.4026 0.211 Uiso 1 1 calc R . . H20N H 1.0980 0.4158 0.4400 0.211 Uiso 1 1 calc R . . C208 C 1.052(2) 0.4341(9) 0.3656(7) 0.179(10) Uani 1 1 d U . . H20O H 1.1111 0.4466 0.3574 0.214 Uiso 1 1 calc R . . H20P H 1.0184 0.4138 0.3360 0.214 Uiso 1 1 calc R . . C209 C 0.9902(13) 0.5159(7) 0.3324(6) 0.119(5) Uani 1 1 d . . . H20Q H 0.9597 0.4986 0.3004 0.143 Uiso 1 1 calc R . . H20R H 1.0511 0.5298 0.3280 0.143 Uiso 1 1 calc R . . C210 C 0.9336(14) 0.5605(11) 0.3441(9) 0.163(9) Uani 1 1 d . . . H21A H 0.9545 0.5707 0.3799 0.195 Uiso 1 1 calc R . . H21B H 0.9427 0.5923 0.3234 0.195 Uiso 1 1 calc R . . C211 C 0.788(2) 0.5943(9) 0.3461(11) 0.184(9) Uani 1 1 d U . . H21C H 0.8017 0.6261 0.3265 0.221 Uiso 1 1 calc R . . H21D H 0.8035 0.6034 0.3824 0.221 Uiso 1 1 calc R . . C212 C 0.6789(15) 0.5767(8) 0.3293(8) 0.142(7) Uani 1 1 d U . . H21E H 0.6375 0.6079 0.3312 0.171 Uiso 1 1 calc R . . H21F H 0.6655 0.5619 0.2946 0.171 Uiso 1 1 calc R . . C213 C 0.9594(13) 0.3310(7) 0.3722(7) 0.116(5) Uani 1 1 d U . . H21G H 0.9972 0.2981 0.3818 0.139 Uiso 1 1 calc R . . H21H H 0.9754 0.3447 0.3406 0.139 Uiso 1 1 calc R . . C214 C 0.853(2) 0.3124(8) 0.3591(8) 0.173(9) Uani 1 1 d U . . H21I H 0.8470 0.2804 0.3366 0.207 Uiso 1 1 calc R . . H21J H 0.8333 0.3015 0.3905 0.207 Uiso 1 1 calc R . . C215 C 0.7067(17) 0.3389(10) 0.3073(7) 0.160(9) Uani 1 1 d . . . H21K H 0.6732 0.3186 0.3296 0.192 Uiso 1 1 calc R . . H21L H 0.7156 0.3148 0.2794 0.192 Uiso 1 1 calc R . . C216 C 0.6472(14) 0.3935(9) 0.2845(7) 0.133(6) Uani 1 1 d U . . H21M H 0.6803 0.4132 0.2616 0.159 Uiso 1 1 calc R . . H21N H 0.5856 0.3827 0.2652 0.159 Uiso 1 1 calc R . . C217 C 0.590(2) 0.4736(12) 0.3013(8) 0.233(15) Uani 1 1 d U . . H21O H 0.5292 0.4640 0.2805 0.280 Uiso 1 1 calc R . . H21P H 0.6270 0.4921 0.2795 0.280 Uiso 1 1 calc R . . C218 C 0.5773(16) 0.5107(12) 0.3435(12) 0.227(16) Uani 1 1 d . . . H21Q H 0.5323 0.5395 0.3304 0.273 Uiso 1 1 calc R . . H21R H 0.5531 0.4899 0.3694 0.273 Uiso 1 1 calc R . . K3 K 0.20329(14) 0.15180(10) 0.41916(8) 0.0644(5) Uani 1 1 d . . . O31 O 0.2884(6) 0.2408(4) 0.3823(3) 0.094(2) Uani 1 1 d . . . O32 O 0.1623(6) 0.1673(4) 0.3193(3) 0.089(2) Uani 1 1 d . . . O33 O 0.3718(5) 0.1153(3) 0.4949(3) 0.077(2) Uani 1 1 d . . . O34 O 0.2632(5) 0.0426(3) 0.4175(2) 0.0712(19) Uani 1 1 d . . . O35 O 0.1324(6) 0.2156(3) 0.4799(3) 0.089(2) Uani 1 1 d . . . O36 O 0.0145(5) 0.1299(3) 0.4192(3) 0.0725(19) Uani 1 1 d . . . N31 N 0.3363(8) 0.2324(5) 0.4900(4) 0.095(3) Uani 1 1 d . . . N32 N 0.0762(6) 0.0711(4) 0.3446(3) 0.067(2) Uani 1 1 d . . . C301 C 0.3821(14) 0.2675(7) 0.4631(7) 0.132(6) Uani 1 1 d . . . H30A H 0.4368 0.2491 0.4548 0.159 Uiso 1 1 calc R . . H30B H 0.4039 0.2997 0.4840 0.159 Uiso 1 1 calc R . . C302 C 0.3157(14) 0.2858(7) 0.4135(7) 0.132(6) Uani 1 1 d . . . H30C H 0.2604 0.3035 0.4218 0.158 Uiso 1 1 calc R . . H30D H 0.3476 0.3124 0.3955 0.158 Uiso 1 1 calc R . . C303 C 0.2229(11) 0.2548(6) 0.3345(6) 0.107(5) Uani 1 1 d . . . H30E H 0.1636 0.2672 0.3424 0.128 Uiso 1 1 calc R . . H30F H 0.2490 0.2849 0.3176 0.128 Uiso 1 1 calc R . . C304 C 0.2060(10) 0.2089(6) 0.3010(6) 0.101(4) Uani 1 1 d . . . H30G H 0.1680 0.2208 0.2685 0.122 Uiso 1 1 calc R . . H30H H 0.2659 0.1958 0.2943 0.122 Uiso 1 1 calc R . . C305 C 0.1278(9) 0.1241(6) 0.2834(4) 0.088(4) Uani 1 1 d . . . H30I H 0.1782 0.0976 0.2833 0.106 Uiso 1 1 calc R . . H30J H 0.1115 0.1400 0.2493 0.106 Uiso 1 1 calc R . . C306 C 0.0467(8) 0.0951(6) 0.2941(4) 0.082(3) Uani 1 1 d . . . H30K H 0.0268 0.0665 0.2687 0.099 Uiso 1 1 calc R . . H30L H -0.0055 0.1205 0.2936 0.099 Uiso 1 1 calc R . . C307 C 0.4077(9) 0.2023(6) 0.5307(5) 0.099(4) Uani 1 1 d . . . H30M H 0.4591 0.2275 0.5440 0.118 Uiso 1 1 calc R . . H30N H 0.3775 0.1925 0.5590 0.118 Uiso 1 1 calc R . . C308 C 0.4461(9) 0.1533(6) 0.5126(5) 0.096(4) Uani 1 1 d . . . H30O H 0.4780 0.1626 0.4849 0.115 Uiso 1 1 calc R . . H30P H 0.4917 0.1367 0.5402 0.115 Uiso 1 1 calc R . . C309 C 0.4053(9) 0.0645(6) 0.4808(4) 0.091(4) Uani 1 1 d . . . H30Q H 0.4490 0.0491 0.5099 0.109 Uiso 1 1 calc R . . H30R H 0.4395 0.0703 0.4533 0.109 Uiso 1 1 calc R . . C310 C 0.3304(8) 0.0256(5) 0.4641(4) 0.078(3) Uani 1 1 d . . . H31A H 0.2961 0.0203 0.4916 0.093 Uiso 1 1 calc R . . H31B H 0.3577 -0.0097 0.4577 0.093 Uiso 1 1 calc R . . C311 C 0.1891(9) 0.0037(5) 0.3980(4) 0.082(3) Uani 1 1 d . . . H31C H 0.1485 0.0000 0.4228 0.099 Uiso 1 1 calc R . . H31D H 0.2172 -0.0322 0.3944 0.099 Uiso 1 1 calc R . . C312 C 0.1296(8) 0.0203(5) 0.3467(4) 0.084(3) Uani 1 1 d . . . H31E H 0.1709 0.0232 0.3222 0.101 Uiso 1 1 calc R . . H31F H 0.0855 -0.0095 0.3352 0.101 Uiso 1 1 calc R . . C313 C 0.2795(14) 0.2674(6) 0.5112(6) 0.120(6) Uani 1 1 d . . . H31G H 0.2554 0.2964 0.4868 0.144 Uiso 1 1 calc R . . H31H H 0.3162 0.2847 0.5417 0.144 Uiso 1 1 calc R . . C314 C 0.2001(11) 0.2368(6) 0.5249(5) 0.102(4) Uani 1 1 d . . . H31I H 0.1669 0.2610 0.5445 0.123 Uiso 1 1 calc R . . H31J H 0.2248 0.2060 0.5469 0.123 Uiso 1 1 calc R . . C315 C 0.0476(10) 0.1948(6) 0.4862(5) 0.099(4) Uani 1 1 d . . . H31K H 0.0163 0.2227 0.5030 0.118 Uiso 1 1 calc R . . H31L H 0.0598 0.1633 0.5092 0.118 Uiso 1 1 calc R . . C316 C -0.0210(9) 0.1762(5) 0.4370(6) 0.101(5) Uani 1 1 d . . . H31M H -0.0828 0.1687 0.4445 0.121 Uiso 1 1 calc R . . H31N H -0.0276 0.2052 0.4112 0.121 Uiso 1 1 calc R . . C317 C -0.0498(7) 0.1115(5) 0.3728(5) 0.079(3) Uani 1 1 d . . . H31O H -0.1125 0.1050 0.3796 0.094 Uiso 1 1 calc R . . H31P H -0.0542 0.1390 0.3458 0.094 Uiso 1 1 calc R . . C318 C -0.0097(7) 0.0610(5) 0.3583(4) 0.078(3) Uani 1 1 d . . . H31Q H -0.0009 0.0352 0.3868 0.093 Uiso 1 1 calc R . . H31R H -0.0526 0.0444 0.3295 0.093 Uiso 1 1 calc R . . C1S C 0.424(3) 0.3184(13) 0.2939(11) 0.28(2) Uani 1 1 d U . . H1T H 0.4853 0.3349 0.2982 0.423 Uiso 1 1 calc R . . H3T H 0.4221 0.2935 0.3219 0.423 Uiso 1 1 calc R . . H2T H 0.3772 0.3468 0.2933 0.423 Uiso 1 1 calc R . . C2S C 0.4014(12) 0.2843(7) 0.2400(7) 0.27(2) Uani 1 1 d GD . . C3S C 0.3132(11) 0.2697(6) 0.2208(7) 0.135(6) Uani 1 1 d G . . H3SA H 0.2651 0.2794 0.2378 0.162 Uiso 1 1 calc R . . C4S C 0.2934(11) 0.2411(6) 0.1775(7) 0.156(8) Uani 1 1 d G . . H4S H 0.2314 0.2308 0.1640 0.187 Uiso 1 1 calc R . . C5S C 0.3618(16) 0.2272(7) 0.1533(6) 0.242(19) Uani 1 1 d G . . H5S H 0.3478 0.2071 0.1228 0.291 Uiso 1 1 calc R . . C6S C 0.4500(14) 0.2419(8) 0.1725(8) 0.34(4) Uani 1 1 d G . . H6S H 0.4981 0.2321 0.1555 0.411 Uiso 1 1 calc R . . C7S C 0.4698(10) 0.2705(7) 0.2159(8) 0.218(17) Uani 1 1 d GD . . H7S H 0.5318 0.2808 0.2294 0.262 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 0.0815(5) 0.1111(7) 0.0726(5) 0.0345(5) 0.0251(4) 0.0057(5) Sn2 0.0597(5) 0.1349(8) 0.0824(5) 0.0310(5) 0.0315(4) 0.0328(5) Sn5 0.0917(6) 0.0873(5) 0.0693(5) 0.0383(4) 0.0419(4) 0.0287(4) Sn8 0.0674(5) 0.0998(6) 0.1064(6) 0.0507(5) 0.0515(4) 0.0201(4) Sn9 0.0854(5) 0.0949(6) 0.0788(5) 0.0327(4) 0.0398(4) 0.0294(4) Sn3 0.0504(10) 0.111(3) 0.0622(15) 0.0371(17) 0.0093(9) -0.0157(15) Sn4 0.0631(11) 0.072(2) 0.113(3) 0.0342(15) 0.0400(12) 0.0104(12) Sn6 0.0910(17) 0.149(3) 0.0624(12) 0.0290(16) 0.0276(10) -0.0104(17) Sn7 0.0453(12) 0.137(3) 0.097(2) 0.0666(18) 0.0023(10) -0.0117(13) Sn3A 0.077(3) 0.043(2) 0.058(3) 0.0099(14) 0.042(3) 0.0092(19) Sn4A 0.133(7) 0.065(4) 0.084(3) 0.034(3) 0.078(4) 0.057(4) Sn6A 0.067(2) 0.048(2) 0.085(3) 0.0055(13) 0.061(2) 0.0137(13) Sn7A 0.073(3) 0.062(2) 0.066(2) 0.0365(16) 0.047(3) 0.037(2) Zn1 0.0815(9) 0.1212(12) 0.0908(10) 0.0469(9) 0.0282(8) -0.0103(8) C1 0.103(9) 0.096(9) 0.097(9) 0.046(7) 0.040(8) 0.003(7) C2 0.167(15) 0.086(9) 0.101(10) 0.007(8) 0.061(10) -0.027(10) C3 0.26(2) 0.097(11) 0.112(12) -0.002(10) 0.101(14) -0.046(13) C4 0.152(15) 0.082(10) 0.133(14) -0.015(9) 0.054(12) -0.016(10) C5 0.139(13) 0.098(10) 0.107(11) 0.029(9) 0.043(10) 0.006(10) C6 0.111(11) 0.102(10) 0.097(10) 0.028(8) 0.023(8) -0.023(8) C9 0.27(3) 0.29(3) 0.094(12) 0.053(15) 0.032(15) -0.17(3) C7 0.28(3) 0.112(13) 0.133(14) 0.001(11) 0.116(16) -0.075(15) C8 0.34(3) 0.112(14) 0.162(19) -0.041(13) 0.11(2) -0.074(18) K1 0.0448(10) 0.0727(13) 0.0494(10) 0.0074(9) 0.0097(8) -0.0036(9) O11 0.060(4) 0.079(5) 0.076(4) 0.002(4) 0.023(3) -0.004(3) O12 0.050(4) 0.103(6) 0.063(4) 0.001(4) 0.015(3) 0.001(4) O13 0.052(4) 0.102(6) 0.068(4) 0.009(4) 0.005(3) -0.009(4) O14 0.076(5) 0.100(6) 0.071(5) -0.032(4) 0.024(4) -0.021(4) O15 0.068(5) 0.117(7) 0.074(5) -0.013(5) 0.030(4) 0.005(4) O16 0.090(5) 0.099(6) 0.064(4) 0.027(4) 0.041(4) 0.012(4) N11 0.060(5) 0.080(6) 0.092(6) -0.002(5) 0.026(5) 0.005(4) N12 0.096(7) 0.078(6) 0.076(6) 0.001(5) 0.032(5) 0.019(5) C101 0.094(9) 0.066(7) 0.102(9) -0.013(6) 0.021(7) 0.004(6) C102 0.079(8) 0.076(8) 0.094(8) -0.005(6) 0.024(6) -0.007(6) C103 0.059(6) 0.101(9) 0.085(7) -0.005(7) 0.032(6) -0.022(6) C104 0.046(5) 0.119(10) 0.069(6) -0.008(6) 0.020(5) 0.002(6) C105 0.083(8) 0.119(11) 0.087(9) 0.002(8) 0.009(7) 0.030(8) C106 0.090(9) 0.095(9) 0.091(8) -0.012(7) 0.036(7) 0.021(7) C107 0.069(7) 0.095(9) 0.106(10) 0.007(7) 0.003(7) 0.010(7) C108 0.061(7) 0.095(9) 0.110(10) 0.021(7) 0.010(6) 0.013(6) C109 0.060(6) 0.124(10) 0.050(5) -0.013(6) 0.012(5) -0.008(7) C110 0.093(9) 0.144(12) 0.057(7) -0.032(7) 0.017(6) -0.040(9) C111 0.097(10) 0.094(10) 0.124(12) -0.044(9) 0.044(9) -0.003(8) C112 0.128(13) 0.076(9) 0.172(16) -0.001(10) 0.090(12) 0.002(9) C113 0.085(9) 0.117(11) 0.142(13) -0.006(10) 0.067(9) 0.019(8) C114 0.087(9) 0.132(13) 0.116(12) -0.045(10) 0.052(8) 0.002(8) C115 0.077(8) 0.166(15) 0.071(8) -0.035(9) 0.038(6) -0.005(8) C116 0.083(8) 0.154(14) 0.060(7) 0.012(8) 0.035(6) -0.013(8) C117 0.24(2) 0.108(12) 0.141(14) 0.057(11) 0.124(15) 0.033(13) C118 0.24(2) 0.139(14) 0.115(12) 0.070(11) 0.104(14) 0.104(14) K2 0.115(2) 0.0748(15) 0.0624(13) 0.0063(11) 0.0370(13) -0.0095(14) O21 0.178(10) 0.109(7) 0.058(5) 0.010(5) 0.032(6) -0.003(7) O22 0.153(10) 0.146(9) 0.098(7) -0.019(7) 0.065(7) -0.012(8) O23 0.144(9) 0.128(9) 0.110(8) 0.018(7) 0.052(7) -0.017(7) O24 0.195(14) 0.141(11) 0.167(12) 0.030(9) 0.078(11) -0.011(10) O25 0.272(18) 0.133(10) 0.102(8) -0.018(8) 0.079(10) -0.049(12) O26 0.233(16) 0.278(19) 0.085(7) -0.036(10) 0.066(9) -0.135(15) N21 0.189(16) 0.109(10) 0.139(12) 0.025(10) 0.075(12) 0.024(10) N22 0.165(16) 0.158(15) 0.160(15) -0.005(13) 0.045(13) 0.012(12) C201 0.30(3) 0.110(13) 0.120(14) 0.044(12) 0.093(17) 0.052(16) C202 0.24(3) 0.163(19) 0.115(14) 0.068(15) 0.049(16) 0.051(19) C203 0.25(3) 0.138(15) 0.069(9) -0.003(9) 0.063(13) -0.031(16) C204 0.149(16) 0.21(2) 0.079(10) 0.007(12) 0.067(11) 0.005(15) C205 0.16(2) 0.23(3) 0.146(18) -0.053(18) 0.088(16) 0.005(19) C206 0.24(3) 0.19(2) 0.143(19) -0.028(18) 0.061(19) 0.06(2) C207 0.160(18) 0.162(18) 0.24(3) 0.087(18) 0.120(18) 0.048(15) C208 0.31(3) 0.134(15) 0.112(13) 0.011(12) 0.088(16) 0.063(18) C209 0.135(14) 0.133(13) 0.096(10) 0.028(10) 0.040(10) -0.039(11) C210 0.107(14) 0.22(2) 0.168(19) -0.049(17) 0.033(13) -0.083(16) C211 0.213(18) 0.118(13) 0.225(17) 0.009(13) 0.051(15) 0.027(13) C212 0.173(18) 0.110(12) 0.151(15) 0.042(12) 0.048(14) 0.030(12) C213 0.136(14) 0.093(10) 0.132(13) 0.000(10) 0.060(11) -0.003(10) C214 0.30(3) 0.086(11) 0.147(16) 0.035(11) 0.072(18) 0.028(16) C215 0.20(2) 0.18(2) 0.108(13) -0.045(14) 0.046(14) -0.096(19) C216 0.141(12) 0.144(13) 0.121(11) -0.035(11) 0.047(10) -0.020(11) C217 0.37(3) 0.23(2) 0.112(14) 0.077(16) 0.079(18) 0.20(2) C218 0.118(16) 0.25(3) 0.29(3) -0.17(3) -0.016(18) 0.018(18) K3 0.0473(11) 0.0871(15) 0.0606(12) 0.0067(11) 0.0154(9) 0.0045(10) O31 0.089(6) 0.095(6) 0.095(6) 0.019(5) 0.013(5) -0.008(5) O32 0.085(5) 0.113(7) 0.072(5) 0.023(5) 0.022(4) -0.011(5) O33 0.054(4) 0.112(6) 0.065(4) 0.005(4) 0.007(3) -0.012(4) O34 0.064(4) 0.093(5) 0.061(4) 0.014(4) 0.022(3) 0.031(4) O35 0.105(6) 0.088(5) 0.085(5) -0.013(4) 0.045(5) 0.003(5) O36 0.059(4) 0.080(5) 0.089(5) 0.007(4) 0.038(4) 0.018(4) N31 0.110(8) 0.083(7) 0.094(7) -0.012(6) 0.024(7) -0.022(6) N32 0.057(5) 0.082(6) 0.062(5) 0.003(4) 0.015(4) 0.011(4) C301 0.158(16) 0.117(12) 0.125(13) 0.012(10) 0.034(12) -0.070(11) C302 0.174(17) 0.102(12) 0.122(13) 0.032(10) 0.036(12) -0.040(12) C303 0.112(11) 0.106(11) 0.099(10) 0.038(9) 0.015(9) 0.019(9) C304 0.104(10) 0.107(11) 0.094(9) 0.043(9) 0.021(8) 0.022(8) C305 0.079(8) 0.128(11) 0.062(7) 0.017(7) 0.025(6) 0.011(7) C306 0.062(6) 0.122(10) 0.063(6) -0.011(6) 0.012(5) 0.001(6) C307 0.087(9) 0.122(11) 0.075(8) 0.001(8) -0.010(7) -0.035(8) C308 0.071(8) 0.129(12) 0.082(8) -0.002(8) 0.006(6) -0.009(8) C309 0.090(9) 0.128(11) 0.057(6) 0.016(7) 0.019(6) 0.062(9) C310 0.065(7) 0.103(9) 0.069(7) 0.016(6) 0.022(5) 0.025(6) C311 0.092(8) 0.074(7) 0.082(8) -0.004(6) 0.020(6) 0.018(6) C312 0.081(8) 0.102(9) 0.071(7) -0.020(6) 0.020(6) 0.001(7) C313 0.189(18) 0.073(9) 0.090(10) -0.008(7) 0.011(11) -0.037(10) C314 0.136(13) 0.091(9) 0.083(9) -0.012(7) 0.027(9) 0.004(9) C315 0.115(11) 0.095(9) 0.105(10) 0.006(8) 0.066(9) 0.035(8) C316 0.074(8) 0.096(9) 0.153(13) 0.021(9) 0.073(9) 0.022(7) C317 0.047(6) 0.095(8) 0.101(9) 0.018(7) 0.032(6) 0.009(5) C318 0.055(6) 0.104(9) 0.075(7) -0.001(6) 0.013(5) -0.010(6) C1S 0.45(5) 0.21(3) 0.15(2) 0.03(2) -0.02(3) -0.07(3) C2S 0.15(2) 0.30(4) 0.35(5) 0.24(4) 0.03(3) 0.03(3) C3S 0.114(14) 0.158(17) 0.142(16) 0.027(13) 0.043(12) -0.020(12) C4S 0.18(2) 0.127(15) 0.19(2) -0.014(14) 0.107(19) -0.025(14) C5S 0.47(6) 0.134(18) 0.16(2) 0.076(16) 0.15(3) 0.09(3) C6S 0.18(3) 0.75(11) 0.092(16) 0.07(3) 0.016(17) -0.04(4) C7S 0.109(14) 0.22(2) 0.36(4) 0.23(3) 0.124(19) 0.094(15) _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 Sn2 2.9044(15) . ? Sn1 Sn5 2.9164(13) . ? Sn1 Sn3 2.939(4) . ? Sn1 Sn4 3.056(4) . ? Sn1 Sn3A 3.153(9) . ? Sn1 Sn4A 3.250(13) . ? Sn2 Sn9 2.9757(14) . ? Sn2 Sn5 2.9896(10) . ? Sn2 Sn6 3.076(4) . ? Sn2 Sn3A 3.092(8) . ? Sn2 Sn6A 3.131(8) . ? Sn2 Sn3 3.282(5) . ? Sn5 Sn9 2.9244(14) . ? Sn5 Sn8 3.1703(13) . ? Sn5 Sn4A 3.257(10) . ? Sn5 Sn4 3.317(5) . ? Sn8 Sn4A 2.709(12) . ? Sn8 Zn1 2.719(2) . ? Sn8 Sn7 2.968(4) . ? Sn8 Sn7A 3.012(6) . ? Sn8 Sn4 3.081(5) . ? Sn8 Sn9 3.0940(11) . ? Sn9 Zn1 2.9656(17) . ? Sn9 Sn6A 2.992(6) . ? Sn9 Sn6 3.089(4) . ? Sn3 Sn4A 2.888(10) . ? Sn3 Sn4 2.950(5) . ? Sn3 Sn6 2.998(5) . ? Sn3 Sn7 3.110(5) . ? Sn3 Sn7A 3.263(9) . ? Sn3 Sn6A 3.358(8) . ? Sn4 Sn7 2.997(6) . ? Sn4 Sn3A 3.123(8) . ? Sn4 Sn7A 3.345(8) . ? Sn6 Sn3A 2.558(7) . ? Sn6 Zn1 2.777(4) . ? Sn6 Sn7A 2.818(8) . ? Sn6 Sn7 3.049(4) . ? Sn7 Sn4A 2.620(10) . ? Sn7 Sn3A 2.951(10) . ? Sn7 Zn1 2.989(7) . ? Sn7 Sn6A 3.371(7) . ? Sn3A Sn6A 2.917(8) . ? Sn3A Sn4A 3.002(11) . ? Sn3A Sn7A 3.052(12) . ? Sn4A Sn7A 2.954(12) . ? Sn6A Zn1 2.756(6) . ? Sn6A Sn7A 3.117(7) . ? Sn7A Zn1 2.673(7) . ? Zn1 C1 2.087(16) . ? C1 C2 1.355(17) . ? C1 C6 1.370(19) . ? C2 C3 1.46(2) . ? C2 C7 1.49(2) . ? C3 C4 1.36(2) . ? C3 H3 0.9500 . ? C4 C5 1.34(2) . ? C4 C8 1.67(3) . ? C5 C6 1.44(2) . ? C5 H5 0.9500 . ? C6 C9 1.47(2) . ? C9 H9C 0.9800 . ? C9 H9B 0.9800 . ? C9 H9A 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? O11 C103 1.360(12) . ? O11 C102 1.443(14) . ? O12 C105 1.420(14) . ? O12 C104 1.452(13) . ? O13 C108 1.419(14) . ? O13 C109 1.439(13) . ? O14 C111 1.433(15) . ? O14 C110 1.454(15) . ? O15 C115 1.399(16) . ? O15 C114 1.434(17) . ? O16 C116 1.317(13) . ? O16 C117 1.383(17) . ? N11 C113 1.371(14) . ? N11 C107 1.530(15) . ? N11 C101 1.541(15) . ? N12 C106 1.413(15) . ? N12 C118 1.434(17) . ? N12 C112 1.53(2) . ? C101 C102 1.424(16) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.491(16) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.549(19) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.557(17) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.480(18) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.51(2) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.55(2) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.52(2) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.40(2) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? O21 C203 1.363(18) . ? O21 C202 1.53(3) . ? O22 C205 1.40(3) . ? O22 C204 1.44(2) . ? O23 C208 1.31(2) . ? O23 C209 1.418(17) . ? O24 C210 1.40(2) . ? O24 C211 1.44(2) . ? O25 C215 1.39(2) . ? O25 C214 1.50(2) . ? O26 C216 1.32(2) . ? O26 C217 1.44(2) . ? N21 C207 1.40(2) . ? N21 C213 1.43(2) . ? N21 C201 1.47(2) . ? N22 C212 1.46(2) . ? N22 C206 1.47(3) . ? N22 C218 1.48(3) . ? C201 C202 1.47(3) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.48(3) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.56(3) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.47(3) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.45(3) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.64(3) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.60(3) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.66(3) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.51(3) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? O31 C302 1.403(18) . ? O31 C303 1.494(16) . ? O32 C304 1.358(15) . ? O32 C305 1.463(15) . ? O33 C309 1.427(14) . ? O33 C308 1.450(15) . ? O34 C311 1.471(14) . ? O34 C310 1.501(12) . ? O35 C315 1.393(16) . ? O35 C314 1.508(16) . ? O36 C316 1.384(14) . ? O36 C317 1.487(14) . ? N31 C301 1.391(17) . ? N31 C313 1.40(2) . ? N31 C307 1.554(17) . ? N32 C318 1.411(13) . ? N32 C306 1.475(13) . ? N32 C312 1.475(14) . ? C301 C302 1.56(2) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.44(2) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.470(16) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.461(19) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.465(18) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.543(16) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.50(2) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.57(2) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 C318 1.465(16) . ? C317 H31O 0.9900 . ? C317 H31P 0.9900 . ? C318 H31Q 0.9900 . ? C318 H31R 0.9900 . ? C1S C2S 1.66(3) . ? C1S H1T 0.9800 . ? C1S H3T 0.9800 . ? C1S H2T 0.9800 . ? C2S C7S 1.351 . ? C2S C3S 1.351 . ? C3S C4S 1.351 . ? C3S H3SA 0.9500 . ? C4S C5S 1.351 . ? C4S H4S 0.9500 . ? C5S C6S 1.351 . ? C5S H5S 0.9500 . ? C6S C7S 1.351 . ? C6S H6S 0.9500 . ? C7S H7S 0.9500 . ? 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 Sn2 Sn1 Sn5 61.81(3) . . ? Sn2 Sn1 Sn3 68.34(14) . . ? Sn5 Sn1 Sn3 96.99(11) . . ? Sn2 Sn1 Sn4 97.79(12) . . ? Sn5 Sn1 Sn4 67.43(9) . . ? Sn3 Sn1 Sn4 58.92(11) . . ? Sn2 Sn1 Sn3A 61.23(11) . . ? Sn5 Sn1 Sn3A 91.39(15) . . ? Sn3 Sn1 Sn3A 7.37(17) . . ? Sn4 Sn1 Sn3A 60.37(19) . . ? Sn2 Sn1 Sn4A 90.60(18) . . ? Sn5 Sn1 Sn4A 63.50(18) . . ? Sn3 Sn1 Sn4A 55.35(17) . . ? Sn4 Sn1 Sn4A 7.2(2) . . ? Sn3A Sn1 Sn4A 55.9(2) . . ? Sn1 Sn2 Sn9 113.74(3) . . ? Sn1 Sn2 Sn5 59.29(3) . . ? Sn9 Sn2 Sn5 58.71(3) . . ? Sn1 Sn2 Sn6 108.32(15) . . ? Sn9 Sn2 Sn6 61.35(9) . . ? Sn5 Sn2 Sn6 98.37(9) . . ? Sn1 Sn2 Sn3A 63.35(13) . . ? Sn9 Sn2 Sn3A 97.18(17) . . ? Sn5 Sn2 Sn3A 91.22(14) . . ? Sn6 Sn2 Sn3A 49.01(15) . . ? Sn1 Sn2 Sn6A 115.46(8) . . ? Sn9 Sn2 Sn6A 58.61(11) . . ? Sn5 Sn2 Sn6A 101.12(10) . . ? Sn6 Sn2 Sn6A 7.20(17) . . ? Sn3A Sn2 Sn6A 55.91(16) . . ? Sn1 Sn2 Sn3 56.34(11) . . ? Sn9 Sn2 Sn3 101.55(8) . . ? Sn5 Sn2 Sn3 88.60(8) . . ? Sn6 Sn2 Sn3 56.14(10) . . ? Sn3A Sn2 Sn3 7.26(16) . . ? Sn6A Sn2 Sn3 63.09(13) . . ? Sn1 Sn5 Sn9 114.94(3) . . ? Sn1 Sn5 Sn2 58.90(3) . . ? Sn9 Sn5 Sn2 60.41(3) . . ? Sn1 Sn5 Sn8 110.53(3) . . ? Sn9 Sn5 Sn8 60.86(3) . . ? Sn2 Sn5 Sn8 100.46(3) . . ? Sn1 Sn5 Sn4A 63.2(2) . . ? Sn9 Sn5 Sn4A 95.0(2) . . ? Sn2 Sn5 Sn4A 88.97(14) . . ? Sn8 Sn5 Sn4A 49.8(2) . . ? Sn1 Sn5 Sn4 58.29(7) . . ? Sn9 Sn5 Sn4 102.28(11) . . ? Sn2 Sn5 Sn4 90.70(8) . . ? Sn8 Sn5 Sn4 56.65(9) . . ? Sn4A Sn5 Sn4 7.6(2) . . ? Sn4A Sn8 Zn1 112.53(19) . . ? Sn4A Sn8 Sn7 54.7(2) . . ? Zn1 Sn8 Sn7 63.25(16) . . ? Sn4A Sn8 Sn7A 61.9(2) . . ? Zn1 Sn8 Sn7A 55.32(13) . . ? Sn7 Sn8 Sn7A 7.93(19) . . ? Sn4A Sn8 Sn4 4.7(3) . . ? Zn1 Sn8 Sn4 116.95(11) . . ? Sn7 Sn8 Sn4 59.37(14) . . ? Sn7A Sn8 Sn4 66.57(17) . . ? Sn4A Sn8 Sn9 103.5(2) . . ? Zn1 Sn8 Sn9 60.95(4) . . ? Sn7 Sn8 Sn9 98.47(11) . . ? Sn7A Sn8 Sn9 93.67(9) . . ? Sn4 Sn8 Sn9 104.02(9) . . ? Sn4A Sn8 Sn5 66.7(2) . . ? Zn1 Sn8 Sn5 113.13(4) . . ? Sn7 Sn8 Sn5 106.83(8) . . ? Sn7A Sn8 Sn5 109.34(15) . . ? Sn4 Sn8 Sn5 64.07(10) . . ? Sn9 Sn8 Sn5 55.64(3) . . ? Sn5 Sn9 Zn1 113.32(5) . . ? Sn5 Sn9 Sn2 60.88(3) . . ? Zn1 Sn9 Sn2 112.99(4) . . ? Sn5 Sn9 Sn6A 106.08(12) . . ? Zn1 Sn9 Sn6A 55.11(14) . . ? Sn2 Sn9 Sn6A 63.28(15) . . ? Sn5 Sn9 Sn6 99.51(14) . . ? Zn1 Sn9 Sn6 54.55(8) . . ? Sn2 Sn9 Sn6 60.93(8) . . ? Sn6A Sn9 Sn6 7.19(16) . . ? Sn5 Sn9 Sn8 63.50(3) . . ? Zn1 Sn9 Sn8 53.26(4) . . ? Sn2 Sn9 Sn8 102.56(4) . . ? Sn6A Sn9 Sn8 86.73(9) . . ? Sn6 Sn9 Sn8 80.98(12) . . ? Sn4A Sn3 Sn1 67.8(2) . . ? Sn4A Sn3 Sn4 8.6(3) . . ? Sn1 Sn3 Sn4 62.51(12) . . ? Sn4A Sn3 Sn6 91.8(2) . . ? Sn1 Sn3 Sn6 109.53(16) . . ? Sn4 Sn3 Sn6 99.85(16) . . ? Sn4A Sn3 Sn7 51.6(2) . . ? Sn1 Sn3 Sn7 116.21(14) . . ? Sn4 Sn3 Sn7 59.21(13) . . ? Sn6 Sn3 Sn7 59.87(12) . . ? Sn4A Sn3 Sn7A 57.0(3) . . ? Sn1 Sn3 Sn7A 119.20(17) . . ? Sn4 Sn3 Sn7A 64.91(15) . . ? Sn6 Sn3 Sn7A 53.30(17) . . ? Sn7 Sn3 Sn7A 6.96(16) . . ? Sn4A Sn3 Sn2 90.3(2) . . ? Sn1 Sn3 Sn2 55.33(8) . . ? Sn4 Sn3 Sn2 92.08(14) . . ? Sn6 Sn3 Sn2 58.45(10) . . ? Sn7 Sn3 Sn2 103.23(13) . . ? Sn7A Sn3 Sn2 99.62(18) . . ? Sn4A Sn3 Sn6A 93.5(2) . . ? Sn1 Sn3 Sn6A 108.1(2) . . ? Sn4 Sn3 Sn6A 101.51(16) . . ? Sn6 Sn3 Sn6A 2.86(18) . . ? Sn7 Sn3 Sn6A 62.70(14) . . ? Sn7A Sn3 Sn6A 56.15(16) . . ? Sn2 Sn3 Sn6A 56.25(17) . . ? Sn3 Sn4 Sn7 63.05(13) . . ? Sn3 Sn4 Sn1 58.57(11) . . ? Sn7 Sn4 Sn1 116.13(14) . . ? Sn3 Sn4 Sn8 100.29(13) . . ? Sn7 Sn4 Sn8 58.44(11) . . ? Sn1 Sn4 Sn8 109.26(16) . . ? Sn3 Sn4 Sn3A 7.77(17) . . ? Sn7 Sn4 Sn3A 57.61(19) . . ? Sn1 Sn4 Sn3A 61.4(2) . . ? Sn8 Sn4 Sn3A 92.53(17) . . ? Sn3 Sn4 Sn5 88.61(13) . . ? Sn7 Sn4 Sn5 102.56(14) . . ? Sn1 Sn4 Sn5 54.28(8) . . ? Sn8 Sn4 Sn5 59.27(9) . . ? Sn3A Sn4 Sn5 84.85(18) . . ? Sn3 Sn4 Sn7A 62.06(15) . . ? Sn7 Sn4 Sn7A 4.13(17) . . ? Sn1 Sn4 Sn7A 113.39(19) . . ? Sn8 Sn4 Sn7A 55.73(14) . . ? Sn3A Sn4 Sn7A 56.2(2) . . ? Sn5 Sn4 Sn7A 98.46(17) . . ? Sn3A Sn6 Zn1 120.0(3) . . ? Sn3A Sn6 Sn7A 69.0(3) . . ? Zn1 Sn6 Sn7A 57.08(19) . . ? Sn3A Sn6 Sn3 1.6(2) . . ? Zn1 Sn6 Sn3 118.6(2) . . ? Sn7A Sn6 Sn3 68.2(2) . . ? Sn3A Sn6 Sn7 62.8(2) . . ? Zn1 Sn6 Sn7 61.53(17) . . ? Sn7A Sn6 Sn7 6.8(2) . . ? Sn3 Sn6 Sn7 61.90(12) . . ? Sn3A Sn6 Sn2 65.8(2) . . ? Zn1 Sn6 Sn2 115.56(11) . . ? Sn7A Sn6 Sn2 116.0(2) . . ? Sn3 Sn6 Sn2 65.40(14) . . ? Sn7 Sn6 Sn2 109.80(14) . . ? Sn3A Sn6 Sn9 107.0(2) . . ? Zn1 Sn6 Sn9 60.47(8) . . ? Sn7A Sn6 Sn9 97.79(17) . . ? Sn3 Sn6 Sn9 105.71(15) . . ? Sn7 Sn6 Sn9 96.86(12) . . ? Sn2 Sn6 Sn9 57.72(7) . . ? Sn4A Sn7 Sn3A 64.9(3) . . ? Sn4A Sn7 Sn8 57.6(3) . . ? Sn3A Sn7 Sn8 98.45(19) . . ? Sn4A Sn7 Zn1 107.0(2) . . ? Sn3A Sn7 Zn1 102.13(17) . . ? Sn8 Sn7 Zn1 54.30(9) . . ? Sn4A Sn7 Sn4 4.6(3) . . ? Sn3A Sn7 Sn4 63.33(17) . . ? Sn8 Sn7 Sn4 62.19(14) . . ? Zn1 Sn7 Sn4 111.46(15) . . ? Sn4A Sn7 Sn6 96.1(2) . . ? Sn3A Sn7 Sn6 50.44(15) . . ? Sn8 Sn7 Sn6 83.68(12) . . ? Zn1 Sn7 Sn6 54.74(10) . . ? Sn4 Sn7 Sn6 97.66(14) . . ? Sn4A Sn7 Sn3 59.8(3) . . ? Sn3A Sn7 Sn3 7.88(15) . . ? Sn8 Sn7 Sn3 99.23(13) . . ? Zn1 Sn7 Sn3 109.02(11) . . ? Sn4 Sn7 Sn3 57.74(12) . . ? Sn6 Sn7 Sn3 58.23(10) . . ? Sn4A Sn7 Sn6A 98.4(3) . . ? Sn3A Sn7 Sn6A 54.47(16) . . ? Sn8 Sn7 Sn6A 82.23(16) . . ? Zn1 Sn7 Sn6A 50.92(15) . . ? Sn4 Sn7 Sn6A 100.21(18) . . ? Sn6 Sn7 Sn6A 4.04(19) . . ? Sn3 Sn7 Sn6A 62.24(15) . . ? Sn6 Sn3A Sn6A 3.4(2) . . ? Sn6 Sn3A Sn7 66.8(2) . . ? Sn6A Sn3A Sn7 70.1(2) . . ? Sn6 Sn3A Sn4A 98.6(3) . . ? Sn6A Sn3A Sn4A 100.8(3) . . ? Sn7 Sn3A Sn4A 52.2(2) . . ? Sn6 Sn3A Sn7A 59.5(2) . . ? Sn6A Sn3A Sn7A 62.9(2) . . ? Sn7 Sn3A Sn7A 7.71(17) . . ? Sn4A Sn3A Sn7A 58.4(3) . . ? Sn6 Sn3A Sn2 65.18(16) . . ? Sn6A Sn3A Sn2 62.72(19) . . ? Sn7 Sn3A Sn2 112.0(2) . . ? Sn4A Sn3A Sn2 91.9(3) . . ? Sn7A Sn3A Sn2 108.9(3) . . ? Sn6 Sn3A Sn4 106.1(3) . . ? Sn6A Sn3A Sn4 108.1(3) . . ? Sn7 Sn3A Sn4 59.1(2) . . ? Sn4A Sn3A Sn4 7.9(3) . . ? Sn7A Sn3A Sn4 65.6(2) . . ? Sn2 Sn3A Sn4 92.6(2) . . ? Sn6 Sn3A Sn1 115.8(3) . . ? Sn6A Sn3A Sn1 114.4(3) . . ? Sn7 Sn3A Sn1 114.6(3) . . ? Sn4A Sn3A Sn1 63.7(3) . . ? Sn7A Sn3A Sn1 119.2(3) . . ? Sn2 Sn3A Sn1 55.42(15) . . ? Sn4 Sn3A Sn1 58.28(16) . . ? Sn7 Sn4A Sn8 67.7(3) . . ? Sn7 Sn4A Sn3 68.6(2) . . ? Sn8 Sn4A Sn3 111.6(3) . . ? Sn7 Sn4A Sn7A 5.09(19) . . ? Sn8 Sn4A Sn7A 64.1(3) . . ? Sn3 Sn4A Sn7A 67.9(2) . . ? Sn7 Sn4A Sn3A 62.9(3) . . ? Sn8 Sn4A Sn3A 103.3(3) . . ? Sn3 Sn4A Sn3A 8.39(17) . . ? Sn7A Sn4A Sn3A 61.6(3) . . ? Sn7 Sn4A Sn1 121.8(3) . . ? Sn8 Sn4A Sn1 113.9(3) . . ? Sn3 Sn4A Sn1 56.9(2) . . ? Sn7A Sn4A Sn1 119.2(3) . . ? Sn3A Sn4A Sn1 60.4(2) . . ? Sn7 Sn4A Sn5 113.6(3) . . ? Sn8 Sn4A Sn5 63.4(2) . . ? Sn3 Sn4A Sn5 90.9(3) . . ? Sn7A Sn4A Sn5 108.5(3) . . ? Sn3A Sn4A Sn5 87.9(3) . . ? Sn1 Sn4A Sn5 53.26(18) . . ? Zn1 Sn6A Sn3A 109.0(2) . . ? Zn1 Sn6A Sn9 61.96(12) . . ? Sn3A Sn6A Sn9 100.7(3) . . ? Zn1 Sn6A Sn7A 53.73(17) . . ? Sn3A Sn6A Sn7A 60.7(2) . . ? Sn9 Sn6A Sn7A 93.61(18) . . ? Zn1 Sn6A Sn2 114.5(2) . . ? Sn3A Sn6A Sn2 61.4(2) . . ? Sn9 Sn6A Sn2 58.10(14) . . ? Sn7A Sn6A Sn2 106.3(2) . . ? Zn1 Sn6A Sn3 108.26(14) . . ? Sn3A Sn6A Sn3 1.3(2) . . ? Sn9 Sn6A Sn3 99.49(19) . . ? Sn7A Sn6A Sn3 60.38(18) . . ? Sn2 Sn6A Sn3 60.65(15) . . ? Zn1 Sn6A Sn7 57.35(13) . . ? Sn3A Sn6A Sn7 55.40(19) . . ? Sn9 Sn6A Sn7 92.18(14) . . ? Sn7A