# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jose Goicoechea' _publ_contact_author_email JOSE.GOICOECHEA@CHEM.OX.AC.UK _publ_section_title ; [Hg3(Ge9)4]10-: A nanometric molecular rod precursor to polymeric mercury-linked cluster chains. ; _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' # Attachment 'manuscript.cif' data_[Hg3(Ge9)4] _database_code_depnum_ccdc_archive 'CCDC 693235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)10][Hg3(Ge9)4]*2en*2tol ; _chemical_name_common (K-(2,2,2-crypt)10)(Hg3(Ge9)4)*2en*2tol _chemical_melting_point ? _chemical_formula_moiety '10(C18 H36 K N2 O6), Ge9 Hg3, 2(C7 H8), 2(C2 H8 N2)' _chemical_formula_sum 'C198 H392 Ge36 Hg3 K10 N24 O60' _chemical_formula_weight 7672.95 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' Ge Ge 0.1550 1.8000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3890 9.2270 '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' _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 14.0120(1) _cell_length_b 18.0241(1) _cell_length_c 30.5830(1) _cell_angle_alpha 78.5788(2) _cell_angle_beta 88.0124(2) _cell_angle_gamma 72.0656(2) _cell_volume 7200.17(7) _cell_formula_units_Z 1 _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-green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3809 _exptl_absorpt_coefficient_mu 5.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1371 _exptl_absorpt_correction_T_max 0.8101 _exptl_absorpt_process_details 'Blessing, R.H. (1995) Acta Cryst. A51, 33-38' _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64671 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 27.51 _reflns_number_total 32797 _reflns_number_gt 25261 _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^)+(0.0739P)^2^+7.5347P] 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 32797 _refine_ls_number_parameters 1492 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.044 _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 Ge1A Ge 0.35024(4) 0.63003(3) 0.200010(18) 0.03393(12) Uani 1 1 d . . . Ge2A Ge 0.30742(4) 0.71852(3) 0.120359(18) 0.03254(12) Uani 1 1 d . . . Ge3A Ge 0.26575(4) 0.77509(3) 0.204861(18) 0.03417(12) Uani 1 1 d . . . Ge4A Ge 0.17908(4) 0.66046(3) 0.235317(17) 0.03032(12) Uani 1 1 d . . . Ge5A Ge 0.22891(5) 0.60385(3) 0.14659(2) 0.03835(13) Uani 1 1 d . . . Ge6A Ge 0.17601(5) 0.85205(3) 0.13079(2) 0.04470(15) Uani 1 1 d . . . Ge7A Ge 0.06157(4) 0.80203(4) 0.18884(2) 0.04019(14) Uani 1 1 d . . . Ge8A Ge 0.05042(5) 0.66756(5) 0.17694(2) 0.04894(17) Uani 1 1 d . . . Ge9A Ge 0.11248(4) 0.74437(4) 0.106732(19) 0.04109(14) Uani 1 1 d . . . Ge1B Ge 0.30693(4) 0.78370(3) 0.467502(19) 0.03550(13) Uani 1 1 d . . . Ge2B Ge 0.29049(4) 