Sn6A Sn7 5.8(2) . . ? Sn2 Sn6A Sn7 100.78(17) . . ? Sn3 Sn6A Sn7 55.06(14) . . ? Zn1 Sn7A Sn6 60.68(15) . . ? Zn1 Sn7A Sn4A 106.6(3) . . ? Sn6 Sn7A Sn4A 94.1(3) . . ? Zn1 Sn7A Sn8 56.75(13) . . ? Sn6 Sn7A Sn8 86.96(18) . . ? Sn4A Sn7A Sn8 54.0(3) . . ? Zn1 Sn7A Sn3A 107.4(2) . . ? Sn6 Sn7A Sn3A 51.49(17) . . ? Sn4A Sn7A Sn3A 60.0(3) . . ? Sn8 Sn7A Sn3A 95.3(3) . . ? Zn1 Sn7A Sn6A 56.22(15) . . ? Sn6 Sn7A Sn6A 4.9(2) . . ? Sn4A Sn7A Sn6A 97.4(3) . . ? Sn8 Sn7A Sn6A 85.97(19) . . ? Sn3A Sn7A Sn6A 56.4(2) . . ? Zn1 Sn7A Sn3 113.2(2) . . ? Sn6 Sn7A Sn3 58.53(17) . . ? Sn4A Sn7A Sn3 55.1(3) . . ? Sn8 Sn7A Sn3 95.0(2) . . ? Sn3A Sn7A Sn3 7.14(15) . . ? Sn6A Sn7A Sn3 63.5(2) . . ? Zn1 Sn7A Sn4 110.1(2) . . ? Sn6 Sn7A Sn4 94.8(2) . . ? Sn4A Sn7A Sn4 3.7(3) . . ? Sn8 Sn7A Sn4 57.69(15) . . ? Sn3A Sn7A Sn4 58.22(19) . . ? Sn6A Sn7A Sn4 98.4(3) . . ? Sn3 Sn7A Sn4 53.03(15) . . ? C1 Zn1 Sn7A 128.1(4) . . ? C1 Zn1 Sn8 133.0(4) . . ? Sn7A Zn1 Sn8 67.92(14) . . ? C1 Zn1 Sn6A 127.2(4) . . ? Sn7A Zn1 Sn6A 70.04(17) . . ? Sn8 Zn1 Sn6A 99.53(15) . . ? C1 Zn1 Sn6 133.2(4) . . ? Sn7A Zn1 Sn6 62.2(2) . . ? Sn8 Zn1 Sn6 93.85(13) . . ? Sn6A Zn1 Sn6 8.14(18) . . ? C1 Zn1 Sn9 127.6(4) . . ? Sn7A Zn1 Sn9 104.23(18) . . ? Sn8 Zn1 Sn9 65.79(4) . . ? Sn6A Zn1 Sn9 62.93(15) . . ? Sn6 Zn1 Sn9 64.98(9) . . ? C1 Zn1 Sn7 131.5(4) . . ? Sn7A Zn1 Sn7 5.48(19) . . ? Sn8 Zn1 Sn7 62.45(11) . . ? Sn6A Zn1 Sn7 71.73(12) . . ? Sn6 Zn1 Sn7 63.73(14) . . ? Sn9 Zn1 Sn7 100.91(9) . . ? C2 C1 C6 110.6(14) . . ? C2 C1 Zn1 122.2(11) . . ? C6 C1 Zn1 127.2(10) . . ? C1 C2 C3 121.8(14) . . ? C1 C2 C7 116.4(15) . . ? C3 C2 C7 121.9(13) . . ? C4 C3 C2 126.4(14) . . ? C4 C3 H3 116.8 . . ? C2 C3 H3 116.8 . . ? C5 C4 C3 111.9(17) . . ? C5 C4 C8 121.8(17) . . ? C3 C4 C8 126.2(16) . . ? C4 C5 C6 121.5(15) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 127.5(13) . . ? C1 C6 C9 115.0(15) . . ? C5 C6 C9 117.2(14) . . ? C6 C9 H9C 109.5 . . ? C6 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? C6 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8C 109.5 . . ? C4 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C103 O11 C102 114.0(9) . . ? C105 O12 C104 107.6(9) . . ? C108 O13 C109 107.7(8) . . ? C111 O14 C110 116.5(10) . . ? C115 O15 C114 113.9(11) . . ? C116 O16 C117 110.6(11) . . ? C113 N11 C107 103.7(10) . . ? C113 N11 C101 107.0(11) . . ? C107 N11 C101 115.8(9) . . ? C106 N12 C118 102.8(12) . . ? C106 N12 C112 113.4(10) . . ? C118 N12 C112 114.3(14) . . ? C102 C101 N11 113.2(10) . . ? C102 C101 H10A 108.9 . . ? N11 C101 H10A 108.9 . . ? C102 C101 H10B 108.9 . . ? N11 C101 H10B 108.9 . . ? H10A C101 H10B 107.8 . . ? C101 C102 O11 111.0(10) . . ? C101 C102 H10C 109.4 . . ? O11 C102 H10C 109.4 . . ? C101 C102 H10D 109.4 . . ? O11 C102 H10D 109.4 . . ? H10C C102 H10D 108.0 . . ? O11 C103 C104 113.9(9) . . ? O11 C103 H10E 108.8 . . ? C104 C103 H10E 108.8 . . ? O11 C103 H10F 108.8 . . ? C104 C103 H10F 108.8 . . ? H10E C103 H10F 107.7 . . ? O12 C104 C103 106.1(8) . . ? O12 C104 H10G 110.5 . . ? C103 C104 H10G 110.5 . . ? O12 C104 H10H 110.5 . . ? C103 C104 H10H 110.5 . . ? H10G C104 H10H 108.7 . . ? O12 C105 C106 104.2(10) . . ? O12 C105 H10I 110.9 . . ? C106 C105 H10I 110.9 . . ? O12 C105 H10J 110.9 . . ? C106 C105 H10J 110.9 . . ? H10I C105 H10J 108.9 . . ? N12 C106 C105 115.9(10) . . ? N12 C106 H10K 108.3 . . ? C105 C106 H10K 108.3 . . ? N12 C106 H10L 108.3 . . ? C105 C106 H10L 108.3 . . ? H10K C106 H10L 107.4 . . ? N11 C107 C108 117.6(11) . . ? N11 C107 H10M 107.9 . . ? C108 C107 H10M 107.9 . . ? N11 C107 H10N 107.9 . . ? C108 C107 H10N 107.9 . . ? H10M C107 H10N 107.2 . . ? O13 C108 C107 104.8(9) . . ? O13 C108 H10O 110.8 . . ? C107 C108 H10O 110.8 . . ? O13 C108 H10P 110.8 . . ? C107 C108 H10P 110.8 . . ? H10O C108 H10P 108.9 . . ? O13 C109 C110 105.0(9) . . ? O13 C109 H10Q 110.7 . . ? C110 C109 H10Q 110.7 . . ? O13 C109 H10R 110.7 . . ? C110 C109 H10R 110.7 . . ? H10Q C109 H10R 108.8 . . ? O14 C110 C109 115.2(9) . . ? O14 C110 H11A 108.5 . . ? C109 C110 H11A 108.5 . . ? O14 C110 H11B 108.5 . . ? C109 C110 H11B 108.5 . . ? H11A C110 H11B 107.5 . . ? O14 C111 C112 112.7(11) . . ? O14 C111 H11C 109.0 . . ? C112 C111 H11C 109.0 . . ? O14 C111 H11D 109.0 . . ? C112 C111 H11D 109.0 . . ? H11C C111 H11D 107.8 . . ? C111 C112 N12 119.1(12) . . ? C111 C112 H11E 107.6 . . ? N12 C112 H11E 107.6 . . ? C111 C112 H11F 107.6 . . ? N12 C112 H11F 107.6 . . ? H11E C112 H11F 107.0 . . ? N11 C113 C114 109.2(11) . . ? N11 C113 H11G 109.8 . . ? C114 C113 H11G 109.8 . . ? N11 C113 H11H 109.8 . . ? C114 C113 H11H 109.8 . . ? H11G C113 H11H 108.3 . . ? O15 C114 C113 111.3(11) . . ? O15 C114 H11I 109.4 . . ? C113 C114 H11I 109.4 . . ? O15 C114 H11J 109.4 . . ? C113 C114 H11J 109.4 . . ? H11I C114 H11J 108.0 . . ? O15 C115 C116 112.6(10) . . ? O15 C115 H11K 109.1 . . ? C116 C115 H11K 109.1 . . ? O15 C115 H11L 109.1 . . ? C116 C115 H11L 109.1 . . ? H11K C115 H11L 107.8 . . ? O16 C116 C115 107.6(11) . . ? O16 C116 H11M 110.2 . . ? C115 C116 H11M 110.2 . . ? O16 C116 H11N 110.2 . . ? C115 C116 H11N 110.2 . . ? H11M C116 H11N 108.5 . . ? O16 C117 C118 111.8(14) . . ? O16 C117 H11O 109.2 . . ? C118 C117 H11O 109.2 . . ? O16 C117 H11P 109.3 . . ? C118 C117 H11P 109.3 . . ? H11O C117 H11P 107.9 . . ? C117 C118 N12 106.9(15) . . ? C117 C118 H11Q 110.3 . . ? N12 C118 H11Q 110.3 . . ? C117 C118 H11R 110.3 . . ? N12 C118 H11R 110.3 . . ? H11Q C118 H11R 108.6 . . ? C203 O21 C202 108.1(17) . . ? C205 O22 C204 116.8(16) . . ? C208 O23 C209 116.5(15) . . ? C210 O24 C211 109(2) . . ? C215 O25 C214 114.3(18) . . ? C216 O26 C217 107.6(17) . . ? C207 N21 C213 115.1(17) . . ? C207 N21 C201 110(2) . . ? C213 N21 C201 107.3(15) . . ? C212 N22 C206 102.7(19) . . ? C212 N22 C218 103(2) . . ? C206 N22 C218 120(2) . . ? C202 C201 N21 109.6(15) . . ? C202 C201 H20A 109.7 . . ? N21 C201 H20A 109.7 . . ? C202 C201 H20B 109.7 . . ? N21 C201 H20B 109.7 . . ? H20A C201 H20B 108.2 . . ? C201 C202 O21 102(2) . . ? C201 C202 H20C 111.5 . . ? O21 C202 H20C 111.5 . . ? C201 C202 H20D 111.5 . . ? O21 C202 H20D 111.5 . . ? H20C C202 H20D 109.3 . . ? O21 C203 C204 103.0(16) . . ? O21 C203 H20E 111.2 . . ? C204 C203 H20E 111.2 . . ? O21 C203 H20F 111.2 . . ? C204 C203 H20F 111.2 . . ? H20E C203 H20F 109.1 . . ? O22 C204 C203 111.4(15) . . ? O22 C204 H20G 109.3 . . ? C203 C204 H20G 109.3 . . ? O22 C204 H20H 109.3 . . ? C203 C204 H20H 109.3 . . ? H20G C204 H20H 108.0 . . ? O22 C205 C206 117.3(18) . . ? O22 C205 H20I 108.0 . . ? C206 C205 H20I 108.0 . . ? O22 C205 H20J 108.0 . . ? C206 C205 H20J 108.0 . . ? H20I C205 H20J 107.2 . . ? N22 C206 C205 108(2) . . ? N22 C206 H20K 110.2 . . ? C205 C206 H20K 110.2 . . ? N22 C206 H20L 110.2 . . ? C205 C206 H20L 110.2 . . ? H20K C206 H20L 108.5 . . ? N21 C207 C208 105(2) . . ? N21 C207 H20M 110.8 . . ? C208 C207 H20M 110.8 . . ? N21 C207 H20N 110.8 . . ? C208 C207 H20N 110.8 . . ? H20M C207 H20N 108.8 . . ? O23 C208 C207 117.0(17) . . ? O23 C208 H20O 108.1 . . ? C207 C208 H20O 108.1 . . ? O23 C208 H20P 108.1 . . ? C207 C208 H20P 108.1 . . ? H20O C208 H20P 107.3 . . ? O23 C209 C210 110.1(16) . . ? O23 C209 H20Q 109.6 . . ? C210 C209 H20Q 109.6 . . ? O23 C209 H20R 109.6 . . ? C210 C209 H20R 109.6 . . ? H20Q C209 H20R 108.2 . . ? O24 C210 C209 112.8(18) . . ? O24 C210 H21A 109.0 . . ? C209 C210 H21A 109.0 . . ? O24 C210 H21B 109.0 . . ? C209 C210 H21B 109.0 . . ? H21A C210 H21B 107.8 . . ? O24 C211 C212 105.0(19) . . ? O24 C211 H21C 110.7 . . ? C212 C211 H21C 110.7 . . ? O24 C211 H21D 110.7 . . ? C212 C211 H21D 110.7 . . ? H21C C211 H21D 108.8 . . ? N22 C212 C211 103.5(17) . . ? N22 C212 H21E 111.1 . . ? C211 C212 H21E 111.1 . . ? N22 C212 H21F 111.1 . . ? C211 C212 H21F 111.1 . . ? H21E C212 H21F 109.0 . . ? N21 C213 C214 120.2(16) . . ? N21 C213 H21G 107.3 . . ? C214 C213 H21G 107.3 . . ? N21 C213 H21H 107.3 . . ? C214 C213 H21H 107.3 . . ? H21G C213 H21H 106.9 . . ? O25 C214 C213 111.8(16) . . ? O25 C214 H21I 109.3 . . ? C213 C214 H21I 109.3 . . ? O25 C214 H21J 109.3 . . ? C213 C214 H21J 109.3 . . ? H21I C214 H21J 107.9 . . ? O25 C215 C216 107.1(17) . . ? O25 C215 H21K 110.3 . . ? C216 C215 H21K 110.3 . . ? O25 C215 H21L 110.3 . . ? C216 C215 H21L 110.3 . . ? H21K C215 H21L 108.5 . . ? O26 C216 C215 109.0(18) . . ? O26 C216 H21M 109.9 . . ? C215 C216 H21M 109.9 . . ? O26 C216 H21N 109.9 . . ? C215 C216 H21N 109.9 . . ? H21M C216 H21N 108.3 . . ? O26 C217 C218 109.0(19) . . ? O26 C217 H21O 109.9 . . ? C218 C217 H21O 109.9 . . ? O26 C217 H21P 109.9 . . ? C218 C217 H21P 109.9 . . ? H21O C217 H21P 108.3 . . ? N22 C218 C217 109(2) . . ? N22 C218 H21Q 110.0 . . ? C217 C218 H21Q 110.0 . . ? N22 C218 H21R 110.0 . . ? C217 C218 H21R 110.0 . . ? H21Q C218 H21R 108.3 . . ? C302 O31 C303 113.5(12) . . ? C304 O32 C305 115.8(10) . . ? C309 O33 C308 112.2(10) . . ? C311 O34 C310 116.1(9) . . ? C315 O35 C314 119.7(10) . . ? C316 O36 C317 108.9(9) . . ? C301 N31 C313 102.9(14) . . ? C301 N31 C307 109.7(13) . . ? C313 N31 C307 112.3(12) . . ? C318 N32 C306 101.5(8) . . ? C318 N32 C312 109.8(9) . . ? C306 N32 C312 115.7(9) . . ? N31 C301 C302 110.0(14) . . ? N31 C301 H30A 109.7 . . ? C302 C301 H30A 109.7 . . ? N31 C301 H30B 109.7 . . ? C302 C301 H30B 109.7 . . ? H30A C301 H30B 108.2 . . ? O31 C302 C301 110.2(13) . . ? O31 C302 H30C 109.6 . . ? C301 C302 H30C 109.6 . . ? O31 C302 H30D 109.6 . . ? C301 C302 H30D 109.6 . . ? H30C C302 H30D 108.1 . . ? C304 C303 O31 111.5(12) . . ? C304 C303 H30E 109.3 . . ? O31 C303 H30E 109.3 . . ? C304 C303 H30F 109.3 . . ? O31 C303 H30F 109.3 . . ? H30E C303 H30F 108.0 . . ? O32 C304 C303 113.5(13) . . ? O32 C304 H30G 108.9 . . ? C303 C304 H30G 108.9 . . ? O32 C304 H30H 108.9 . . ? C303 C304 H30H 108.9 . . ? H30G C304 H30H 107.7 . . ? O32 C305 C306 114.4(9) . . ? O32 C305 H30I 108.7 . . ? C306 C305 H30I 108.7 . . ? O32 C305 H30J 108.7 . . ? C306 C305 H30J 108.7 . . ? H30I C305 H30J 107.6 . . ? C305 C306 N32 106.0(9) . . ? C305 C306 H30K 110.5 . . ? N32 C306 H30K 110.5 . . ? C305 C306 H30L 110.5 . . ? N32 C306 H30L 110.5 . . ? H30K C306 H30L 108.7 . . ? C308 C307 N31 114.2(11) . . ? C308 C307 H30M 108.7 . . ? N31 C307 H30M 108.7 . . ? C308 C307 H30N 108.7 . . ? N31 C307 H30N 108.7 . . ? H30M C307 H30N 107.6 . . ? O33 C308 C307 109.2(11) . . ? O33 C308 H30O 109.8 . . ? C307 C308 H30O 109.8 . . ? O33 C308 H30P 109.8 . . ? C307 C308 H30P 109.8 . . ? H30O C308 H30P 108.3 . . ? O33 C309 C310 112.1(10) . . ? O33 C309 H30Q 109.2 . . ? C310 C309 H30Q 109.2 . . ? O33 C309 H30R 109.2 . . ? C310 C309 H30R 109.2 . . ? H30Q C309 H30R 107.9 . . ? C309 C310 O34 114.1(10) . . ? C309 C310 H31A 108.7 . . ? O34 C310 H31A 108.7 . . ? C309 C310 H31B 108.7 . . ? O34 C310 H31B 108.7 . . ? H31A C310 H31B 107.6 . . ? O34 C311 C312 113.6(10) . . ? O34 C311 H31C 108.8 . . ? C312 C311 H31C 108.8 . . ? O34 C311 H31D 108.8 . . ? C312 C311 H31D 108.8 . . ? H31C C311 H31D 107.7 . . ? N32 C312 C311 117.6(9) . . ? N32 C312 H31E 107.9 . . ? C311 C312 H31E 107.9 . . ? N32 C312 H31F 107.9 . . ? C311 C312 H31F 107.9 . . ? H31E C312 H31F 107.2 . . ? N31 C313 C314 110.5(11) . . ? N31 C313 H31G 109.5 . . ? C314 C313 H31G 109.5 . . ? N31 C313 H31H 109.5 . . ? C314 C313 H31H 109.5 . . ? H31G C313 H31H 108.1 . . ? C313 C314 O35 113.5(11) . . ? C313 C314 H31I 108.9 . . ? O35 C314 H31I 108.9 . . ? C313 C314 H31J 108.9 . . ? O35 C314 H31J 108.9 . . ? H31I C314 H31J 107.7 . . ? O35 C315 C316 116.5(10) . . ? O35 C315 H31K 108.2 . . ? C316 C315 H31K 108.2 . . ? O35 C315 H31L 108.2 . . ? C316 C315 H31L 108.2 . . ? H31K C315 H31L 107.3 . . ? O36 C316 C315 108.1(10) . . ? O36 C316 H31M 110.1 . . ? C315 C316 H31M 110.1 . . ? O36 C316 H31N 110.1 . . ? C315 C316 H31N 110.1 . . ? H31M C316 H31N 108.4 . . ? C318 C317 O36 105.2(8) . . ? C318 C317 H31O 110.7 . . ? O36 C317 H31O 110.7 . . ? C318 C317 H31P 110.7 . . ? O36 C317 H31P 110.7 . . ? H31O C317 H31P 108.8 . . ? N32 C318 C317 110.7(10) . . ? N32 C318 H31Q 109.5 . . ? C317 C318 H31Q 109.5 . . ? N32 C318 H31R 109.5 . . ? C317 C318 H31R 109.5 . . ? H31Q C318 H31R 108.1 . . ? C2S C1S H1T 109.5 . . ? C2S C1S H3T 109.5 . . ? H1T C1S H3T 109.5 . . ? C2S C1S H2T 109.5 . . ? H1T C1S H2T 109.5 . . ? H3T C1S H2T 109.5 . . ? C7S C2S C3S 120.0 . . ? C7S C2S C1S 121(2) . . ? C3S C2S C1S 119(2) . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3SA 120.0 . . ? C2S C3S H3SA 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C7S C6S C5S 120.0 . . ? C7S C6S H6S 120.0 . . ? C5S C6S H6S 120.0 . . ? C6S C7S C2S 120.0 . . ? C6S C7S H7S 120.0 . . ? C2S C7S H7S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.629 _refine_diff_density_min -1.702 _refine_diff_density_rms 0.128 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 700662' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)]3[Ge9Zn(iPr)]*en*2tol ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K-(2,2,2-crypt))3(Ge9Zn(iPr))*en*2tol _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), C3 H7 Ge9 Zn, 2(C7 H8), C2 H6 N2' _chemical_formula_sum 'C73 H139 Ge9 K3 N8 O18 Zn' _chemical_formula_weight 2252.90 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' K K 0.2009 0.2494 '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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.86500(10) _cell_length_b 15.17060(10) _cell_length_c 26.0077(2) _cell_angle_alpha 75.4570(10) _cell_angle_beta 85.3940(10) _cell_angle_gamma 69.1790(10) _cell_volume 4949.15(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 3.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3163 _exptl_absorpt_correction_T_max 0.6040 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43107 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 22374 _reflns_number_gt 18451 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. Due to poorly resolved electon density around the two toluene solvent molecules (presumably due to crystallographic disorder which could not be modelled) it was necessary to constrain the atomic positions of the aromatic rings to fit a planar geometry employing the AFIX 69 command' ; _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^)+(0.0280P)^2^+7.9296P] 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 22374 _refine_ls_number_parameters 987 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.18676(2) 0.96230(2) 0.343324(12) 0.02695(7) Uani 1 1 d . . . Ge3 Ge 0.14097(2) 0.80885(2) 0.354555(12) 0.02455(7) Uani 1 1 d . . . Ge4 Ge 0.34519(2) 0.80363(2) 0.363516(12) 0.02448(7) Uani 1 1 d . . . Ge5 Ge 0.31922(2) 0.94864(2) 0.267982(12) 0.02617(7) Uani 1 1 d . . . Ge2 Ge 0.11416(2) 0.95517(2) 0.257363(12) 0.02662(7) Uani 1 1 d . . . Ge7 Ge 0.30109(2) 0.67227(2) 0.335961(12) 0.02354(7) Uani 1 1 d . . . Ge8 Ge 0.42426(2) 0.76873(2) 0.275525(12) 0.02521(7) Uani 1 1 d . . . Ge9 Ge 0.26571(2) 0.87155(2) 0.203172(11) 0.02687(7) Uani 1 1 d . . . Ge6 Ge 0.14071(2) 0.77722(2) 0.262520(12) 0.02641(7) Uani 1 1 d . . . Zn1 Zn 0.32578(3) 0.68245(3) 0.235070(15) 0.03416(9) Uani 1 1 d . . . C1 C 0.3849(2) 0.5809(2) 0.19238(13) 0.0315(7) Uani 1 1 d . . . H1 H 0.4292 0.5206 0.2173 0.038 Uiso 1 1 calc R . . C2 C 0.4546(3) 0.6109(3) 0.14920(16) 0.0500(9) Uani 1 1 d . . . H2A H 0.5060 0.6276 0.1647 0.075 Uiso 1 1 calc R . . H2B H 0.4133 0.6674 0.1225 0.075 Uiso 1 1 calc R . . H2C H 0.4898 0.5570 0.1323 0.075 Uiso 1 1 calc R . . C3 C 0.3054(3) 0.5543(3) 0.16965(17) 0.0516(10) Uani 1 1 d . . . H3A H 0.2613 0.5347 0.1982 0.077 Uiso 1 1 calc R . . H3B H 0.3402 0.5004 0.1528 0.077 Uiso 1 1 calc R . . H3C H 0.2631 0.6106 0.1432 0.077 Uiso 1 1 calc R . . K1 K 0.12714(4) 0.53592(4) 0.64668(2) 0.02521(13) Uani 1 1 d . . . K2 K 0.77300(6) -0.09446(5) 0.07620(3) 0.03660(16) Uani 1 1 d . . . K3 K 0.60428(5) 0.12799(4) 0.38868(3) 0.02694(13) Uani 1 1 d . . . N11 N 0.21956(19) 0.49363(18) 0.54245(10) 0.0300(5) Uani 1 1 d . . . N12 N 0.0347(2) 0.5719(2) 0.75307(11) 0.0374(6) Uani 1 1 d . . . N21 N 0.7060(4) -0.2470(4) 0.05116(19) 0.0911(17) Uani 1 1 d . . . N22 N 0.8425(2) 0.0578(2) 0.10055(12) 0.0445(7) Uani 1 1 d . . . N31 N 0.4192(2) 0.2863(2) 0.32913(14) 0.0451(8) Uani 1 1 d . . . N32 N 0.78863(18) -0.03112(18) 0.44946(10) 0.0273(5) Uani 1 1 d . . . O11 O 0.04319(17) 0.44187(15) 0.58902(9) 0.0346(5) Uani 1 1 d . . . O12 O -0.02012(17) 0.45864(18) 0.69328(9) 0.0390(5) Uani 1 1 d . . . O13 O 0.11948(16) 0.69005(15) 0.55894(8) 0.0304(5) Uani 1 1 d . . . O14 O 0.00097(17) 0.72317(15) 0.65330(9) 0.0347(5) Uani 1 1 d . . . O15 O 0.33660(15) 0.46331(16) 0.63769(9) 0.0344(5) Uani 1 1 d . . . O16 O 0.25500(17) 0.52720(17) 0.73095(9) 0.0402(5) Uani 1 1 d . . . O21 O 0.5908(2) -0.1176(2) 0.12009(10) 0.0522(7) Uani 1 1 d . . . O22 O 0.67217(18) 0.00272(18) 0.15646(9) 0.0408(5) Uani 1 1 d . . . O23 O 0.7103(3) -0.0740(3) -0.02752(11) 0.0751(10) Uani 1 1 d . . . O24 O 0.7492(2) 0.0810(2) -0.00069(10) 0.0559(7) Uani 1 1 d . . . O25 O 0.9142(3) -0.2878(2) 0.08853(14) 0.0843(12) Uani 1 1 d . . . O26 O 0.9840(2) -0.1403(2) 0.09747(10) 0.0576(7) Uani 1 1 d . . . O31 O 0.51905(16) 0.31219(15) 0.41412(9) 0.0348(5) Uani 1 1 d . . . O32 O 0.66885(16) 0.15017(14) 0.48126(8) 0.0289(4) Uani 1 1 d . . . O33 O 0.6226(2) 0.21003(17) 0.27902(9) 0.0429(6) Uani 1 1 d . . . O34 O 0.80054(16) 0.08850(16) 0.34250(8) 0.0326(5) Uani 1 1 d . . . O35 O 0.41711(17) 0.09325(16) 0.38822(11) 0.0413(6) Uani 1 1 d . . . O36 O 0.60263(16) -0.06235(15) 0.42791(8) 0.0302(5) Uani 1 1 d . . . C101 C 0.1603(3) 0.4514(3) 0.51827(13) 0.0392(8) Uani 1 1 d . . . H10A H 0.2054 0.4144 0.4937 0.047 Uiso 1 1 calc R . . H10B H 0.1027 0.5045 0.4971 0.047 Uiso 1 1 calc R . . C102 C 0.1172(3) 0.3852(2) 0.55831(15) 0.0407(8) Uani 1 1 d . . . H10C H 0.0842 0.3531 0.5400 0.049 Uiso 1 1 calc R . . H10D H 0.1732 0.3343 0.5816 0.049 Uiso 1 1 calc R . . C103 C -0.0152(3) 0.3882(3) 0.62129(15) 0.0432(9) Uani 1 1 d . . . H10E H 0.0319 0.3266 0.6431 0.052 Uiso 1 1 calc R . . H10F H -0.0573 0.3722 0.5985 0.052 Uiso 1 1 calc R . . C104 C -0.0829(3) 0.4470(3) 0.65604(15) 0.0443(9) Uani 1 1 d . . . H10G H -0.1249 0.5113 0.6345 0.053 Uiso 1 1 calc R . . H10H H -0.1302 0.4143 0.6753 0.053 Uiso 1 1 calc R . . C105 C -0.0753(3) 0.4793(3) 0.73926(15) 0.0458(9) Uani 1 1 d . . . H10I H -0.0989 0.4250 0.7574 0.055 Uiso 1 1 calc R . . H10J H -0.1369 0.5388 0.7293 0.055 Uiso 1 1 calc R . . C106 C -0.0070(3) 0.4937(3) 0.77597(14) 0.0476(9) Uani 1 1 d . . . H10K H -0.0467 0.5080 0.8081 0.057 Uiso 1 1 calc R . . H10L H 0.0515 0.4321 0.7874 0.057 Uiso 1 1 calc R . . C107 C 0.2239(3) 0.5836(2) 0.50603(13) 0.0363(7) Uani 1 1 d . . . H10M H 0.2339 0.5744 0.4694 0.044 Uiso 1 1 calc R . . H10N H 0.2841 0.5970 0.5156 0.044 Uiso 1 1 calc R . . C108 C 0.1274(3) 0.6697(2) 0.50769(13) 0.0367(7) Uani 1 1 d . . . H10O H 0.1302 0.7270 0.4800 0.044 Uiso 1 1 calc R . . H10P H 0.0661 0.6554 0.5006 0.044 Uiso 1 1 calc R . . C109 C 0.0316(2) 0.7742(2) 0.56142(14) 0.0353(7) Uani 1 1 d . . . H10Q H -0.0321 0.7629 0.5551 0.042 Uiso 1 1 calc R . . H10R H 0.0361 0.8304 0.5335 0.042 Uiso 1 1 calc R . . C110 C 0.0271(3) 0.7955(2) 0.61454(14) 0.0364(7) Uani 1 1 d . . . H11A H 0.0949 0.7961 0.6235 0.044 Uiso 1 1 calc R . . H11B H -0.0252 0.8602 0.6141 0.044 Uiso 1 1 calc R . . C111 C -0.0146(3) 0.7451(2) 0.70422(14) 0.0427(8) Uani 1 1 d . . . H11C H -0.0686 0.8097 0.7018 0.051 Uiso 1 1 calc R . . H11D H 0.0501 0.7464 0.7170 0.051 Uiso 1 1 calc R . . C112 C -0.0473(3) 0.6684(3) 0.74236(15) 0.0447(9) Uani 1 1 d . . . H11E H -0.0677 0.6882 0.7763 0.054 Uiso 1 1 calc R . . H11F H -0.1085 0.6639 0.7275 0.054 Uiso 1 1 calc R . . C113 C 0.3237(2) 0.4218(2) 0.55677(14) 0.0394(8) Uani 1 1 d . . . H11G H 0.3614 0.4107 0.5237 0.047 Uiso 1 1 calc R . . H11H H 0.3169 0.3595 0.5767 0.047 Uiso 1 1 calc R . . C114 C 0.3873(2) 0.4501(3) 0.58954(14) 0.0401(8) Uani 1 1 d . . . H11I H 0.4560 0.3986 0.5970 0.048 Uiso 1 1 calc R . . H11J H 0.3973 0.5110 0.5697 0.048 Uiso 1 1 calc R . . C115 C 0.3926(2) 0.4933(3) 0.66934(16) 0.0413(8) Uani 1 1 d . . . H11K H 0.3781 0.5640 0.6569 0.050 Uiso 1 1 calc R . . H11L H 0.4676 0.4593 0.6662 0.050 Uiso 1 1 calc R . . C116 C 0.3607(2) 0.4695(3) 0.72536(15) 0.0427(8) Uani 1 1 d . . . H11M H 0.3693 0.3998 0.7365 0.051 Uiso 1 1 calc R . . H11N H 0.4050 0.4823 0.7485 0.051 Uiso 1 1 calc R . . C117 C 0.2177(3) 0.4957(3) 0.78221(14) 0.0484(9) Uani 1 1 d . . . H11O H 0.2658 0.4907 0.8098 0.058 Uiso 1 1 calc R . . H11P H 0.2128 0.4308 0.7861 0.058 Uiso 1 1 calc R . . C118 C 0.1128(3) 0.5680(3) 0.78896(15) 0.0492(9) Uani 1 1 d . . . H11Q H 0.0904 0.5506 0.8261 0.059 Uiso 1 1 calc R . . H11R H 0.1180 0.6332 0.7826 0.059 Uiso 1 1 calc R . . C201 C 0.6023(6) -0.2382(5) 0.0743(3) 0.118(3) Uani 1 1 d . . . H20A H 0.5913 -0.3006 0.0784 0.142 Uiso 1 1 calc R . . H20B H 0.5492 -0.1878 0.0492 0.142 Uiso 1 1 calc R . . C202 C 0.5877(5) -0.2124(4) 0.1273(2) 0.094(2) Uani 1 1 d . . . H20C H 0.5206 -0.2146 0.1424 0.112 Uiso 1 1 calc R . . H20D H 0.6431 -0.2596 0.1523 0.112 Uiso 1 1 calc R . . C203 C 0.5546(3) -0.0826(3) 0.16617(15) 0.0495(9) Uani 1 1 d . . . H20E H 0.5945 -0.1295 0.1976 0.059 Uiso 1 1 calc R . . H20F H 0.4812 -0.0761 0.1717 0.059 Uiso 1 1 calc R . . C204 C 0.5657(3) 0.0122(3) 0.16057(16) 0.0485(9) Uani 1 1 d . . . H20G H 0.5279 0.0585 0.1284 0.058 Uiso 1 1 calc R . . H20H H 0.5354 0.0384 0.1918 0.058 Uiso 1 1 calc R . . C205 C 0.6864(3) 0.0908(3) 0.15730(16) 0.0512(10) Uani 1 1 d . . . H20I H 0.6609 0.1089 0.1912 0.061 Uiso 1 1 calc R . . H20J H 0.6467 0.1439 0.1278 0.061 Uiso 1 1 calc R . . C206 C 0.8001(3) 0.0767(3) 0.15146(17) 0.0567(11) Uani 1 1 d . . . H20K H 0.8106 0.1357 0.1558 0.068 Uiso 1 1 calc R . . H20L H 0.8389 0.0217 0.1803 0.068 Uiso 1 1 calc R . . C207 C 0.6995(6) -0.2331(7) -0.0062(3) 0.121(3) Uani 1 1 d . . . H20M H 0.6595 -0.2712 -0.0136 0.145 Uiso 1 1 calc R . . H20N H 0.7699 -0.2589 -0.0201 0.145 Uiso 1 1 calc R . . C208 C 0.6501(5) -0.1292(7) -0.0352(2) 0.109(3) Uani 1 1 d . . . H20O H 0.6450 -0.1249 -0.0735 0.131 Uiso 1 1 calc R . . H20P H 0.5795 -0.1025 -0.0217 0.131 Uiso 1 1 calc R . . C209 C 0.6731(5) 0.0219(6) -0.05735(18) 0.108(3) Uani 1 1 d . . . H20Q H 0.6042 0.0560 -0.0442 0.129 Uiso 1 1 calc R . . H20R H 0.6653 0.0226 -0.0950 0.129 Uiso 1 1 calc R . . C210 C 0.7442(4) 0.0736(4) -0.05367(14) 0.0753(16) Uani 1 1 d . . . H21A H 0.8140 0.0379 -0.0652 0.090 Uiso 1 1 calc R . . H21B H 0.7197 0.1394 -0.0776 0.090 Uiso 1 1 calc R . . C211 C 0.8165(4) 0.1302(3) 0.00386(16) 0.0602(11) Uani 1 1 d . . . H21C H 0.7978 0.1929 -0.0230 0.072 Uiso 1 1 calc R . . H21D H 0.8884 0.0906 -0.0026 0.072 Uiso 1 1 calc R . . C212 C 0.8084(4) 0.1476(3) 0.05835(18) 0.0649(12) Uani 1 1 d . . . H21E H 0.8506 0.1874 0.0603 0.078 Uiso 1 1 calc R . . H21F H 0.7357 0.1852 0.0647 0.078 Uiso 1 1 calc R . . C213 C 0.7833(7) -0.3436(4) 0.0748(3) 0.131(3) Uani 1 1 d . . . H21G H 0.7741 -0.3586 0.1138 0.157 Uiso 1 1 calc R . . H21H H 0.7697 -0.3935 0.0612 0.157 Uiso 1 1 calc R . . C214 C 0.8910(6) -0.3501(4) 0.0634(3) 0.116(3) Uani 1 1 d . . . H21I H 0.9380 -0.4178 0.0768 0.139 Uiso 1 1 calc R . . H21J H 0.9005 -0.3309 0.0246 0.139 Uiso 1 1 calc R . . C215 C 1.0200(4) -0.2956(4) 0.0841(2) 0.093(2) Uani 1 1 d . . . H21K H 1.0359 -0.2699 0.0467 0.112 Uiso 1 1 calc R . . H21L H 1.0650 -0.3646 0.0953 0.112 Uiso 1 1 calc R . . C216 C 1.0388(4) -0.2393(4) 0.1184(2) 0.091(2) Uani 1 1 d . . . H21M H 1.0155 -0.2600 0.1549 0.110 Uiso 1 1 calc R . . H21N H 1.1135 -0.2505 0.1198 0.110 Uiso 1 1 calc R . . C217 C 1.0006(3) -0.0843(4) 0.13002(16) 0.0683(14) Uani 1 1 d . . . H21O H 1.0755 -0.1025 0.1360 0.082 Uiso 1 1 calc R . . H21P H 0.9678 -0.0976 0.1649 0.082 Uiso 1 1 calc R . . C218 C 0.9563(3) 0.0197(4) 0.10384(18) 0.0612(12) Uani 1 1 d . . . H21Q H 0.9841 0.0305 0.0674 0.073 Uiso 1 1 calc R . . H21R H 0.9789 0.0571 0.1236 0.073 Uiso 1 1 calc R . . C301 C 0.4011(3) 0.3801(2) 0.34164(17) 0.0466(9) Uani 1 1 d . . . H30A H 0.3300 0.4238 0.3307 0.056 Uiso 1 1 calc R . . H30B H 0.4492 0.4101 0.3208 0.056 Uiso 1 1 calc R . . C302 C 0.4153(3) 0.3715(3) 0.39906(17) 0.0468(9) Uani 1 1 d . . . H30C H 0.4002 0.4367 0.4055 0.056 Uiso 1 1 calc R . . H30D H 0.3672 0.3421 0.4205 0.056 Uiso 1 1 calc R . . C303 C 0.5404(3) 0.3077(2) 0.46761(13) 0.0382(8) Uani 1 1 d . . . H30E H 0.4960 0.2778 0.4920 0.046 Uiso 1 1 calc R . . H30F H 0.5250 0.3742 0.4722 0.046 Uiso 1 1 calc R . . C304 C 0.6506(3) 0.2494(2) 0.48080(13) 0.0339(7) Uani 1 1 d . . . H30G H 0.6952 0.2749 0.4541 0.041 Uiso 1 1 calc R . . H30H H 0.6676 0.2539 0.5161 0.041 Uiso 1 1 calc R . . C305 C 0.7696(2) 0.0914(2) 0.50122(13) 0.0344(7) Uani 1 1 d . . . H30I H 0.7771 0.0979 0.5375 0.041 Uiso 1 1 calc R . . H30J H 0.8214 0.1132 0.4783 0.041 Uiso 1 1 calc R . . C306 C 0.7880(2) -0.0128(2) 0.50238(12) 0.0324(7) Uani 1 1 d . . . H30K H 0.8550 -0.0539 0.5202 0.039 Uiso 1 1 calc R . . H30L H 0.7335 -0.0325 0.5238 0.039 Uiso 1 1 calc R . . C307 C 0.4398(3) 0.2936(3) 0.27264(19) 0.0621(13) Uani 1 1 d . . . H30M H 0.3861 0.3519 0.2522 0.074 Uiso 1 1 calc R . . H30N H 0.4342 0.2362 0.2634 0.074 Uiso 1 1 calc R . . C308 C 0.5441(4) 0.2999(3) 0.25588(16) 0.0564(11) Uani 1 1 d . . . H30O H 0.5490 0.3136 0.2167 0.068 Uiso 1 1 calc R . . H30P H 0.5535 0.3536 0.2677 0.068 Uiso 1 1 calc R . . C309 C 0.7228(3) 0.2139(3) 0.26723(14) 0.0468(9) Uani 1 1 d . . . H30Q H 0.7345 0.2600 0.2849 0.056 Uiso 1 1 calc R . . H30R H 0.7293 0.2371 0.2284 0.056 Uiso 1 1 calc R . . C310 C 0.8016(3) 0.1149(3) 0.28624(13) 0.0428(8) Uani 1 1 d . . . H31A