0.83155(3) 0.382174(18) 0.02860(11) Uani 1 1 d . . . Ge3B Ge 0.22373(4) 0.93399(3) 0.441256(18) 0.02924(11) Uani 1 1 d . . . Ge4B Ge 0.12123(4) 0.82942(3) 0.486188(17) 0.03100(12) Uani 1 1 d . . . Ge5B Ge 0.19036(4) 0.72973(3) 0.426203(19) 0.03395(13) Uani 1 1 d . . . Ge6B Ge 0.15193(4) 0.96958(3) 0.360570(18) 0.03185(12) Uani 1 1 d . . . Ge7B Ge 0.02996(4) 0.95772(3) 0.423900(18) 0.03460(13) Uani 1 1 d . . . Ge8B Ge 0.00226(4) 0.82462(4) 0.42520(2) 0.04294(15) Uani 1 1 d . . . Ge9B Ge 0.11279(4) 0.83935(3) 0.356846(17) 0.02992(11) Uani 1 1 d . . . Hg1 Hg 0.153340(15) 0.774862(12) 0.286506(7) 0.03319(6) Uani 1 1 d . . . Hg2 Hg 0.0000 1.0000 0.5000 0.03612(7) Uani 1 2 d S . . K1 K 0.65292(8) -0.02128(6) 0.08929(4) 0.0315(2) Uani 1 1 d . . . N11 N 0.8316(4) 0.0031(3) 0.03784(16) 0.0434(11) Uani 1 1 d . . . N12 N 0.4777(3) -0.0526(3) 0.14019(15) 0.0389(10) Uani 1 1 d . . . O11 O 0.7824(3) 0.0454(2) 0.12631(12) 0.0399(9) Uani 1 1 d . . . O12 O 0.6304(3) 0.0001(2) 0.17722(12) 0.0381(8) Uani 1 1 d . . . O13 O 0.7908(4) -0.1512(3) 0.0590(2) 0.100(3) Uani 1 1 d . . . O14 O 0.6418(3) -0.1760(3) 0.11159(17) 0.0602(13) Uani 1 1 d . . . O15 O 0.6186(3) 0.0843(2) 0.00610(12) 0.0409(9) Uani 1 1 d . . . O16 O 0.4539(3) 0.0739(3) 0.06001(13) 0.0458(10) Uani 1 1 d . . . C101 C 0.8762(5) 0.0495(5) 0.0604(2) 0.0571(18) Uani 1 1 d . . . H10A H 0.8361 0.1063 0.0523 0.069 Uiso 1 1 calc R . . H10B H 0.9447 0.0444 0.0494 0.069 Uiso 1 1 calc R . . C102 C 0.8821(5) 0.0247(4) 0.1105(2) 0.0504(15) Uani 1 1 d . . . H10C H 0.9149 -0.0333 0.1193 0.061 Uiso 1 1 calc R . . H10D H 0.9219 0.0523 0.1234 0.061 Uiso 1 1 calc R . . C103 C 0.7829(4) 0.0319(4) 0.17349(19) 0.0424(13) Uani 1 1 d . . . H10E H 0.8188 0.0646 0.1843 0.051 Uiso 1 1 calc R . . H10F H 0.8182 -0.0248 0.1859 0.051 Uiso 1 1 calc R . . C104 C 0.6781(4) 0.0531(3) 0.18854(19) 0.0401(13) Uani 1 1 d . . . H10G H 0.6774 0.0498 0.2212 0.048 Uiso 1 1 calc R . . H10H H 0.6413 0.1084 0.1741 0.048 Uiso 1 1 calc R . . C105 C 0.5326(4) 0.0111(4) 0.19569(19) 0.0413(13) Uani 1 1 d . . . H10I H 0.4863 0.0633 0.1813 0.050 Uiso 1 1 calc R . . H10J H 0.5363 0.0098 0.2281 0.050 Uiso 1 1 calc R . . C106 C 0.4949(4) -0.0543(4) 0.1877(2) 0.0451(14) Uani 1 1 d . . . H10K H 0.5440 -0.1060 0.2009 0.054 Uiso 1 1 calc R . . H10L H 0.4311 -0.0507 0.2034 0.054 Uiso 1 1 calc R . . C107 C 0.9056(4) -0.0742(4) 0.0365(2) 0.0540(17) Uani 1 1 d . . . H10M H 0.9433 -0.0942 0.0654 0.065 Uiso 1 1 calc R . . H10N H 0.9541 -0.0663 0.0130 0.065 Uiso 1 1 calc R . . C108 C 0.8620(5) -0.1374(4) 0.0273(2) 0.0576(18) Uani 1 1 d . . . H10O H 0.8298 -0.1202 -0.0028 0.069 Uiso 1 1 calc R . . H10P H 0.9170 -0.1876 0.0278 0.069 Uiso 1 1 calc R . . C109 C 0.8086(6) -0.2091(7) 