H 0.7856 0.0672 0.2717 0.051 Uiso 1 1 calc R . . H31B H 0.8709 0.1152 0.2738 0.051 Uiso 1 1 calc R . . C311 C 0.8752(2) -0.0063(2) 0.36190(13) 0.0366(7) Uani 1 1 d . . . H31C H 0.9429 -0.0098 0.3455 0.044 Uiso 1 1 calc R . . H31D H 0.8534 -0.0558 0.3524 0.044 Uiso 1 1 calc R . . C312 C 0.8843(2) -0.0265(2) 0.42120(13) 0.0342(7) Uani 1 1 d . . . H31E H 0.9409 -0.0890 0.4340 0.041 Uiso 1 1 calc R . . H31F H 0.9031 0.0251 0.4302 0.041 Uiso 1 1 calc R . . C313 C 0.3272(3) 0.2580(3) 0.3448(2) 0.0675(14) Uani 1 1 d . . . H31G H 0.2706 0.2995 0.3192 0.081 Uiso 1 1 calc R . . H31H H 0.3044 0.2707 0.3802 0.081 Uiso 1 1 calc R . . C314 C 0.3452(3) 0.1526(3) 0.3473(2) 0.0689(15) Uani 1 1 d . . . H31I H 0.2793 0.1402 0.3543 0.083 Uiso 1 1 calc R . . H31J H 0.3719 0.1375 0.3129 0.083 Uiso 1 1 calc R . . C315 C 0.4334(2) -0.0066(2) 0.39125(14) 0.0351(7) Uani 1 1 d . . . H31K H 0.4648 -0.0236 0.3579 0.042 Uiso 1 1 calc R . . H31L H 0.3663 -0.0170 0.3956 0.042 Uiso 1 1 calc R . . C316 C 0.5022(2) -0.0700(2) 0.43682(14) 0.0354(7) Uani 1 1 d . . . H31M H 0.4733 -0.0502 0.4699 0.043 Uiso 1 1 calc R . . H31N H 0.5074 -0.1382 0.4409 0.043 Uiso 1 1 calc R . . C317 C 0.6742(3) -0.1300(2) 0.46778(13) 0.0361(7) Uani 1 1 d . . . H31O H 0.6741 -0.1963 0.4706 0.043 Uiso 1 1 calc R . . H31P H 0.6542 -0.1138 0.5026 0.043 Uiso 1 1 calc R . . C318 C 0.7804(2) -0.1262(2) 0.45324(13) 0.0343(7) Uani 1 1 d . . . H31Q H 0.8305 -0.1754 0.4802 0.041 Uiso 1 1 calc R . . H31R H 0.7996 -0.1436 0.4187 0.041 Uiso 1 1 calc R . . N1R N 0.6710(3) 0.7961(3) 0.34610(13) 0.0525(8) Uani 1 1 d . . . H1R3 H 0.6463 0.8448 0.3634 0.079 Uiso 0.67 1 calc PR . . H1R4 H 0.7103 0.7408 0.3688 0.079 Uiso 0.67 1 calc PR . . H1R5 H 0.6172 0.7857 0.3339 0.079 Uiso 0.67 1 calc PR . . C1R C 0.7336(3) 0.8233(3) 0.30155(15) 0.0473(9) Uani 1 1 d . . . H1R1 H 0.7914 0.8357 0.3148 0.057 Uiso 1 1 calc R . . H1R2 H 0.6910 0.8841 0.2772 0.057 Uiso 1 1 calc R . . C2R C 0.7759(3) 0.7448(3) 0.27177(17) 0.0564(10) Uani 1 1 d . . . H2R1 H 0.8182 0.6843 0.2964 0.068 Uiso 1 1 calc R . . H2R2 H 0.7177 0.7322 0.2591 0.068 Uiso 1 1 calc R . . N2R N 0.8390(4) 0.7688(4) 0.22632(17) 0.0936(15) Uani 1 1 d . . . H2R3 H 0.8625 0.7188 0.2099 0.140 Uiso 0.67 1 calc PR . . H2R4 H 0.8937 0.7790 0.2378 0.140 Uiso 0.67 1 calc PR . . H2R5 H 0.8003 0.8235 0.2030 0.140 Uiso 0.67 1 calc PR . . C1S C 0.5177(8) 0.3486(7) 0.0146(6) 0.259(8) Uani 1 1 d DU . . H1S1 H 0.5116 0.3469 -0.0224 0.389 Uiso 1 1 calc R . . H1S2 H 0.4535 0.3938 0.0251 0.389 Uiso 1 1 calc R . . H1S3 H 0.5306 0.2835 0.0376 0.389 Uiso 1 1 calc R . . C2S C 0.6084(5) 0.3826(3) 0.0199(3) 0.236(11) Uani 1 1 d GU . . C3S C 0.5960(4) 0.3790(3) 0.0719(3) 0.180(7) Uani 1 1 d GDU . . H3S H 0.5391 0.3645 0.0898 0.216 Uiso 1 1 calc R . . C4S C 0.6638(5) 0.3957(3) 0.0985(2) 0.130(3) Uani 1 1 d GU . . H4S H 0.6550 0.3931 0.1354 0.156 Uiso 1 1 calc R . . C5S C 0.7440(4) 0.4161(3) 0.0732(2) 0.0917(18) Uani 1 1 d GU . . H5S H 0.7921 0.4280 0.0921 0.110 Uiso 1 1 calc R . . C6S C 0.7563(4) 0.4198(3) 0.0212(2) 0.103(2) Uani 1 1 d GU . . H6S H 0.8133 0.4343 0.0033 0.123 Uiso 1 1 calc R . . C7S C 0.6886(6) 0.4031(4) -0.0054(2) 0.161(5) Uani 1 1 d GDU . . H7S H 0.6974 0.4057 -0.0423 0.194 Uiso 1 1 calc R . . C1T C 0.0396(6) 0.2511(9) 0.1045(4) 0.165(4) Uani 1 1 d U . . H1T1 H -0.0057 0.3101 0.0808 0.248 Uiso 1 1 calc R . . H1T2 H 0.0012 0.2323 0.1362 0.248 Uiso 1 1 calc R . . H1T3 H 0.0640 0.1985 0.0860 0.248 Uiso 1 1 calc R . . C2T C 0.1216(3) 0.2684(3) 0.11934(15) 0.274(10) Uani 1 1 d GU . . C3T C 0.1292(5) 0.3598(3) 0.10040(16) 0.163(5) Uani 1 1 d GU . . H3T H 0.0780 0.4090 0.0767 0.195 Uiso 1 1 calc R . . C4T C 0.2114(6) 0.3792(4) 0.1161(2) 0.151(4) Uani 1 1 d GU . . H4T H 0.2165 0.4417 0.1031 0.182 Uiso 1 1 calc R . . C5T C 0.2861(5) 0.3073(5) 0.1507(2) 0.107(2) Uani 1 1 d GU . . H5T H 0.3424 0.3206 0.1614 0.128 Uiso 1 1 calc R . . C6T C 0.2785(4) 0.2159(4) 0.16963(17) 0.138(3) Uani 1 1 d GU . . H6T H 0.3297 0.1667 0.1933 0.166 Uiso 1 1 calc R . . C7T C 0.1963(3) 0.1965(3) 0.15396(16) 0.0666(13) Uani 1 1 d GU . . H7T H 0.1912 0.1339 0.1669 0.080 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 Ge1 0.02746(16) 0.02338(15) 0.02946(16) -0.01240(13) 0.00306(12) -0.00461(12) Ge3 0.02375(15) 0.02546(15) 0.02267(15) -0.00555(12) 0.00739(11) -0.00812(12) Ge4 0.02515(15) 0.02528(15) 0.02238(15) -0.00789(12) -0.00277(11) -0.00585(12) Ge5 0.02790(16) 0.02270(15) 0.02937(16) -0.00585(12) 0.00437(12) -0.01164(13) Ge2 0.02292(15) 0.02496(15) 0.02607(16) -0.00266(12) -0.00168(12) -0.00319(12) Ge7 0.02529(15) 0.01865(14) 0.02469(15) -0.00411(11) 0.00152(11) -0.00625(12) Ge8 0.01986(14) 0.02608(15) 0.02877(16) -0.00904(12) 0.00544(11) -0.00630(12) Ge9 0.03073(16) 0.03163(17) 0.01740(14) -0.00393(12) 0.00323(12) -0.01176(13) Ge6 0.02657(15) 0.03028(16) 0.02537(15) -0.00627(13) -0.00145(12) -0.01334(13) Zn1 0.0413(2) 0.0331(2) 0.03178(19) -0.01805(16) 0.00697(16) -0.01171(17) C1 0.0348(16) 0.0261(15) 0.0346(17) -0.0132(13) 0.0035(13) -0.0085(13) C2 0.055(2) 0.053(2) 0.049(2) -0.0249(19) 0.0184(18) -0.0224(19) C3 0.043(2) 0.057(2) 0.067(3) -0.036(2) 0.0034(18) -0.0178(19) K1 0.0210(3) 0.0247(3) 0.0300(3) -0.0083(2) 0.0014(2) -0.0070(2) K2 0.0398(4) 0.0394(4) 0.0328(4) -0.0098(3) 0.0080(3) -0.0172(3) K3 0.0230(3) 0.0225(3) 0.0352(3) -0.0075(3) -0.0012(2) -0.0069(2) N11 0.0314(13) 0.0292(13) 0.0303(13) -0.0121(11) 0.0050(10) -0.0091(11) N12 0.0359(15) 0.0381(15) 0.0315(14) -0.0118(12) 0.0014(11) -0.0029(12) N21 0.120(4) 0.103(4) 0.106(3) -0.077(3) 0.077(3) -0.085(3) N22 0.0537(18) 0.0532(19) 0.0363(16) -0.0180(14) 0.0081(13) -0.0269(16) N31 0.0335(15) 0.0265(14) 0.071(2) -0.0047(14) -0.0186(14) -0.0067(12) N32 0.0249(12) 0.0280(13) 0.0289(13) -0.0114(10) 0.0032(10) -0.0067(10) O11 0.0399(12) 0.0293(11) 0.0411(13) -0.0084(10) 0.0016(10) -0.0199(10) O12 0.0313(12) 0.0487(14) 0.0422(13) -0.0110(11) 0.0090(10) -0.0219(11) O13 0.0281(11) 0.0259(11) 0.0306(11) -0.0049(9) -0.0006(8) -0.0026(9) O14 0.0394(12) 0.0262(11) 0.0382(12) -0.0130(9) 0.0059(10) -0.0085(10) O15 0.0216(10) 0.0388(12) 0.0458(13) -0.0150(10) 0.0020(9) -0.0112(9) O16 0.0314(12) 0.0414(13) 0.0416(13) -0.0154(11) -0.0106(10) 0.0008(10) O21 0.0609(17) 0.0670(18) 0.0483(15) -0.0289(13) 0.0262(13) -0.0408(15) O22 0.0373(13) 0.0498(15) 0.0378(13) -0.0164(11) 0.0057(10) -0.0153(11) O23 0.075(2) 0.149(3) 0.0335(15) -0.0290(19) 0.0114(14) -0.075(2) O24 0.0615(17) 0.0660(18) 0.0290(13) 0.0061(12) 0.0025(12) -0.0211(15) O25 0.112(3) 0.0386(17) 0.074(2) -0.0119(15) 0.038(2) -0.0014(18) O26 0.0445(15) 0.0659(18) 0.0400(15) -0.0025(13) -0.0074(12) 0.0024(13) O31 0.0290(11) 0.0251(11) 0.0442(13) -0.0097(10) 0.0069(9) -0.0026(9) O32 0.0328(11) 0.0215(10) 0.0330(11) -0.0102(9) 0.0038(9) -0.0082(9) O33 0.0532(15) 0.0313(12) 0.0371(13) -0.0029(10) -0.0099(11) -0.0076(11) O34 0.0303(11) 0.0366(12) 0.0276(11) -0.0119(9) 0.0052(9) -0.0060(9) O35 0.0312(12) 0.0296(12) 0.0685(17) -0.0140(11) -0.0111(11) -0.0128(10) O36 0.0286(11) 0.0271(11) 0.0347(12) -0.0040(9) 0.0019(9) -0.0122(9) C101 0.048(2) 0.0420(19) 0.0345(18) -0.0213(15) 0.0034(15) -0.0156(16) C102 0.051(2) 0.0328(18) 0.049(2) -0.0200(16) -0.0036(16) -0.0186(16) C103 0.053(2) 0.042(2) 0.047(2) -0.0010(16) -0.0077(17) -0.0349(18) C104 0.0355(18) 0.053(2) 0.050(2) 0.0008(17) -0.0014(15) -0.0303(17) C105 0.0397(19) 0.048(2) 0.047(2) -0.0068(17) 0.0180(16) -0.0177(17) C106 0.053(2) 0.047(2) 0.0351(19) -0.0086(16) 0.0155(16) -0.0121(18) C107 0.0418(18) 0.0371(18) 0.0287(16) -0.0086(14) 0.0080(13) -0.0133(15) C108 0.0411(18) 0.0368(18) 0.0273(16) -0.0040(14) -0.0030(13) -0.0094(15) C109 0.0271(15) 0.0232(15) 0.0457(19) 0.0004(14) -0.0015(13) -0.0022(13) C110 0.0335(17) 0.0240(15) 0.049(2) -0.0119(14) 0.0025(14) -0.0056(13) C111 0.047(2) 0.0325(18) 0.044(2) -0.0218(15) 0.0037(16) 0.0005(15) C112 0.0399(19) 0.044(2) 0.042(2) -0.0179(16) 0.0100(15) -0.0019(16) C113 0.0321(17) 0.0342(18) 0.045(2) -0.0167(15) 0.0125(14) -0.0013(14) C114 0.0227(15) 0.0427(19) 0.049(2) -0.0092(16) 0.0093(14) -0.0070(14) C115 0.0227(15) 0.0348(18) 0.068(2) -0.0132(17) -0.0090(15) -0.0088(14) C116 0.0276(16) 0.0405(19) 0.057(2) -0.0159(17) -0.0153(15) -0.0026(15) C117 0.048(2) 0.054(2) 0.0358(19) -0.0159(17) -0.0126(16) -0.0023(18) C118 0.051(2) 0.056(2) 0.0350(19) -0.0208(17) -0.0032(16) -0.0039(18) C201 0.159(6) 0.164(6) 0.129(5) -0.112(5) 0.107(5) -0.142(6) C202 0.133(5) 0.103(4) 0.096(4) -0.062(3) 0.077(4) -0.093(4) C203 0.045(2) 0.073(3) 0.040(2) -0.0227(19) 0.0169(16) -0.029(2) C204 0.0359(19) 0.066(3) 0.044(2) -0.0243(19) 0.0070(15) -0.0120(18) C205 0.060(2) 0.056(2) 0.046(2) -0.0282(19) 0.0096(18) -0.021(2) C206 0.067(3) 0.075(3) 0.050(2) -0.036(2) 0.013(2) -0.040(2) C207 0.146(6) 0.195(8) 0.122(6) -0.127(6) 0.088(5) -0.138(7) C208 0.098(4) 0.240(9) 0.072(4) -0.096(5) 0.042(3) -0.124(6) C209 0.096(4) 0.220(8) 0.024(2) 0.009(3) -0.007(2) -0.098(5) C210 0.072(3) 0.131(5) 0.0185(18) 0.013(2) -0.0051(18) -0.050(3) C211 0.083(3) 0.043(2) 0.048(2) -0.0009(18) 0.017(2) -0.024(2) C212 0.096(4) 0.045(2) 0.059(3) -0.018(2) 0.024(2) -0.031(2) C213 0.199(8) 0.067(4) 0.160(7) -0.068(4) 0.107(6) -0.083(5) C214 0.163(7) 0.055(3) 0.136(6) -0.050(4) 0.082(5) -0.046(4) C215 0.086(4) 0.059(3) 0.075(4) 0.005(3) 0.030(3) 0.025(3) C216 0.071(3) 0.090(4) 0.050(3) 0.000(3) -0.004(2) 0.038(3) C217 0.039(2) 0.128(5) 0.036(2) -0.016(3) -0.0073(17) -0.028(3) C218 0.054(2) 0.100(4) 0.052(2) -0.030(3) 0.009(2) -0.046(3) C301 0.0308(17) 0.0240(16) 0.077(3) -0.0055(17) -0.0134(17) -0.0014(14) C302 0.0300(17) 0.0279(17) 0.073(3) -0.0087(17) 0.0085(17) -0.0025(14) C303 0.050(2) 0.0224(15) 0.0396(18) -0.0105(13) 0.0203(15) -0.0110(14) C304 0.0493(19) 0.0261(15) 0.0303(16) -0.0114(13) 0.0090(14) -0.0168(14) C305 0.0344(17) 0.0422(18) 0.0305(16) -0.0160(14) -0.0001(13) -0.0129(15) C306 0.0330(16) 0.0324(17) 0.0271(16) -0.0082(13) -0.0021(12) -0.0048(13) C307 0.059(3) 0.037(2) 0.080(3) -0.005(2) -0.044(2) -0.0018(19) C308 0.078(3) 0.036(2) 0.039(2) 0.0033(16) -0.016(2) -0.005(2) C309 0.064(2) 0.044(2) 0.0303(18) -0.0075(15) 0.0076(16) -0.0184(19) C310 0.050(2) 0.047(2) 0.0292(17) -0.0118(15) 0.0079(15) -0.0148(17) C311 0.0274(16) 0.0415(19) 0.0382(18) -0.0181(15) 0.0081(13) -0.0044(14) C312 0.0209(14) 0.0401(18) 0.0379(18) -0.0121(14) 0.0023(12) -0.0046(13) C313 0.0307(19) 0.037(2) 0.130(4) -0.007(2) -0.027(2) -0.0097(17) C314 0.050(2) 0.039(2) 0.118(4) 0.000(2) -0.047(3) -0.0182(19) C315 0.0326(16) 0.0304(16) 0.050(2) -0.0147(15) 0.0004(14) -0.0163(14) C316 0.0355(17) 0.0335(17) 0.0432(19) -0.0120(14) 0.0079(14) -0.0185(14) C317 0.0434(19) 0.0242(15) 0.0384(18) -0.0034(13) -0.0027(14) -0.0112(14) C318 0.0357(17) 0.0237(15) 0.0389(18) -0.0095(13) -0.0043(14) -0.0022(13) N1R 0.0518(19) 0.057(2) 0.0443(18) -0.0146(16) -0.0001(15) -0.0112(16) C1R 0.062(2) 0.041(2) 0.042(2) -0.0130(16) -0.0033(17) -0.0187(18) C2R 0.062(3) 0.055(2) 0.051(2) -0.023(2) 0.001(2) -0.012(2) N2R 0.086(3) 0.132(4) 0.061(3) -0.044(3) 0.023(2) -0.026(3) C1S 0.180(10) 0.119(8) 0.46(2) -0.034(10) -0.183(13) -0.015(7) C2S 0.199(13) 0.084(6) 0.41(2) -0.110(12) -0.227(16) 0.047(8) C3S 0.062(5) 0.047(4) 0.41(2) -0.026(7) -0.001(7) -0.011(3) C4S 0.138(7) 0.055(4) 0.144(7) -0.002(4) 0.063(6) 0.003(4) C5S 0.123(5) 0.059(3) 0.093(5) -0.022(3) -0.019(4) -0.025(3) C6S 0.114(5) 0.061(3) 0.106(5) -0.003(4) 0.015(4) -0.013(3) C7S 0.242(14) 0.087(6) 0.097(6) -0.040(4) -0.061(8) 0.038(7) C1T 0.099(6) 0.305(13) 0.137(7) -0.132(8) 0.035(5) -0.078(7) C2T 0.062(4) 0.56(3) 0.124(7) -0.221(12) -0.034(4) 0.078(8) C3T 0.327(13) 0.024(2) 0.076(4) -0.017(3) 0.110(6) -0.007(4) C4T 0.238(12) 0.142(9) 0.101(6) -0.032(6) 0.024(7) -0.100(9) C5T 0.149(7) 0.115(6) 0.080(4) -0.023(4) -0.006(4) -0.073(5) C6T 0.151(8) 0.134(7) 0.131(7) -0.070(6) 0.063(6) -0.038(6) C7T 0.090(4) 0.057(3) 0.065(3) -0.029(2) 0.023(3) -0.034(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 Ge1 Ge2 2.5658(4) . ? Ge1 Ge3 2.5665(4) . ? Ge1 Ge5 2.5712(4) . ? Ge1 Ge4 2.5859(4) . ? Ge3 Ge7 2.5528(4) . ? Ge3 Ge6 2.5572(4) . ? Ge3 Ge4 2.8311(4) . ? Ge3 Ge2 2.8638(4) . ? Ge4 Ge8 2.5519(4) . ? Ge4 Ge7 2.5520(4) . ? Ge4 Ge5 2.8245(4) . ? Ge5 Ge8 2.5612(4) . ? Ge5 Ge9 2.5626(4) . ? Ge5 Ge2 2.8428(4) . ? Ge2 Ge9 2.5570(4) . ? Ge2 Ge6 2.5615(4) . ? Ge7 Zn1 2.5915(5) . ? Ge7 Ge8 2.7782(4) . ? Ge7 Ge6 2.7868(4) . ? Ge8 Zn1 2.6225(5) . ? Ge8 Ge9 2.7494(4) . ? Ge9 Zn1 2.6132(5) . ? Ge9 Ge6 2.7674(4) . ? Ge6 Zn1 2.5999(5) . ? Zn1 C1 2.023(3) . ? C1 C3 1.506(5) . ? C1 C2 1.511(5) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? K1 O15 2.729(2) . ? K1 O12 2.757(2) . ? K1 O14 2.797(2) . ? K1 O13 2.805(2) . ? K1 O11 2.859(2) . ? K1 O16 2.877(2) . ? K1 N11 3.022(3) . ? K1 N12 3.048(3) . ? K2 O21 2.789(3) . ? K2 O23 2.810(3) . ? K2 O26 2.823(3) . ? K2 O24 2.829(3) . ? K2 O25 2.843(3) . ? K2 O22 2.845(2) . ? K2 N21 3.004(4) . ? K2 N22 3.013(3) . ? K3 O32 2.771(2) . ? K3 O34 2.808(2) . ? K3 O36 2.818(2) . ? K3 O35 2.827(2) . ? K3 O33 2.841(2) . ? K3 O31 2.846(2) . ? K3 N31 3.024(3) . ? K3 N32 3.034(3) . ? N11 C101 1.464(4) . ? N11 C107 1.470(4) . ? N11 C113 1.475(4) . ? N12 C118 1.461(5) . ? N12 C106 1.474(5) . ? N12 C112 1.475(4) . ? N21 C207 1.459(8) . ? N21 C201 1.487(6) . ? N21 C213 1.487(9) . ? N22 C206 1.458(5) . ? N22 C212 1.470(5) . ? N22 C218 1.476(5) . ? N31 C307 1.458(6) . ? N31 C301 1.468(4) . ? N31 C313 1.482(5) . ? N32 C318 1.465(4) . ? N32 C306 1.469(4) . ? N32 C312 1.480(4) . ? O11 C102 1.420(4) . ? O11 C103 1.429(4) . ? O12 C105 1.409(4) . ? O12 C104 1.434(4) . ? O13 C109 1.429(4) . ? O13 C108 1.429(4) . ? O14 C110 1.421(4) . ? O14 C111 1.426(4) . ? O15 C114 1.410(4) . ? O15 C115 1.424(4) . ? O16 C117 1.421(5) . ? O16 C116 1.433(4) . ? O21 C203 1.415(4) . ? O21 C202 1.418(5) . ? O22 C205 1.424(4) . ? O22 C204 1.429(4) . ? O23 C209 1.396(8) . ? O23 C208 1.430(6) . ? O24 C211 1.414(5) . ? O24 C210 1.420(5) . ? O25 C214 1.409(7) . ? O25 C215 1.426(7) . ? O26 C216 1.405(6) . ? O26 C217 1.422(6) . ? O31 C302 1.424(4) . ? O31 C303 1.425(4) . ? O32 C305 1.420(4) . ? O32 C304 1.432(3) . ? O33 C309 1.416(5) . ? O33 C308 1.430(4) . ? O34 C310 1.417(4) . ? O34 C311 1.434(4) . ? O35 C314 1.411(4) . ? O35 C315 1.433(4) . ? O36 C317 1.421(4) . ? O36 C316 1.433(4) . ? C101 C102 1.501(5) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.472(5) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.501(6) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.509(5) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.488(5) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.505(5) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.503(5) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.481(5) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.508(5) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 C202 1.505(7) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.471(6) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.515(6) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.497(10) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.483(7) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.494(6) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.472(10) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.474(9) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.473(7) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? C301 C302 1.489(6) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.485(5) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.503(4) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.505(6) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.497(5) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.502(5) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.514(5) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.482(5) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 C318 1.509(5) . ? C317 H31O 0.9900 . ? C317 H31P 0.9900 . ? C318 H31Q 0.9900 . ? C318 H31R 0.9900 . ? N1R C1R 1.455(5) . ? N1R H1R3 0.9100 . ? N1R H1R4 0.9100 . ? N1R H1R5 0.9100 . ? C1R C2R 1.502(5) . ? C1R H1R1 0.9900 . ? C1R H1R2 0.9900 . ? C2R N2R 1.463(6) . ? C2R H2R1 0.9900 . ? C2R H2R2 0.9900 . ? N2R H2R3 0.9100 . ? N2R H2R4 0.9100 . ? N2R H2R5 0.9100 . ? C1S C2S 1.547(10) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.338 . ? C2S C7S 1.338 . ? C3S C4S 1.338 . ? C3S H3S 0.9500 . ? C4S C5S 1.338 . ? C4S H4S 0.9500 . ? C5S C6S 1.338 . ? C5S H5S 0.9500 . ? C6S C7S 1.338 . ? C6S H6S 0.9500 . ? C7S H7S 0.9500 . ? C1T C2T 1.358(9) . ? C1T H1T1 0.9800 . ? C1T H1T2 0.9800 . ? C1T H1T3 0.9800 . ? C2T C3T 1.388 . ? C2T C7T 1.388 . ? C3T C4T 1.388 . ? C3T H3T 0.9500 . ? C4T C5T 1.388 . ? C4T H4T 0.9500 . ? C5T C6T 1.388 . ? C5T H5T 0.9500 . ? C6T C7T 1.388 . ? C6T H6T 0.9500 . ? C7T H7T 0.9500 . ? 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 Ge2 Ge1 Ge3 67.836(12) . . ? Ge2 Ge1 Ge5 67.202(12) . . ? Ge3 Ge1 Ge5 102.742(14) . . ? Ge2 Ge1 Ge4 102.604(14) . . ? Ge3 Ge1 Ge4 66.662(12) . . ? Ge5 Ge1 Ge4 66.417(12) . . ? Ge7 Ge3 Ge6 66.099(12) . . ? Ge7 Ge3 Ge1 108.795(14) . . ? Ge6 Ge3 Ge1 107.904(14) . . ? Ge7 Ge3 Ge4 56.303(11) . . ? Ge6 Ge3 Ge4 102.264(13) . . ? Ge1 Ge3 Ge4 56.997(11) . . ? Ge7 Ge3 Ge2 102.380(13) . . ? Ge6 Ge3 Ge2 56.052(11) . . ? Ge1 Ge3 Ge2 56.071(11) . . ? Ge4 Ge3 Ge2 89.819(12) . . ? Ge8 Ge4 Ge7 65.959(12) . . ? Ge8 Ge4 Ge1 108.423(14) . . ? Ge7 Ge4 Ge1 108.215(14) . . ? Ge8 Ge4 Ge5 56.625(11) . . ? Ge7 Ge4 Ge5 102.956(13) . . ? Ge1 Ge4 Ge5 56.542(11) . . ? Ge8 Ge4 Ge3 102.500(13) . . ? Ge7 Ge4 Ge3 56.329(11) . . ? Ge1 Ge4 Ge3 56.341(11) . . ? Ge5 Ge4 Ge3 90.415(12) . . ? Ge8 Ge5 Ge9 64.904(12) . . ? Ge8 Ge5 Ge1 108.591(14) . . ? Ge9 Ge5 Ge1 107.716(14) . . ? Ge8 Ge5 Ge4 56.310(11) . . ? Ge9 Ge5 Ge4 101.535(13) . . ? Ge1 Ge5 Ge4 57.040(11) . . ? Ge8 Ge5 Ge2 102.200(13) . . ? Ge9 Ge5 Ge2 56.175(11) . . ? Ge1 Ge5 Ge2 56.308(11) . . ? Ge4 Ge5 Ge2 90.378(12) . . ? Ge9 Ge2 Ge6 65.459(12) . . ? Ge9 Ge2 Ge1 108.055(14) . . ? Ge6 Ge2 Ge1 107.793(14) . . ? Ge9 Ge2 Ge5 56.363(11) . . ? Ge6 Ge2 Ge5 102.225(13) . . ? Ge1 Ge2 Ge5 56.490(11) . . ? Ge9 Ge2 Ge3 101.231(13) . . ? Ge6 Ge2 Ge3 55.909(11) . . ? Ge1 Ge2 Ge3 56.094(11) . . ? Ge5 Ge2 Ge3 89.387(12) . . ? Ge4 Ge7 Ge3 67.367(12) . . ? Ge4 Ge7 Zn1 112.040(15) . . ? Ge3 Ge7 Zn1 111.679(15) . . ? Ge4 Ge7 Ge8 57.018(11) . . ? Ge3 Ge7 Ge8 103.950(13) . . ? Zn1 Ge7 Ge8 58.346(12) . . ? Ge4 Ge7 Ge6 103.629(13) . . ? Ge3 Ge7 Ge6 57.027(11) . . ? Zn1 Ge7 Ge6 57.679(12) . . ? Ge8 Ge7 Ge6 89.757(12) . . ? Ge4 Ge8 Ge5 67.065(12) . . ? Ge4 Ge8 Zn1 111.026(15) . . ? Ge5 Ge8 Zn1 112.188(15) . . ? Ge4 Ge8 Ge9 103.889(13) . . ? Ge5 Ge8 Ge9 57.573(12) . . ? Zn1 Ge8 Ge9 58.158(13) . . ? Ge4 Ge8 Ge7 57.023(11) . . ? Ge5 Ge8 Ge7 104.007(13) . . ? Zn1 Ge8 Ge7 57.262(12) . . ? Ge9 Ge8 Ge7 90.015(12) . . ? Ge2 Ge9 Ge5 67.462(12) . . ? Ge2 Ge9 Zn1 111.958(15) . . ? Ge5 Ge9 Zn1 112.452(15) . . ? Ge2 Ge9 Ge8 104.927(13) . . ? Ge5 Ge9 Ge8 57.523(11) . . ? Zn1 Ge9 Ge8 58.490(12) . . ? Ge2 Ge9 Ge6 57.350(11) . . ? Ge5 Ge9 Ge6 104.293(13) . . ? Zn1 Ge9 Ge6 57.704(12) . . ? Ge8 Ge9 Ge6 90.759(12) . . ? Ge3 Ge6 Ge2 68.040(12) . . ? Ge3 Ge6 Zn1 111.260(15) . . ? Ge2 Ge6 Zn1 112.249(15) . . ? Ge3 Ge6 Ge9 103.875(14) . . ? Ge2 Ge6 Ge9 57.192(11) . . ? Zn1 Ge6 Ge9 58.170(12) . . ? Ge3 Ge6 Ge7 56.875(11) . . ? Ge2 Ge6 Ge7 104.296(14) . . ? Zn1 Ge6 Ge7 57.388(12) . . ? Ge9 Ge6 Ge7 89.469(12) . . ? C1 Zn1 Ge7 133.11(9) . . ? C1 Zn1 Ge6 134.52(9) . . ? Ge7 Zn1 Ge6 64.933(13) . . ? C1 Zn1 Ge9 129.29(9) . . ? Ge7 Zn1 Ge9 97.369(15) . . ? Ge6 Zn1 Ge9 64.126(13) . . ? C1 Zn1 Ge8 127.85(9) . . ? Ge7 Zn1 Ge8 64.392(12) . . ? Ge6 Zn1 Ge8 97.508(15) . . ? Ge9 Zn1 Ge8 63.352(13) . . ? C3 C1 C2 110.6(3) . . ? C3 C1 Zn1 114.5(2) . . ? C2 C1 Zn1 110.9(2) . . ? C3 C1 H1 106.8 . . ? C2 C1 H1 106.8 . . ? Zn1 C1 H1 106.8 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O15 K1 O12 134.54(7) . . ? O15 K1 O14 128.71(7) . . ? O12 K1 O14 91.98(7) . . ? O15 K1 O13 89.49(7) . . ? O12 K1 O13 132.20(7) . . ? O14 K1 O13 62.14(6) . . ? O15 K1 O11 107.18(7) . . ? O12 K1 O11 60.41(7) . . ? O14 K1 O11 115.95(7) . . ? O13 K1 O11 93.87(6) . . ? O15 K1 O16 60.80(7) . . ? O12 K1 O16 107.03(7) . . ? O14 K1 O16 89.67(7) . . ? O13 K1 O16 111.83(7) . . ? O11 K1 O16 150.51(7) . . ? O15 K1 N11 60.76(7) . . ? O12 K1 N11 119.05(7) . . ? O14 K1 N11 121.37(7) . . ? O13 K1 N11 60.28(7) . . ? O11 K1 N11 59.26(7) . . ? O16 K1 N11 120.96(7) . . ? O15 K1 N12 119.01(7) . . ? O12 K1 N12 59.68(8) . . ? O14 K1 N12 60.28(7) . . ? O13 K1 N12 121.47(7) . . ? O11 K1 N12 119.67(7) . . ? O16 K1 N12 59.11(7) . . ? N11 K1 N12 178.21(8) . . ? O21 K2 O23 92.68(8) . . ? O21 K2 O26 143.76(9) . . ? O23 K2 O26 119.23(9) . . ? O21 K2 O24 115.68(9) . . ? O23 K2 O24 60.62(10) . . ? O26 K2 O24 96.02(8) . . ? O21 K2 O25 104.00(10) . . ? O23 K2 O25 95.68(12) . . ? O26 K2 O25 59.19(11) . . ? O24 K2 O25 133.47(9) . . ? O21 K2 O22 60.27(7) . . ? O23 K2 O22 131.01(10) . . ? O26 K2 O22 103.04(8) . . ? O24 K2 O22 93.27(8) . . ? O25 K2 O22 128.49(9) . . ? O21 K2 N21 61.08(9) . . ? O23 K2 N21 59.98(13) . . ? O26 K2 N21 118.51(13) . . ? O24 K2 N21 120.14(13) . . ? O25 K2 N21 59.90(15) . . ? O22 K2 N21 120.56(9) . . ? O21 K2 N22 119.61(8) . . ? O23 K2 N22 119.79(10) . . ? O26 K2 N22 60.96(9) . . ? O24 K2 N22 59.72(9) . . ? O25 K2 N22 119.63(11) . . ? O22 K2 N22 60.11(7) . . ? N21 K2 N22 179.31(10) . . ? O32 K3 O34 94.03(6) . . ? O32 K3 O36 97.71(6) . . ? O34 K3 O36 100.21(6) . . ? O32 K3 O35 119.27(7) . . ? O34 K3 O35 142.29(7) . . ? O36 K3 O35 60.71(6) . . ? O32 K3 O33 133.68(7) . . ? O34 K3 O33 60.50(7) . . ? O36 K3 O33 123.05(7) . . ? O35 K3 O33 100.84(8) . . ? O32 K3 O31 61.29(6) . . ? O34 K3 O31 115.29(7) . . ? O36 K3 O31 138.85(7) . . ? O35 K3 O31 97.16(7) . . ? O33 K3 O31 93.48(7) . . ? O32 K3 N31 118.88(8) . . ? O34 K3 N31 120.24(8) . . ? O36 K3 N31 120.40(7) . . ? O35 K3 N31 60.57(7) . . ? O33 K3 N31 60.84(9) . . ? O31 K3 N31 58.58(8) . . ? O32 K3 N32 60.80(6) . . ? O34 K3 N32 60.36(6) . . ? O36 K3 N32 59.32(6) . . ? O35 K3 N32 119.06(7) . . ? O33 K3 N32 119.77(7) . . ? O31 K3 N32 121.20(7) . . ? N31 K3 N32 179.39(9) . . ? C101 N11 C107 110.2(3) . . ? C101 N11 C113 109.5(3) . . ? C107 N11 C113 111.5(3) . . ? C101 N11 K1 111.35(18) . . ? C107 N11 K1 109.59(17) . . ? C113 N11 K1 104.55(18) . . ? C118 N12 C106 109.6(3) . . ? C118 N12 C112 110.4(3) . . ? C106 N12 C112 111.8(3) . . ? C118 N12 K1 111.5(2) . . ? C106 N12 K1 105.97(19) . . ? C112 N12 K1 107.51(19) . . ? C207 N21 C201 108.9(5) . . ? C207 N21 C213 110.2(5) . . ? C201 N21 C213 110.8(5) . . ? C207 N21 K2 110.3(3) . . ? C201 N21 K2 108.7(3) . . ? C213 N21 K2 108.0(4) . . ? C206 N22 C212 110.2(3) . . ? C206 N22 C218 109.5(3) . . ? C212 N22 C218 109.3(3) . . ? C206 N22 K2 109.1(2) . . ? C212 N22 K2 110.5(2) . . ? C218 N22 K2 108.1(2) . . ? C307 N31 C301 110.1(3) . . ? C307 N31 C313 111.1(3) . . ? C301 N31 C313 108.7(3) . . ? C307 N31 K3 107.0(2) . . ? C301 N31 K3 111.8(2) . . ? C313 N31 K3 108.2(2) . . ? C318 N32 C306 111.1(2) . . ? C318 N32 C312 109.5(2) . . ? C306 N32 C312 110.3(2) . . ? C318 N32 K3 109.81(17) . . ? C306 N32 K3 106.95(17) . . ? C312 N32 K3 109.19(17) . . ? C102 O11 C103 111.6(3) . . ? C102 O11 K1 113.64(18) . . ? C103 O11 K1 113.37(19) . . ? C105 O12 C104 111.8(3) . . ? C105 O12 K1 124.6(2) . . ? C104 O12 K1 113.97(18) . . ? C109 O13 C108 111.0(2) . . ? C109 O13 K1 110.97(17) . . ? C108 O13 K1 116.62(18) . . ? C110 O14 C111 111.8(2) . . ? C110 O14 K1 111.66(17) . . ? C111 O14 K1 118.35(18) . . ? C114 O15 C115 111.4(2) . . ? C114 O15 K1 123.54(18) . . ? C115 O15 K1 115.13(18) . . ? C117 O16 C116 111.1(3) . . ? C117 O16 K1 112.8(2) . . ? C116 O16 K1 111.88(18) . . ? C203 O21 C202 110.1(3) . . ? C203 O21 K2 117.0(2) . . ? C202 O21 K2 114.7(3) . . ? C205 O22 C204 111.6(3) . . ? C205 O22 K2 118.3(2) . . ? C204 O22 K2 111.80(19) . . ? C209 O23 C208 112.4(5) . . ? C209 O23 K2 114.2(3) . . ? C208 O23 K2 118.5(3) . . ? C211 O24 C210 111.4(3) . . ? C211 O24 K2 116.6(2) . . ? C210 O24 K2 113.6(3) . . ? C214 O25 C215 113.2(4) . . ? C214 O25 K2 118.4(4) . . ? C215 O25 K2 114.3(3) . . ? C216 O26 C217 109.7(4) . . ? C216 O26 K2 115.0(3) . . ? C217 O26 K2 112.8(2) . . ? C302 O31 C303 111.7(3) . . ? C302 O31 K3 119.3(2) . . ? C303 O31 K3 112.48(17) . . ? C305 O32 C304 109.7(2) . . ? C305 O32 K3 118.84(16) . . ? C304 O32 K3 113.14(17) . . ? C309 O33 C308 111.8(3) . . ? C309 O33 K3 111.25(19) . . ? C308 O33 K3 117.1(2) . . ? C310 O34 C311 110.2(2) . . ? C310 O34 K3 115.63(19) . . ? C311 O34 K3 117.00(17) . . ? C314 O35 C315 109.2(3) . . ? C314 O35 K3 117.5(2) . . ? C315 O35 K3 112.43(17) . . ? C317 O36 C316 111.4(2) . . ? C317 O36 K3 120.85(17) . . ? C316 O36 K3 115.21(17) . . ? N11 C101 C102 113.1(3) . . ? N11 C101 H10A 109.0 . . ? C102 C101 H10A 109.0 . . ? N11 C101 H10B 109.0 . . ? C102 C101 H10B 109.0 . . ? H10A C101 H10B 107.8 . . ? O11 C102 C101 108.2(3) . . ? O11 C102 H10C 110.1 . . ? C101 C102 H10C 110.1 . . ? O11 C102 H10D 110.1 . . ? C101 C102 H10D 110.1 . . ? H10C C102 H10D 108.4 . . ? O11 C103 C104 109.1(3) . . ? O11 C103 H10E 109.9 . . ? C104 C103 H10E 109.9 . . ? O11 C103 H10F 109.9 . . ? C104 C103 H10F 109.9 . . ? H10E C103 H10F 108.3 . . ? O12 C104 C103 108.8(3) . . ? O12 C104 H10G 109.9 . . ? C103 C104 H10G 109.9 . . ? O12 C104 H10H 109.9 . . ? C103 C104 H10H 109.9 . . ? H10G C104 H10H 108.3 . . ? O12 C105 C106 109.5(3) . . ? O12 C105 H10I 109.8 . . ? C106 C105 H10I 109.8 . . ? O12 