0.0879(4) 0.118(4) Uani 1 1 d U . . H10Q H 0.8609 -0.2050 0.1074 0.141 Uiso 1 1 calc R . . H10R H 0.8412 -0.2545 0.0732 0.141 Uiso 1 1 calc R . . C110 C 0.7382(4) -0.2338(4) 0.1173(2) 0.0503(15) Uani 1 1 d U . . H11A H 0.7331 -0.2846 0.1115 0.060 Uiso 1 1 calc R . . H11B H 0.7625 -0.2431 0.1485 0.060 Uiso 1 1 calc R . . C111 C 0.5690(5) -0.1958(4) 0.1419(2) 0.0495(15) Uani 1 1 d . . . H11C H 0.5933 -0.2040 0.1731 0.059 Uiso 1 1 calc R . . H11D H 0.5590 -0.2459 0.1374 0.059 Uiso 1 1 calc R . . C112 C 0.4726(5) -0.1307(4) 0.1342(2) 0.0525(16) Uani 1 1 d . . . H11E H 0.4479 -0.1250 0.1034 0.063 Uiso 1 1 calc R . . H11F H 0.4228 -0.1459 0.1549 0.063 Uiso 1 1 calc R . . C113 C 0.7953(5) 0.0464(4) -0.0074(2) 0.0510(16) Uani 1 1 d . . . H11G H 0.7840 0.0086 -0.0246 0.061 Uiso 1 1 calc R . . H11H H 0.8482 0.0674 -0.0223 0.061 Uiso 1 1 calc R . . C114 C 0.7004(5) 0.1141(4) -0.0086(2) 0.0523(16) Uani 1 1 d . . . H11I H 0.7085 0.1496 0.0109 0.063 Uiso 1 1 calc R . . H11J H 0.6860 0.1454 -0.0395 0.063 Uiso 1 1 calc R . . C115 C 0.5246(5) 0.1448(3) 0.0014(2) 0.0481(15) Uani 1 1 d . . . H11K H 0.5137 0.1740 -0.0299 0.058 Uiso 1 1 calc R . . H11L H 0.5244 0.1831 0.0206 0.058 Uiso 1 1 calc R . . C116 C 0.4431(4) 0.1097(4) 0.0142(2) 0.0516(16) Uani 1 1 d . . . H11M H 0.3774 0.1516 0.0083 0.062 Uiso 1 1 calc R . . H11N H 0.4455 0.0692 -0.0039 0.062 Uiso 1 1 calc R . . C117 C 0.3777(4) 0.0380(4) 0.0739(2) 0.0516(16) Uani 1 1 d . . . H11O H 0.3860 -0.0078 0.0593 0.062 Uiso 1 1 calc R . . H11P H 0.3110 0.0769 0.0648 0.062 Uiso 1 1 calc R . . C118 C 0.3835(4) 0.0101(4) 0.1241(2) 0.0487(15) Uani 1 1 d . . . H11Q H 0.3769 0.0561 0.1384 0.058 Uiso 1 1 calc R . . H11R H 0.3264 -0.0103 0.1334 0.058 Uiso 1 1 calc R . . K2 K 0.81434(9) 0.45995(7) 0.07434(4) 0.0364(2) Uani 1 1 d . . . N21 N 0.6890(6) 0.5924(5) 0.0057(2) 0.098(3) Uani 1 1 d . . . N22 N 0.9430(7) 0.3260(4) 0.1429(2) 0.086(2) Uani 1 1 d . . . O21 O 0.6246(4) 0.5503(4) 0.0976(2) 0.0844(19) Uani 1 1 d . . . O22 O 0.7570(5) 0.4426(4) 0.16482(16) 0.0789(17) Uani 1 1 d . . . O23 O 0.8752(5) 0.5941(3) 0.0409(2) 0.0814(18) Uani 1 1 d . . . O24 O 1.0109(3) 0.4593(3) 0.09443(19) 0.0645(14) Uani 1 1 d . . . O25 O 0.7581(4) 0.4247(3) -0.00340(15) 0.0649(14) Uani 1 1 d . . . O26 O 0.8556(4) 0.2982(3) 0.06413(15) 0.0673(14) Uani 1 1 d . . . C201 C 0.5858(8) 0.6119(6) 0.0212(4) 0.124(5) Uani 1 1 d . . . H20A H 0.5590 0.5678 0.0193 0.149 Uiso 1 1 calc R . . H20B H 0.5441 0.6602 0.0010 0.149 Uiso 1 1 calc R . . C202 C 0.5765(6) 0.6259(6) 0.0680(4) 0.107(4) Uani 1 1 d . . . H20C H 0.6096 0.6658 0.0714 0.128 Uiso 1 1 calc R . . H20D H 0.5049 0.6462 0.0752 0.128 Uiso 1 1 calc R . . C203 C 0.6173(7) 0.5619(7) 0.1416(4) 