C105 H10J 109.8 . . ? C106 C105 H10J 109.8 . . ? H10I C105 H10J 108.2 . . ? N12 C106 C105 114.9(3) . . ? N12 C106 H10K 108.5 . . ? C105 C106 H10K 108.5 . . ? N12 C106 H10L 108.5 . . ? C105 C106 H10L 108.5 . . ? H10K C106 H10L 107.5 . . ? N11 C107 C108 112.4(3) . . ? N11 C107 H10M 109.1 . . ? C108 C107 H10M 109.1 . . ? N11 C107 H10N 109.1 . . ? C108 C107 H10N 109.1 . . ? H10M C107 H10N 107.8 . . ? O13 C108 C107 109.1(3) . . ? O13 C108 H10O 109.9 . . ? C107 C108 H10O 109.9 . . ? O13 C108 H10P 109.9 . . ? C107 C108 H10P 109.9 . . ? H10O C108 H10P 108.3 . . ? O13 C109 C110 109.8(3) . . ? O13 C109 H10Q 109.7 . . ? C110 C109 H10Q 109.7 . . ? O13 C109 H10R 109.7 . . ? C110 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O14 C110 C109 109.3(3) . . ? O14 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O14 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.3 . . ? O14 C111 C112 108.8(3) . . ? O14 C111 H11C 109.9 . . ? C112 C111 H11C 109.9 . . ? O14 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? H11C C111 H11D 108.3 . . ? N12 C112 C111 112.9(3) . . ? N12 C112 H11E 109.0 . . ? C111 C112 H11E 109.0 . . ? N12 C112 H11F 109.0 . . ? C111 C112 H11F 109.0 . . ? H11E C112 H11F 107.8 . . ? N11 C113 C114 114.9(3) . . ? N11 C113 H11G 108.5 . . ? C114 C113 H11G 108.5 . . ? N11 C113 H11H 108.5 . . ? C114 C113 H11H 108.5 . . ? H11G C113 H11H 107.5 . . ? O15 C114 C113 109.5(3) . . ? O15 C114 H11I 109.8 . . ? C113 C114 H11I 109.8 . . ? O15 C114 H11J 109.8 . . ? C113 C114 H11J 109.8 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 108.6(3) . . ? O15 C115 H11K 110.0 . . ? C116 C115 H11K 110.0 . . ? O15 C115 H11L 110.0 . . ? C116 C115 H11L 110.0 . . ? H11K C115 H11L 108.3 . . ? O16 C116 C115 110.0(3) . . ? O16 C116 H11M 109.7 . . ? C115 C116 H11M 109.7 . . ? O16 C116 H11N 109.7 . . ? C115 C116 H11N 109.7 . . ? H11M C116 H11N 108.2 . . ? O16 C117 C118 108.8(3) . . ? O16 C117 H11O 109.9 . . ? C118 C117 H11O 109.9 . . ? O16 C117 H11P 109.9 . . ? C118 C117 H11P 109.9 . . ? H11O C117 H11P 108.3 . . ? N12 C118 C117 113.1(3) . . ? N12 C118 H11Q 109.0 . . ? C117 C118 H11Q 109.0 . . ? N12 C118 H11R 109.0 . . ? C117 C118 H11R 109.0 . . ? H11Q C118 H11R 107.8 . . ? N21 C201 C202 113.7(5) . . ? N21 C201 H20A 108.8 . . ? C202 C201 H20A 108.8 . . ? N21 C201 H20B 108.8 . . ? C202 C201 H20B 108.8 . . ? H20A C201 H20B 107.7 . . ? O21 C202 C201 108.8(4) . . ? O21 C202 H20C 109.9 . . ? C201 C202 H20C 109.9 . . ? O21 C202 H20D 109.9 . . ? C201 C202 H20D 109.9 . . ? H20C C202 H20D 108.3 . . ? O21 C203 C204 110.2(3) . . ? O21 C203 H20E 109.6 . . ? C204 C203 H20E 109.6 . . ? O21 C203 H20F 109.6 . . ? C204 C203 H20F 109.6 . . ? H20E C203 H20F 108.1 . . ? O22 C204 C203 110.3(3) . . ? O22 C204 H20G 109.6 . . ? C203 C204 H20G 109.6 . . ? O22 C204 H20H 109.6 . . ? C203 C204 H20H 109.6 . . ? H20G C204 H20H 108.1 . . ? O22 C205 C206 109.0(3) . . ? O22 C205 H20I 109.9 . . ? C206 C205 H20I 109.9 . . ? O22 C205 H20J 109.9 . . ? C206 C205 H20J 109.9 . . ? H20I C205 H20J 108.3 . . ? N22 C206 C205 113.8(3) . . ? N22 C206 H20K 108.8 . . ? C205 C206 H20K 108.8 . . ? N22 C206 H20L 108.8 . . ? C205 C206 H20L 108.8 . . ? H20K C206 H20L 107.7 . . ? N21 C207 C208 113.6(5) . . ? N21 C207 H20M 108.9 . . ? C208 C207 H20M 108.9 . . ? N21 C207 H20N 108.9 . . ? C208 C207 H20N 108.9 . . ? H20M C207 H20N 107.7 . . ? O23 C208 C207 109.7(5) . . ? O23 C208 H20O 109.7 . . ? C207 C208 H20O 109.7 . . ? O23 C208 H20P 109.7 . . ? C207 C208 H20P 109.7 . . ? H20O C208 H20P 108.2 . . ? O23 C209 C210 111.0(4) . . ? O23 C209 H20Q 109.4 . . ? C210 C209 H20Q 109.4 . . ? O23 C209 H20R 109.4 . . ? C210 C209 H20R 109.4 . . ? H20Q C209 H20R 108.0 . . ? O24 C210 C209 110.3(3) . . ? O24 C210 H21A 109.6 . . ? C209 C210 H21A 109.6 . . ? O24 C210 H21B 109.6 . . ? C209 C210 H21B 109.6 . . ? H21A C210 H21B 108.1 . . ? O24 C211 C212 109.2(3) . . ? O24 C211 H21C 109.8 . . ? C212 C211 H21C 109.8 . . ? O24 C211 H21D 109.8 . . ? C212 C211 H21D 109.8 . . ? H21C C211 H21D 108.3 . . ? N22 C212 C211 113.4(3) . . ? N22 C212 H21E 108.9 . . ? C211 C212 H21E 108.9 . . ? N22 C212 H21F 108.9 . . ? C211 C212 H21F 108.9 . . ? H21E C212 H21F 107.7 . . ? C214 C213 N21 113.9(5) . . ? C214 C213 H21G 108.8 . . ? N21 C213 H21G 108.8 . . ? C214 C213 H21H 108.8 . . ? N21 C213 H21H 108.8 . . ? H21G C213 H21H 107.7 . . ? O25 C214 C213 108.8(5) . . ? O25 C214 H21I 109.9 . . ? C213 C214 H21I 109.9 . . ? O25 C214 H21J 109.9 . . ? C213 C214 H21J 109.9 . . ? H21I C214 H21J 108.3 . . ? O25 C215 C216 108.3(4) . . ? O25 C215 H21K 110.0 . . ? C216 C215 H21K 110.0 . . ? O25 C215 H21L 110.0 . . ? C216 C215 H21L 110.0 . . ? H21K C215 H21L 108.4 . . ? O26 C216 C215 108.7(4) . . ? O26 C216 H21M 110.0 . . ? C215 C216 H21M 110.0 . . ? O26 C216 H21N 110.0 . . ? C215 C216 H21N 110.0 . . ? H21M C216 H21N 108.3 . . ? O26 C217 C218 109.6(3) . . ? O26 C217 H21O 109.8 . . ? C218 C217 H21O 109.8 . . ? O26 C217 H21P 109.8 . . ? C218 C217 H21P 109.8 . . ? H21O C217 H21P 108.2 . . ? C217 C218 N22 114.0(3) . . ? C217 C218 H21Q 108.8 . . ? N22 C218 H21Q 108.8 . . ? C217 C218 H21R 108.8 . . ? N22 C218 H21R 108.8 . . ? H21Q C218 H21R 107.6 . . ? N31 C301 C302 113.2(3) . . ? N31 C301 H30A 108.9 . . ? C302 C301 H30A 108.9 . . ? N31 C301 H30B 108.9 . . ? C302 C301 H30B 108.9 . . ? H30A C301 H30B 107.8 . . ? O31 C302 C301 108.8(3) . . ? O31 C302 H30C 109.9 . . ? C301 C302 H30C 109.9 . . ? O31 C302 H30D 109.9 . . ? C301 C302 H30D 109.9 . . ? H30C C302 H30D 108.3 . . ? O31 C303 C304 110.0(2) . . ? O31 C303 H30E 109.7 . . ? C304 C303 H30E 109.7 . . ? O31 C303 H30F 109.7 . . ? C304 C303 H30F 109.7 . . ? H30E C303 H30F 108.2 . . ? O32 C304 C303 109.3(3) . . ? O32 C304 H30G 109.8 . . ? C303 C304 H30G 109.8 . . ? O32 C304 H30H 109.8 . . ? C303 C304 H30H 109.8 . . ? H30G C304 H30H 108.3 . . ? O32 C305 C306 109.6(2) . . ? O32 C305 H30I 109.8 . . ? C306 C305 H30I 109.8 . . ? O32 C305 H30J 109.8 . . ? C306 C305 H30J 109.8 . . ? H30I C305 H30J 108.2 . . ? N32 C306 C305 113.6(3) . . ? N32 C306 H30K 108.8 . . ? C305 C306 H30K 108.8 . . ? N32 C306 H30L 108.8 . . ? C305 C306 H30L 108.8 . . ? H30K C306 H30L 107.7 . . ? N31 C307 C308 114.3(3) . . ? N31 C307 H30M 108.7 . . ? C308 C307 H30M 108.7 . . ? N31 C307 H30N 108.7 . . ? C308 C307 H30N 108.7 . . ? H30M C307 H30N 107.6 . . ? O33 C308 C307 109.4(3) . . ? O33 C308 H30O 109.8 . . ? C307 C308 H30O 109.8 . . ? O33 C308 H30P 109.8 . . ? C307 C308 H30P 109.8 . . ? H30O C308 H30P 108.3 . . ? O33 C309 C310 109.6(3) . . ? O33 C309 H30Q 109.8 . . ? C310 C309 H30Q 109.8 . . ? O33 C309 H30R 109.8 . . ? C310 C309 H30R 109.8 . . ? H30Q C309 H30R 108.2 . . ? O34 C310 C309 108.9(3) . . ? O34 C310 H31A 109.9 . . ? C309 C310 H31A 109.9 . . ? O34 C310 H31B 109.9 . . ? C309 C310 H31B 109.9 . . ? H31A C310 H31B 108.3 . . ? O34 C311 C312 109.2(2) . . ? O34 C311 H31C 109.8 . . ? C312 C311 H31C 109.8 . . ? O34 C311 H31D 109.8 . . ? C312 C311 H31D 109.8 . . ? H31C C311 H31D 108.3 . . ? N32 C312 C311 113.5(3) . . ? N32 C312 H31E 108.9 . . ? C311 C312 H31E 108.9 . . ? N32 C312 H31F 108.9 . . ? C311 C312 H31F 108.9 . . ? H31E C312 H31F 107.7 . . ? N31 C313 C314 114.0(4) . . ? N31 C313 H31G 108.7 . . ? C314 C313 H31G 108.7 . . ? N31 C313 H31H 108.7 . . ? C314 C313 H31H 108.7 . . ? H31G C313 H31H 107.6 . . ? O35 C314 C313 109.0(3) . . ? O35 C314 H31I 109.9 . . ? C313 C314 H31I 109.9 . . ? O35 C314 H31J 109.9 . . ? C313 C314 H31J 109.9 . . ? H31I C314 H31J 108.3 . . ? O35 C315 C316 110.1(3) . . ? O35 C315 H31K 109.6 . . ? C316 C315 H31K 109.6 . . ? O35 C315 H31L 109.6 . . ? C316 C315 H31L 109.6 . . ? H31K C315 H31L 108.1 . . ? O36 C316 C315 109.6(3) . . ? O36 C316 H31M 109.8 . . ? C315 C316 H31M 109.8 . . ? O36 C316 H31N 109.8 . . ? C315 C316 H31N 109.8 . . ? H31M C316 H31N 108.2 . . ? O36 C317 C318 109.0(3) . . ? O36 C317 H31O 109.9 . . ? C318 C317 H31O 109.9 . . ? O36 C317 H31P 109.9 . . ? C318 C317 H31P 109.9 . . ? H31O C317 H31P 108.3 . . ? N32 C318 C317 113.8(3) . . ? N32 C318 H31Q 108.8 . . ? C317 C318 H31Q 108.8 . . ? N32 C318 H31R 108.8 . . ? C317 C318 H31R 108.8 . . ? H31Q C318 H31R 107.7 . . ? C1R N1R H1R3 109.5 . . ? C1R N1R H1R4 109.5 . . ? H1R3 N1R H1R4 109.5 . . ? C1R N1R H1R5 109.5 . . ? H1R3 N1R H1R5 109.5 . . ? H1R4 N1R H1R5 109.5 . . ? N1R C1R C2R 111.2(3) . . ? N1R C1R H1R1 109.4 . . ? C2R C1R H1R1 109.4 . . ? N1R C1R H1R2 109.4 . . ? C2R C1R H1R2 109.4 . . ? H1R1 C1R H1R2 108.0 . . ? N2R C2R C1R 113.4(4) . . ? N2R C2R H2R1 108.9 . . ? C1R C2R H2R1 108.9 . . ? N2R C2R H2R2 108.9 . . ? C1R C2R H2R2 108.9 . . ? H2R1 C2R H2R2 107.7 . . ? C2R N2R H2R3 109.5 . . ? C2R N2R H2R4 109.5 . . ? H2R3 N2R H2R4 109.5 . . ? C2R N2R H2R5 109.5 . . ? H2R3 N2R H2R5 109.5 . . ? H2R4 N2R H2R5 109.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3S C2S C7S 120.0 . . ? C3S C2S C1S 95.4(7) . . ? C7S C2S C1S 144.3(7) . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C7S C6S C5S 120.0 . . ? C7S C6S H6S 120.0 . . ? C5S C6S H6S 120.0 . . ? C6S C7S C2S 120.0 . . ? C6S C7S H7S 120.0 . . ? C2S C7S H7S 120.0 . . ? C2T C1T H1T1 109.5 . . ? C2T C1T H1T2 109.5 . . ? H1T1 C1T H1T2 109.5 . . ? C2T C1T H1T3 109.5 . . ? H1T1 C1T H1T3 109.5 . . ? H1T2 C1T H1T3 109.5 . . ? C1T C2T C3T 119.3(6) . . ? C1T C2T C7T 120.7(6) . . ? C3T C2T C7T 120.0 . . ? C2T C3T C4T 120.0 . . ? C2T C3T H3T 120.0 . . ? C4T C3T H3T 120.0 . . ? C5T C4T C3T 120.0 . . ? C5T C4T H4T 120.0 . . ? C3T C4T H4T 120.0 . . ? C6T C5T C4T 120.0 . . ? C6T C5T H5T 120.0 . . ? C4T C5T H5T 120.0 . . ? C5T C6T C7T 120.0 . . ? C5T C6T H6T 120.0 . . ? C7T C6T H6T 120.0 . . ? C6T C7T C2T 120.0 . . ? C6T C7T H7T 120.0 . . ? C2T C7T H7T 120.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.982 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.077 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 700663' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)]3[Sn9Zn(iPr)]*0.5en ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K-(2,2,2-crypt))3(Sn9Zn(iPr))*0.5en _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), C3 H7 Sn9 Zn, 0.5(C2 H8 N2)' _chemical_formula_sum 'C58 H115 K3 N7 O18 Sn9 Zn' _chemical_formula_weight 2453.48 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' K K 0.2009 0.2494 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.00060(10) _cell_length_b 14.58550(10) _cell_length_c 21.8839(2) _cell_angle_alpha 86.8242(4) _cell_angle_beta 86.3706(5) _cell_angle_gamma 79.6696(4) _cell_volume 4383.15(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour 'dark orange-yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2394 _exptl_absorpt_coefficient_mu 2.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4299 _exptl_absorpt_correction_T_max 0.5594 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36870 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19739 _reflns_number_gt 15600 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0273P)^2^+75.4777P] 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 19739 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _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 0.15558(5) 0.83175(4) 0.37151(3) 0.02865(14) Uani 1 1 d . . . Sn3 Sn 0.09800(4) 0.66196(4) 0.32906(3) 0.02674(13) Uani 1 1 d . . . Sn4 Sn 0.31861(4) 0.68153(4) 0.33706(3) 0.02698(13) Uani 1 1 d . . . Sn5 Sn 0.27876(5) 0.88230(4) 0.26564(3) 0.02776(13) Uani 1 1 d . . . Sn2 Sn 0.05705(4) 0.86530(4) 0.25611(3) 0.02692(13) Uani 1 1 d . . . Sn7 Sn 0.25457(4) 0.56207(4) 0.24835(3) 0.02628(13) Uani 1 1 d . . . Sn8 Sn 0.38356(4) 0.71300(4) 0.20773(3) 0.02940(14) Uani 1 1 d . . . Sn9 Sn 0.19723(4) 0.83920(4) 0.15269(3) 0.02685(13) Uani 1 1 d . . . Sn6 Sn 0.07196(4) 0.68755(4) 0.19583(3) 0.02774(13) Uani 1 1 d . . . Zn1 Zn 0.25477(8) 0.65034(8) 0.13296(5) 0.0343(2) Uani 1 1 d . . . C1 C 0.2895(9) 0.6037(7) 0.0481(5) 0.046(3) Uani 1 1 d . . . H1 H 0.2781 0.5379 0.0480 0.055 Uiso 1 1 calc R . . C2 C 0.3911(9) 0.6047(9) 0.0287(6) 0.063(4) Uani 1 1 d . . . H2A H 0.4334 0.5661 0.0577 0.094 Uiso 1 1 calc R . . H2B H 0.4033 0.6689 0.0275 0.094 Uiso 1 1 calc R . . H2C H 0.4048 0.5798 -0.0122 0.094 Uiso 1 1 calc R . . C3 C 0.22124(6) 0.66427(6) 0.00225(4) 0.062(3) Uani 1 1 d . . . H3A H 0.1534 0.6627 0.0155 0.093 Uiso 1 1 calc R . . H3B H 0.2349 0.6395 -0.0387 0.093 Uiso 1 1 calc R . . H3C H 0.2325 0.7288 0.0011 0.093 Uiso 1 1 calc R . . K1 K 0.66561(6) 0.78629(6) 0.47109(4) 0.0240(3) Uani 1 1 d R . . K2 K 0.78852(6) 0.32428(6) 0.30723(4) 0.0265(4) Uani 1 1 d R . . K3 K 0.24847(6) 1.13750(6) 0.03814(4) 0.0354(4) Uani 1 1 d R B . N11 N 0.69379(6) 0.77038(6) 0.33387(4) 0.0301(16) Uani 1 1 d R . . N12 N 0.62207(6) 0.80018(6) 0.60475(4) 0.0274(15) Uani 1 1 d R . . N21 N 0.63882(6) 0.39019(6) 0.21298(4) 0.0312(16) Uani 1 1 d R . . N22 N 0.93847(6) 0.25590(6) 0.40191(4) 0.0291(16) Uani 1 1 d R . . N31 N 0.31709(6) 1.19762(6) 0.15432(4) 0.054(3) Uani 1 1 d R . . N32 N 0.18245(6) 1.08312(6) -0.08058(4) 0.0396(19) Uani 1 1 d R . . O11 O 0.53769(6) 0.90003(6) 0.39829(4) 0.0275(13) Uani 1 1 d R . . O12 O 0.47717(6) 0.81776(6) 0.51391(4) 0.0315(14) Uani 1 1 d R . . O13 O 0.79638(6) 0.88448(6) 0.40798(4) 0.0321(14) Uani 1 1 d R . . O14 O 0.72628(6) 0.92637(6) 0.52932(4) 0.0360(15) Uani 1 1 d R . . O15 O 0.75566(6) 0.61905(6) 0.42116(4) 0.0409(16) Uani 1 1 d R . . O16 O 0.75617(6) 0.64343(6) 0.54925(4) 0.0361(15) Uani 1 1 d R . . O21 O 0.59826(6) 0.40851(6) 0.34666(4) 0.0310(13) Uani 1 1 d R . . O22 O 0.74687(6) 0.36895(6) 0.43211(4) 0.0281(13) Uani 1 1 d R . . O23 O 0.82801(6) 0.45376(6) 0.21287(4) 0.0400(16) Uani 1 1 d R . . O24 O 0.97555(6) 0.37053(6) 0.29193(4) 0.0323(14) Uani 1 1 d R . . O25 O 0.72412(6) 0.19180(6) 0.23260(4) 0.0353(14) Uani 1 1 d R . . O26 O 0.84497(6) 0.13215(6) 0.33200(4) 0.0378(15) Uani 1 1 d R . . O31 O 0.35403(6) 1.29035(6) 0.03484(4) 0.053(2) Uani 1 1 d R . . O32 O 0.27390(6) 1.24803(6) -0.07289(4) 0.0389(16) Uani 1 1 d R . . O33 O 0.10875(6) 1.20052(6) 0.13440(4) 0.0467(18) Uani 1 1 d R . . O34 O 0.05001(6) 1.12597(6) 0.02932(4) 0.0405(16) Uani 1 1 d R . . O35 O 0.38920(6) 1.01656(6) 0.10035(4) 0.051(2) Uani 1 1 d R . . O36 O 0.34609(6) 0.96599(6) -0.01547(4) 0.0422(17) Uani 1 1 d R . . C101 C 0.60867(6) 0.82438(6) 0.30450(4) 0.038(2) Uani 1 1 d R . . H10I H 0.5570 0.7859 0.3053 0.046 Uiso 1 1 calc R . . H10J H 0.6270 0.8389 0.2611 0.046 Uiso 1 1 calc R . . C102 C 0.5693(7) 0.9138(7) 0.3354(4) 0.035(2) Uani 1 1 d . . . H10C H 0.6203 0.9530 0.3332 0.042 Uiso 1 1 calc R . . H10D H 0.5138 0.9480 0.3128 0.042 Uiso 1 1 calc R . . C103 C 0.4599(7) 0.8511(7) 0.4063(4) 0.036(2) Uani 1 1 d . . . H10A H 0.4838 0.7836 0.4017 0.043 Uiso 1 1 calc R . . H10B H 0.4119 0.8731 0.3750 0.043 Uiso 1 1 calc R . . C104 C 0.4126(7) 0.8676(8) 0.4698(5) 0.041(2) Uani 1 1 d . . . H10K H 0.4000 0.9351 0.4773 0.049 Uiso 1 1 calc R . . H10L H 0.3497 0.8451 0.4735 0.049 Uiso 1 1 calc R . . C105 C 0.4523(7) 0.8479(7) 0.5736(4) 0.036(2) Uani 1 1 d . . . H10E H 0.3844 0.8410 0.5853 0.044 Uiso 1 1 calc R . . H10F H 0.4568 0.9147 0.5750 0.044 Uiso 1 1 calc R . . C106 C 0.5188(7) 0.7921(8) 0.6180(4) 0.038(2) Uani 1 1 d . . . H10G H 0.4986 0.8131 0.6598 0.046 Uiso 1 1 calc R . . H10H H 0.5124 0.7257 0.6171 0.046 Uiso 1 1 calc R . . C107 C 0.7830(7) 0.8075(7) 0.3163(4) 0.037(2) Uani 1 1 d . . . H10O H 0.7648 0.8706 0.2968 0.045 Uiso 1 1 calc R . . H10P H 0.8216 0.7673 0.2853 0.045 Uiso 1 1 calc R . . C108 C 0.8456(7) 0.8135(7) 0.3684(4) 0.036(2) Uani 1 1 d . . . H10M H 0.8581 0.7527 0.3916 0.043 Uiso 1 1 calc R . . H10N H 0.9088 0.8291 0.3525 0.043 Uiso 1 1 calc R . . C109 C 0.8597(7) 0.8967(7) 0.4555(5) 0.038(2) Uani 1 1 d . . . H10Q H 0.9177 0.9204 0.4374 0.046 Uiso 1 1 calc R . . H10R H 0.8816 0.8365 0.4779 0.046 Uiso 1 1 calc R . . C110 C 0.8022(7) 0.9657(8) 0.4983(5) 0.040(2) Uani 1 1 d . . . H11I H 0.8453 0.9825 0.5284 0.048 Uiso 1 1 calc R . . H11J H 0.7745 1.0232 0.4748 0.048 Uiso 1 1 calc R . . C111 C 0.7320(7) 0.9178(7) 0.5943(4) 0.033(2) Uani 1 1 d . . . H11E H 0.7408 0.9779 0.6101 0.039 Uiso 1 1 calc R . . H11F H 0.7884 0.8697 0.6053 0.039 Uiso 1 1 calc R . . C112 C 0.6394(7) 0.8907(7) 0.6222(4) 0.033(2) Uani 1 1 d . . . H11A H 0.6411 0.8899 0.6674 0.040 Uiso 1 1 calc R . . H11B H 0.5840 0.9391 0.6100 0.040 Uiso 1 1 calc R . . C113 C 0.7046(9) 0.6708(7) 0.3217(5) 0.043(3) Uani 1 1 d . . . H11G H 0.7211 0.6626 0.2775 0.052 Uiso 1 1 calc R . . H11H H 0.6415 0.6503 0.3315 0.052 Uiso 1 1 calc R . . C114 C 0.7808(9) 0.6093(8) 0.3575(5) 0.049(3) Uani 1 1 d . . . H11O H 0.7849 0.5435 0.3470 0.058 Uiso 1 1 calc R . . H11P H 0.8450 0.6274 0.3473 0.058 Uiso 1 1 calc R . . C115 C 0.8293(9) 0.5712(7) 0.4582(6) 0.054(3) Uani 1 1 d . . . H11Q H 0.8816 0.6084 0.4596 0.065 Uiso 1 1 calc R . . H11R H 0.8578 0.5106 0.4406 0.065 Uiso 1 1 calc R . . C116 C 0.7863(9) 0.5551(7) 0.5223(5) 0.048(3) Uani 1 1 d . . . H11M H 0.7299 0.5231 0.5206 0.058 Uiso 1 1 calc R . . H11N H 0.8354 0.5151 0.5473 0.058 Uiso 1 1 calc R . . C117 C 0.7006(8) 0.6341(6) 0.6055(4) 0.036(2) Uani 1 1 d . . . H11K H 0.7356 0.5832 0.6318 0.044 Uiso 1 1 calc R . . H11L H 0.6372 0.6178 0.5970 0.044 Uiso 1 1 calc R . . C118 C 0.6843(8) 0.7235(7) 0.6382(4) 0.038(2) Uani 1 1 d . . . H11C H 0.6534 0.7135 0.6794 0.046 Uiso 1 1 calc R . . H11D H 0.7478 0.7418 0.6437 0.046 Uiso 1 1 calc R . . C201 C 0.5417(7) 0.4193(7) 0.2442(5) 0.037(2) Uani 1 1 d . . . H20G H 0.5119 0.3634 0.2544 0.045 Uiso 1 1 calc R . . H20H H 0.4994 0.4606 0.2157 0.045 Uiso 1 1 calc R . . C202 C 0.5453(7) 0.4695(6) 0.3017(5) 0.037(2) Uani 1 1 d . . . H20C H 0.5771 0.5244 0.2922 0.045 Uiso 1 1 calc R . . H20D H 0.4783 0.4921 0.3183 0.045 Uiso 1 1 calc R . . C203 C 0.5906(6) 0.4491(7) 0.4052(4) 0.033(2) Uani 1 1 d . . . H20K H 0.5214 0.4641 0.4199 0.040 Uiso 1 1 calc R . . H20L H 0.6174 0.5077 0.4019 0.040 Uiso 1 1 calc R . . C204 C 0.6457(7) 0.3816(7) 0.4493(4) 0.037(2) Uani 1 1 d . . . H20I H 0.6341 0.4053 0.4911 0.044 Uiso 1 1 calc R . . H20J H 0.6230 0.3211 0.4495 0.044 Uiso 1 1 calc R . . C205 C 0.8014(7) 0.3087(7) 0.4762(4) 0.034(2) Uani 1 1 d . . . H20E H 0.7828 0.2462 0.4773 0.041 Uiso 1 1 calc R . . H20F H 0.7868 0.3341 0.5174 0.041 Uiso 1 1 calc R . . C206 C 0.9085(7) 0.3006(6) 0.4592(4) 0.033(2) Uani 1 1 d . . . H20A H 0.9253 0.3639 0.4562 0.040 Uiso 1 1 calc R . . H20B H 0.9456 0.2646 0.4924 0.040 Uiso 1 1 calc R . . C207 C 0.6675(8) 0.4705(8) 0.1780(5) 0.047(3) Uani 1 1 d . . . H20Q H 0.6498 0.5262 0.2030 0.057 Uiso 1 1 calc R . . H20R H 0.6301 0.4824 0.1406 0.057 Uiso 1 1 calc R . . C208 C 0.7749(8) 0.4579(9) 0.1595(5) 0.048(3) Uani 1 1 d . . . H20M H 0.7951 0.3997 0.1373 0.058 Uiso 1 1 calc R . . H20N H 0.7881 0.5108 0.1319 0.058 Uiso 1 1 calc R . . C209 C 0.9296(7) 0.4478(8) 0.1972(5) 0.040(2) Uani 1 1 d . . . H20O H 0.9398 0.5002 0.1683 0.048 Uiso 1 1 calc R . . H20P H 0.9548 0.3888 0.1768 0.048 Uiso 1 1 calc R . . C210 C 0.9830(8) 0.4514(7) 0.2529(5) 0.039(2) Uani 1 1 d . . . H21O H 1.0522 0.4532 0.2414 0.046 Uiso 1 1 calc R . . H21P H 0.9553 0.5085 0.2748 0.046 Uiso 1 1 calc R . . C211 C 1.0265(8) 0.3715(7) 0.3463(4) 0.038(2) Uani 1 1 d . . . H21Q H 0.9914 0.4205 0.3731 0.046 Uiso 1 1 calc R . . H21R H 1.0925 0.3852 0.3356 0.046 Uiso 1 1 calc R . . C212 C 1.0332(7) 0.2777(7) 0.3788(5) 0.037(2) Uani 1 1 d . . . H21M H 1.0645 0.2293 0.3504 0.044 Uiso 1 1 calc R . . H21N H 1.0755 0.2750 0.4137 0.044 Uiso 1 1 calc R . . C213 C 0.6361(8) 0.3149(8) 0.1715(4) 0.041(2) Uani 1 1 d . . . H21A H 0.6934 0.3100 0.1421 0.049 Uiso 1 1 calc R . . H21B H 0.5771 0.3312 0.1477 0.049 Uiso 1 1 calc R . . C214 C 0.6359(7) 0.2207(6) 0.2049(4) 0.034(2) Uani 1 1 d . . . H21C H 0.5815 0.2258 0.2365 0.041 Uiso 1 1 calc R . . H21D H 0.6265 0.1743 0.1756 0.041 Uiso 1 1 calc R . . C215 C 0.7277(7) 0.1031(6) 0.2656(5) 0.036(2) Uani 1 1 d . . . H21E H 0.7113 0.0567 0.2385 0.043 Uiso 1 1 calc R . . H21F H 0.6800 0.1092 0.3011 0.043 Uiso 1 1 calc R . . C216 C 0.8280(8) 0.0718(6) 0.2870(5) 0.040(2) Uani 1 1 d . . . H21K H 0.8348 0.0071 0.3045 0.048 Uiso 1 1 calc R . . H21L H 0.8762 0.0731 0.2520 0.048 Uiso 1 1 calc R . . C217 C 0.9428(8) 0.1047(7) 0.3530(5) 0.044(2) Uani 1 1 d . . . H21I H 0.9909 0.1224 0.3215 0.052 Uiso 1 1 calc R . . H21J H 0.9577 0.0363 0.3611 0.052 Uiso 1 1 calc R . . C218 C 0.9470(8) 0.1542(6) 0.4108(5) 0.039(2) Uani 1 1 d . . . H21G H 0.8939 0.1405 0.4400 0.047 Uiso 1 1 calc R . . H21H H 1.0093 0.1289 0.4296 0.047 Uiso 1 1 calc R . . C301 C 0.3840(11) 1.2637(10) 0.1407(6) 0.066(4) Uani 1 1 d . B . H30G H 0.4484 1.2289 0.1270 0.080 Uiso 1 1 calc R . . H30H H 0.3921 1.2946 0.1787 0.080 Uiso 1 1 calc R . . C302 C 0.3489(12) 1.3382(9) 0.0914(6) 0.065(4) Uani 1 1 d . B . H30I H 0.2812 1.3689 0.1018 0.079 Uiso 1 1 calc R . . H30J H 0.3909 1.3863 0.0877 0.079 Uiso 1 1 calc R . . C303 C 0.3437(8) 1.3511(7) -0.0160(5) 0.044(2) Uani 1 1 d . B . H30C H 0.3953 1.3897 -0.0180 0.053 Uiso 1 1 calc R . . H30D H 0.2800 1.3934 -0.0123 0.053 Uiso 1 1 calc R . . C304 C 0.3500(8) 1.2997(7) -0.0730(5) 0.043(2) Uani 1 1 d . B . H30E H 0.3460 1.3445 -0.1089 0.052 Uiso 1 1 calc R . . H30F H 0.4133 1.2570 -0.0766 0.052 Uiso 1 1 calc R . . C305 C 0.2724(9) 1.2032(8) -0.1285(5) 0.048(3) Uani 1 1 d . B . H30Q H 0.3308 1.1542 -0.1332 0.058 Uiso 1 1 calc R A 1 H30R H 0.2733 1.2491 -0.1635 0.058 Uiso 1 1 calc R A 1 C306 C 0.1833(9) 1.1606(8) -0.1286(4) 0.046(3) Uani 1 1 d . B 1 H30A H 0.1794 1.1359 -0.1694 0.055 Uiso 1 1 calc R B 1 H30B H 0.1253 1.2094 -0.1214 0.055 Uiso 1 1 calc R B 1 C307 C 0.2310(12) 1.2419(10) 0.1927(6) 0.067(4) Uani 1 1 d . B 1 H30O H 0.2090 1.3065 0.1764 0.081 Uiso 1 1 calc R B 1 H30P H 0.2505 1.2454 0.2351 0.081 Uiso 1 1 calc R B 1 C308 C 0.1474(10) 1.1893(9) 0.1941(5) 0.053(3) Uani 1 1 d . B 1 H30M H 0.1702 1.1224 0.2046 0.064 Uiso 1 1 calc R B 1 H30N H 0.0966 1.2144 0.2254 0.064 Uiso 1 1 calc R B 1 C309 C 0.0234(8) 1.1617(8) 0.1333(5) 0.045(2) Uani 1 1 d . B 1 H30K H -0.0259 1.1902 0.1644 0.054 Uiso 1 1 calc R B 1 H30L H 0.0382 1.0936 0.1428 0.054 Uiso 1 1 calc R B 1 C310 C -0.0143(8) 1.1801(8) 0.0715(5) 0.043(2) Uani 1 1 d . B 1 H31O H -0.0799 1.1636 0.0714 0.052 Uiso 1 1 calc R B 1 H31P H -0.0195 1.2472 0.0595 0.052 Uiso 1 1 calc R B 1 C311 C 0.0156(8) 1.1369(9) -0.0311(5) 0.048(3) Uani 1 1 d . B 1 H31Q H 0.0172 1.2010 -0.0481 0.058 Uiso 1 1 calc R B 1 H31R H -0.0522 1.1259 -0.0303 0.058 Uiso 1 1 calc R B 1 C312 C 0.0809(8) 1.0671(9) -0.0698(5) 0.048(3) Uani 1 1 d . B 1 H31M H 0.0824 1.0042 -0.0499 0.058 Uiso 1 1 calc R B 1 H31N H 0.0522 1.0671 -0.1100 0.058 Uiso 1 1 calc R B 1 C313 C 0.3685(9) 1.1142(9) 0.1857(5) 0.054(3) Uani 1 1 d . B 1 H31G H 0.3199 1.0787 0.2053 0.065 Uiso 1 1 calc R B 1 H31H H 0.4046 1.1338 0.2188 0.065 Uiso 1 1 calc R B 1 C314 C 0.4391(9) 1.0500(10) 0.1455(6) 0.062(4) Uani 1 1 d . B 1 H31K H 0.4887 1.0842 0.1258 0.075 Uiso 1 1 calc R B 1 H31L H 0.4727 0.9970 0.1707 0.075 Uiso 1 1 calc R B 1 C315 C 0.4459(8) 0.9400(8) 0.0701(5) 0.050(3) Uani 1 1 d . B 1 H31C H 0.4732 0.8919 0.1010 0.059 Uiso 1 1 calc R B 1 H31D H 0.5009 0.9613 0.0461 0.059 Uiso 1 1 calc R B 1 C316 C 0.3878(8) 0.8993(8) 0.0292(5) 0.050(3) Uani 1 1 d . B 1 H31I H 0.4295 0.8467 0.0084 0.061 Uiso 1 1 calc R B 1 H31J H 0.3354 0.8744 0.0536 0.061 Uiso 1 1 calc R B 1 C317 C 0.2796(9) 0.9304(8) -0.0499(5) 0.049(3) Uani 1 1 d . B 1 H31E H 0.2230 0.9191 -0.0229 0.059 Uiso 1 1 calc R B 1 H31F H 0.3114 0.8703 -0.0668 0.059 Uiso 1 1 calc R B 1 C318 C 0.2456(9) 0.9996(8) -0.1018(5) 0.049(3) Uani 1 1 d . B 1 H31A H 0.3030 1.0176 -0.1249 0.059 Uiso 1 1 calc R B 1 H31B H 0.2103 0.9690 -0.1303 0.059 Uiso 1 1 calc R B 1 N1S N 0.9417(18) 0.5958(17) 0.0482(12) 0.113(10) Uiso 0.74(4) 1 d P C 1 C1S C 0.968(2) 0.5448(19) -0.0049(16) 0.151(10) Uiso 1 1 d . . . N2S N 0.913(4) 0.541(4) -0.054(3) 0.10(2) Uiso 0.26(4) 1 d P C 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 0.0350(3) 0.0273(3) 0.0221(3) -0.0014(2) -0.0004(2) -0.0016(2) Sn3 0.0265(3) 0.0254(3) 0.0273(3) 0.0039(2) 0.0029(2) -0.0049(2) Sn4 0.0267(3) 0.0277(3) 0.0250(3) 0.0024(2) -0.0062(2) 0.0001(2) Sn5 0.0324(3) 0.0253(3) 0.0272(3) 0.0017(2) -0.0030(2) -0.0097(2) Sn2 0.0250(3) 0.0255(3) 0.0270(3) 0.0022(2) -0.0005(2) 0.0033(2) Sn7 0.0282(3) 0.0207(3) 0.0279(3) 0.0015(2) -0.0021(2) 0.0008(2) Sn8 0.0216(3) 0.0338(3) 0.0310(3) 0.0007(2) 0.0028(2) -0.0023(2) Sn9 0.0304(3) 0.0279(3) 0.0209(3) 0.0046(2) -0.0001(2) -0.0036(2) Sn6 0.0260(3) 0.0274(3) 0.0304(3) 0.0023(2) -0.0071(2) -0.0053(2) Zn1 0.0410(6) 0.0357(6) 0.0240(5) -0.0039(4) 0.0010(4) -0.0006(5) C1 0.067(7) 0.032(5) 0.040(6) 0.002(4) -0.003(5) -0.012(5) C2 0.055(8) 0.060(8) 0.067(8) -0.013(6) 0.027(6) 0.000(6) C3 0.079(9) 0.075(9) 0.032(6) -0.007(6) -0.007(6) -0.007(7) K1 0.0233(8) 0.0240(8) 0.0237(8) 0.0007(7) -0.0007(7) -0.0025(7) K2 0.0267(9) 0.0250(9) 0.0276(9) -0.0004(7) -0.0011(7) -0.0041(7) K3 0.0346(11) 0.0430(11) 0.0291(10) 0.0043(8) -0.0083(8) -0.0080(9) N11 0.033(4) 0.032(4) 0.025(4) -0.008(3) 0.007(3) -0.006(3) N12 0.027(4) 0.032(4) 0.024(4) 0.002(3) -0.005(3) -0.009(3) N21 0.030(4) 0.031(4) 0.033(4) 0.004(3) -0.006(3) -0.007(3) N22 0.028(4) 0.022(3) 0.037(4) 0.000(3) -0.007(3) -0.001(3) N31 0.068(7) 0.055(6) 0.047(5) 0.020(4) -0.031(5) -0.032(5) N32 0.044(5) 0.046(5) 0.030(4) -0.006(4) -0.003(4) -0.008(4) O11 0.023(3) 0.029(3) 0.028(3) -0.002(2) -0.001(2) 0.001(2) O12 0.025(3) 0.042(4) 0.026(3) 0.001(3) -0.002(2) -0.004(3) O13 0.032(3) 0.034(3) 0.031(3) -0.008(3) 0.004(3) -0.006(3) O14 0.035(4) 0.050(4) 0.027(3) -0.007(3) 0.003(3) -0.020(3) O15 0.045(4) 