0.095(3) Uani 1 1 d . . . H20E H 0.5474 0.5911 0.1477 0.114 Uiso 1 1 calc R . . H20F H 0.6614 0.5931 0.1470 0.114 Uiso 1 1 calc R . . C204 C 0.6486(8) 0.4833(8) 0.1703(3) 0.100(4) Uani 1 1 d . . . H20G H 0.6083 0.4510 0.1626 0.120 Uiso 1 1 calc R . . H20H H 0.6367 0.4883 0.2018 0.120 Uiso 1 1 calc R . . C205 C 0.7878(11) 0.3679(8) 0.1887(3) 0.115(5) Uani 1 1 d . . . H20I H 0.7575 0.3337 0.1759 0.138 Uiso 1 1 calc R . . H20J H 0.7661 0.3675 0.2199 0.138 Uiso 1 1 calc R . . C206 C 0.9015(12) 0.3358(6) 0.1879(3) 0.115(5) Uani 1 1 d . . . H20K H 0.9302 0.3723 0.1993 0.138 Uiso 1 1 calc R . . H20L H 0.9239 0.2836 0.2085 0.138 Uiso 1 1 calc R . . C207 C 0.7262(10) 0.6620(5) -0.0001(3) 0.117(5) Uani 1 1 d . . . H20M H 0.6975 0.6990 -0.0282 0.141 Uiso 1 1 calc R . . H20N H 0.7030 0.6903 0.0248 0.141 Uiso 1 1 calc R . . C208 C 0.8364(11) 0.6389(5) -0.0012(4) 0.134(5) Uani 1 1 d . . . H20O H 0.8609 0.6069 -0.0245 0.160 Uiso 1 1 calc R . . H20P H 0.8586 0.6870 -0.0083 0.160 Uiso 1 1 calc R . . C209 C 0.9811(9) 0.5837(6) 0.0460(5) 0.123(5) Uani 1 1 d . . . H20Q H 0.9922 0.6363 0.0418 0.147 Uiso 1 1 calc R . . H20R H 1.0189 0.5554 0.0232 0.147 Uiso 1 1 calc R . . C210 C 1.0170(7) 0.5382(6) 0.0903(5) 0.099(4) Uani 1 1 d . . . H21A H 1.0873 0.5361 0.0952 0.119 Uiso 1 1 calc R . . H21B H 0.9756 0.5643 0.1132 0.119 Uiso 1 1 calc R . . C211 C 1.0547(6) 0.4123(6) 0.1357(3) 0.091(3) Uani 1 1 d . . . H21C H 1.0204 0.4368 0.1606 0.109 Uiso 1 1 calc R . . H21D H 1.1264 0.4089 0.1373 0.109 Uiso 1 1 calc R . . C212 C 1.0447(9) 0.3290(6) 0.1399(3) 0.117(5) Uani 1 1 d . . . H21E H 1.0753 0.3071 0.1137 0.140 Uiso 1 1 calc R . . H21F H 1.0834 0.2943 0.1668 0.140 Uiso 1 1 calc R . . C213 C 0.6948(12) 0.5613(6) -0.0356(3) 0.165(7) Uani 1 1 d . . . H21G H 0.7612 0.5587 -0.0485 0.198 Uiso 1 1 calc R . . H21H H 0.6435 0.6001 -0.0571 0.198 Uiso 1 1 calc R . . C214 C 0.6804(9) 0.4821(6) -0.0316(3) 0.135(6) Uani 1 1 d . . . H21I H 0.6143 0.4830 -0.0189 0.162 Uiso 1 1 calc R . . H21J H 0.6826 0.4682 -0.0614 0.162 Uiso 1 1 calc R . . C215 C 0.7537(6) 0.3461(5) -0.0017(2) 0.065(2) Uani 1 1 d . . . H21K H 0.7442 0.3382 -0.0322 0.078 Uiso 1 1 calc R . . H21L H 0.6966 0.3377 0.0164 0.078 Uiso 1 1 calc R . . C216 C 0.8488(7) 0.2893(4) 0.0186(2) 0.062(2) Uani 1 1 d . . . H21M H 0.8505 0.2343 0.0178 0.074 Uiso 1 1 calc R . . H21N H 0.9063 0.3003 0.0017 0.074 Uiso 1 1 calc R . . C217 C 0.9444(10) 0.2443(4) 0.0854(3) 0.110(4) Uani 1 1 d . . . H21O H 1.0034 0.2588 0.0724 0.132 Uiso 1 1 calc R . . H21P H 0.9510 0.1897 0.0815 0.132 Uiso 1 1 calc R . . C218 C 0.9386(12) 0.2481(5) 0.1351(3) 0.139(6) Uani 1 1 d . . . H21Q H 0.8751 0.2396 0.1468 0.167 Uiso 1 1 calc R . . H21R H 0.9949 0.2049 0.1517 