0.030(3) 0.044(4) -0.009(3) 0.005(3) 0.003(3) O16 0.043(4) 0.021(3) 0.043(4) 0.006(3) -0.010(3) 0.000(3) O21 0.032(3) 0.029(3) 0.030(3) -0.006(2) -0.005(3) 0.004(3) O22 0.023(3) 0.033(3) 0.026(3) 0.003(2) 0.000(2) 0.000(2) O23 0.040(4) 0.056(4) 0.028(3) 0.011(3) -0.007(3) -0.023(3) O24 0.029(3) 0.028(3) 0.040(4) 0.005(3) -0.005(3) -0.007(3) O25 0.036(4) 0.033(3) 0.039(4) 0.000(3) -0.003(3) -0.010(3) O26 0.037(4) 0.025(3) 0.050(4) -0.010(3) -0.008(3) 0.002(3) O31 0.070(5) 0.044(4) 0.051(5) 0.014(4) -0.019(4) -0.027(4) O32 0.042(4) 0.045(4) 0.029(3) 0.005(3) -0.001(3) -0.008(3) O33 0.063(5) 0.061(5) 0.023(3) 0.001(3) -0.006(3) -0.028(4) O34 0.032(4) 0.057(4) 0.032(4) -0.004(3) -0.008(3) -0.005(3) O35 0.041(4) 0.059(5) 0.056(5) 0.019(4) -0.017(4) -0.015(4) O36 0.032(4) 0.042(4) 0.050(4) 0.013(3) 0.000(3) -0.006(3) C101 0.049(6) 0.043(5) 0.025(5) 0.002(4) -0.006(4) -0.015(5) C102 0.036(5) 0.043(5) 0.025(4) 0.009(4) -0.004(4) -0.005(4) C103 0.036(5) 0.036(5) 0.036(5) 0.009(4) -0.020(4) -0.008(4) C104 0.025(5) 0.055(6) 0.044(6) 0.015(5) -0.007(4) -0.010(4) C105 0.023(4) 0.051(6) 0.035(5) -0.007(4) 0.005(4) -0.008(4) C106 0.035(5) 0.058(6) 0.024(4) -0.002(4) 0.005(4) -0.018(5) C107 0.043(6) 0.040(5) 0.031(5) -0.010(4) 0.010(4) -0.014(4) C108 0.027(5) 0.039(5) 0.039(5) -0.006(4) 0.014(4) -0.004(4) C109 0.021(4) 0.041(5) 0.052(6) -0.001(4) -0.002(4) -0.004(4) C110 0.036(5) 0.049(6) 0.042(6) -0.006(5) -0.001(4) -0.022(5) C111 0.040(5) 0.038(5) 0.024(4) -0.002(4) -0.004(4) -0.015(4) C112 0.036(5) 0.036(5) 0.027(4) -0.003(4) -0.003(4) -0.004(4) C113 0.061(7) 0.035(5) 0.037(5) -0.017(4) 0.014(5) -0.020(5) C114 0.065(7) 0.036(5) 0.045(6) -0.009(5) 0.009(5) -0.011(5) C115 0.061(7) 0.029(5) 0.066(8) -0.004(5) -0.007(6) 0.011(5) C116 0.062(7) 0.020(5) 0.058(7) -0.003(4) -0.010(6) 0.008(5) C117 0.047(6) 0.029(5) 0.034(5) 0.013(4) -0.015(4) -0.008(4) C118 0.046(6) 0.046(6) 0.027(5) 0.011(4) -0.014(4) -0.019(5) C201 0.033(5) 0.036(5) 0.044(6) 0.004(4) -0.014(4) -0.008(4) C202 0.034(5) 0.026(4) 0.048(6) -0.005(4) -0.012(4) 0.007(4) C203 0.021(4) 0.036(5) 0.041(5) -0.014(4) 0.003(4) 0.001(4) C204 0.033(5) 0.048(6) 0.032(5) -0.005(4) 0.004(4) -0.013(4) C205 0.039(5) 0.039(5) 0.023(4) 0.009(4) -0.009(4) -0.004(4) C206 0.037(5) 0.031(5) 0.031(5) 0.003(4) -0.012(4) -0.001(4) C207 0.055(7) 0.044(6) 0.050(6) 0.020(5) -0.025(5) -0.023(5) C208 0.053(7) 0.063(7) 0.036(5) 0.021(5) -0.015(5) -0.031(6) C209 0.036(5) 0.049(6) 0.036(5) 0.013(4) 0.001(4) -0.013(4) C210 0.040(5) 0.040(5) 0.038(5) 0.001(4) 0.002(4) -0.018(4) C211 0.040(5) 0.043(5) 0.036(5) -0.004(4) -0.009(4) -0.016(4) C212 0.031(5) 0.039(5) 0.042(5) 0.001(4) -0.007(4) -0.007(4) C213 0.040(6) 0.060(7) 0.027(5) -0.004(4) -0.003(4) -0.022(5) C214 0.037(5) 0.033(5) 0.033(5) -0.009(4) 0.002(4) -0.007(4) C215 0.044(6) 0.026(4) 0.040(5) -0.001(4) -0.009(4) -0.009(4) C216 0.048(6) 0.022(4) 0.050(6) -0.010(4) -0.005(5) -0.002(4) C217 0.042(6) 0.028(5) 0.059(7) -0.002(4) -0.014(5) 0.004(4) C218 0.046(6) 0.024(4) 0.044(6) 0.000(4) -0.012(5) 0.002(4) C301 0.096(10) 0.072(9) 0.049(7) 0.017(6) -0.035(7) -0.057(8) C302 0.112(12) 0.049(7) 0.050(7) 0.006(5) -0.029(7) -0.045(7) C303 0.045(6) 0.029(5) 0.055(6) 0.009(4) -0.004(5) -0.004(4) C304 0.054(6) 0.037(5) 0.038(5) 0.008(4) 0.005(5) -0.009(5) C305 0.059(7) 0.056(7) 0.027(5) 0.003(5) -0.002(5) -0.006(5) C306 0.059(7) 0.053(6) 0.024(5) 0.005(4) -0.010(5) -0.006(5) C307 0.099(11) 0.069(8) 0.043(7) -0.009(6) -0.032(7) -0.027(8) C308 0.068(8) 0.069(8) 0.021(5) -0.004(5) -0.002(5) -0.011(6) C309 0.044(6) 0.048(6) 0.042(6) -0.007(5) 0.007(5) -0.009(5) C310 0.035(5) 0.045(6) 0.049(6) -0.007(5) 0.004(5) -0.005(4) C311 0.039(6) 0.065(7) 0.045(6) -0.002(5) -0.012(5) -0.016(5) C312 0.043(6) 0.065(7) 0.041(6) -0.016(5) -0.012(5) -0.015(5) C313 0.066(8) 0.062(7) 0.041(6) 0.022(5) -0.028(6) -0.026(6) C314 0.041(6) 0.087(10) 0.062(8) 0.025(7) -0.025(6) -0.022(6) C315 0.033(5) 0.059(7) 0.049(6) 0.026(5) 0.003(5) 0.003(5) C316 0.039(6) 0.047(6) 0.056(7) 0.020(5) 0.013(5) 0.006(5) C317 0.051(7) 0.045(6) 0.052(7) -0.012(5) 0.015(5) -0.013(5) C318 0.054(7) 0.059(7) 0.035(6) -0.013(5) 0.002(5) -0.010(6) _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 Sn2 2.9295(8) . ? Sn1 Sn5 2.9405(8) . ? Sn1 Sn3 2.9515(9) . ? Sn1 Sn4 2.9581(8) . ? Sn3 Sn7 2.9490(8) . ? Sn3 Sn6 2.9561(8) . ? Sn3 Sn4 3.1688(9) . ? Sn3 Sn2 3.2641(8) . ? Sn4 Sn8 2.9543(8) . ? Sn4 Sn7 2.9603(9) . ? Sn4 Sn5 3.2167(8) . ? Sn5 Sn9 2.9316(9) . ? Sn5 Sn8 2.9442(9) . ? Sn5 Sn2 3.1787(9) . ? Sn2 Sn9 2.8955(8) . ? Sn2 Sn6 2.9420(9) . ? Sn7 Zn1 2.7702(12) . ? Sn7 Sn6 3.1094(8) . ? Sn7 Sn8 3.1471(8) . ? Sn8 Zn1 2.8095(13) . ? Sn8 Sn9 3.1739(8) . ? Sn9 Zn1 2.7776(13) . ? Sn9 Sn6 3.1321(8) . ? Sn6 Zn1 2.8066(13) . ? Zn1 C1 2.014(11) . ? C1 C2 1.461(17) . ? C1 C3 1.557(11) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? K1 O12 2.7110 . ? K1 O11 2.7388 . ? K1 O14 2.7509 . ? K1 O13 2.7770 . ? K1 O15 2.7842 . ? K1 O16 2.7940 . ? K1 N12 2.9603 . ? K1 N11 3.0203 . ? K1 C103 3.255 . ? K1 C108 3.331 . ? K1 C109 3.389 . ? K1 C104 3.530 . ? K2 O26 2.8041 . ? K2 O24 2.8144 . ? K2 O23 2.8167 . ? K2 O21 2.8289 . ? K2 O22 2.8448 . ? K2 O25 2.8940 . ? K2 N21 3.0292 . ? K2 N22 3.0440 . ? K3 O35 2.7702 . ? K3 O34 2.8329 . ? K3 O33 2.8560 . ? K3 O32 2.8797 . ? K3 O31 2.8827 . ? K3 O36 2.8979 . ? K3 N31 3.0023 . ? K3 N32 3.0049 . ? N11 C101 1.4690 . ? N11 C107 1.469 . ? N11 C113 1.471 . ? N12 C112 1.460 . ? N12 C118 1.479 . ? N12 C106 1.480 . ? N21 C207 1.466 . ? N21 C213 1.470 . ? N21 C201 1.485 . ? N22 C206 1.448 . ? N22 C218 1.470 . ? N22 C212 1.471 . ? N31 C313 1.459 . ? N31 C301 1.467 . ? N31 C307 1.493 . ? N32 C318 1.451 . ? N32 C312 1.484 . ? N32 C306 1.501 . ? O11 C103 1.403 . ? O11 C102 1.433 . ? O12 C105 1.405 . ? O12 C104 1.441 . ? O13 C108 1.437 . ? O13 C109 1.447 . ? O14 C110 1.415 . ? O14 C111 1.427 . ? O15 C115 1.411 . ? O15 C114 1.424 . ? O16 C117 1.427 . ? O16 C116 1.430 . ? O21 C203 1.432 . ? O21 C202 1.439 . ? O22 C204 1.424 . ? O22 C205 1.429 . ? O23 C208 1.417 . ? O23 C209 1.431 . ? O24 C211 1.427 . ? O24 C210 1.433 . ? O25 C214 1.397 . ? O25 C215 1.440 . ? O26 C216 1.415 . ? O26 C217 1.453 . ? O31 C303 1.382 . ? O31 C302 1.447 . ? O32 C304 1.411 . ? O32 C305 1.416 . ? O33 C309 1.414 . ? O33 C308 1.436 . ? O34 C310 1.417 . ? O34 C311 1.426 . ? O35 C314 1.401 . ? O35 C315 1.418 . ? O36 C316 1.415 . ? O36 C317 1.417 . ? C101 C102 1.501 . ? C101 H10I 0.9900 . ? C101 H10J 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.512(14) . ? C103 H10A 0.9900 . ? C103 H10B 0.9900 . ? C104 H10K 0.9900 . ? C104 H10L 0.9900 . ? C105 C106 1.492(14) . ? C105 H10E 0.9900 . ? C105 H10F 0.9900 . ? C106 H10G 0.9900 . ? C106 H10H 0.9900 . ? C107 C108 1.497(14) . ? C107 H10O 0.9900 . ? C107 H10P 0.9900 . ? C108 H10M 0.9900 . ? C108 H10N 0.9900 . ? C109 C110 1.502(14) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11I 0.9900 . ? C110 H11J 0.9900 . ? C111 C112 1.506(13) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? C112 H11A 0.9900 . ? C112 H11B 0.9900 . ? C113 C114 1.497(17) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11O 0.9900 . ? C114 H11P 0.9900 . ? C115 C116 1.514(17) . ? C115 H11Q 0.9900 . ? C115 H11R 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.497(14) . ? C117 H11K 0.9900 . ? C117 H11L 0.9900 . ? C118 H11C 0.9900 . ? C118 H11D 0.9900 . ? C201 C202 1.497(14) . ? C201 H20G 0.9900 . ? C201 H20H 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.487(14) . ? C203 H20K 0.9900 . ? C203 H20L 0.9900 . ? C204 H20I 0.9900 . ? C204 H20J 0.9900 . ? C205 C206 1.508(13) . ? C205 H20E 0.9900 . ? C205 H20F 0.9900 . ? C206 H20A 0.9900 . ? C206 H20B 0.9900 . ? C207 C208 1.515(16) . ? C207 H20Q 0.9900 . ? C207 H20R 0.9900 . ? C208 H20M 0.9900 . ? C208 H20N 0.9900 . ? C209 C210 1.477(14) . ? C209 H20O 0.9900 . ? C209 H20P 0.9900 . ? C210 H21O 0.9900 . ? C210 H21P 0.9900 . ? C211 C212 1.499(13) . ? C211 H21Q 0.9900 . ? C211 H21R 0.9900 . ? C212 H21M 0.9900 . ? C212 H21N 0.9900 . ? C213 C214 1.521(14) . ? C213 H21A 0.9900 . ? C213 H21B 0.9900 . ? C214 H21C 0.9900 . ? C214 H21D 0.9900 . ? C215 C216 1.492(14) . ? C215 H21E 0.9900 . ? C215 H21F 0.9900 . ? C216 H21K 0.9900 . ? C216 H21L 0.9900 . ? C217 C218 1.500(14) . ? C217 H21I 0.9900 . ? C217 H21J 0.9900 . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C301 C302 1.526(17) . ? C301 H30G 0.9900 . ? C301 H30H 0.9900 . ? C302 H30I 0.9900 . ? C302 H30J 0.9900 . ? C303 C304 1.481(15) . ? C303 H30C 0.9900 . ? C303 H30D 0.9900 . ? C304 H30E 0.9900 . ? C304 H30F 0.9900 . ? C305 C306 1.489(16) . ? C305 H30Q 0.9900 . ? C305 H30R 0.9900 . ? C306 H30A 0.9900 . ? C306 H30B 0.9900 . ? C307 C308 1.508(19) . ? C307 H30O 0.9900 . ? C307 H30P 0.9900 . ? C308 H30M 0.9900 . ? C308 H30N 0.9900 . ? C309 C310 1.476(15) . ? C309 H30K 0.9900 . ? C309 H30L 0.9900 . ? C310 H31O 0.9900 . ? C310 H31P 0.9900 . ? C311 C312 1.501(16) . ? C311 H31Q 0.9900 . ? C311 H31R 0.9900 . ? C312 H31M 0.9900 . ? C312 H31N 0.9900 . ? C313 C314 1.510(19) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31K 0.9900 . ? C314 H31L 0.9900 . ? C315 C316 1.465(18) . ? C315 H31C 0.9900 . ? C315 H31D 0.9900 . ? C316 H31I 0.9900 . ? C316 H31J 0.9900 . ? C317 C318 1.520(16) . ? C317 H31E 0.9900 . ? C317 H31F 0.9900 . ? C318 H31A 0.9900 . ? C318 H31B 0.9900 . ? N1S C1S 1.41(4) . ? C1S N2S 1.37(6) . ? C1S C1S 1.46(5) 2_765 ? 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 Sn2 Sn1 Sn5 65.57(2) . . ? Sn2 Sn1 Sn3 67.42(2) . . ? Sn5 Sn1 Sn3 100.89(2) . . ? Sn2 Sn1 Sn4 100.56(2) . . ? Sn5 Sn1 Sn4 66.09(2) . . ? Sn3 Sn1 Sn4 64.85(2) . . ? Sn7 Sn3 Sn1 110.14(2) . . ? Sn7 Sn3 Sn6 63.55(2) . . ? Sn1 Sn3 Sn6 108.29(2) . . ? Sn7 Sn3 Sn4 57.744(19) . . ? Sn1 Sn3 Sn4 57.67(2) . . ? Sn6 Sn3 Sn4 102.07(2) . . ? Sn7 Sn3 Sn2 100.54(2) . . ? Sn1 Sn3 Sn2 55.968(19) . . ? Sn6 Sn3 Sn2 56.193(18) . . ? Sn4 Sn3 Sn2 89.48(2) . . ? Sn8 Sn4 Sn1 109.42(2) . . ? Sn8 Sn4 Sn7 64.29(2) . . ? Sn1 Sn4 Sn7 109.65(2) . . ? Sn8 Sn4 Sn3 103.35(2) . . ? Sn1 Sn4 Sn3 57.47(2) . . ? Sn7 Sn4 Sn3 57.400(19) . . ? Sn8 Sn4 Sn5 56.802(19) . . ? Sn1 Sn4 Sn5 56.692(19) . . ? Sn7 Sn4 Sn5 101.34(2) . . ? Sn3 Sn4 Sn5 90.70(2) . . ? Sn9 Sn5 Sn1 109.14(3) . . ? Sn9 Sn5 Sn8 65.39(2) . . ? Sn1 Sn5 Sn8 110.19(2) . . ? Sn9 Sn5 Sn2 56.397(19) . . ? Sn1 Sn5 Sn2 57.047(19) . . ? Sn8 Sn5 Sn2 102.92(2) . . ? Sn9 Sn5 Sn4 102.09(2) . . ? Sn1 Sn5 Sn4 57.216(19) . . ? Sn8 Sn5 Sn4 57.104(19) . . ? Sn2 Sn5 Sn4 90.16(2) . . ? Sn9 Sn2 Sn1 110.45(3) . . ? Sn9 Sn2 Sn6 64.89(2) . . ? Sn1 Sn2 Sn6 109.26(2) . . ? Sn9 Sn2 Sn5 57.49(2) . . ? Sn1 Sn2 Sn5 57.380(19) . . ? Sn6 Sn2 Sn5 102.40(2) . . ? Sn9 Sn2 Sn3 102.14(2) . . ? Sn1 Sn2 Sn3 56.608(19) . . ? Sn6 Sn2 Sn3 56.604(19) . . ? Sn5 Sn2 Sn3 89.66(2) . . ? Zn1 Sn7 Sn3 110.21(3) . . ? Zn1 Sn7 Sn4 109.20(3) . . ? Sn3 Sn7 Sn4 64.86(2) . . ? Zn1 Sn7 Sn6 56.67(3) . . ? Sn3 Sn7 Sn6 58.338(19) . . ? Sn4 Sn7 Sn6 103.40(2) . . ? Zn1 Sn7 Sn8 56.26(3) . . ? Sn3 Sn7 Sn8 104.00(2) . . ? Sn4 Sn7 Sn8 57.762(19) . . ? Sn6 Sn7 Sn8 91.17(2) . . ? Zn1 Sn8 Sn5 107.76(3) . . ? Zn1 Sn8 Sn4 108.29(3) . . ? Sn5 Sn8 Sn4 66.09(2) . . ? Zn1 Sn8 Sn7 55.08(3) . . ? Sn5 Sn8 Sn7 103.36(2) . . ? Sn4 Sn8 Sn7 57.946(19) . . ? Zn1 Sn8 Sn9 54.91(3) . . ? Sn5 Sn8 Sn9 57.115(19) . . ? Sn4 Sn8 Sn9 102.60(2) . . ? Sn7 Sn8 Sn9 88.56(2) . . ? Zn1 Sn9 Sn2 110.13(3) . . ? Zn1 Sn9 Sn5 108.99(3) . . ? Sn2 Sn9 Sn5 66.11(2) . . ? Zn1 Sn9 Sn6 56.32(3) . . ? Sn2 Sn9 Sn6 58.27(2) . . ? Sn5 Sn9 Sn6 103.77(2) . . ? Zn1 Sn9 Sn8 55.86(3) . . ? Sn2 Sn9 Sn8 104.17(2) . . ? Sn5 Sn9 Sn8 57.50(2) . . ? Sn6 Sn9 Sn8 90.26(2) . . ? Zn1 Sn6 Sn2 108.00(3) . . ? Zn1 Sn6 Sn3 109.00(3) . . ? Sn2 Sn6 Sn3 67.20(2) . . ? Zn1 Sn6 Sn7 55.56(3) . . ? Sn2 Sn6 Sn7 104.40(2) . . ? Sn3 Sn6 Sn7 58.117(19) . . ? Zn1 Sn6 Sn9 55.45(3) . . ? Sn2 Sn6 Sn9 56.836(19) . . ? Sn3 Sn6 Sn9 103.95(2) . . ? Sn7 Sn6 Sn9 90.00(2) . . ? C1 Zn1 Sn7 133.1(3) . . ? C1 Zn1 Sn9 121.5(3) . . ? Sn7 Zn1 Sn9 105.40(4) . . ? C1 Zn1 Sn6 129.2(4) . . ? Sn7 Zn1 Sn6 67.77(3) . . ? Sn9 Zn1 Sn6 68.23(3) . . ? C1 Zn1 Sn8 124.9(4) . . ? Sn7 Zn1 Sn8 68.66(3) . . ? Sn9 Zn1 Sn8 69.23(3) . . ? Sn6 Zn1 Sn8 105.46(4) . . ? C2 C1 C3 110.1(9) . . ? C2 C1 Zn1 112.7(9) . . ? C3 C1 Zn1 109.0(6) . . ? C2 C1 H1 108.3 . . ? C3 C1 H1 108.3 . . ? Zn1 C1 H1 108.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O12 K1 O11 63.9 . . ? O12 K1 O14 97.9 . . ? O11 K1 O14 96.5 . . ? O12 K1 O13 138.2 . . ? O11 K1 O13 81.7 . . ? O14 K1 O13 61.6 . . ? O12 K1 O15 123.0 . . ? O11 K1 O15 115.6 . . ? O14 K1 O15 135.6 . . ? O13 K1 O15 92.1 . . ? O12 K1 O16 104.4 . . ? O11 K1 O16 164.9 . . ? O14 K1 O16 94.6 . . ? O13 K1 O16 112.8 . . ? O15 K1 O16 61.3 . . ? O12 K1 N12 61.3 . . ? O11 K1 N12 115.6 . . ? O14 K1 N12 61.5 . . ? O13 K1 N12 121.9 . . ? O15 K1 N12 121.3 . . ? O16 K1 N12 61.6 . . ? O12 K1 N11 114.4 . . ? O11 K1 N11 61.6 . . ? O14 K1 N11 121.5 . . ? O13 K1 N11 61.8 . . ? O15 K1 N11 59.5 . . ? O16 K1 N11 120.1 . . ? N12 K1 N11 175.5 . . ? O12 K1 C103 46.26 . . ? O11 K1 C103 25.25 . . ? O14 K1 C103 113.95 . . ? O13 K1 C103 105.99 . . ? O15 K1 C103 107.30 . . ? O16 K1 C103 139.62 . . ? N12 K1 C103 106.56 . . ? N11 K1 C103 69.39 . . ? O12 K1 C108 153.22 . . ? O11 K1 C108 89.33 . . ? O14 K1 C108 84.20 . . ? O13 K1 C108 25.17 . . ? O15 K1 C108 67.31 . . ? O16 K1 C108 102.01 . . ? N12 K1 C108 138.52 . . ? N11 K1 C108 45.91 . . ? C103 K1 C108 108.5 . . ? O12 K1 C109 139.57 . . ? O11 K1 C109 101.00 . . ? O14 K1 C109 44.21 . . ? O13 K1 C109 24.69 . . ? O15 K1 C109 97.44 . . ? O16 K1 C109 94.14 . . ? N12 K1 C109 99.35 . . ? N11 K1 C109 84.77 . . ? C103 K1 C109 126.2 . . ? C108 K1 C109 41.0 . . ? O12 K1 C104 22.09 . . ? O11 K1 C104 42.07 . . ? O14 K1 C104 101.58 . . ? O13 K1 C104 121.05 . . ? O15 K1 C104 122.9 . . ? O16 K1 C104 125.22 . . ? N12 K1 C104 81.22 . . ? N11 K1 C104 94.73 . . ? C103 K1 C104 25.3 . . ? C108 K1 C104 131.3 . . ? C109 K1 C104 132.7 . . ? O26 K2 O24 97.8 . . ? O26 K2 O23 136.1 . . ? O24 K2 O23 60.5 . . ? O26 K2 O21 117.9 . . ? O24 K2 O21 138.6 . . ? O23 K2 O21 100.0 . . ? O26 K2 O22 95.1 . . ? O24 K2 O22 98.7 . . ? O23 K2 O22 124.0 . . ? O21 K2 O22 60.2 . . ? O26 K2 O25 59.8 . . ? O24 K2 O25 122.8 . . ? O23 K2 O25 98.2 . . ? O21 K2 O25 94.4 . . ? O22 K2 O25 132.4 . . ? O26 K2 N21 118.9 . . ? O24 K2 N21 120.6 . . ? O23 K2 N21 60.7 . . ? O21 K2 N21 60.6 . . ? O22 K2 N21 120.3 . . ? O25 K2 N21 59.6 . . ? O26 K2 N22 60.5 . . ? O24 K2 N22 59.8 . . ? O23 K2 N22 119.8 . . ? O21 K2 N22 119.4 . . ? O22 K2 N22 59.9 . . ? O25 K2 N22 119.8 . . ? N21 K2 N22 179.4 . . ? O35 K3 O34 128.4 . . ? O35 K3 O33 102.5 . . ? O34 K3 O33 59.6 . . ? O35 K3 O32 128.0 . . ? O34 K3 O32 98.3 . . ? O33 K3 O32 122.6 . . ? O35 K3 O31 93.6 . . ? O34 K3 O31 133.8 . . ? O33 K3 O31 97.5 . . ? O32 K3 O31 58.6 . . ? O35 K3 O36 59.4 . . ? O34 K3 O36 102.1 . . ? O33 K3 O36 140.3 . . ? O32 K3 O36 93.2 . . ? O31 K3 O36 117.4 . . ? O35 K3 N31 61.0 . . ? O34 K3 N31 120.1 . . ? O33 K3 N31 60.8 . . ? O32 K3 N31 118.1 . . ? O31 K3 N31 59.8 . . ? O36 K3 N31 119.9 . . ? O35 K3 N32 120.0 . . ? O34 K3 N32 61.0 . . ? O33 K3 N32 120.0 . . ? O32 K3 N32 59.9 . . ? O31 K3 N32 118.1 . . ? O36 K3 N32 60.8 . . ? N31 K3 N32 177.9 . . ? C101 N11 C107 112.1 . . ? C101 N11 C113 110.8 . . ? C107 N11 C113 111.9 . . ? C101 N11 K1 109.3 . . ? C107 N11 K1 105.4 . . ? C113 N11 K1 106.9 . . ? C112 N12 C118 110.7 . . ? C112 N12 C106 110.5 . . ? C118 N12 C106 109.1 . . ? C112 N12 K1 108.2 . . ? C118 N12 K1 110.0 . . ? C106 N12 K1 108.2 . . ? C207 N21 C213 109.7 . . ? C207 N21 C201 109.2 . . ? C213 N21 C201 110.3 . . ? C207 N21 K2 107.9 . . ? C213 N21 K2 109.8 . . ? C201 N21 K2 109.9 . . ? C206 N22 C218 110.3 . . ? C206 N22 C212 110.0 . . ? C218 N22 C212 108.9 . . ? C206 N22 K2 109.9 . . ? C218 N22 K2 108.4 . . ? C212 N22 K2 109.2 . . ? C313 N31 C301 109.1 . . ? C313 N31 C307 110.9 . . ? C301 N31 C307 110.0 . . ? C313 N31 K3 107.2 . . ? C301 N31 K3 110.7 . . ? C307 N31 K3 108.9 . . ? C318 N32 C312 110.7 . . ? C318 N32 C306 109.2 . . ? C312 N32 C306 108.2 . . ? C318 N32 K3 110.3 . . ? C312 N32 K3 107.9 . . ? C306 N32 K3 110.5 . . ? C103 O11 C102 113.7 . . ? C103 O11 K1 98.4 . . ? C102 O11 K1 116.8 . . ? C105 O12 C104 112.3 . . ? C105 O12 K1 120.4 . . ? C104 O12 K1 112.9 . . ? C108 O13 C109 109.4 . . ? C108 O13 K1 99.5 . . ? C109 O13 K1 102.0 . . ? C110 O14 C111 114.1 . . ? C110 O14 K1 115.9 . . ? C111 O14 K1 118.5 . . ? C115 O15 C114 112.3 . . ? C115 O15 K1 111.4 . . ? C114 O15 K1 123.5 . . ? C117 O16 C116 111.0 . . ? C117 O16 K1 112.4 . . ? C116 O16 K1 115.2 . . ? C203 O21 C202 112.1 . . ? C203 O21 K2 114.9 . . ? C202 O21 K2 115.2 . . ? C204 O22 C205 110.4 . . ? C204 O22 K2 112.8 . . ? C205 O22 K2 116.2 . . ? C208 O23 C209 110.8 . . ? C208 O23 K2 116.8 . . ? C209 O23 K2 113.1 . . ? C211 O24 C210 110.8 . . ? C211 O24 K2 116.6 . . ? C210 O24 K2 115.3 . . ? C214 O25 C215 112.0 . . ? C214 O25 K2 117.0 . . ? C215 O25 K2 110.5 . . ? C216 O26 C217 110.4 . . ? C216 O26 K2 117.1 . . ? C217 O26 K2 114.6 . . ? C303 O31 C302 112.6 . . ? C303 O31 K3 116.5 . . ? C302 O31 K3 115.3 . . ? C304 O32 C305 112.8 . . ? C304 O32 K3 114.6 . . ? C305 O32 K3 116.2 . . ? C309 O33 C308 111.6 . . ? C309 O33 K3 112.5 . . ? C308 O33 K3 113.7 . . ? C310 O34 C311 112.0 . . ? C310 O34 K3 114.4 . . ? C311 O34 K3 115.7 . . ? C314 O35 C315 112.8 . . ? C314 O35 K3 119.9 . . ? C315 O35 K3 119.8 . . ? C316 O36 C317 111.6 . . ? C316 O36 K3 112.2 . . ? C317 O36 K3 109.1 . . ? N11 C101 C102 112.6 . . ? N11 C101 H10I 109.1 . . ? C102 C101 H10I 109.1 . . ? N11 C101 H10J 109.1 . . ? C102 C101 H10J 109.1 . . ? H10I C101 H10J 107.8 . . ? O11 C102 C101 113.4 . . ? O11 C102 H10C 108.9 . . ? C101 C102 H10C 108.9 . . ? O11 C102 H10D 108.9 . . ? C101 C102 H10D 108.9 . . ? H10C C102 H10D 107.7 . . ? O11 C103 C104 108.6 . . ? O11 C103 K1 56.4 . . ? C104 C103 K1 87.6 . . ? O11 C103 H10A 110.0 . . ? C104 C103 H10A 110.0 . . ? K1 C103 H10A 69.6 . . ? O11 C103 H10B 110.0 . . ? C104 C103 H10B 110.0 . . ? K1 C103 H10B 161.4 . . ? H10A C103 H10B 108.4 . . ? O12 C104 C103 108.4 . . ? O12 C104 K1 45.0 . . ? C103 C104 K1 67.1 . . ? O12 C104 H10K 110.0 . . ? C103 C104 H10K 110.0 . . ? K1 C104 H10K 108.3 . . ? O12 C104 H10L 110.0 . . ? C103 C104 H10L 110.0 . . ? K1 C104 H10L 141.5 . . ? H10K C104 H10L 108.4 . . ? O12 C105 C106 110.4 . . ? O12 C105 H10E 109.6 . . ? C106 C105 H10E 109.6 . . ? O12 C105 H10F 109.6 . . ? C106 C105 H10F 109.6 . . ? H10E C105 H10F 108.1 . . ? N12 C106 C105 113.2 . . ? N12 C106 H10G 108.9 . . ? C105 C106 H10G 108.9 . . ? N12 C106 H10H 108.9 . . ? C105 C106 H10H 108.9 . . ? H10G C106 H10H 107.7 . . ? N11 C107 C108 114.4 . . ? N11 C107 H10O 108.7 . . ? C108 C107 H10O 108.7 . . ? N11 C107 H10P 108.7 . . ? C108 C107 H10P 108.7 . . ? H10O C107 H10P 107.6 . . ? O13 C108 C107 108.8 . . ? O13 C108 K1 55.3 . . ? C107 C108 K1 91.7 . . ? O13 C108 H10M 109.9 . . ? C107 C108 H10M 109.9 . . ? K1 C108 H10M 67.6 . . ? O13 C108 H10N 109.9 . . ? C107 C108 H10N 109.9 . . ? K1 C108 H10N 157.6 . . ? H10M C108 H10N 108.3 . . ? O13 C109 C110 107.1 . . ? O13 C109 K1 53.3 . . ? C110 C109 K1 85.7 . . ? O13 C109 H10Q 110.3 . . ? C110 C109 H10Q 110.3 . . ? K1 C109 H10Q 161.0 . . ? O13 C109 H10R 110.3 . . ? C110 C109 H10R 110.3 . . ? K1 C109 H10R 73.5 . . ? H10Q C109 H10R 108.5 . . ? O14 C110 C109 109.6 . . ? O14 C110 H11I 109.7 . . ? C109 C110 H11I 109.7 . . ? O14 C110 H11J 109.7 . . ? C109 C110 H11J 109.7 . . ? H11I C110 H11J 108.2 . . ? O14 C111 C112 108.7 . . ? O14 C111 H11E 110.0 . . ? C112 C111 H11E 110.0 . . ? O14 C111 H11F 110.0 . . ? C112 C111 H11F 110.0 . . ? H11E C111 H11F 108.3 . . ? N12 C112 C111 114.6 . . ? N12 C112 H11A 108.6 . . ? C111 C112 H11A 108.6 . . ? N12 C112 H11B 108.6 . . ? C111 C112 H11B 108.6 . . ? H11A C112 H11B 107.6 . . ? N11 C113 C114 114.0(8) . . ? N11 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? N11 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? O15 C114 C113 108.7 . . ? O15 C114 H11O 109.9 . . ? C113 C114 H11O 109.9 . . ? O15 C114 H11P 109.9 . . ? C113 C114 H11P 109.9 . . ? H11O C114 H11P 108.3 . . ? O15 C115 C116 109.4 . . ? O15 C115 H11Q 109.8 . . ? C116 C115 H11Q 109.8 . . ? O15 C115 H11R 109.8 . . ? C116 C115 H11R 109.8 . . ? H11Q C115 H11R 108.2 . . ? O16 C116 C115 108.6 . . ? O16 C116 H11M 110.0 . . ? C115 C116 H11M 110.0 . . ? O16 C116 H11N 110.0 . . ? C115 C116 H11N 110.0 . . ? H11M C116 H11N 108.4 . . ? O16 C117 C118 110.2 . . ? O16 C117 H11K 109.6 . . ? C118 C117 H11K 109.6 . . ? O16 C117 H11L 109.6 . . ? C118 C117 H11L 109.6 . . ? H11K C117 H11L 108.1 . . ? N12 C118 C117 112.4 . . ? N12 C118 H11C 109.1 . . ? C117 C118 H11C 109.1 . . ? N12 C118 H11D 109.1 . . ? C117 C118 H11D 109.1 . . ? H11C C118 H11D 107.9 . . ? N21 C201 C202 113.3 . . ? N21 C201 H20G 108.9 . . ? C202 C201 H20G 108.9 . . ? N21 C201 H20H 108.9 . . ? C202 C201 H20H 108.9 . . ? H20G C201 H20H 107.7 . . ? O21 C202 C201 110.4 . . ? O21 C202 H20C 109.6 . . ? C201 C202 H20C 109.6 . . ? O21 C202 H20D 109.6 . . ? C201 C202 H20D 109.6 . . ? H20C C202 H20D 108.1 . . ? O21 C203 C204 108.9 . . ? O21 C203 H20K 109.9 . . ? C204 C203 H20K 109.9 . . ? O21 C203 H20L 109.9 . . ? C204 C203 H20L 109.9 . . ? H20K C203 H20L 108.3 . . ? O22 C204 C203 109.8 . . ? O22 C204 H20I 109.7 . . ? C203 C204 H20I 109.7 . . ? O22 C204 H20J 109.7 . . ? C203 C204 H20J 109.7 . . ? H20I C204 H20J 108.2 . . ? O22 C205 C206 109.6 . . ? O22 C205 H20E 109.8 . . ? C206 C205 H20E 109.8 . . ? O22 C205 H20F 109.8 . . ? C206 C205 H20F 109.8 . . ? H20E C205 H20F 108.2 . . ? N22 C206 C205 113.8 . . ? N22 C206 H20A 108.8 . . ? C205 C206 H20A 108.8 . . ? N22 C206 H20B 108.8 . . ? C205 C206 H20B 108.8 . . ? H20A C206 H20B 107.7 . . ? N21 C207 C208 113.9 . . ? N21 C207 H20Q 108.8 . . ? C208 C207 H20Q 108.8 . . ? N21 C207 H20R 108.8 . . ? C208 C207 H20R 108.8 . . ? H20Q C207 H20R 107.7 . . ? O23 C208 C207 108.9 . . ? O23 C208 H20M 109.9 . . ? C207 C208 H20M 109.9 . . ? O23 C208 H20N 109.9 . . ? C207 C208 H20N 109.9 . . ? H20M C208 H20N 108.3 . . ? O23 C209 C210 110.2 . . ? O23 C209 H20O 109.6 . . ? C210 C209 H20O 109.6 . . ? O23 C209 H20P 109.6 . . ? C210 C209 H20P 109.6 . . ? H20O C209 H20P 108.1 . . ? O24 C210 C209 109.3 . . ? O24 C210 H21O 109.8 . . ? C209 C210 H21O 109.8 . . ? O24 C210 H21P 109.8 . . ? C209 C210 H21P 109.8 . . ? H21O C210 H21P 108.3 . . ? O24 C211 C212 108.2 . . ? O24 C211 H21Q 110.1 . . ? C212 C211 H21Q 110.1 . . ? O24 C211 H21R 110.1 . . ? C212 C211 H21R 110.1 . . ? H21Q C211 H21R 108.4 . . ? N22 C212 C211 113.6 . . ? N22 C212 H21M 108.8 . . ? C211 C212 H21M 108.8 . . ? N22 C212 H21N 108.8 . . ? C211 C212 H21N 108.8 . . ? H21M C212 H21N 107.7 . . ? N21 C213 C214 113.1 . . ? N21 C213 H21A 109.0 . . ? C214 C213 H21A 109.0 . . ? N21 C213 H21B 109.0 . . ? C214 C213 H21B 109.0 . . ? H21A C213 H21B 107.8 . . ? O25 C214 C213 109.5 . . ? O25 C214 H21C 109.8 . . ? C213 C214 H21C 109.8 . . ? O25 C214 H21D 109.8 . . ? C213 C214 H21D 109.8 . . ? H21C C214 H21D 108.2 . . ? O25 C215 C216 108.5 . . ? O25 C215 H21E 110.0 . . ? C216 C215 H21E 110.0 . . ? O25 C215 H21F 110.0 . . ? C216 C215 H21F 110.0 . . ? H21E C215 H21F 108.4 . . ? O26 C216 C215 109.0 . . ? O26 C216 H21K 109.9 . . ? C215 C216 H21K 109.9 . . ? O26 C216 H21L 109.9 . . ? C215 C216 H21L 109.9 . . ? H21K C216 H21L 108.3 . . ? O26 C217 C218 107.3 . . ? O26 C217 H21I 110.3 . . ? C218 C217 H21I 110.3 . . ? O26 C217 H21J 110.3 . . ? C218 C217 H21J 110.3 . . ? H21I C217 H21J 108.5 . . ? N22 C218 C217 114.2 . . ? N22 C218 H21G 108.7 . . ? C217 C218 H21G 108.7 . . ? N22 C218 H21H 108.7 . . ? C217 C218 H21H 108.7 . . ? H21G C218 H21H 107.6 . . ? N31 C301 C302 113.0 . . ? N31 C301 H30G 109.0 . . ? C302 C301 H30G 109.0 . . ? N31 C301 H30H 109.0 . . ? C302 C301 H30H 109.0 . . ? H30G C301 H30H 107.8 . . ? O31 C302 C301 106.2 . . ? O31 C302 H30I 110.5 . . ? C301 C302 H30I 110.5 . . ? O31 C302 H30J 110.5 . . ? C301 C302 H30J 110.5 . . ? H30I C302 H30J 108.7 . . ? O31 C303 C304 111.1 . . ? O31 C303 H30C 109.4 . . ? C304 C303 H30C 109.4 . . ? O31 C303 H30D 109.4 . . ? C304 C303 H30D 109.4 . . ? H30C C303 H30D 108.0 . . ? O32 C304 C303 110.6 . . ? O32 C304 H30E 109.5 . . ? C303 C304 H30E 109.5 . . ? O32 C304 H30F 109.5 . . ? C303 C304 H30F 109.5 . . ? H30E C304 H30F 108.1 . . ? O32 C305 C306 110.0 . . ? O32 C305 H30Q 109.7 . . ? C306 C305 H30Q 109.7 . . ? O32 C305 H30R 109.7 . . ? C306 C305 H30R 109.7 . . ? H30Q C305 H30R 108.2 . . ? C305 C306 N32 112.3 . . ? C305 C306 H30A 109.1 . . ? N32 C306 H30A 109.1 . . ? C305 C306 H30B 109.1 . . ? N32 C306 H30B 109.1 . . ? H30A C306 H30B 107.9 . . ? N31 C307 C308 112.8 . . ? N31 C307 H30O 109.0 . . ? C308 C307 H30O 109.0 . . ? N31 C307 H30P 109.0 . . ? C308 C307 H30P 109.0 . . ? H30O C307 H30P 107.8 . . ? O33 C308 C307 107.7 . . ? O33 C308 H30M 110.2 . . ? C307 C308 H30M 110.2 . . ? O33 C308 H30N 110.2 . . ? C307 C308 H30N 110.2 . . ? H30M C308 H30N 108.5 . . ? O33 C309 C310 108.2 . . ? O33 C309 H30K 110.1 . . ? C310 C309 H30K 110.1 . . ? O33 C309 H30L 110.1 . . ? C310 C309 H30L 110.1 . . ? H30K C309 H30L 108.4 . . ? O34 C310 C309 108.9 . . ? O34 C310 H31O 109.9 . . ? C309 C310 H31O 109.9 . . ? O34 C310 H31P 109.9 . . ? C309 C310 H31P 109.9 . . ? H31O C310 H31P 108.3 . . ? O34 C311 C312 107.6 . . ? O34 C311 H31Q 110.2 . . ? C312 C311 H31Q 110.2 . . ? O34 C311 H31R 110.2 . . ? C312 C311 H31R 110.2 . . ? H31Q C311 H31R 108.5 . . ? N32 C312 C311 115.3 . . ? N32 C312 H31M 108.5 . . ? C311 C312 H31M 108.5 . . ? N32 C312 H31N 108.5 . . ? C311 C312 H31N 108.5 . . ? H31M C312 H31N 107.5 . . ? N31 C313 C314 115.1 . . ? N31 C313 H31G 108.5 . . ? C314 C313 H31G 108.5 . . ? N31 C313 H31H 108.5 . . ? C314 C313 H31H 108.5 . . ? H31G C313 H31H 107.5 . . ? O35 C314 C313 109.9 . . ? O35 C314 H31K 109.7 . . ? C313 C314 H31K 109.7 . . ? O35 C314 H31L 109.7 . . ? C313 C314 H31L 109.7 . . ? H31K C314 H31L 108.2 . . ? O35 C315 C316 111.3 . . ? O35 C315 H31C 109.4 . . ? C316 C315 H31C 109.4 . . ? O35 C315 H31D 109.4 . . ? C316 C315 H31D 109.4 . . ? H31C C315 H31D 108.0 . . ? O36 C316 C315 111.5 . . ? O36 C316 H31I 109.3 . . ? C315 C316 H31I 109.3 . . ? O36 C316 H31J 109.3 . . ? C315 C316 H31J 109.3 . . ? H31I C316 H31J 108.0 . . ? O36 C317 C318 109.9 . . ? O36 C317 H31E 109.7 . . ? C318 C317 H31E 109.7 . . ? O36 C317 H31F 109.7 . . ? C318 C317 H31F 109.7 . . ? H31E C317 H31F 108.2 . . ? N32 C318 C317 112.8 . . ? N32 C318 H31A 109.0 . . ? C317 C318 H31A 109.0 . . ? N32 C318 H31B 109.0 . . ? C317 C318 H31B 109.0 . . ? H31A C318 H31B 107.8 . . ? N2S C1S N1S 128(4) . . ? N2S C1S C1S 110(4) . 2_765 ? N1S C1S C1S 115(4) . 2_765 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.092 _refine_diff_density_min -1.760 _refine_diff_density_rms 0.198 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 700664' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)]6[Pb9Zn(iPr)]2*en ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K-(2,2,2-crypt))6(Pb9Zn(iPr))2*en _chemical_melting_point ? _chemical_formula_moiety '6(C18 H36 K N2 O6), 2(C3 H7 Pb9 Zn), C2 H8 N2' _chemical_formula_sum 'C116 H238 K6 N14 O36 Pb18 Zn2' _chemical_formula_weight 6498.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3940 10.1110 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2840 1.4300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.08810(10) _cell_length_b 25.57220(20) _cell_length_c 27.13480(20) _cell_angle_alpha 112.1484(3) _cell_angle_beta 100.0104(3) _cell_angle_gamma 92.2170(3) _cell_volume 8858.104(116) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark purple/black' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5938 _exptl_absorpt_coefficient_mu 17.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1448 _exptl_absorpt_correction_T_max 0.3349 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54321 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 30777 _reflns_number_gt 23264 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0779P)^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 30777 _refine_ls_number_parameters 1729 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Pb11 Pb 0.61934(3) 0.274257(17) -0.101217(16) 0.02265(10) Uani 1 1 d . . . Pb13 Pb 0.56624(3) 0.338601(16) 0.009988(17) 0.02196(10) Uani 1 1 d . . . Pb14 Pb 0.79257(3) 0.328542(16) -0.005668(16) 0.01817(10) Uani 1 1 d . . . Pb15 Pb 0.73864(3) 0.186118(16) -0.076631(16) 0.01815(10) Uani 1 1 d . . . Pb12 Pb 0.51415(3) 0.199100(17) -0.057813(16) 0.02184(10) Uani 1 1 d . . . Pb17 Pb 0.73430(3) 0.343271(15) 0.102823(15) 0.01787(10) Uani 1 1 d . . . Pb18 Pb 0.85771(3) 0.239854(16) 0.041825(16) 0.01855(10) Uani 1 1 d . . . Pb19 Pb 0.66027(3) 0.148933(15) 0.004974(16) 0.01892(10) Uani 1 1 d . . . Pb16 Pb 0.53914(3) 0.253837(16) 0.065097(16) 0.02042(10) Uani 1 1 d . . . Zn11 Zn 0.72733(9) 0.23544(5) 0.10979(5) 0.0221(3) Uani 1 1 d . . . C11 C 0.7504(7) 0.2134(4) 0.1755(4) 0.015(2) Uani 1 1 d U . . H11 H 0.7297 0.2438 0.2063 0.018 Uiso 1 1 calc R . . C12 C 0.8576(8) 0.2092(5) 0.1930(5) 0.031(3) Uani 1 1 d . . . H12A H 0.8955 0.2454 0.2008 0.047 Uiso 1 1 calc R . . H12B H 0.8790 0.1788 0.1637 0.047 Uiso 1 1 calc R . . H12C H 0.8675 0.2006 0.2257 0.047 Uiso 1 1 calc R . . C13 C 0.6903(8) 0.1585(5) 0.1632(5) 0.033(3) Uani 1 1 d . . . H13A H 0.6217 0.1622 0.1522 0.049 Uiso 1 1 calc R . . H13B H 0.6995 0.1496 0.1957 0.049 Uiso 1 1 calc R . . H13C H 0.7105 0.1279 0.1336 0.049 Uiso 1 1 calc R . . Pb1 Pb 0.34928(3) 0.232493(16) 0.616655(16) 0.01833(10) Uani 1 1 d . . . Pb3 Pb 0.17737(3) 0.173250(15) 0.520490(16) 0.01649(9) Uani 1 1 d . . . Pb4 Pb 0.40647(3) 0.166726(15) 0.507471(16) 0.01641(9) Uani 1 1 d . . . Pb5 Pb 0.45059(3) 0.311185(15) 0.575925(16) 0.01778(10) Uani 1 1 d . . . Pb2 Pb 0.21969(3) 0.314506(15) 0.587556(16) 0.01702(10) Uani 1 1 d . . . Pb7 Pb 0.24267(3) 0.157716(15) 0.412997(15) 0.01547(9) Uani 1 1 d . . . Pb8 Pb 0.43144(3) 0.251601(15) 0.452324(16) 0.01675(9) Uani 1 1 d . . . Pb9 Pb 0.30335(3) 0.351782(15) 0.507131(16) 0.01643(10) Uani 1 1 d . . . Pb6 Pb 0.10861(3) 0.257780(16) 0.469226(16) 0.01751(10) Uani 1 1 d . . . Zn1 Zn 0.24124(9) 0.26265(5) 0.40269(5) 0.0208(3) Uani 1 1 d . . . C1 C 0.2022(8) 0.2820(4) 0.3369(4) 0.023(2) Uani 1 1 d . . . H21 H 0.2142 0.2497 0.3044 0.028 Uiso 1 1 calc R . . C2 C 0.2614(9) 0.3350(5) 0.3423(5) 0.035(3) Uani 1 1 d . . . H22A H 0.3305 0.3297 0.3476 0.053 Uiso 1 1 calc R . . H22B H 0.2499 0.3673 0.3736 0.053 Uiso 1 1 calc R . . H22C H 0.2424 0.3424 0.3093 0.053 Uiso 1 1 calc R . . C3 C 0.0906(8) 0.2883(5) 0.3279(5) 0.029(3) Uani 1 1 d . . . H23A H 0.0540 0.2530 0.3238 0.044 Uiso 1 1 calc R . . H23B H 0.0710 0.2959 0.2950 0.044 Uiso 1 1 calc R . . H23C H 0.0773 0.3199 0.3592 0.044 Uiso 1 1 calc R . . K1 K 0.70799(15) 0.02038(9) 0.32246(9) 0.0153(5) Uani 1 1 d . . . K2 K 0.73475(16) 0.51351(9) 0.81327(9) 0.0171(5) Uani 1 1 d . . . K3 K 0.26638(16) 0.55250(9) 0.59292(9) 0.0191(5) Uani 1 1 d . . . K4 K 0.77292(16) -0.05714(9) -0.10215(9) 0.0189(5) Uani 1 1 d . . . K5 K -0.15346(15) 0.15840(9) 0.63781(9) 0.0172(5) Uani 1 1 d . . . K6 K 0.16147(15) 0.33671(8) -0.12956(9) 0.0146(4) Uani 1 1 d . . . N11 N 0.5520(6) -0.0602(3) 0.3288(4) 0.021(2) Uani 1 1 d . . . N12 N 0.8641(6) 0.1012(3) 0.3166(3) 0.0174(19) Uani 1 1 d . . . N21 N 0.5971(6) 0.4308(3) 0.8309(3) 0.021(2) Uani 1 1 d . . . N22 N 0.8742(6) 0.5943(4) 0.7938(4) 0.025(2) Uani 1 1 d . . . N31 N 0.2134(7) 0.5273(4) 0.6873(4) 0.025(2) Uani 1 1 d . . . N32 N 0.3155(6) 0.5825(4) 0.5008(4) 0.020(2) Uani 1 1 d . . . N41 N 0.7190(7) -0.0543(4) 0.0000(4) 0.024(2) Uani 1 1 d . . . N42 N 0.8296(6) -0.0608(4) -0.2043(4) 0.024(2) Uani 1 1 d . . . N51 N -0.1103(6) 0.1001(4) 0.7133(4) 0.020(2) Uani 1 1 d . . . N52 N -0.1808(6) 0.2167(4) 0.5603(3) 0.022(2) Uani 1 1 d . . . N61 N 0.1622(6) 0.2584(4) -0.0694(4) 0.023(2) Uani 1 1 d . . . N62 N 0.1572(6) 0.4134(3) -0.1914(3) 0.0191(19) Uani 1 1 d . . . O11 O 0.6191(5) -0.0747(3) 0.2282(3) 0.0248(17) Uani 1 1 d . . . O12 O 0.7468(5) 0.0113(3) 0.2214(3) 0.0194(16) Uani 1 1 d . . . O13 O 0.7516(5) -0.0344(3) 0.3951(3) 0.0205(16) Uani 1 1 d . . . O14 O 0.9033(5) 0.0278(3) 0.3786(3) 0.0149(15) Uani 1 1 d . . . O15 O 0.5318(5) 0.0580(3) 0.3462(3) 0.0188(16) Uani 1 1 d . . . O16 O 0.6867(5) 0.1376(3) 0.3558(3) 0.0183(16) Uani 1 1 d . . . O21 O 0.7884(5) 0.4800(3) 0.9021(3) 0.0262(18) Uani 1 1 d . . . O22 O 0.9245(5) 0.5443(3) 0.8765(3) 0.0258(17) Uani 1 1 d . . . O23 O 0.5473(5) 0.5397(3) 0.8264(3) 0.0231(17) Uani 1 1 d . . . O24 O 0.6831(5) 0.6212(3) 0.8221(3) 0.0252(17) Uani 1 1 d . . . O25 O 0.6849(6) 0.4022(3) 0.7334(3) 0.0273(18) Uani 1 1 d . . . O26 O 0.7944(5) 0.4821(3) 0.7090(3) 0.0246(17) Uani 1 1 d . . . O31 O 0.4140(5) 0.5358(3) 0.6694(3) 0.0233(17) Uani 1 1 d . . . O32 O 0.4584(5) 0.5495(3) 0.5765(3) 0.0206(16) Uani 1 1 d . . . O33 O 0.1678(6) 0.6294(3) 0.6680(3) 0.0307(19) Uani 1 1 d . . . O34 O 0.2271(5) 0.6614(3) 0.5874(3) 0.0232(17) Uani 1 1 d . . . O35 O 0.1265(5) 0.4631(3) 0.5705(3) 0.0267(18) Uani 1 1 d . . . O36 O 0.1558(5) 0.4945(3) 0.4848(3) 0.0242(17) Uani 1 1 d . . . O41 O 0.8300(6) -0.1411(3) -0.0626(3) 0.0285(18) Uani 1 1 d . . . O42 O 0.8516(5) -0.1549(3) -0.1677(3) 0.0240(17) Uani 1 1 d . . . O43 O 0.8506(6) 0.0311(3) -0.0043(3) 0.0277(18) Uani 1 1 d . . . O44 O 0.9303(5) 0.0249(3) -0.0941(3) 0.0236(17) Uani 1 1 d . . . O45 O 0.5743(5) -0.0694(3) -0.1002(3) 0.0261(18) Uani 1 1 d . . . O46 O 0.6318(5) -0.0507(3) -0.1871(3) 0.0217(17) Uani 1 1 d . . . O51 O 0.0353(5) 0.1598(3) 0.6834(3) 0.0169(15) Uani 1 1 d . . . O52 O -0.0308(5) 0.2551(3) 0.6623(3) 0.0186(16) Uani 1 1 d . . . O53 O -0.2233(5) 0.1979(3) 0.7355(3) 0.0224(17) Uani 1 1 d . . . O54 O -0.2931(5) 0.2322(3) 0.6486(3) 0.0265(18) Uani 1 1 d . . . O55 O -0.2338(5) 0.0452(3) 0.6030(3) 0.0288(19) Uani 1 1 d . . . O56 O -0.2321(5) 0.0965(3) 0.5270(3) 0.0294(19) Uani 1 1 d . . . O61 O -0.0131(5) 0.2715(3) -0.1390(3) 0.0224(17) Uani 1 1 d . . . O62 O -0.0164(5) 0.3630(3) -0.1754(3) 0.0233(17) Uani 1 1 d . . . O63 O 0.2797(5) 0.2506(3) -0.1498(3) 0.0244(17) Uani 1 1 d . . . O64 O 0.2563(5) 0.3096(3) -0.2164(3) 0.0163(15) Uani 1 1 d . . . O65 O 0.2299(5) 0.3807(3) -0.0186(3) 0.0250(17) Uani 1 1 d . . . O66 O 0.2652(6) 0.4455(3) -0.0819(3) 0.0291(19) Uani 1 1 d . . . C101 C 0.5355(9) -0.1122(4) 0.2794(5) 0.031(3) Uani 1 1 d . . . H10A H 0.4745 -0.1344 0.2770 0.038 Uiso 1 1 calc R . . H10B H 0.5892 -0.1355 0.2819 0.038 Uiso 1 1 calc R . . C102 C 0.5289(8) -0.1002(5) 0.2284(5) 0.028(3) Uani 1 1 d . . . H10C H 0.5101 -0.1362 0.1960 0.034 Uiso 1 1 calc R . . H10D H 0.4786 -0.0746 0.2270 0.034 Uiso 1 1 calc R . . C103 C 0.6153(9) -0.0627(5) 0.1813(4) 0.032(3) Uani 1 1 d . . . H10E H 0.5727 -0.0326 0.1823 0.038 Uiso 1 1 calc R . . H10F H 0.5883 -0.0972 0.1484 0.038 Uiso 1 1 calc R . . C104 C 0.7139(10) -0.0438(5) 0.1791(5) 0.038(3) Uani 1 1 d U . . H10G H 0.7586 -0.0714 0.1836 0.046 Uiso 1 1 calc R . . H10H H 0.7139 -0.0420 0.1433 0.046 Uiso 1 1 calc R . . C105 C 0.8417(9) 0.0313(5) 0.2204(5) 0.031(3) Uani 1 1 d . . . H10I H 0.8456 0.0284 0.1834 0.038 Uiso 1 1 calc R . . H10J H 0.8900 0.0086 0.2314 0.038 Uiso 1 1 calc R . . C106 C 0.8613(9) 0.0922(4) 0.2597(5) 0.026(3) Uani 1 1 d . . . H10K H 0.9242 0.1084 0.2571 0.031 Uiso 1 1 calc R . . H10L H 0.8104 0.1134 0.2485 0.031 Uiso 1 1 calc R . . C107 C 0.5859(8) -0.0744(5) 0.3769(5) 0.028(3) Uani 1 1 d . . . H10M H 0.5770 -0.0425 0.4100 0.033 Uiso 1 1 calc R . . H10N H 0.5447 -0.1084 0.3733 0.033 Uiso 1 1 calc R . . C108 C 0.6890(8) -0.0856(4) 0.3841(5) 0.028(3) Uani 1 1 d . . . H10O H 0.7049 -0.0981 0.4147 0.034 Uiso 1 1 calc R . . H10P H 0.6996 -0.1164 0.3508 0.034 Uiso 1 1 calc R . . C109 C 0.8502(7) -0.0422(4) 0.4091(5) 0.022(2) Uani 1 1 d . . . H10Q H 0.8693 -0.0720 0.3779 0.026 Uiso 1 1 calc R . . H10R H 0.8593 -0.0547 0.4399 0.026 Uiso 1 1 calc R . . C110 C 0.9121(8) 0.0130(4) 0.4249(5) 0.024(3) Uani 1 1 d . . . H11A H 0.8906 0.0433 0.4548 0.029 Uiso 1 1 calc R . . H11B H 0.9807 0.0091 0.4376 0.029 Uiso 1 1 calc R . . C111 C 0.9625(7) 0.0798(4) 0.3913(4) 0.021(2) Uani 1 1 d . . . H11C H 1.0300 0.0775 0.4075 0.026 Uiso 1 1 calc R . . H11D H 0.9375 0.1118 0.4179 0.026 Uiso 1 1 calc R . . C112 C 0.9603(7) 0.0897(5) 0.3403(4) 0.021(2) Uani 1 1 d . . . H11E H 1.0088 0.1223 0.3480 0.025 Uiso 1 1 calc R . . H11F H 0.9799 0.0558 0.3130 0.025 Uiso 1 1 calc R . . C113 C 0.4608(7) -0.0347(4) 0.3342(5) 0.025(3) Uani 1 1 d . . . H11G H 0.4207 -0.0546 0.3498 0.031 Uiso 1 1 calc R . . H11H H 0.4243 -0.0400 0.2977 0.031 Uiso 1 1 calc R . . C114 C 0.4778(8) 0.0281(4) 0.3700(4) 0.022(2) Uani 1 1 d . . . H11I H 0.4148 0.0434 0.3739 0.026 Uiso 1 1 calc R . . H11J H 0.5144 0.0338 0.4066 0.026 Uiso 1 1 calc R . . C115 C 0.5320(7) 0.1177(4) 0.3729(4) 0.020(2) Uani 1 1 d . . . H11K H 0.5615 0.1299 0.4119 0.024 Uiso 1 1 calc R . . H11L H 0.4645 0.1274 0.3698 0.024 Uiso 1 1 calc R . . C116 C 0.5885(7) 0.1481(4) 0.3478(4) 0.019(2) Uani 1 1 d . . . H11M H 0.5609 0.1346 0.3084 0.022 Uiso 1 1 calc R . . H11N H 0.5842 0.1894 0.3645 0.022 Uiso 1 1 calc R . . C117 C 0.7430(8) 0.1701(4) 0.3362(5) 0.022(2) Uani 1 1 d . . . H11O H 0.7362 0.2110 0.3544 0.027 Uiso 1 1 calc R . . H11P H 0.7194 0.1586 0.2966 0.027 Uiso 1 1 calc R . . C118 C 0.8477(7) 0.1604(4) 0.3474(5) 0.021(2) Uani 1 1 d . . . H11Q H 0.8875 0.1864 0.3378 0.025 Uiso 1 1 calc R . . H11R H 0.8692 0.1696 0.3868 0.025 Uiso 1 1 calc R . . C201 C 0.6323(8) 0.4280(4) 0.8837(4) 0.023(2) Uani 1 1 d . . . H20A H 0.5993 0.3934 0.8841 0.028 Uiso 1 1 calc R . . H20B H 0.6134 0.4612 0.9121 0.028 Uiso 1 1 calc R . . C202 C 0.7386(9) 0.4273(4) 0.8981(5) 0.029(3) Uani 1 1 d U . . H20C H 0.7555 0.4231 0.9333 0.035 Uiso 1 1 calc R . . H20D H 0.7592 0.3947 0.8700 0.035 Uiso 1 1 calc R . . C203 C 0.8898(8) 0.4822(5) 0.9202(5) 0.027(3) Uani 1 1 d . . . H20E H 0.9170 0.4522 0.8928 0.033 Uiso 1 1 calc R . . H20F H 0.9033 0.4765 0.9548 0.033 Uiso 1 1 calc R . . C204 C 0.9350(8) 0.5414(5) 0.9286(5) 0.029(3) Uani 1 1 d . . . H20G H 0.9017 0.5712 0.9523 0.035 Uiso 1 1 calc R . . H20H H 1.0046 0.5473 0.9460 0.035 Uiso 1 1 calc R . . C205 C 0.9691(10) 0.5988(5) 0.8832(5) 0.038(3) Uani 1 1 d . . . H20I H 1.0364 0.6059 0.9044 0.045 Uiso 1 1 calc R . . H20J H 0.9323 0.6294 0.9029 0.045 Uiso 1 1 calc R . . C206 C 0.9694(8) 0.5982(5) 0.8264(5) 0.030(3) Uani 1 1 d . . . H20K H 1.0081 0.6332 0.8305 0.036 Uiso 1 1 calc R . . H20L H 1.0023 0.5655 0.8065 0.036 Uiso 1 1 calc R . . C207 C 0.5001(7) 0.4494(5) 0.8269(5) 0.024(2) Uani 1 1 d . . . H20M H 0.4605 0.4306 0.8436 0.029 Uiso 1 1 calc R . . H20N H 0.4691 0.4368 0.7880 0.029 Uiso 1 1 calc R . . C208 C 0.4994(8) 0.5136(4) 0.8543(4) 0.020(2) Uani 1 1 d . . . H20O H 0.4318 0.5230 0.8531 0.023 Uiso 1 1 calc R . . H20P H 0.5331 0.5274 0.8929 0.023 Uiso 1 1 calc R . . C209 C 0.5365(8) 0.5991(4) 0.8470(5) 0.021(2) Uani 1 1 d . . . H20Q H 0.5704 0.6178 0.8855 0.025 Uiso 1 1 calc R . . H20R H 0.4670 0.6049 0.8446 0.025 Uiso 1 1 calc R . . C210 C 0.5816(8) 0.6242(5) 0.8117(5) 0.030(3) Uani 1 1 d . . . H21A H 0.5533 0.6022 0.7727 0.037 Uiso 1 1 calc R . . H21B H 0.5684 0.6642 0.8209 0.037 Uiso 1 1 calc R . . C211 C 0.7289(9) 0.6477(5) 0.7935(5) 0.030(3) Uani 1 1 d . . . H21C H 0.7105 0.6866 0.8021 0.036 Uiso 1 1 calc R . . H21D H 0.7080 0.6258 0.7539 0.036 Uiso 1 1 calc R . . C212 C 0.8372(9) 0.6498(4) 0.8104(5) 0.033(3) Uani 1 1 d . . . H21E H 0.8693 0.6732 0.7948 0.039 Uiso 1 1 calc R . . H21F H 0.8556 0.6690 0.8505 0.039 Uiso 1 1 calc R . . C213 C 0.5932(9) 0.3739(4) 0.7879(5) 0.029(3) Uani 1 1 d . . . H21G H 0.5334 0.3506 0.7853 0.035 Uiso 1 1 calc R . . H21H H 0.6493 0.3553 0.7982 0.035 Uiso 1 1 calc R . . C214 C 0.5947(9) 0.3752(5) 0.7319(5) 0.033(3) Uani 1 1 d . . . H21I H 0.5845 0.3359 0.7040 0.039 Uiso 1 1 calc R . . H21J H 0.5417 0.3960 0.7222 0.039 Uiso 1 1 calc R . . C215 C 0.6917(8) 0.3953(5) 0.6799(4) 0.024(3) Uani 1 1 d . . . H21K H 0.6401 0.4137 0.6651 0.029 Uiso 1 1 calc R . . H21L H 0.6833 0.3544 0.6562 0.029 Uiso 1 1 calc R . . C216 C 0.7910(9) 0.4224(4) 0.6814(4) 0.028(3) Uani 1 1 d . . . H21M H 0.8427 0.4077 0.7007 0.033 Uiso 1 1 calc R . . H21N H 0.8012 0.4131 0.6440 0.033 Uiso 1 1 calc R . . C217 C 0.8845(8) 0.5103(5) 0.7096(5) 0.026(3) Uani 1 1 d . . . H21O H 0.8952 0.4997 0.6721 0.031 Uiso 1 1 calc R . . H21P H 0.9389 0.4994 0.7308 0.031 Uiso 1 1 calc R . . C218 C 0.8784(8) 0.5735(5) 0.7356(5) 0.031(3) Uani 1 1 d . . . H21Q H 0.9357 0.5941 0.7316 0.037 Uiso 1 1 calc R . . H21R H 0.8199 0.5827 0.7158 0.037 Uiso 1 1 calc R . . C301 C 0.3032(8) 0.5267(5) 0.7226(5) 0.027(3) Uani 1 1 d U . . H30A H 0.2886 0.5062 0.7455 0.033 Uiso 1 1 calc R . . H30B H 0.3286 0.5663 0.7472 0.033 Uiso 1 1 calc R . . C302 C 0.3807(8) 0.4996(5) 0.6937(5) 0.028(3) Uani 1 1 d U . . H30C H 0.4350 0.4949 0.7196 0.033 Uiso 1 1 calc R . . H30D H 0.3544 0.4617 0.6653 0.033 Uiso 1 1 calc R . . C303 C 0.4971(7) 0.5173(4) 0.6475(5) 0.024(3) Uani 1 1 d . . . H30E H 0.4812 0.4783 0.6191 0.029 Uiso 1 1 calc R . . H30F H 0.5501 0.5167 0.6764 0.029 Uiso 1 1 calc R . . C304 C 0.5290(8) 0.5574(4) 0.6234(4) 0.025(3) Uani 1 1 d . . . H30G H 0.5350 0.5971 0.6501 0.030 Uiso 1 1 calc R . . H30H H 0.5930 0.5494 0.6137 0.030 Uiso 1 1 calc R . . C305 C 0.4852(8) 0.5860(5) 0.5505(4) 0.023(2) Uani 1 1 d . . . H30I H 0.5527 0.5821 0.5451 0.027 Uiso 1 1 calc R . . H30J H 0.4814 0.6262 0.5736 0.027 Uiso 1 1 calc R . . C306 C 0.4166(8) 0.5692(5) 0.4966(5) 0.027(3) Uani 1 1 d . . . H30K H 0.4419 0.5889 0.4756 0.032 Uiso 1 1 calc R . . H30L H 0.4152 0.5278 0.4761 0.032 Uiso 1 1 calc R . . C307 C 0.1554(9) 0.5706(4) 0.7166(5) 0.033(3) Uani 1 1 d . . . H30M H 0.1606 0.5712 0.7537 0.040 Uiso 1 1 calc R . . H30N H 0.0865 0.5593 0.6979 0.040 Uiso 1 1 calc R . . C308 C 0.1845(10) 0.6307(5) 0.7214(5) 0.032(3) Uani 1 1 d U . . H30O H 0.1451 0.6578 0.7435 0.039 Uiso 1 1 calc R . . H30P H 0.2538 0.6427 0.7389 0.039 Uiso 1 1 calc R . . C309 C 0.1637(8) 0.6843(4) 0.6671(4) 0.024(3) Uani 1 1 d . . . H30Q H 0.2258 0.7083 0.6871 0.029 Uiso 1 1 calc R . . H30R H 0.1110 0.7025 0.6847 0.029 Uiso 1 1 calc R . . C310 C 0.1455(8) 0.6782(5) 0.6099(5) 0.025(3) Uani 1 1 d . . . H31A H 0.0889 0.6495 0.5889 0.030 Uiso 1 1 calc R . . H31B H 0.1303 0.7149 0.6079 0.030 Uiso 1 1 calc R . . C311 C 0.2212(9) 0.6644(5) 0.5360(5) 0.029(3) Uani 1 1 d . . . H31C H 0.2174 0.7042 0.5395 0.035 Uiso 1 1 calc R . . H31D H 0.1620 0.6409 0.5106 0.035 Uiso 1 1 calc R . . C312 C 0.3109(8) 0.6428(5) 0.5139(5) 0.027(3) Uani 1 1 d U . . H31E H 0.3114 0.6504 0.4807 0.032 Uiso 1 1 calc R . . H31F H 0.3696 0.6644 0.5412 0.032 Uiso 1 1 calc R . . C313 C 0.1573(8) 0.4715(4) 0.6631(5) 0.026(3) Uani 1 1 d . . . H31G H 0.1240 0.4664 0.6905 0.032 Uiso 1 1 calc R . . H31H H 0.2028 0.4424 0.6543 0.032 Uiso 1 1 calc R . . C314 C 0.0814(8) 0.4606(5) 0.6117(5) 0.027(3) Uani 1 1 d . . . H31I H 0.0444 0.4227 0.5996 0.032 Uiso 1 1 calc R . . H31J H 0.0353 0.4895 0.6195 0.032 Uiso 1 1 calc R . . C315 C 0.0584(8) 0.4427(5) 0.5195(5) 0.028(3) Uani 1 1 d . . . H31K H 0.0075 0.4686 0.5211 0.034 Uiso 1 1 calc R . . H31L H 0.0268 0.4045 0.5121 0.034 Uiso 1 1 calc R . . C316 C 0.1117(9) 0.4397(5) 0.4743(5) 0.033(3) Uani 1 1 d . . . H31M H 0.1618 0.4134 0.4724 0.040 Uiso 1 1 calc R . . H31N H 0.0653 0.4252 0.4390 0.040 Uiso 1 1 calc R . . C317 C 0.2158(8) 0.4893(5) 0.4462(4) 0.023(2) Uani 1 1 d . . . H31O H 0.1787 0.4663 0.4091 0.028 Uiso 1 1 calc R . . H31P H 0.2724 0.4698 0.4537 0.028 Uiso 1 1 calc R . . C318 C 0.2496(8) 0.5474(4) 0.4499(4) 0.024(2) Uani 1 1 d . . . H31Q H 0.2828 0.5430 0.4194 0.029 Uiso 1 1 calc R . . H31R H 0.1922 0.5675 0.4453 0.029 Uiso 1 1 calc R . . C401 C 0.7758(10) -0.0918(5) 0.0187(5) 0.036(3) Uani 1 1 d . . . H40A H 0.7476 -0.0976 0.0475 0.043 Uiso 1 1 calc R . . H40B H 0.8424 -0.0723 0.0356 0.043 Uiso 1 1 calc R . . C402 C 0.7826(10) -0.1496(5) -0.0241(6) 0.040(3) Uani 1 1 d . . . H40C H 0.8196 -0.1727 -0.0072 0.048 Uiso 1 1 calc R . . H40D H 0.7169 -0.1699 -0.0421 0.048 Uiso 1 1 calc R . . C403 C 0.8452(11) -0.1951(5) -0.1021(6) 0.045(4) Uani 1 1 d . . . H40E H 0.7818 -0.2169 -0.1233 0.054 Uiso 1 1 calc R . . H40F H 0.8795 -0.2175 -0.0832 0.054 Uiso 1 1 calc R . . C404 C 0.9040(10) -0.1857(5) -0.1395(5) 0.037(3) Uani 1 1 d . . . H40G H 0.9674 -0.1639 -0.1184 0.044 Uiso 1 1 calc R . . H40H H 0.9161 -0.2227 -0.1659 0.044 Uiso 1 1 calc R . . C405 C 0.9040(9) -0.1479(5) -0.2047(5) 0.031(3) Uani 1 1 d . . . H40I H 0.9171 -0.1855 -0.2295 0.038 Uiso 1 1 calc R . . H40J H 0.9669 -0.1248 -0.1848 0.038 Uiso 1 1 calc R . . C406 C 0.8463(8) -0.1188(5) -0.2370(5) 0.027(3) Uani 1 1 d . . . H40K H 0.8809 -0.1176 -0.2653 0.032 Uiso 1 1 calc R . . H40L H 0.7827 -0.1417 -0.2555 0.032 Uiso 1 1 calc R . . C407 C 0.7351(9) 0.0038(5) 0.0379(4) 0.029(3) Uani 1 1 d . . . H40M H 0.7247 0.0051 0.0735 0.035 Uiso 1 1 calc R . . H40N H 0.6861 0.0251 0.0253 0.035 Uiso 1 1 calc R . . C408 C 0.8361(9) 0.0337(5) 0.0460(5) 0.031(3) Uani 1 1 d . . . H40O H 0.8410 0.0738 0.0715 0.037 Uiso 1 1 calc R . . H40P H 0.8861 0.0148 0.0614 0.037 Uiso 1 1 calc R . . C409 C 0.9334(8) 0.0678(5) 0.0002(5) 0.033(3) Uani 1 1 d . . . H40Q H 0.9932 0.0505 0.0072 0.039 Uiso 1 1 calc R . . H40R H 0.9361 0.1045 0.0311 0.039 Uiso 1 1 calc R . . C410 C 0.9281(9) 0.0778(5) -0.0508(5) 0.033(3) Uani 1 1 d . . . H41A H 0.8674 0.0940 -0.0587 0.039 Uiso 1 1 calc R . . H41B H 0.9837 0.1050 -0.0468 0.039 Uiso 1 1 calc R . . C411 C 0.9222(9) 0.0342(5) -0.1440(5) 0.029(3) Uani 1 1 d U . . H41C H 0.9780 0.0606 -0.1413 0.034 Uiso 1 1 calc R . . H41D H 0.8619 0.0512 -0.1507 0.034 Uiso 1 1 calc R . . C412 C 0.9206(9) -0.0224(5) -0.1901(5) 0.032(3) Uani 1 1 d . . . H41E H 0.9300 -0.0157 -0.2226 0.038 Uiso 1 1 calc R . . H41F H 0.9758 -0.0417 -0.1799 0.038 Uiso 1 1 calc R . . C413 C 0.6149(9) -0.0760(5) -0.0128(5) 0.034(3) Uani 1 1 d U . . H41G H 0.5921 -0.0673 0.0217 0.041 Uiso 1 1 calc R . . H41H H 0.6078 -0.1179 -0.0319 0.041 Uiso 1 1 calc R . . C414 C 0.5506(9) -0.0516(5) -0.0474(5) 0.034(3) Uani 1 1 d . . . H41I H 0.4817 -0.0647 -0.0510 0.041 Uiso 1 1 calc R . . H41J H 0.5596 -0.0096 -0.0297 0.041 Uiso 1 1 calc R . . C415 C 0.5151(8) -0.0459(5) -0.1322(5) 0.027(3) Uani 1 1 d . . . H41K H 0.5293 -0.0040 -0.1163 0.032 Uiso 1 1 calc R . . H41L H 0.4459 -0.0558 -0.1333 0.032 Uiso 1 1 calc R . . C416 C 0.5352(8) -0.0695(5) -0.1891(5) 0.027(3) Uani 1 1 d . . . H41M H 0.5254 -0.1116 -0.2040 0.032 Uiso 1 1 calc R . . H41N H 0.4899 -0.0564 -0.2130 0.032 Uiso 1 1 calc R . . C417 C 0.6522(8) -0.0676(5) -0.2400(5) 0.030(3) Uani 1 1 d . . . H41O H 0.6042 -0.0545 -0.2628 0.036 Uiso 1 1 calc R . . H41P H 0.6476 -0.1095 -0.2572 0.036 Uiso 1 1 calc R . . C418 C 0.7535(8) -0.0420(5) -0.2362(5) 0.031(3) Uani 1 1 d . . . H41Q H 0.7660 -0.0525 -0.2733 0.037 Uiso 1 1 calc R . . H41R H 0.7569 -0.0001 -0.2193 0.037 Uiso 1 1 calc R . . C501 C -0.0064(8) 0.0926(5) 0.7214(5) 0.027(3) Uani 1 1 d . . . H50A H 0.0049 0.0602 0.6896 0.032 Uiso 1 1 calc R . . H50B H 0.0112 0.0831 0.7537 0.032 Uiso 1 1 calc R . . C502 C 0.0596(8) 0.1447(5) 0.7292(5) 0.025(3) Uani 1 1 d . . . H50C H 0.0524 0.1768 0.7626 0.029 Uiso 1 1 calc R . . H50D H 0.1280 0.1366 0.7337 0.029 Uiso 1 1 calc R . . C503 C 0.0985(8) 0.2071(5) 0.6884(5) 0.029(3) Uani 1 1 d . . . H50E H 0.1627 0.1951 0.6819 0.034 Uiso 1 1 calc R . . H50F H 0.1075 0.2369 0.7255 0.034 Uiso 1 1 calc R . . C504 C 0.0547(8) 0.2301(4) 0.6476(4) 0.023(2) Uani 1 1 d U . . H50G H 0.1020 0.2591 0.6465 0.028 Uiso 1 1 calc R . . H50H H 0.0378 0.1991 0.6111 0.028 Uiso 1 1 calc R . . C505 C -0.0635(8) 0.2925(4) 0.6352(4) 0.024(3) Uani 1 1 d . . . H50I H -0.0097 0.3221 0.6423 0.029 Uiso 1 1 calc R . . H50J H -0.1174 0.3118 0.6507 0.029 Uiso 1 1 calc R . . C506 C -0.0974(8) 0.2609(5) 0.5745(5) 0.027(3) Uani 1 1 d . . . H50K H -0.1166 0.2884 0.5580 0.033 Uiso 1 1 calc R . . H50L H -0.0428 0.2426 0.5589 0.033 Uiso 1 1 calc R . . C507 C -0.1335(9) 0.1343(5) 0.7654(5) 0.032(3) Uani 1 1 d . . . H50M H -0.0814 0.1661 0.7855 0.038 Uiso 1 1 calc R . . H50N H -0.1346 0.1106 0.7869 0.038 Uiso 1 1 calc R . . C508 C -0.2330(8) 0.1590(5) 0.7605(5) 0.028(3) Uani 1 1 d . . . H50O H -0.2858 0.1282 0.7382 0.033 Uiso 1 1 calc R . . H50P H -0.2481 0.1785 0.7969 0.033 Uiso 1 1 calc R . . C509 C -0.3087(8) 0.2271(5) 0.7313(5) 0.029(3) Uani 1 1 d . . . H50Q H -0.3549 0.2172 0.7510 0.034 Uiso 1 1 calc R . . H50R H -0.2898 0.2686 0.7485 0.034 Uiso 1 1 calc R . . C510 C -0.3552(8) 0.2113(5) 0.6750(5) 0.030(3) Uani 1 1 d . . . H51A H -0.3686 0.1694 0.6567 0.036 Uiso 1 1 calc R . . H51B H -0.4177 0.2275 0.6728 0.036 Uiso 1 1 calc R . . C511 C -0.3343(9) 0.2182(5) 0.5930(5) 0.035(3) Uani 1 1 d . . . H51C H -0.3982 0.2329 0.5902 0.042 Uiso 1 1 calc R . . H51D H -0.3451 0.1764 0.5738 0.042 Uiso 1 1 calc R . . C512 C -0.2730(8) 0.2417(6) 0.5665(5) 0.034(3) Uani 1 1 d . . . H51E H -0.2580 0.2832 0.5878 0.040 Uiso 1 1 calc R . . H51F H -0.3101 0.2361 0.5300 0.040 Uiso 1 1 calc R . . C513 C -0.1675(8) 0.0438(5) 0.6894(5) 0.032(3) Uani 1 1 d . . . H51G H -0.2334 0.0482 0.6973 0.039 Uiso 1 1 calc R . . H51H H -0.1370 0.0195 0.7072 0.039 Uiso 1 1 calc R . . C514 C -0.1759(8) 0.0149(4) 0.6301(5) 0.031(3) Uani 1 1 d . . . H51I H -0.1106 0.0136 0.6212 0.038 Uiso 1 1 calc R . . H51J H -0.2066 -0.0247 0.6175 0.038 Uiso 1 1 calc R . . C515 C -0.2578(11) 0.0129(5) 0.5457(5) 0.046(4) Uani 1 1 d . . . H51K H -0.3047 -0.0206 0.5375 0.055 Uiso 1 1 calc R . . H51L H -0.1987 -0.0009 0.5323 0.055 Uiso 1 1 calc R . . C516 C -0.3016(10) 0.0501(6) 0.5176(6) 0.046(4) Uani 1 1 d . . . H51M H -0.3220 0.0275 0.4781 0.055 Uiso 1 1 calc R . . H51N H -0.3596 0.0646 0.5318 0.055 Uiso 1 1 calc R . . C517 C -0.2585(10) 0.1246(5) 0.4909(5) 0.036(3) Uani 1 1 d . . . H51O H -0.3234 0.1375 0.4938 0.043 Uiso 1 1 calc R . . H51P H -0.2615 0.0979 0.4529 0.043 Uiso 1 1 calc R . . C518 C -0.1855(9) 0.1744(5) 0.5050(5) 0.032(3) Uani 1 1 d . . . H51Q H -0.1209 0.1611 0.5020 0.038 Uiso 1 1 calc R . . H51R H -0.2023 0.1924 0.4786 0.038 Uiso 1 1 calc R . . C601 C 0.0722(8) 0.2213(4) -0.0894(5) 0.024(3) Uani 1 1 d U . . H60A H 0.0652 0.2031 -0.0636 0.029 Uiso 1 1 calc R . . H60B H 0.0753 0.1908 -0.1247 0.029 Uiso 1 1 calc R . . C602 C -0.0156(8) 0.2504(5) -0.0970(5) 0.029(3) Uani 1 1 d . . . H60C H -0.0747 0.2234 -0.1070 0.035 Uiso 1 1 calc R . . H60D H -0.0179 0.2824 -0.0625 0.035 Uiso 1 1 calc R . . C603 C -0.0975(8) 0.3000(5) -0.1453(5) 0.029(3) Uani 1 1 d . . . H60E H -0.0973 0.3331 -0.1112 0.035 Uiso 1 1 calc R . . H60F H -0.1571 0.2738 -0.1535 0.035 Uiso 1 1 calc R . . C604 C -0.0954(8) 0.3192(5) -0.1911(5) 0.029(3) Uani 1 1 d . . . H60G H -0.0873 0.2866 -0.2239 0.035 Uiso 1 1 calc R . . H60H H -0.1574 0.3338 -0.2000 0.035 Uiso 1 1 calc R . . C605 C -0.0219(8) 0.3880(5) -0.2144(5) 0.032(3) Uani 1 1 d . . . H60I H -0.0841 0.4043 -0.2177 0.039 Uiso 1 1 calc R . . H60J H -0.0193 0.3586 -0.2504 0.039 Uiso 1 1 calc R . . C606 C 0.0628(8) 0.4346(4) -0.1969(5) 0.026(3) Uani 1 1 d . . . H60K H 0.0580 0.4522 -0.2240 0.031 Uiso 1 1 calc R . . H60L H 0.0579 0.4646 -0.1616 0.031 Uiso 1 1 calc R . . C607 C 0.2434(8) 0.2258(4) -0.0775(4) 0.022(2) Uani 1 1 d . . . H60M H 0.2333 0.1930 -0.0672 0.026 Uiso 1 1 calc R . . H60N H 0.3029 0.2498 -0.0531 0.026 Uiso 1 1 calc R . . C608 C 0.2588(8) 0.2038(4) -0.1359(5) 0.024(3) Uani 1 1 d . . . H60O H 0.3132 0.1802 -0.1394 0.029 Uiso 1 1 calc R . . H60P H 0.1996 0.1799 -0.1609 0.029 Uiso 1 1 calc R . . C609 C 0.3252(8) 0.2347(5) -0.1951(5) 0.027(3) Uani 1 1 d . . . H60Q H 0.2827 0.2048 -0.2270 0.033 Uiso 1 1 calc R . . H60R H 0.3870 0.2196 -0.1868 0.033 Uiso 1 1 calc R . . C610 C 0.3446(7) 0.2870(4) -0.2071(4) 0.022(2) Uani 1 1 d . . . H61A H 0.3905 0.3159 -0.1760 0.026 Uiso 1 1 calc R . . H61B H 0.3741 0.2768 -0.2396 0.026 Uiso 1 1 calc R . . C611 C 0.2650(8) 0.3474(4) -0.2433(4) 0.021(2) Uani 1 1 d U . . H61C H 0.2742 0.3258 -0.2807 0.025 Uiso 1 1 calc R . . H61D H 0.3225 0.3758 -0.2236 0.025 Uiso 1 1 calc R . . C612 C 0.1754(9) 0.3771(5) -0.2453(4) 0.028(3) Uani 1 1 d . . . H61E H 0.1808 0.4009 -0.2665 0.034 Uiso 1 1 calc R . . H61F H 0.1187 0.3481 -0.2650 0.034 Uiso 1 1 calc R . . C613 C 0.1708(8) 0.2948(5) -0.0117(4) 0.024(2) Uani 1 1 d U . . H61G H 0.1833 0.2714 0.0101 0.028 Uiso 1 1 calc R . . H61H H 0.1085 0.3104 -0.0063 0.028 Uiso 1 1 calc R . . C614 C 0.2512(9) 0.3435(5) 0.0087(4) 0.030(3) Uani 1 1 d U . . H61I H 0.2576 0.3646 0.0483 0.036 Uiso 1 1 calc R . . H61J H 0.3135 0.3285 0.0022 0.036 Uiso 1 1 calc R . . C615 C 0.3088(10) 0.4245(5) -0.0027(5) 0.041(3) Uani 1 1 d . . . H61K H 0.3658 0.4080 -0.0167 0.049 Uiso 1 1 calc R . . H61L H 0.3273 0.4425 0.0375 0.049 Uiso 1 1 calc R . . C616 C 0.2792(9) 0.4679(5) -0.0247(5) 0.036(3) Uani 1 1 d . . . H61M H 0.2182 0.4813 -0.0136 0.043 Uiso 1 1 calc R . . H61N H 0.3298 0.5009 -0.0091 0.043 Uiso 1 1 calc R . . C617 C 0.2376(9) 0.4869(4) -0.1025(5) 0.031(3) Uani 1 1 d . . . H61O H 0.2856 0.5212 -0.0849 0.037 Uiso 1 1 calc R . . H61P H 0.1736 0.4980 -0.0946 0.037 Uiso 1 1 calc R . . C618 C 0.2323(8) 0.4625(4) -0.1627(5) 0.027(3) Uani 1 1 d . . . H61Q H 0.2180 0.4923 -0.1770 0.032 Uiso 1 1 calc R . . H61R H 0.2961 0.4505 -0.1700 0.032 Uiso 1 1 calc R . . N1S N 0.4318(12) 0.2251(6) 0.1827(8) 0.097(5) Uani 1 1 d U . . H1S3 H 0.4545 0.2151 0.1513 0.146 Uiso 0.67 1 calc PR . . H1S4 H 0.3889 0.2510 0.1837 0.146 Uiso 0.67 1 calc PR . . H1S5 H 0.4016 0.1937 0.1841 0.146 Uiso 0.67 1 calc PR . . C1S C 0.5169(13) 0.2512(8) 0.2316(7) 0.078(6) Uani 1 1 d . . . H1S1 H 0.5487 0.2856 0.2300 0.094 Uiso 1 1 calc R . . H1S2 H 0.5653 0.2237 0.2288 0.094 Uiso 1 1 calc R . . C2S C 0.486(2) 0.2680(10) 0.2881(17) 0.200(18) Uani 1 1 d U . . H2S1 H 0.5430 0.2714 0.3169 0.241 Uiso 1 1 calc R . . H2S2 H 0.4587 0.3047 0.2982 0.241 Uiso 1 1 calc R . . N2S N 0.4126(12) 0.2217(7) 0.2815(8) 0.105(6) Uani 1 1 d . . . H2S3 H 0.3898 0.2304 0.3127 0.158 Uiso 0.67 1 calc PR . . H2S4 H 0.4399 0.1887 0.2740 0.158 Uiso 0.67 1 calc PR . . H2S5 H 0.3626 0.2178 0.2536 0.158 Uiso 0.67 1 calc PR . . 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 Pb11 0.0333(2) 0.0229(2) 0.0146(2) 0.01228(17) 0.00011(18) 0.00558(18) Pb13 0.0262(2) 0.0200(2) 0.0211(2) 0.00937(18) 0.00329(18) 0.01109(17) Pb14 0.0249(2) 0.0167(2) 0.0174(2) 0.01188(17) 0.00405(17) -0.00043(16) Pb15 0.0255(2) 0.0180(2) 0.0165(2) 0.01033(17) 0.00935(17) 0.00645(16) Pb12 0.0197(2) 0.0231(2) 0.0176(2) 0.00476(17) -0.00106(17) -0.00218(16) Pb17 0.0252(2) 0.01456(19) 0.0136(2) 0.00620(16) 0.00191(17) 0.00101(16) Pb18 0.0181(2) 0.0215(2) 0.0211(2) 0.01404(17) 0.00315(17) 0.00531(16) Pb19 0.0283(2) 0.01348(19) 0.0200(2) 0.01036(17) 0.00883(18) 0.00253(16) Pb16 0.0215(2) 0.0217(2) 0.0194(2) 0.00747(17) 0.00853(17) 0.00334(16) Zn11 0.0311(7) 0.0233(6) 0.0178(7) 0.0153(5) 0.0032(5) 0.0033(5) C11 0.021(4) 0.016(4) 0.014(4) 0.013(3) 0.002(3) 0.002(3) C12 0.027(6) 0.034(7) 0.041(8) 0.024(6) 0.006(6) 0.004(5) C13 0.031(7) 0.035(7) 0.037(8) 0.020(6) 0.006(6) 0.002(5) Pb1 0.0280(2) 0.0168(2) 0.0135(2) 0.01045(16) 0.00195(17) 0.00338(16) Pb3 0.0213(2) 0.01603(19) 0.0163(2) 0.01096(16) 0.00438(16) -0.00055(15) Pb4 0.0210(2) 0.01380(19) 0.0171(2) 0.00886(16) 0.00322(16) 0.00601(15) Pb5 0.0188(2) 0.01523(19) 0.0187(2) 0.00862(16) -0.00183(17) -0.00098(15) Pb2 0.0252(2) 0.01504(19) 0.0157(2) 0.00894(16) 0.00897(17) 0.00605(16) Pb7 0.0209(2) 0.01320(19) 0.0134(2) 0.00704(16) 0.00238(16) -0.00010(15) Pb8 0.0184(2) 0.01524(19) 0.0206(2) 0.00959(17) 0.00810(17) 0.00246(15) Pb9 0.0220(2) 0.01296(19) 0.0205(2) 0.01245(17) 0.00609(17) 0.00430(15) Pb6 0.0160(2) 0.0218(2) 0.0201(2) 0.01398(17) 0.00353(17) 0.00397(16) Zn1 0.0274(7) 0.0226(6) 0.0185(7) 0.0152(5) 0.0033(5) 0.0028(5) C1 0.028(6) 0.021(6) 0.018(6) 0.008(5) -0.003(5) 0.003(5) C2 0.049(8) 0.020(6) 0.047(8) 0.021(6) 0.018(6) 0.007(5) C3 0.036(7) 0.030(6) 0.019(6) 0.011(5) -0.002(5) 0.005(5) K1 0.0201(11) 0.0152(10) 0.0126(11) 0.0079(9) 0.0024(9) 0.0030(9) K2 0.0241(12) 0.0115(10) 0.0148(12) 0.0059(9) -0.0004(9) 0.0023(9) K3 0.0263(12) 0.0181(11) 0.0193(12) 0.0130(10) 0.0079(10) 0.0017(9) K4 0.0254(12) 0.0229(12) 0.0149(12) 0.0139(10) 0.0054(10) 0.0056(10) K5 0.0174(11) 0.0165(11) 0.0170(12) 0.0074(9) 0.0001(9) 0.0018(9) K6 0.0187(11) 0.0148(10) 0.0136(11) 0.0093(9) 0.0036(9) 0.0018(9) N11 0.027(5) 0.016(4) 0.018(5) 0.004(4) 0.005(4) 0.002(4) N12 0.019(5) 0.024(5) 0.017(5) 0.015(4) 0.009(4) 0.007(4) N21 0.035(5) 0.017(4) 0.016(5) 0.010(4) 0.007(4) 0.004(4) N22 0.023(5) 0.024(5) 0.027(6) 0.012(4) 0.000(4) 0.007(4) N31 0.039(6) 0.017(5) 0.034(6) 0.019(4) 0.022(5) 0.009(4) N32 0.028(5) 0.023(5) 0.020(5) 0.017(4) 0.010(4) 0.009(4) N41 0.041(6) 0.027(5) 0.021(5) 0.020(4) 0.018(4) 0.019(4) N42 0.016(5) 0.042(6) 0.025(5) 0.022(5) 0.010(4) 0.003(4) N51 0.017(5) 0.027(5) 0.020(5) 0.015(4) 0.004(4) -0.002(4) N52 0.031(5) 0.024(5) 0.014(5) 0.011(4) 0.001(4) 0.010(4) N61 0.027(5) 0.025(5) 0.021(5) 0.014(4) 0.005(4) 0.003(4) N62 0.032(5) 0.013(4) 0.019(5) 0.013(4) 0.006(4) 0.001(4) O11 0.029(4) 0.022(4) 0.019(4) 0.005(3) 0.003(3) 0.002(3) O12 0.031(4) 0.018(4) 0.007(4) 0.002(3) 0.005(3) -0.002(3) O13 0.019(4) 0.015(4) 0.035(5) 0.017(3) 0.008(3) -0.001(3) O14 0.019(4) 0.014(3) 0.011(4) 0.007(3) -0.002(3) -0.001(3) O15 0.024(4) 0.024(4) 0.013(4) 0.011(3) 0.009(3) 0.003(3) O16 0.021(4) 0.017(4) 0.018(4) 0.008(3) 0.003(3) 0.002(3) O21 0.028(4) 0.027(4) 0.026(4) 0.016(4) -0.003(3) 0.002(3) O22 0.034(4) 0.028(4) 0.017(4) 0.011(3) 0.003(3) -0.002(3) O23 0.032(4) 0.019(4) 0.026(4) 0.015(3) 0.009(3) 0.007(3) O24 0.032(4) 0.022(4) 0.030(5) 0.016(3) 0.013(4) 0.010(3) O25 0.038(5) 0.025(4) 0.012(4) 0.003(3) -0.001(3) -0.003(3) O26 0.030(4) 0.028(4) 0.027(4) 0.017(4) 0.016(3) 0.016(3) O31 0.033(4) 0.021(4) 0.026(4) 0.018(3) 0.012(3) -0.001(3) O32 0.022(4) 0.028(4) 0.018(4) 0.016(3) 0.006(3) 0.001(3) O33 0.049(5) 0.021(4) 0.034(5) 0.017(4) 0.025(4) 0.009(4) O34 0.027(4) 0.020(4) 0.032(5) 0.019(3) 0.009(3) 0.009(3) O35 0.027(4) 0.020(4) 0.029(5) 0.007(3) 0.004(4) 0.000(3) O36 0.024(4) 0.019(4) 0.029(5) 0.010(3) 0.004(3) 0.004(3) O41 0.048(5) 0.024(4) 0.029(5) 0.021(4) 0.021(4) 0.014(4) O42 0.032(4) 0.025(4) 0.015(4) 0.005(3) 0.013(3) 0.006(3) O43 0.038(5) 0.024(4) 0.023(4) 0.010(3) 0.010(4) 0.007(3) O44 0.034(4) 0.018(4) 0.022(4) 0.012(3) 0.004(3) 0.006(3) O45 0.029(4) 0.026(4) 0.025(4) 0.010(3) 0.009(4) 0.007(3) O46 0.021(4) 0.036(4) 0.009(4) 0.012(3) -0.003(3) 0.002(3) O51 0.015(4) 0.020(4) 0.017(4) 0.013(3) -0.005(3) -0.008(3) O52 0.019(4) 0.025(4) 0.019(4) 0.014(3) 0.007(3) 0.006(3) O53 0.027(4) 0.028(4) 0.022(4) 0.016(3) 0.015(3) 0.011(3) O54 0.022(4) 0.029(4) 0.027(5) 0.013(4) -0.002(3) 0.005(3) O55 0.027(4) 0.017(4) 0.030(5) -0.005(3) 0.009(4) -0.005(3) O56 0.030(4) 0.032(4) 0.016(4) 0.003(3) -0.004(3) -0.002(4) O61 0.023(4) 0.027(4) 0.027(4) 0.019(3) 0.012(3) 0.005(3) O62 0.022(4) 0.028(4) 0.029(5) 0.024(4) -0.002(3) 0.001(3) O63 0.030(4) 0.026(4) 0.034(5) 0.023(4) 0.019(4) 0.017(3) O64 0.019(4) 0.018(4) 0.021(4) 0.016(3) 0.008(3) 0.005(3) O65 0.034(4) 0.020(4) 0.019(4) 0.010(3) -0.005(3) -0.001(3) O66 0.046(5) 0.015(4) 0.026(5) 0.010(3) -0.001(4) 0.004(3) C101 0.030(7) 0.015(6) 0.040(8) 0.003(5) 0.005(6) -0.005(5) C102 0.026(6) 0.025(6) 0.024(7) 0.003(5) -0.004(5) -0.003(5) C103 0.058(8) 0.019(6) 0.010(6) 0.003(5) -0.004(6) -0.002(5) C104 0.068(9) 0.025(6) 0.012(6) -0.003(5) 0.011(6) 0.000(6) C105 0.054(8) 0.028(6) 0.027(7) 0.017(5) 0.026(6) 0.011(6) C106 0.034(7) 0.023(6) 0.026(7) 0.013(5) 0.011(5) 0.005(5) C107 0.036(7) 0.021(6) 0.028(7) 0.009(5) 0.014(5) -0.011(5) C108 0.036(7) 0.015(5) 0.029(7) 0.008(5) -0.002(5) -0.009(5) C109 0.024(6) 0.021(6) 0.028(6) 0.017(5) 0.006(5) 0.004(5) C110 0.023(6) 0.025(6) 0.027(7) 0.019(5) -0.005(5) -0.001(5) C111 0.013(5) 0.022(5) 0.027(6) 0.011(5) -0.002(5) -0.009(4) C112 0.014(5) 0.034(6) 0.027(6) 0.022(5) 0.010(5) 0.011(5) C113 0.018(6) 0.023(6) 0.030(7) 0.005(5) 0.005(5) -0.009(5) C114 0.028(6) 0.022(6) 0.021(6) 0.011(5) 0.012(5) 0.003(5) C115 0.011(5) 0.019(5) 0.026(6) 0.002(5) 0.005(4) 0.008(4) C116 0.012(5) 0.026(6) 0.016(6) 0.003(5) 0.007(4) 0.006(4) C117 0.031(6) 0.021(6) 0.027(6) 0.017(5) 0.017(5) 0.008(5) C118 0.022(6) 0.018(5) 0.033(7) 0.017(5) 0.013(5) 0.004(4) C201 0.038(7) 0.014(5) 0.023(6) 0.011(5) 0.014(5) 0.001(5) C202 0.047(7) 0.019(5) 0.028(6) 0.020(5) -0.001(5) -0.003(5) C203 0.029(6) 0.037(7) 0.020(6) 0.017(5) 0.001(5) 0.006(5) C204 0.018(6) 0.037(7) 0.026(7) 0.010(5) -0.002(5) -0.001(5) C205 0.046(8) 0.035(7) 0.025(7) 0.009(6) 0.000(6) -0.008(6) C206 0.028(7) 0.028(6) 0.035(7) 0.016(6) 0.003(5) -0.012(5) C207 0.019(6) 0.033(6) 0.021(6) 0.013(5) 0.005(5) -0.005(5) C208 0.021(6) 0.026(6) 0.017(6) 0.011(5) 0.011(5) 0.001(4) C209 0.020(6) 0.016(5) 0.030(7) 0.009(5) 0.008(5) 0.005(4) C210 0.039(7) 0.028(6) 0.026(7) 0.010(5) 0.008(5) 0.017(5) C211 0.042(7) 0.029(6) 0.035(7) 0.025(6) 0.020(6) 0.011(5) C212 0.041(7) 0.015(6) 0.052(8) 0.016(6) 0.026(6) 0.008(5) C213 0.041(7) 0.012(5) 0.032(7) 0.008(5) 0.002(6) -0.001(5) C214 0.041(7) 0.027(6) 0.024(7) 0.007(5) -0.002(6) 0.003(5) C215 0.034(7) 0.025(6) 0.005(5) -0.002(5) -0.001(5) 0.002(5) C216 0.048(8) 0.025(6) 0.012(6) 0.008(5) 0.006(5) 0.023(5) C217 0.028(6) 0.041(7) 0.022(6) 0.024(6) 0.012(5) 0.010(5) C218 0.029(7) 0.045(7) 0.038(7) 0.035(6) 0.013(6) 0.007(5) C301 0.044(6) 0.021(5) 0.023(5) 0.015(4) 0.009(5) -0.009(4) C302 0.036(6) 0.031(5) 0.027(6) 0.027(5) -0.001(5) 0.001(4) C303 0.019(6) 0.024(6) 0.031(7) 0.013(5) 0.003(5) 0.010(5) C304 0.030(6) 0.023(6) 0.022(6) 0.005(5) 0.010(5) 0.007(5) C305 0.024(6) 0.029(6) 0.021(6) 0.015(5) 0.006(5) 0.004(5) C306 0.028(6) 0.041(7) 0.023(6) 0.020(6) 0.019(5) 0.009(5) C307 0.050(8) 0.020(6) 0.041(8) 0.014(6) 0.033(6) 0.010(5) C308 0.055(7) 0.025(5) 0.028(6) 0.016(5) 0.026(5) 0.002(5) C309 0.036(7) 0.013(5) 0.022(6) 0.003(5) 0.012(5) 0.013(5) C310 0.017(6) 0.021(6) 0.031(7) 0.003(5) 0.002(5) -0.002(4) C311 0.049(8) 0.022(6) 0.027(7) 0.022(5) 0.006(6) 0.006(5) C312 0.035(5) 0.030(4) 0.024(4) 0.021(4) 0.009(4) -0.003(3) C313 0.038(7) 0.025(6) 0.032(7) 0.021(5) 0.022(6) 0.010(5) C314 0.035(7) 0.024(6) 0.036(7) 0.022(5) 0.019(6) 0.016(5) C315 0.021(6) 0.029(6) 0.043(8) 0.023(6) 0.006(5) 0.003(5) C316 0.035(7) 0.032(7) 0.038(8) 0.024(6) -0.004(6) 0.004(5) C317 0.026(6) 0.030(6) 0.016(6) 0.011(5) 0.008(5) 0.005(5) C318 0.031(6) 0.031(6) 0.015(6) 0.011(5) 0.010(5) 0.011(5) C401 0.061(9) 0.037(7) 0.030(7) 0.026(6) 0.027(6) 0.023(6) C402 0.063(9) 0.025(6) 0.049(9) 0.025(6) 0.027(7) 0.020(6) C403 0.077(10) 0.021(6) 0.047(9) 0.015(6) 0.028(8) 0.023(7) C404 0.057(9) 0.025(6) 0.038(8) 0.012(6) 0.030(7) 0.017(6) C405 0.031(7) 0.030(6) 0.025(7) -0.001(5) 0.011(5) 0.004(5) C406 0.022(6) 0.048(7) 0.020(6) 0.024(6) 0.005(5) 0.006(5) C407 0.040(7) 0.032(6) 0.013(6) 0.004(5) 0.008(5) 0.011(5) C408 0.048(8) 0.028(6) 0.014(6) 0.007(5) 0.003(5) 0.012(6) C409 0.028(7) 0.019(6) 0.044(8) 0.006(6) 0.006(6) 0.008(5) C410 0.031(7) 0.024(6) 0.048(8) 0.017(6) 0.011(6) 0.008(5) C411 0.034(6) 0.035(6) 0.032(6) 0.029(5) 0.009(5) -0.002(4) C412 0.035(7) 0.046(7) 0.033(7) 0.030(6) 0.021(6) 0.007(6) C413 0.056(8) 0.035(6) 0.031(7) 0.023(6) 0.034(6) 0.015(6) C414 0.038(7) 0.038(7) 0.040(8) 0.022(6) 0.025(6) 0.017(6) C415 0.020(6) 0.022(6) 0.040(7) 0.012(5) 0.008(5) 0.014(5) C416 0.026(6) 0.028(6) 0.023(7) 0.007(5) 0.003(5) 0.009(5) C417 0.032(7) 0.036(7) 0.023(7) 0.017(5) -0.006(5) -0.002(5) C418 0.036(7) 0.046(7) 0.019(6) 0.025(6) 0.004(5) 0.001(6) C501 0.024(6) 0.031(6) 0.032(7) 0.018(5) 0.011(5) 0.004(5) C502 0.027(6) 0.031(6) 0.023(6) 0.019(5) 0.003(5) 0.009(5) C503 0.025(6) 0.021(6) 0.042(8) 0.016(5) 0.003(5) -0.002(5) C504 0.037(6) 0.021(5) 0.020(5) 0.012(4) 0.017(4) 0.001(4) C505 0.038(7) 0.015(5) 0.025(6) 0.016(5) 0.004(5) 0.001(5) C506 0.035(7) 0.035(7) 0.027(7) 0.025(6) 0.012(5) 0.014(5) C507 0.034(7) 0.034(7) 0.028(7) 0.010(6) 0.009(6) 0.012(5) C508 0.029(6) 0.026(6) 0.039(7) 0.020(6) 0.019(6) 0.004(5) C509 0.032(7) 0.026(6) 0.031(7) 0.012(5) 0.011(5) 0.002(5) C510 0.019(6) 0.029(6) 0.042(8) 0.018(6) -0.004(5) 0.002(5) C511 0.041(7) 0.036(7) 0.025(7) 0.012(6) -0.006(6) 0.023(6) C512 0.034(7) 0.059(8) 0.014(6) 0.022(6) 0.003(5) 0.013(6) C513 0.028(7) 0.034(7) 0.053(9) 0.029(6) 0.025(6) 0.019(5) C514 0.029(6) 0.008(5) 0.051(9) 0.005(5) 0.011(6) -0.004(5) C515 0.063(10) 0.025(7) 0.035(8) 0.002(6) -0.002(7) -0.011(6) C516 0.038(8) 0.053(9) 0.031(8) 0.006(7) -0.005(6) -0.007(7) C517 0.050(8) 0.043(7) 0.015(6) 0.011(6) 0.007(6) 0.019(6) C518 0.033(7) 0.042(7) 0.027(7) 0.024(6) -0.001(5) 0.007(6) C601 0.032(5) 0.018(5) 0.033(6) 0.020(4) 0.006(5) 0.009(4) C602 0.031(7) 0.032(6) 0.035(7) 0.022(6) 0.013(6) 0.000(5) C603 0.015(6) 0.043(7) 0.032(7) 0.018(6) 0.003(5) 0.002(5) C604 0.014(6) 0.040(7) 0.031(7) 0.011(6) 0.004(5) 0.002(5) C605 0.025(6) 0.047(7) 0.029(7) 0.020(6) 0.004(5) 0.009(5) C606 0.029(6) 0.021(6) 0.040(7) 0.025(5) 0.009(5) 0.012(5) C607 0.030(6) 0.018(5) 0.023(6) 0.015(5) 0.001(5) 0.008(5) C608 0.028(6) 0.017(5) 0.038(7) 0.018(5) 0.015(5) 0.017(5) C609 0.017(6) 0.043(7) 0.022(6) 0.013(5) 0.004(5) 0.010(5) C610 0.020(6) 0.026(6) 0.015(6) 0.005(5) 0.004(5) -0.009(5) C611 0.029(5) 0.028(5) 0.010(5) 0.013(4) 0.007(4) 0.000(4) C612 0.042(7) 0.026(6) 0.021(6) 0.017(5) -0.001(5) 0.009(5) C613 0.037(6) 0.032(5) 0.012(5) 0.017(4) 0.010(4) 0.011(4) C614 0.044(7) 0.036(6) 0.012(6) 0.014(5) -0.001(5) 0.019(5) C615 0.057(9) 0.034(7) 0.026(7) 0.013(6) -0.010(6) -0.002(6) C616 0.042(8) 0.026(6) 0.029(7) 0.003(5) -0.001(6) -0.002(5) C617 0.043(7) 0.016(6) 0.037(7) 0.012(5) 0.009(6) 0.004(5) C618 0.037(7) 0.021(6) 0.031(7) 0.018(5) 0.012(5) -0.004(5) N1S 0.109(11) 0.063(8) 0.172(14) 0.087(9) 0.061(10) 0.045(8) C1S 0.073(13) 0.092(14) 0.063(12) 0.015(11) 0.026(10) 0.041(11) C2S 0.27(3) 0.099(17) 0.40(5) 0.17(2) 0.29(4) 0.13(2) N2S 0.106(13) 0.101(13) 0.171(18) 0.083(13) 0.106(13) 0.072(11) _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 Pb11 Pb12 3.0611(6) . ? Pb11 Pb15 3.0638(5) . ? Pb11 Pb14 3.0707(5) . ? Pb11 Pb13 3.0836(6) . ? Pb13 Pb17 3.1054(5) . ? Pb13 Pb16 3.1079(6) . ? Pb13 Pb14 3.2962(6) . ? Pb13 Pb12 3.3209(5) . ? Pb14 Pb17 3.0838(6) . ? Pb14 Pb18 3.0984(5) . ? Pb14 Pb15 3.3970(5) . ? Pb15 Pb19 3.0632(5) . ? Pb15 Pb18 3.1066(5) . ? Pb15 Pb12 3.2997(6) . ? Pb12 Pb16 3.0397(6) . ? Pb12 Pb19 3.0691(5) . ? Pb17 Zn11 2.8332(12) . ? Pb17 Pb16 3.2570(5) . ? Pb17 Pb18 3.2881(5) . ? Pb18 Zn11 2.8470(13) . ? Pb18 Pb19 3.3049(5) . ? Pb19 Zn11 2.8347(13) . ? Pb19 Pb16 3.2852(5) . ? Pb16 Zn11 2.8513(13) . ? Zn11 C11 2.044(9) . ? C11 C13 1.501(14) . ? C11 C12 1.523(14) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Pb1 Pb5 3.0514(5) . ? Pb1 Pb2 3.0657(5) . ? Pb1 Pb4 3.0713(6) . ? Pb1 Pb3 3.0835(5) . ? Pb3 Pb6 3.0833(5) . ? Pb3 Pb7 3.0983(6) . ? Pb3 Pb4 3.3111(5) . ? Pb3 Pb2 3.3489(5) . ? Pb4 Pb7 3.0671(5) . ? Pb4 Pb8 3.1059(5) . ? Pb4 Pb5 3.4250(5) . ? Pb5 Pb9 3.0244(5) . ? Pb5 Pb8 3.0730(6) . ? Pb5 Pb2 3.3237(6) . ? Pb2 Pb6 3.0706(5) . ? Pb2 Pb9 3.0718(5) . ? Pb7 Zn1 2.8013(12) . ? Pb7 Pb8 3.2501(5) . ? Pb7 Pb6 3.2977(5) . ? Pb8 Zn1 2.8574(12) . ? Pb8 Pb9 3.2325(5) . ? Pb9 Zn1 2.8471(13) . ? Pb9 Pb6 3.3179(5) . ? Pb6 Zn1 2.8445(13) . ? Zn1 C1 2.021(10) . ? C1 C2 1.508(15) . ? C1 C3 1.572(15) . ? C1 H21 1.0000 . ? C2 H22A 0.9800 . ? C2 H22B 0.9800 . ? C2 H22C 0.9800 . ? C3 H23A 0.9800 . ? C3 H23B 0.9800 . ? C3 H23C 0.9800 . ? N11 C101 1.463(14) . ? N11 C113 1.469(13) . ? N11 C107 1.489(14) . ? N12 C106 1.466(14) . ? N12 C118 1.478(13) . ? N12 C112 1.487(12) . ? N21 C201 1.462(13) . ? N21 C207 1.465(13) . ? N21 C213 1.474(13) . ? N22 C206 1.451(14) . ? N22 C212 1.465(13) . ? N22 C218 1.476(15) . ? N31 C301 1.452(14) . ? N31 C313 1.455(14) . ? N31 C307 1.470(14) . ? N32 C312 1.452(13) . ? N32 C318 1.460(14) . ? N32 C306 1.492(13) . ? N41 C407 1.434(14) . ? N41 C401 1.448(13) . ? N41 C413 1.482(15) . ? N42 C406 1.465(14) . ? N42 C418 1.467(13) . ? N42 C412 1.484(14) . ? N51 C507 1.455(14) . ? N51 C513 1.472(14) . ? N51 C501 1.473(13) . ? N52 C518 1.471(15) . ? N52 C512 1.477(14) . ? N52 C506 1.490(14) . ? N61 C607 1.441(13) . ? N61 C601 1.443(14) . ? N61 C613 1.468(14) . ? N62 C606 1.461(13) . ? N62 C618 1.475(13) . ? N62 C612 1.482(14) . ? O11 C102 1.408(13) . ? O11 C103 1.412(13) . ? O12 C105 1.422(14) . ? O12 C104 1.435(12) . ? O13 C109 1.417(12) . ? O13 C108 1.452(12) . ? O14 C110 1.430(12) . ? O14 C111 1.432(11) . ? O15 C115 1.422(12) . ? O15 C114 1.440(12) . ? O16 C116 1.414(11) . ? O16 C117 1.426(12) . ? O21 C203 1.419(13) . ? O21 C202 1.452(12) . ? O22 C204 1.425(13) . ? O22 C205 1.440(13) . ? O23 C208 1.414(12) . ? O23 C209 1.433(12) . ? O24 C211 1.418(13) . ? O24 C210 1.420(13) . ? O25 C214 1.410(14) . ? O25 C215 1.415(13) . ? O26 C216 1.420(12) . ? O26 C217 1.429(13) . ? O31 C303 1.422(13) . ? O31 C302 1.429(12) . ? O32 C304 1.415(13) . ? O32 C305 1.440(12) . ? O33 C308 1.413(13) . ? O33 C309 1.417(12) . ? O34 C310 1.401(13) . ? O34 C311 1.414(13) . ? O35 C314 1.398(14) . ? O35 C315 1.435(13) . ? O36 C316 1.415(13) . ? O36 C317 1.427(13) . ? O41 C402 1.407(15) . ? O41 C403 1.446(14) . ? O42 C405 1.402(14) . ? O42 C404 1.435(14) . ? O43 C408 1.391(14) . ? O43 C409 1.428(14) . ? O44 C410 1.423(14) . ? O44 C411 1.448(13) . ? O45 C415 1.409(12) . ? O45 C414 1.436(14) . ? O46 C416 1.411(13) . ? O46 C417 1.420(14) . ? O51 C503 1.423(12) . ? O51 C502 1.428(12) . ? O52 C504 1.431(12) . ? O52 C505 1.453(11) . ? O53 C508 1.414(12) . ? O53 C509 1.450(13) . ? O54 C511 1.418(13) . ? O54 C510 1.427(14) . ? O55 C515 1.431(15) . ? O55 C514 1.441(13) . ? O56 C516 1.425(15) . ? O56 C517 1.429(13) . ? O61 C603 1.437(12) . ? O61 C602 1.440(13) . ? O62 C605 1.420(13) . ? O62 C604 1.434(13) . ? O63 C609 1.415(13) . ? O63 C608 1.419(12) . ? O64 C610 1.414(12) . ? O64 C611 1.428(11) . ? O65 C614 1.422(12) . ? O65 C615 1.432(14) . ? O66 C617 1.410(13) . ? O66 C616 1.412(14) . ? C101 C102 1.514(17) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.472(18) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.499(15) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.485(16) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.504(14) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.492(14) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.516(14) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.497(15) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.503(14) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 C202 1.483(15) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.537(15) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.534(17) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.526(14) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.541(16) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.507(16) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.533(16) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.524(16) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.515(16) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? C301 C302 1.496(17) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.499(15) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.504(15) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.525(15) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.474(16) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.526(17) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.527(16) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.526(17) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 C318 1.503(15) . ? C317 H31O 0.9900 . ? C317 H31P 0.9900 . ? C318 H31Q 0.9900 . ? C318 H31R 0.9900 . ? C401 C402 1.517(16) . ? C401 H40A 0.9900 . ? C401 H40B 0.9900 . ? C402 H40C 0.9900 . ? C402 H40D 0.9900 . ? C403 C404 1.495(18) . ? C403 H40E 0.9900 . ? C403 H40F 0.9900 . ? C404 H40G 0.9900 . ? C404 H40H 0.9900 . ? C405 C406 1.508(15) . ? C405 H40I 0.9900 . ? C405 H40J 0.9900 . ? C406 H40K 0.9900 . ? C406 H40L 0.9900 . ? C407 C408 1.529(17) . ? C407 H40M 0.9900 . ? C407 H40N 0.9900 . ? C408 H40O 0.9900 . ? C408 H40P 0.9900 . ? C409 C410 1.488(17) . ? C409 H40Q 0.9900 . ? C409 H40R 0.9900 . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 C412 1.512(17) . ? C411 H41C 0.9900 . ? C411 H41D 0.9900 . ? C412 H41E 0.9900 . ? C412 H41F 0.9900 . ? C413 C414 1.511(16) . ? C413 H41G 0.9900 . ? C413 H41H 0.9900 . ? C414 H41I 0.9900 . ? C414 H41J 0.9900 . ? C415 C416 1.513(16) . ? C415 H41K 0.9900 . ? C415 H41L 0.9900 . ? C416 H41M 0.9900 . ? C416 H41N 0.9900 . ? C417 C418 1.516(16) . ? C417 H41O 0.9900 . ? C417 H41P 0.9900 . ? C418 H41Q 0.9900 . ? C418 H41R 0.9900 . ? C501 C502 1.518(15) . ? C501 H50A 0.9900 . ? C501 H50B 0.9900 . ? C502 H50C 0.9900 . ? C502 H50D 0.9900 . ? C503 C504 1.493(15) . ? C503 H50E 0.9900 . ? C503 H50F 0.9900 . ? C504 H50G 0.9900 . ? C504 H50H 0.9900 . ? C505 C506 1.512(15) . ? C505 H50I 0.9900 . ? C505 H50J 0.9900 . ? C506 H50K 0.9900 . ? C506 H50L 0.9900 . ? C507 C508 1.564(15) . ? C507 H50M 0.9900 . ? C507 H50N 0.9900 . ? C508 H50O 0.9900 . ? C508 H50P 0.9900 . ? C509 C510 1.448(16) . ? C509 H50Q 0.9900 . ? C509 H50R 0.9900 . ? C510 H51A 0.9900 . ? C510 H51B 0.9900 . ? C511 C512 1.458(18) . ? C511 H51C 0.9900 . ? C511 H51D 0.9900 . ? C512 H51E 0.9900 . ? C512 H51F 0.9900 . ? C513 C514 1.478(17) . ? C513 H51G 0.9900 . ? C513 H51H 0.9900 . ? C514 H51I 0.9900 . ? C514 H51J 0.9900 . ? C515 C516 1.514(18) . ? C515 H51K 0.9900 . ? C515 H51L 0.9900 . ? C516 H51M 0.9900 . ? C516 H51N 0.9900 . ? C517 C518 1.489(17) . ? C517 H51O 0.9900 . ? C517 H51P 0.9900 . ? C518 H51Q 0.9900 . ? C518 H51R 0.9900 . ? C601 C602 1.492(14) . ? C601 H60A 0.9900 . ? C601 H60B 0.9900 . ? C602 H60C 0.9900 . ? C602 H60D 0.9900 . ? C603 C604 1.504(16) . ? C603 H60E 0.9900 . ? C603 H60F 0.9900 . ? C604 H60G 0.9900 . ? C604 H60H 0.9900 . ? C605 C606 1.530(16) . ? C605 H60I 0.9900 . ? C605 H60J 0.9900 . ? C606 H60K 0.9900 . ? C606 H60L 0.9900 . ? C607 C608 1.526(15) . ? C607 H60M 0.9900 . ? C607 H60N 0.9900 . ? C608 H60O 0.9900 . ? C608 H60P 0.9900 . ? C609 C610 1.517(15) . ? C609 H60Q 0.9900 . ? C609 H60R 0.9900 . ? C610 H61A 0.9900 . ? C610 H61B 0.9900 . ? C611 C612 1.502(14) . ? C611 H61C 0.9900 . ? C611 H61D 0.9900 . ? C612 H61E 0.9900 . ? C612 H61F 0.9900 . ? C613 C614 1.514(16) . ? C613 H61G 0.9900 . ? C613 H61H 0.9900 . ? C614 H61I 0.9900 . ? C614 H61J 0.9900 . ? C615 C616 1.485(16) . ? C615 H61K 0.9900 . ? C615 H61L 0.9900 . ? C616 H61M 0.9900 . ? C616 H61N 0.9900 . ? C617 C618 1.500(16) . ? C617 H61O 0.9900 . ? C617 H61P 0.9900 . ? C618 H61Q 0.9900 . ? C618 H61R 0.9900 . ? N1S C1S 1.54(2) . ? N1S H1S3 0.9100 . ? N1S H1S4 0.9100 . ? N1S H1S5 0.9100 . ? C1S C2S 1.57(4) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S N2S 1.48(3) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? N2S H2S3 0.9100 . ? N2S H2S4 0.9100 . ? N2S H2S5 0.9100 . ? 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 Pb12 Pb11 Pb15 65.196(13) . . ? Pb12 Pb11 Pb14 99.426(15) . . ? Pb15 Pb11 Pb14 67.249(13) . . ? Pb12 Pb11 Pb13 65.428(14) . . ? Pb15 Pb11 Pb13 100.796(15) . . ? Pb14 Pb11 Pb13 64.768(13) . . ? Pb11 Pb13 Pb17 109.945(16) . . ? Pb11 Pb13 Pb16 109.037(15) . . ? Pb17 Pb13 Pb16 63.228(12) . . ? Pb11 Pb13 Pb14 57.426(13) . . ? Pb17 Pb13 Pb14 57.503(12) . . ? Pb16 Pb13 Pb14 101.776(14) . . ? Pb11 Pb13 Pb12 56.959(13) . . ? Pb17 Pb13 Pb12 100.722(14) . . ? Pb16 Pb13 Pb12 56.319(12) . . ? Pb14 Pb13 Pb12 89.960(13) . . ? Pb11 Pb14 Pb17 110.868(16) . . ? Pb11 Pb14 Pb18 109.523(15) . . ? Pb17 Pb14 Pb18 64.263(12) . . ? Pb11 Pb14 Pb13 57.806(13) . . ? Pb17 Pb14 Pb13 58.139(12) . . ? Pb18 Pb14 Pb13 103.397(15) . . ? Pb11 Pb14 Pb15 56.279(12) . . ? Pb17 Pb14 Pb15 101.519(14) . . ? Pb18 Pb14 Pb15 56.922(11) . . ? Pb13 Pb14 Pb15 90.078(13) . . ? Pb19 Pb15 Pb11 110.797(16) . . ? Pb19 Pb15 Pb18 64.774(13) . . ? Pb11 Pb15 Pb18 109.489(15) . . ? Pb19 Pb15 Pb12 57.532(12) . . ? Pb11 Pb15 Pb12 57.362(13) . . ? Pb18 Pb15 Pb12 101.877(15) . . ? Pb19 Pb15 Pb14 101.799(14) . . ? Pb11 Pb15 Pb14 56.472(12) . . ? Pb18 Pb15 Pb14 56.693(11) . . ? Pb12 Pb15 Pb14 88.596(13) . . ? Pb16 Pb12 Pb11 111.462(16) . . ? Pb16 Pb12 Pb19 65.063(13) . . ? Pb11 Pb12 Pb19 110.712(16) . . ? Pb16 Pb12 Pb15 103.470(15) . . ? Pb11 Pb12 Pb15 57.442(12) . . ? Pb19 Pb12 Pb15 57.360(12) . . ? Pb16 Pb12 Pb13 58.297(12) . . ? Pb11 Pb12 Pb13 57.613(13) . . ? Pb19 Pb12 Pb13 103.945(14) . . ? Pb15 Pb12 Pb13 91.355(13) . . ? Zn11 Pb17 Pb14 107.47(3) . . ? Zn11 Pb17 Pb13 108.16(3) . . ? Pb14 Pb17 Pb13 64.358(13) . . ? Zn11 Pb17 Pb16 55.31(3) . . ? Pb14 Pb17 Pb16 103.201(14) . . ? Pb13 Pb17 Pb16 58.422(12) . . ? Zn11 Pb17 Pb18 54.83(3) . . ? Pb14 Pb17 Pb18 58.084(12) . . ? Pb13 Pb17 Pb18 103.428(14) . . ? Pb16 Pb17 Pb18 90.505(13) . . ? Zn11 Pb18 Pb14 106.72(3) . . ? Zn11 Pb18 Pb15 106.19(3) . . ? Pb14 Pb18 Pb15 66.385(12) . . ? Zn11 Pb18 Pb17 54.43(3) . . ? Pb14 Pb18 Pb17 57.653(12) . . ? Pb15 Pb18 Pb17 103.504(14) . . ? Zn11 Pb18 Pb19 54.26(3) . . ? Pb14 Pb18 Pb19 103.137(14) . . ? Pb15 Pb18 Pb19 56.978(12) . . ? Pb17 Pb18 Pb19 89.440(13) . . ? Zn11 Pb19 Pb15 107.67(3) . . ? Zn11 Pb19 Pb12 106.56(3) . . ? Pb15 Pb19 Pb12 65.108(13) . . ? Zn11 Pb19 Pb16 54.94(3) . . ? Pb15 Pb19 Pb16 103.287(14) . . ? Pb12 Pb19 Pb16 57.037(12) . . ? Zn11 Pb19 Pb18 54.61(3) . . ? Pb15 Pb19 Pb18 58.248(12) . . ? Pb12 Pb19 Pb18 102.575(14) . . ? Pb16 Pb19 Pb18 89.719(13) . . ? Zn11 Pb16 Pb12 106.92(3) . . ? Zn11 Pb16 Pb13 107.63(3) . . ? Pb12 Pb16 Pb13 65.384(13) . . ? Zn11 Pb16 Pb17 54.78(3) . . ? Pb12 Pb16 Pb17 103.618(15) . . ? Pb13 Pb16 Pb17 58.350(12) . . ? Zn11 Pb16 Pb19 54.47(3) . . ? Pb12 Pb16 Pb19 57.900(12) . . ? Pb13 Pb16 Pb19 103.911(15) . . ? Pb17 Pb16 Pb19 90.327(13) . . ? C11 Zn11 Pb17 131.1(3) . . ? C11 Zn11 Pb19 118.8(3) . . ? Pb17 Zn11 Pb19 109.87(4) . . ? C11 Zn11 Pb18 128.9(3) . . ? Pb17 Zn11 Pb18 70.74(3) . . ? Pb19 Zn11 Pb18 71.14(3) . . ? C11 Zn11 Pb16 121.4(3) . . ? Pb17 Zn11 Pb16 69.91(3) . . ? Pb19 Zn11 Pb16 70.59(3) . . ? Pb18 Zn11 Pb16 109.33(4) . . ? C13 C11 C12 110.8(9) . . ? C13 C11 Zn11 110.5(7) . . ? C12 C11 Zn11 110.9(7) . . ? C13 C11 H11 108.2 . . ? C12 C11 H11 108.2 . . ? Zn11 C11 H11 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Pb5 Pb1 Pb2 65.821(12) . . ? Pb5 Pb1 Pb4 68.026(13) . . ? Pb2 Pb1 Pb4 101.211(14) . . ? Pb5 Pb1 Pb3 101.145(14) . . ? Pb2 Pb1 Pb3 65.994(12) . . ? Pb4 Pb1 Pb3 65.090(13) . . ? Pb6 Pb3 Pb1 109.374(14) . . ? Pb6 Pb3 Pb7 64.480(12) . . ? Pb1 Pb3 Pb7 109.153(15) . . ? Pb6 Pb3 Pb4 103.313(14) . . ? Pb1 Pb3 Pb4 57.276(12) . . ? Pb7 Pb3 Pb4 57.063(12) . . ? Pb6 Pb3 Pb2 56.849(11) . . ? Pb1 Pb3 Pb2 56.747(11) . . ? Pb7 Pb3 Pb2 101.440(14) . . ? Pb4 Pb3 Pb2 90.812(13) . . ? Pb7 Pb4 Pb1 110.301(15) . . ? Pb7 Pb4 Pb8 63.535(12) . . ? Pb1 Pb4 Pb8 107.623(14) . . ? Pb7 Pb4 Pb3 57.973(12) . . ? Pb1 Pb4 Pb3 57.633(12) . . ? Pb8 Pb4 Pb3 101.722(13) . . ? Pb7 Pb4 Pb5 100.745(13) . . ? Pb1 Pb4 Pb5 55.712(11) . . ? Pb8 Pb4 Pb5 55.881(11) . . ? Pb3 Pb4 Pb5 89.402(12) . . ? Pb9 Pb5 Pb1 110.347(15) . . ? Pb9 Pb5 Pb8 64.023(12) . . ? Pb1 Pb5 Pb8 108.983(15) . . ? Pb9 Pb5 Pb2 57.650(12) . . ? Pb1 Pb5 Pb2 57.296(12) . . ? Pb8 Pb5 Pb2 101.829(14) . . ? Pb9 Pb5 Pb4 101.662(14) . . ? Pb1 Pb5 Pb4 56.262(12) . . ? Pb8 Pb5 Pb4 56.797(11) . . ? Pb2 Pb5 Pb4 89.284(12) . . ? Pb1 Pb2 Pb6 110.183(15) . . ? Pb1 Pb2 Pb9 108.709(15) . . ? Pb6 Pb2 Pb9 65.388(13) . . ? Pb1 Pb2 Pb5 56.883(12) . . ? Pb6 Pb2 Pb5 103.155(15) . . ? Pb9 Pb2 Pb5 56.279(12) . . ? Pb1 Pb2 Pb3 57.258(11) . . ? Pb6 Pb2 Pb3 57.213(11) . . ? Pb9 Pb2 Pb3 102.116(14) . . ? Pb5 Pb2 Pb3 90.502(13) . . ? Zn1 Pb7 Pb4 109.25(3) . . ? Zn1 Pb7 Pb3 107.29(3) . . ? Pb4 Pb7 Pb3 64.963(13) . . ? Zn1 Pb7 Pb8 55.76(3) . . ? Pb4 Pb7 Pb8 58.814(12) . . ? Pb3 Pb7 Pb8 103.280(14) . . ? Zn1 Pb7 Pb6 54.87(3) . . ? Pb4 Pb7 Pb6 103.989(14) . . ? Pb3 Pb7 Pb6 57.540(12) . . ? Pb8 Pb7 Pb6 90.558(13) . . ? Zn1 Pb8 Pb5 107.31(3) . . ? Zn1 Pb8 Pb4 106.73(3) . . ? Pb5 Pb8 Pb4 67.323(13) . . ? Zn1 Pb8 Pb9 55.33(3) . . ? Pb5 Pb8 Pb9 57.258(12) . . ? Pb4 Pb8 Pb9 104.330(15) . . ? Zn1 Pb8 Pb7 54.14(2) . . ? Pb5 Pb8 Pb7 104.638(15) . . ? Pb4 Pb8 Pb7 57.651(11) . . ? Pb9 Pb8 Pb7 90.618(13) . . ? Zn1 Pb9 Pb5 108.91(3) . . ? Zn1 Pb9 Pb2 106.67(3) . . ? Pb5 Pb9 Pb2 66.072(13) . . ? Zn1 Pb9 Pb8 55.63(3) . . ? Pb5 Pb9 Pb8 58.719(12) . . ? Pb2 Pb9 Pb8 103.966(13) . . ? Zn1 Pb9 Pb6 54.31(3) . . ? Pb5 Pb9 Pb6 104.325(14) . . ? Pb2 Pb9 Pb6 57.288(12) . . ? Pb8 Pb9 Pb6 90.506(13) . . ? Zn1 Pb6 Pb2 106.77(3) . . ? Zn1 Pb6 Pb3 106.59(3) . . ? Pb2 Pb6 Pb3 65.938(12) . . ? Zn1 Pb6 Pb7 53.65(2) . . ? Pb2 Pb6 Pb7 103.207(14) . . ? Pb3 Pb6 Pb7 57.980(12) . . ? Zn1 Pb6 Pb9 54.38(3) . . ? Pb2 Pb6 Pb9 57.324(12) . . ? Pb3 Pb6 Pb9 102.575(14) . . ? Pb7 Pb6 Pb9 88.312(13) . . ? C1 Zn1 Pb7 131.1(3) . . ? C1 Zn1 Pb6 122.1(3) . . ? Pb7 Zn1 Pb6 71.47(3) . . ? C1 Zn1 Pb9 119.5(3) . . ? Pb7 Zn1 Pb9 109.35(4) . . ? Pb6 Zn1 Pb9 71.32(3) . . ? C1 Zn1 Pb8 128.0(3) . . ? Pb7 Zn1 Pb8 70.10(3) . . ? Pb6 Zn1 Pb8 109.37(4) . . ? Pb9 Zn1 Pb8 69.03(3) . . ? C2 C1 C3 111.3(9) . . ? C2 C1 Zn1 111.5(8) . . ? C3 C1 Zn1 109.4(7) . . ? C2 C1 H21 108.1 . . ? C3 C1 H21 108.1 . . ? Zn1 C1 H21 108.1 . . ? C1 C2 H22A 109.5 . . ? C1 C2 H22B 109.5 . . ? H22A C2 H22B 109.5 . . ? C1 C2 H22C 109.5 . . ? H22A C2 H22C 109.5 . . ? H22B C2 H22C 109.5 . . ? C1 C3 H23A 109.5 . . ? C1 C3 H23B 109.5 . . ? H23A C3 H23B 109.5 . . ? C1 C3 H23C 109.5 . . ? H23A C3 H23C 109.5 . . ? H23B C3 H23C 109.5 . . ? C101 N11 C113 109.4(8) . . ? C101 N11 C107 109.4(8) . . ? C113 N11 C107 109.0(9) . . ? C106 N12 C118 109.8(8) . . ? C106 N12 C112 109.1(8) . . ? C118 N12 C112 109.9(8) . . ? C201 N21 C207 111.6(8) . . ? C201 N21 C213 109.0(8) . . ? C207 N21 C213 108.8(9) . . ? C206 N22 C212 110.6(9) . . ? C206 N22 C218 110.4(9) . . ? C212 N22 C218 109.5(9) . . ? C301 N31 C313 110.8(8) . . ? C301 N31 C307 111.3(10) . . ? C313 N31 C307 110.5(9) . . ? C312 N32 C318 112.1(8) . . ? C312 N32 C306 109.5(9) . . ? C318 N32 C306 109.1(8) . . ? C407 N41 C401 113.6(9) . . ? C407 N41 C413 110.3(9) . . ? C401 N41 C413 108.9(9) . . ? C406 N42 C418 109.5(9) . . ? C406 N42 C412 108.9(9) . . ? C418 N42 C412 109.0(8) . . ? C507 N51 C513 110.7(9) . . ? C507 N51 C501 109.2(8) . . ? C513 N51 C501 108.9(8) . . ? C518 N52 C512 112.1(8) . . ? C518 N52 C506 109.2(9) . . ? C512 N52 C506 112.0(9) . . ? C607 N61 C601 110.6(8) . . ? C607 N61 C613 111.0(8) . . ? C601 N61 C613 110.2(9) . . ? C606 N62 C618 108.4(8) . . ? C606 N62 C612 110.6(8) . . ? C618 N62 C612 111.8(9) . . ? C102 O11 C103 111.2(8) . . ? C105 O12 C104 111.8(9) . . ? C109 O13 C108 110.3(7) . . ? C110 O14 C111 110.9(7) . . ? C115 O15 C114 110.7(8) . . ? C116 O16 C117 110.3(7) . . ? C203 O21 C202 110.3(8) . . ? C204 O22 C205 108.7(8) . . ? C208 O23 C209 109.1(8) . . ? C211 O24 C210 109.7(8) . . ? C214 O25 C215 109.0(8) . . ? C216 O26 C217 110.7(8) . . ? C303 O31 C302 111.5(8) . . ? C304 O32 C305 111.0(8) . . ? C308 O33 C309 112.5(8) . . ? C310 O34 C311 113.2(8) . . ? C314 O35 C315 110.3(8) . . ? C316 O36 C317 108.4(8) . . ? C402 O41 C403 110.2(9) . . ? C405 O42 C404 109.3(8) . . ? C408 O43 C409 112.7(9) . . ? C410 O44 C411 108.7(8) . . ? C415 O45 C414 109.9(8) . . ? C416 O46 C417 111.4(8) . . ? C503 O51 C502 111.5(8) . . ? C504 O52 C505 113.9(8) . . ? C508 O53 C509 112.7(8) . . ? C511 O54 C510 112.3(9) . . ? C515 O55 C514 110.5(9) . . ? C516 O56 C517 112.6(9) . . ? C603 O61 C602 109.2(8) . . ? C605 O62 C604 110.4(8) . . ? C609 O63 C608 111.7(8) . . ? C610 O64 C611 111.2(8) . . ? C614 O65 C615 110.4(8) . . ? C617 O66 C616 111.0(8) . . ? N11 C101 C102 112.6(9) . . ? N11 C101 H10A 109.1 . . ? C102 C101 H10A 109.1 . . ? N11 C101 H10B 109.1 . . ? C102 C101 H10B 109.1 . . ? H10A C101 H10B 107.8 . . ? O11 C102 C101 109.8(9) . . ? O11 C102 H10C 109.7 . . ? C101 C102 H10C 109.7 . . ? O11 C102 H10D 109.7 . . ? C101 C102 H10D 109.7 . . ? H10C C102 H10D 108.2 . . ? O11 C103 C104 109.1(9) . . ? O11 C103 H10E 109.9 . . ? C104 C103 H10E 109.9 . . ? O11 C103 H10F 109.9 . . ? C104 C103 H10F 109.9 . . ? H10E C103 H10F 108.3 . . ? O12 C104 C103 110.0(10) . . ? O12 C104 H10G 109.7 . . ? C103 C104 H10G 109.7 . . ? O12 C104 H10H 109.7 . . ? C103 C104 H10H 109.7 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 106.8(9) . . ? O12 C105 H10I 110.4 . . ? C106 C105 H10I 110.4 . . ? O12 C105 H10J 110.4 . . ? C106 C105 H10J 110.4 . . ? H10I C105 H10J 108.6 . . ? N12 C106 C105 115.1(9) . . ? N12 C106 H10K 108.5 . . ? C105 C106 H10K 108.5 . . ? N12 C106 H10L 108.5 . . ? C105 C106 H10L 108.5 . . ? H10K C106 H10L 107.5 . . ? C108 C107 N11 114.0(9) . . ? C108 C107 H10M 108.8 . . ? N11 C107 H10M 108.8 . . ? C108 C107 H10N 108.8 . . ? N11 C107 H10N 108.8 . . ? H10M C107 H10N 107.6 . . ? O13 C108 C107 109.8(8) . . ? O13 C108 H10O 109.7 . . ? C107 C108 H10O 109.7 . . ? O13 C108 H10P 109.7 . . ? C107 C108 H10P 109.7 . . ? H10O C108 H10P 108.2 . . ? O13 C109 C110 108.8(8) . . ? O13 C109 H10Q 109.9 . . ? C110 C109 H10Q 109.9 . . ? O13 C109 H10R 109.9 . . ? C110 C109 H10R 109.9 . . ? H10Q C109 H10R 108.3 . . ? O14 C110 C109 108.8(8) . . ? O14 C110 H11A 109.9 . . ? C109 C110 H11A 109.9 . . ? O14 C110 H11B 109.9 . . ? C109 C110 H11B 109.9 . . ? H11A C110 H11B 108.3 . . ? O14 C111 C112 108.8(8) . . ? O14 C111 H11C 109.9 . . ? C112 C111 H11C 109.9 . . ? O14 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? H11C C111 H11D 108.3 . . ? N12 C112 C111 114.0(8) . . ? N12 C112 H11E 108.7 . . ? C111 C112 H11E 108.7 . . ? N12 C112 H11F 108.7 . . ? C111 C112 H11F 108.7 . . ? H11E C112 H11F 107.6 . . ? N11 C113 C114 112.1(8) . . ? N11 C113 H11G 109.2 . . ? C114 C113 H11G 109.2 . . ? N11 C113 H11H 109.2 . . ? C114 C113 H11H 109.2 . . ? H11G C113 H11H 107.9 . . ? O15 C114 C113 109.7(9) . . ? O15 C114 H11I 109.7 . . ? C113 C114 H11I 109.7 . . ? O15 C114 H11J 109.7 . . ? C113 C114 H11J 109.7 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 110.1(8) . . ? O15 C115 H11K 109.6 . . ? C116 C115 H11K 109.6 . . ? O15 C115 H11L 109.6 . . ? C116 C115 H11L 109.6 . . ? H11K C115 H11L 108.2 . . ? O16 C116 C115 109.7(8) . . ? O16 C116 H11M 109.7 . . ? C115 C116 H11M 109.7 . . ? O16 C116 H11N 109.7 . . ? C115 C116 H11N 109.7 . . ? H11M C116 H11N 108.2 . . ? O16 C117 C118 109.4(8) . . ? O16 C117 H11O 109.8 . . ? C118 C117 H11O 109.8 . . ? O16 C117 H11P 109.8 . . ? C118 C117 H11P 109.8 . . ? H11O C117 H11P 108.3 . . ? N12 C118 C117 112.4(9) . . ? N12 C118 H11Q 109.1 . . ? C117 C118 H11Q 109.1 . . ? N12 C118 H11R 109.1 . . ? C117 C118 H11R 109.1 . . ? H11Q C118 H11R 107.8 . . ? N21 C201 C202 115.2(9) . . ? N21 C201 H20A 108.5 . . ? C202 C201 H20A 108.5 . . ? N21 C201 H20B 108.5 . . ? C202 C201 H20B 108.5 . . ? H20A C201 H20B 107.5 . . ? O21 C202 C201 109.5(8) . . ? O21 C202 H20C 109.8 . . ? C201 C202 H20C 109.8 . . ? O21 C202 H20D 109.8 . . ? C201 C202 H20D 109.8 . . ? H20C C202 H20D 108.2 . . ? O21 C203 C204 106.7(8) . . ? O21 C203 H20E 110.4 . . ? C204 C203 H20E 110.4 . . ? O21 C203 H20F 110.4 . . ? C204 C203 H20F 110.4 . . ? H20E C203 H20F 108.6 . . ? O22 C204 C203 107.8(9) . . ? O22 C204 H20G 110.2 . . ? C203 C204 H20G 110.2 . . ? O22 C204 H20H 110.2 . . ? C203 C204 H20H 110.2 . . ? H20G C204 H20H 108.5 . . ? O22 C205 C206 107.9(9) . . ? O22 C205 H20I 110.1 . . ? C206 C205 H20I 110.1 . . ? O22 C205 H20J 110.1 . . ? C206 C205 H20J 110.1 . . ? H20I C205 H20J 108.4 . . ? N22 C206 C205 115.0(10) . . ? N22 C206 H20K 108.5 . . ? C205 C206 H20K 108.5 . . ? N22 C206 H20L 108.5 . . ? C205 C206 H20L 108.5 . . ? H20K C206 H20L 107.5 . . ? N21 C207 C208 114.1(8) . . ? N21 C207 H20M 108.7 . . ? C208 C207 H20M 108.7 . . ? N21 C207 H20N 108.7 . . ? C208 C207 H20N 108.7 . . ? H20M C207 H20N 107.6 . . ? O23 C208 C207 108.2(8) . . ? O23 C208 H20O 110.1 . . ? C207 C208 H20O 110.1 . . ? O23 C208 H20P 110.1 . . ? C207 C208 H20P 110.1 . . ? H20O C208 H20P 108.4 . . ? O23 C209 C210 106.8(9) . . ? O23 C209 H20Q 110.4 . . ? C210 C209 H20Q 110.4 . . ? O23 C209 H20R 110.4 . . ? C210 C209 H20R 110.4 . . ? H20Q C209 H20R 108.6 . . ? O24 C210 C209 107.7(8) . . ? O24 C210 H21A 110.2 . . ? C209 C210 H21A 110.2 . . ? O24 C210 H21B 110.2 . . ? C209 C210 H21B 110.2 . . ? H21A C210 H21B 108.5 . . ? O24 C211 C212 108.5(9) . . ? O24 C211 H21C 110.0 . . ? C212 C211 H21C 110.0 . . ? O24 C211 H21D 110.0 . . ? C212 C211 H21D 110.0 . . ? H21C C211 H21D 108.4 . . ? N22 C212 C211 114.8(9) . . ? N22 C212 H21E 108.6 . . ? C211 C212 H21E 108.6 . . ? N22 C212 H21F 108.6 . . ? C211 C212 H21F 108.6 . . ? H21E C212 H21F 107.5 . . ? N21 C213 C214 113.4(9) . . ? N21 C213 H21G 108.9 . . ? C214 C213 H21G 108.9 . . ? N21 C213 H21H 108.9 . . ? C214 C213 H21H 108.9 . . ? H21G C213 H21H 107.7 . . ? O25 C214 C213 109.4(9) . . ? O25 C214 H21I 109.8 . . ? C213 C214 H21I 109.8 . . ? O25 C214 H21J 109.8 . . ? C213 C214 H21J 109.8 . . ? H21I C214 H21J 108.3 . . ? O25 C215 C216 108.8(8) . . ? O25 C215 H21K 109.9 . . ? C216 C215 H21K 109.9 . . ? O25 C215 H21L 109.9 . . ? C216 C215 H21L 109.9 . . ? H21K C215 H21L 108.3 . . ? O26 C216 C215 108.0(9) . . ? O26 C216 H21M 110.1 . . ? C215 C216 H21M 110.1 . . ? O26 C216 H21N 110.1 . . ? C215 C216 H21N 110.1 . . ? H21M C216 H21N 108.4 . . ? O26 C217 C218 107.0(9) . . ? O26 C217 H21O 110.3 . . ? C218 C217 H21O 110.3 . . ? O26 C217 H21P 110.3 . . ? C218 C217 H21P 110.3 . . ? H21O C217 H21P 108.6 . . ? N22 C218 C217 114.0(8) . . ? N22 C218 H21Q 108.7 . . ? C217 C218 H21Q 108.7 . . ? N22 C218 H21R 108.7 . . ? C217 C218 H21R 108.7 . . ? H21Q C218 H21R 107.6 . . ? N31 C301 C302 114.7(9) . . ? N31 C301 H30A 108.6 . . ? C302 C301 H30A 108.6 . . ? N31 C301 H30B 108.6 . . ? C302 C301 H30B 108.6 . . ? H30A C301 H30B 107.6 . . ? O31 C302 C301 107.8(8) . . ? O31 C302 H30C 110.1 . . ? C301 C302 H30C 110.1 . . ? O31 C302 H30D 110.1 . . ? C301 C302 H30D 110.1 . . ? H30C C302 H30D 108.5 . . ? O31 C303 C304 108.7(8) . . ? O31 C303 H30E 109.9 . . ? C304 C303 H30E 109.9 . . ? O31 C303 H30F 109.9 . . ? C304 C303 H30F 109.9 . . ? H30E C303 H30F 108.3 . . ? O32 C304 C303 107.8(9) . . ? O32 C304 H30G 110.1 . . ? C303 C304 H30G 110.1 . . ? O32 C304 H30H 110.1 . . ? C303 C304 H30H 110.1 . . ? H30G C304 H30H 108.5 . . ? O32 C305 C306 108.4(9) . . ? O32 C305 H30I 110.0 . . ? C306 C305 H30I 110.0 . . ? O32 C305 H30J 110.0 . . ? C306 C305 H30J 110.0 . . ? H30I C305 H30J 108.4 . . ? N32 C306 C305 114.1(9) . . ? N32 C306 H30K 108.7 . . ? C305 C306 H30K 108.7 . . ? N32 C306 H30L 108.7 . . ? C305 C306 H30L 108.7 . . ? H30K C306 H30L 107.6 . . ? N31 C307 C308 115.0(10) . . ? N31 C307 H30M 108.5 . . ? C308 C307 H30M 108.5 . . ? N31 C307 H30N 108.5 . . ? C308 C307 H30N 108.5 . . ? H30M C307 H30N 107.5 . . ? O33 C308 C307 107.0(9) . . ? O33 C308 H30O 110.3 . . ? C307 C308 H30O 110.3 . . ? O33 C308 H30P 110.3 . . ? C307 C308 H30P 110.3 . . ? H30O C308 H30P 108.6 . . ? O33 C309 C310 108.2(8) . . ? O33 C309 H30Q 110.0 . . ? C310 C309 H30Q 110.0 . . ? O33 C309 H30R 110.0 . . ? C310 C309 H30R 110.0 . . ? H30Q C309 H30R 108.4 . . ? O34 C310 C309 110.3(9) . . ? O34 C310 H31A 109.6 . . ? C309 C310 H31A 109.6 . . ? O34 C310 H31B 109.6 . . ? C309 C310 H31B 109.6 . . ? H31A C310 H31B 108.1 . . ? O34 C311 C312 109.2(9) . . ? O34 C311 H31C 109.8 . . ? C312 C311 H31C 109.8 . . ? O34 C311 H31D 109.8 . . ? C312 C311 H31D 109.8 . . ? H31C C311 H31D 108.3 . . ? N32 C312 C311 113.5(9) . . ? N32 C312 H31E 108.9 . . ? C311 C312 H31E 108.9 . . ? N32 C312 H31F 108.9 . . ? C311 C312 H31F 108.9 . . ? H31E C312 H31F 107.7 . . ? N31 C313 C314 115.6(9) . . ? N31 C313 H31G 108.4 . . ? C314 C313 H31G 108.4 . . ? N31 C313 H31H 108.4 . . ? C314 C313 H31H 108.4 . . ? H31G C313 H31H 107.4 . . ? O35 C314 C313 110.1(9) . . ? O35 C314 H31I 109.6 . . ? C313 C314 H31I 109.6 . . ? O35 C314 H31J 109.6 . . ? C313 C314 H31J 109.6 . . ? H31I C314 H31J 108.2 . . ? O35 C315 C316 109.3(9) . . ? O35 C315 H31K 109.8 . . ? C316 C315 H31K 109.8 . . ? O35 C315 H31L 109.8 . . ? C316 C315 H31L 109.8 . . ? H31K C315 H31L 108.3 . . ? O36 C316 C315 109.6(10) . . ? O36 C316 H31M 109.7 . . ? C315 C316 H31M 109.7 . . ? O36 C316 H31N 109.7 . . ? C315 C316 H31N 109.7 . . ? H31M C316 H31N 108.2 . . ? O36 C317 C318 109.6(9) . . ? O36 C317 H31O 109.8 . . ? C318 C317 H31O 109.8 . . ? O36 C317 H31P 109.8 . . ? C318 C317 H31P 109.8 . . ? H31O C317 H31P 108.2 . . ? N32 C318 C317 114.4(9) . . ? N32 C318 H31Q 108.7 . . ? C317 C318 H31Q 108.7 . . ? N32 C318 H31R 108.7 . . ? C317 C318 H31R 108.7 . . ? H31Q C318 H31R 107.6 . . ? N41 C401 C402 116.1(10) . . ? N41 C401 H40A 108.2 . . ? C402 C401 H40A 108.2 . . ? N41 C401 H40B 108.2 . . ? C402 C401 H40B 108.2 . . ? H40A C401 H40B 107.4 . . ? O41 C402 C401 108.0(9) . . ? O41 C402 H40C 110.1 . . ? C401 C402 H40C 110.1 . . ? O41 C402 H40D 110.1 . . ? C401 C402 H40D 110.1 . . ? H40C C402 H40D 108.4 . . ? O41 C403 C404 109.9(10) . . ? O41 C403 H40E 109.7 . . ? C404 C403 H40E 109.7 . . ? O41 C403 H40F 109.7 . . ? C404 C403 H40F 109.7 . . ? H40E C403 H40F 108.2 . . ? O42 C404 C403 108.7(10) . . ? O42 C404 H40G 109.9 . . ? C403 C404 H40G 109.9 . . ? O42 C404 H40H 109.9 . . ? C403 C404 H40H 109.9 . . ? H40G C404 H40H 108.3 . . ? O42 C405 C406 109.5(9) . . ? O42 C405 H40I 109.8 . . ? C406 C405 H40I 109.8 . . ? O42 C405 H40J 109.8 . . ? C406 C405 H40J 109.8 . . ? H40I C405 H40J 108.2 . . ? N42 C406 C405 114.2(9) . . ? N42 C406 H40K 108.7 . . ? C405 C406 H40K 108.7 . . ? N42 C406 H40L 108.7 . . ? C405 C406 H40L 108.7 . . ? H40K C406 H40L 107.6 . . ? N41 C407 C408 114.6(9) . . ? N41 C407 H40M 108.6 . . ? C408 C407 H40M 108.6 . . ? N41 C407 H40N 108.6 . . ? C408 C407 H40N 108.6 . . ? H40M C407 H40N 107.6 . . ? O43 C408 C407 108.3(9) . . ? O43 C408 H40O 110.0 . . ? C407 C408 H40O 110.0 . . ? O43 C408 H40P 110.0 . . ? C407 C408 H40P 110.0 . . ? H40O C408 H40P 108.4 . . ? O43 C409 C410 110.3(9) . . ? O43 C409 H40Q 109.6 . . ? C410 C409 H40Q 109.6 . . ? O43 C409 H40R 109.6 . . ? C410 C409 H40R 109.6 . . ? H40Q C409 H40R 108.1 . . ? O44 C410 C409 108.5(9) . . ? O44 C410 H41A 110.0 . . ? C409 C410 H41A 110.0 . . ? O44 C410 H41B 110.0 . . ? C409 C410 H41B 110.0 . . ? H41A C410 H41B 108.4 . . ? O44 C411 C412 108.4(8) . . ? O44 C411 H41C 110.0 . . ? C412 C411 H41C 110.0 . . ? O44 C411 H41D 110.0 . . ? C412 C411 H41D 110.0 . . ? H41C C411 H41D 108.4 . . ? N42 C412 C411 113.8(10) . . ? N42 C412 H41E 108.8 . . ? C411 C412 H41E 108.8 . . ? N42 C412 H41F 108.8 . . ? C411 C412 H41F 108.8 . . ? H41E C412 H41F 107.7 . . ? N41 C413 C414 114.1(9) . . ? N41 C413 H41G 108.7 . . ? C414 C413 H41G 108.7 . . ? N41 C413 H41H 108.7 . . ? C414 C413 H41H 108.7 . . ? H41G C413 H41H 107.6 . . ? O45 C414 C413 110.0(9) . . ? O45 C414 H41I 109.7 . . ? C413 C414 H41I 109.7 . . ? O45 C414 H41J 109.7 . . ? C413 C414 H41J 109.7 . . ? H41I C414 H41J 108.2 . . ? O45 C415 C416 108.7(8) . . ? O45 C415 H41K 109.9 . . ? C416 C415 H41K 109.9 . . ? O45 C415 H41L 109.9 . . ? C416 C415 H41L 109.9 . . ? H41K C415 H41L 108.3 . . ? O46 C416 C415 108.9(9) . . ? O46 C416 H41M 109.9 . . ? C415 C416 H41M 109.9 . . ? O46 C416 H41N 109.9 . . ? C415 C416 H41N 109.9 . . ? H41M C416 H41N 108.3 . . ? O46 C417 C418 109.5(9) . . ? O46 C417 H41O 109.8 . . ? C418 C417 H41O 109.8 . . ? O46 C417 H41P 109.8 . . ? C418 C417 H41P 109.8 . . ? H41O C417 H41P 108.2 . . ? N42 C418 C417 113.2(9) . . ? N42 C418 H41Q 108.9 . . ? C417 C418 H41Q 108.9 . . ? N42 C418 H41R 108.9 . . ? C417 C418 H41R 108.9 . . ? H41Q C418 H41R 107.8 . . ? N51 C501 C502 113.7(9) . . ? N51 C501 H50A 108.8 . . ? C502 C501 H50A 108.8 . . ? N51 C501 H50B 108.8 . . ? C502 C501 H50B 108.8 . . ? H50A C501 H50B 107.7 . . ? O51 C502 C501 110.1(9) . . ? O51 C502 H50C 109.6 . . ? C501 C502 H50C 109.6 . . ? O51 C502 H50D 109.6 . . ? C501 C502 H50D 109.6 . . ? H50C C502 H50D 108.2 . . ? O51 C503 C504 108.7(9) . . ? O51 C503 H50E 110.0 . . ? C504 C503 H50E 110.0 . . ? O51 C503 H50F 110.0 . . ? C504 C503 H50F 110.0 . . ? H50E C503 H50F 108.3 . . ? O52 C504 C503 109.5(9) . . ? O52 C504 H50G 109.8 . . ? C503 C504 H50G 109.8 . . ? O52 C504 H50H 109.8 . . ? C503 C504 H50H 109.8 . . ? H50G C504 H50H 108.2 . . ? O52 C505 C506 112.4(8) . . ? O52 C505 H50I 109.1 . . ? C506 C505 H50I 109.1 . . ? O52 C505 H50J 109.1 . . ? C506 C505 H50J 109.1 . . ? H50I C505 H50J 107.9 . . ? N52 C506 C505 112.6(9) . . ? N52 C506 H50K 109.1 . . ? C505 C506 H50K 109.1 . . ? N52 C506 H50L 109.1 . . ? C505 C506 H50L 109.1 . . ? H50K C506 H50L 107.8 . . ? N51 C507 C508 113.9(9) . . ? N51 C507 H50M 108.8 . . ? C508 C507 H50M 108.8 . . ? N51 C507 H50N 108.8 . . ? C508 C507 H50N 108.8 . . ? H50M C507 H50N 107.7 . . ? O53 C508 C507 106.5(9) . . ? O53 C508 H50O 110.4 . . ? C507 C508 H50O 110.4 . . ? O53 C508 H50P 110.4 . . ? C507 C508 H50P 110.4 . . ? H50O C508 H50P 108.6 . . ? C510 C509 O53 110.7(9) . . ? C510 C509 H50Q 109.5 . . ? O53 C509 H50Q 109.5 . . ? C510 C509 H50R 109.5 . . ? O53 C509 H50R 109.5 . . ? H50Q C509 H50R 108.1 . . ? O54 C510 C509 109.3(9) . . ? O54 C510 H51A 109.8 . . ? C509 C510 H51A 109.8 . . ? O54 C510 H51B 109.8 . . ? C509 C510 H51B 109.8 . . ? H51A C510 H51B 108.3 . . ? O54 C511 C512 112.5(10) . . ? O54 C511 H51C 109.1 . . ? C512 C511 H51C 109.1 . . ? O54 C511 H51D 109.1 . . ? C512 C511 H51D 109.1 . . ? H51C C511 H51D 107.8 . . ? C511 C512 N52 114.8(9) . . ? C511 C512 H51E 108.6 . . ? N52 C512 H51E 108.6 . . ? C511 C512 H51F 108.6 . . ? N52 C512 H51F 108.6 . . ? H51E C512 H51F 107.5 . . ? N51 C513 C514 113.9(9) . . ? N51 C513 H51G 108.8 . . ? C514 C513 H51G 108.8 . . ? N51 C513 H51H 108.8 . . ? C514 C513 H51H 108.8 . . ? H51G C513 H51H 107.7 . . ? O55 C514 C513 109.4(9) . . ? O55 C514 H51I 109.8 . . ? C513 C514 H51I 109.8 . . ? O55 C514 H51J 109.8 . . ? C513 C514 H51J 109.8 . . ? H51I C514 H51J 108.2 . . ? O55 C515 C516 109.1(10) . . ? O55 C515 H51K 109.9 . . ? C516 C515 H51K 109.9 . . ? O55 C515 H51L 109.9 . . ? C516 C515 H51L 109.9 . . ? H51K C515 H51L 108.3 . . ? O56 C516 C515 109.8(10) . . ? O56 C516 H51M 109.7 . . ? C515 C516 H51M 109.7 . . ? O56 C516 H51N 109.7 . . ? C515 C516 H51N 109.7 . . ? H51M C516 H51N 108.2 . . ? O56 C517 C518 109.5(9) . . ? O56 C517 H51O 109.8 . . ? C518 C517 H51O 109.8 . . ? O56 C517 H51P 109.8 . . ? C518 C517 H51P 109.8 . . ? H51O C517 H51P 108.2 . . ? N52 C518 C517 112.2(10) . . ? N52 C518 H51Q 109.2 . . ? C517 C518 H51Q 109.2 . . ? N52 C518 H51R 109.2 . . ? C517 C518 H51R 109.2 . . ? H51Q C518 H51R 107.9 . . ? N61 C601 C602 114.2(8) . . ? N61 C601 H60A 108.7 . . ? C602 C601 H60A 108.7 . . ? N61 C601 H60B 108.7 . . ? C602 C601 H60B 108.7 . . ? H60A C601 H60B 107.6 . . ? O61 C602 C601 110.0(9) . . ? O61 C602 H60C 109.7 . . ? C601 C602 H60C 109.7 . . ? O61 C602 H60D 109.7 . . ? C601 C602 H60D 109.7 . . ? H60C C602 H60D 108.2 . . ? O61 C603 C604 108.1(9) . . ? O61 C603 H60E 110.1 . . ? C604 C603 H60E 110.1 . . ? O61 C603 H60F 110.1 . . ? C604 C603 H60F 110.1 . . ? H60E C603 H60F 108.4 . . ? O62 C604 C603 109.4(9) . . ? O62 C604 H60G 109.8 . . ? C603 C604 H60G 109.8 . . ? O62 C604 H60H 109.8 . . ? C603 C604 H60H 109.8 . . ? H60G C604 H60H 108.2 . . ? O62 C605 C606 109.5(9) . . ? O62 C605 H60I 109.8 . . ? C606 C605 H60I 109.8 . . ? O62 C605 H60J 109.8 . . ? C606 C605 H60J 109.8 . . ? H60I C605 H60J 108.2 . . ? N62 C606 C605 112.7(8) . . ? N62 C606 H60K 109.0 . . ? C605 C606 H60K 109.0 . . ? N62 C606 H60L 109.0 . . ? C605 C606 H60L 109.0 . . ? H60K C606 H60L 107.8 . . ? N61 C607 C608 113.5(8) . . ? N61 C607 H60M 108.9 . . ? C608 C607 H60M 108.9 . . ? N61 C607 H60N 108.9 . . ? C608 C607 H60N 108.9 . . ? H60M C607 H60N 107.7 . . ? O63 C608 C607 109.3(8) . . ? O63 C608 H60O 109.8 . . ? C607 C608 H60O 109.8 . . ? O63 C608 H60P 109.8 . . ? C607 C608 H60P 109.8 . . ? H60O C608 H60P 108.3 . . ? O63 C609 C610 108.1(9) . . ? O63 C609 H60Q 110.1 . . ? C610 C609 H60Q 110.1 . . ? O63 C609 H60R 110.1 . . ? C610 C609 H60R 110.1 . . ? H60Q C609 H60R 108.4 . . ? O64 C610 C609 109.4(8) . . ? O64 C610 H61A 109.8 . . ? C609 C610 H61A 109.8 . . ? O64 C610 H61B 109.8 . . ? C609 C610 H61B 109.8 . . ? H61A C610 H61B 108.2 . . ? O64 C611 C612 110.0(9) . . ? O64 C611 H61C 109.7 . . ? C612 C611 H61C 109.7 . . ? O64 C611 H61D 109.7 . . ? C612 C611 H61D 109.7 . . ? H61C C611 H61D 108.2 . . ? N62 C612 C611 114.4(8) . . ? N62 C612 H61E 108.7 . . ? C611 C612 H61E 108.7 . . ? N62 C612 H61F 108.7 . . ? C611 C612 H61F 108.7 . . ? H61E C612 H61F 107.6 . . ? N61 C613 C614 113.1(9) . . ? N61 C613 H61G 109.0 . . ? C614 C613 H61G 109.0 . . ? N61 C613 H61H 109.0 . . ? C614 C613 H61H 109.0 . . ? H61G C613 H61H 107.8 . . ? O65 C614 C613 109.8(8) . . ? O65 C614 H61I 109.7 . . ? C613 C614 H61I 109.7 . . ? O65 C614 H61J 109.7 . . ? C613 C614 H61J 109.7 . . ? H61I C614 H61J 108.2 . . ? O65 C615 C616 109.5(10) . . ? O65 C615 H61K 109.8 . . ? C616 C615 H61K 109.8 . . ? O65 C615 H61L 109.8 . . ? C616 C615 H61L 109.8 . . ? H61K C615 H61L 108.2 . . ? O66 C616 C615 111.3(10) . . ? O66 C616 H61M 109.4 . . ? C615 C616 H61M 109.4 . . ? O66 C616 H61N 109.4 . . ? C615 C616 H61N 109.4 . . ? H61M C616 H61N 108.0 . . ? O66 C617 C618 108.7(9) . . ? O66 C617 H61O 110.0 . . ? C618 C617 H61O 110.0 . . ? O66 C617 H61P 110.0 . . ? C618 C617 H61P 110.0 . . ? H61O C617 H61P 108.3 . . ? N62 C618 C617 112.2(9) . . ? N62 C618 H61Q 109.2 . . ? C617 C618 H61Q 109.2 . . ? N62 C618 H61R 109.2 . . ? C617 C618 H61R 109.2 . . ? H61Q C618 H61R 107.9 . . ? C1S N1S H1S3 109.5 . . ? C1S N1S H1S4 109.5 . . ? H1S3 N1S H1S4 109.5 . . ? C1S N1S H1S5 109.5 . . ? H1S3 N1S H1S5 109.5 . . ? H1S4 N1S H1S5 109.5 . . ? N1S C1S C2S 114(2) . . ? N1S C1S H1S1 108.8 . . ? C2S C1S H1S1 108.8 . . ? N1S C1S H1S2 108.8 . . ? C2S C1S H1S2 108.8 . . ? H1S1 C1S H1S2 107.7 . . ? N2S C2S C1S 106(3) . . ? N2S C2S H2S1 110.5 . . ? C1S C2S H2S1 110.5 . . ? N2S C2S H2S2 110.5 . . ? C1S C2S H2S2 110.5 . . ? H2S1 C2S H2S2 108.7 . . ? C2S N2S H2S3 109.5 . . ? C2S N2S H2S4 109.5 . . ? H2S3 N2S H2S4 109.5 . . ? C2S N2S H2S5 109.5 . . ? H2S3 N2S H2S5 109.5 . . ? H2S4 N2S H2S5 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.196 _refine_diff_density_min -4.999 _refine_diff_density_rms 0.339