0.167 Uiso 1 1 calc R . . K3 K 0.74224(7) 0.57258(6) 0.36720(3) 0.0251(2) Uani 1 1 d . . . N31 N 0.8838(3) 0.5498(2) 0.29241(14) 0.0311(9) Uani 1 1 d . . . N32 N 0.6091(3) 0.5874(2) 0.44222(14) 0.0301(9) Uani 1 1 d . . . O31 O 0.6676(2) 0.6310(2) 0.27967(12) 0.0357(8) Uani 1 1 d . . . O32 O 0.5358(2) 0.6101(2) 0.34890(12) 0.0333(8) Uani 1 1 d . . . O33 O 0.8303(3) 0.4160(2) 0.34767(13) 0.0364(8) Uani 1 1 d . . . O34 O 0.7277(3) 0.4388(2) 0.42599(14) 0.0426(9) Uani 1 1 d . . . O35 O 0.9053(2) 0.62969(19) 0.36259(12) 0.0309(7) Uani 1 1 d . . . O36 O 0.7510(2) 0.6769(2) 0.42215(11) 0.0313(7) Uani 1 1 d . . . C301 C 0.8358(4) 0.6133(4) 0.25485(18) 0.0398(13) Uani 1 1 d . . . H30A H 0.8777 0.6062 0.2283 0.048 Uiso 1 1 calc R . . H30B H 0.8336 0.6650 0.2621 0.048 Uiso 1 1 calc R . . C302 C 0.7308(4) 0.6164(4) 0.24314(18) 0.0432(14) Uani 1 1 d . . . H30C H 0.7045 0.6592 0.2168 0.052 Uiso 1 1 calc R . . H30D H 0.7319 0.5653 0.2355 0.052 Uiso 1 1 calc R . . C303 C 0.5684(4) 0.6308(4) 0.27108(19) 0.0411(13) Uani 1 1 d . . . H30E H 0.5686 0.5760 0.2707 0.049 Uiso 1 1 calc R . . H30F H 0.5435 0.6645 0.2416 0.049 Uiso 1 1 calc R . . C304 C 0.5018(4) 0.6620(3) 0.30646(19) 0.0360(12) Uani 1 1 d . . . H30G H 0.5030 0.7163 0.3074 0.043 Uiso 1 1 calc R . . H30H H 0.4320 0.6648 0.2999 0.043 Uiso 1 1 calc R . . C305 C 0.4733(4) 0.6391(3) 0.3834(2) 0.0370(12) Uani 1 1 d . . . H30I H 0.4036 0.6406 0.3776 0.044 Uiso 1 1 calc R . . H30J H 0.4730 0.6940 0.3838 0.044 Uiso 1 1 calc R . . C306 C 0.5109(4) 0.5863(3) 0.4281(2) 0.0402(13) Uani 1 1 d . . . H30K H 0.4615 0.6033 0.4510 0.048 Uiso 1 1 calc R . . H30L H 0.5150 0.5310 0.4267 0.048 Uiso 1 1 calc R . . C307 C 0.9020(4) 0.4706(3) 0.2823(2) 0.0434(14) Uani 1 1 d . . . H30M H 0.9693 0.4366 0.2944 0.052 Uiso 1 1 calc R . . H30N H 0.9026 0.4752 0.2495 0.052 Uiso 1 1 calc R . . C308 C 0.8253(5) 0.4300(4) 0.3010(2) 0.0496(15) Uani 1 1 d . . . H30O H 0.7572 0.4641 0.2901 0.059 Uiso 1 1 calc R . . H30P H 0.8389 0.3790 0.2908 0.059 Uiso 1 1 calc R . . C309 C 0.7682(4) 0.3690(3) 0.3671(2) 0.0483(16) Uani 1 1 d . . . H30Q H 0.7942 0.3154 0.3597 0.058 Uiso 1 1 calc R . . H30R H 0.6992 0.3940 0.3543 0.058 Uiso 1 1 calc R . . C310 C 0.7660(4) 0.3617(3) 0.4158(2) 0.0411(14) Uani 1 1 d . . . H31A H 0.7229 0.3289 0.4286 0.049 Uiso 1 1 calc R . . H31B H 0.8346 0.3353 0.4289 0.049 Uiso 1 1 calc R . . C311 C 0.6765(5) 0.4394(3) 0.4669(2) 0.0477(15) Uani 1 1 d . . . H31C H 0.7184 0.3980 0.4908 0.057 Uiso 1 1 calc R . . H31D H 0.6129 0.4275 0.4639 0.057 Uiso 1 1 calc R . . C312 C 0.6550(5) 0.5193(4) 0.47884(19) 0.0481(15) Uani 1 1 d . . . H31E H 0.6095 0.5221 0.5044 0.058 Uiso 1 1 calc R . . H31F H 0.7186 0.5247 0.4888 0.058 Uiso 1 1 calc R . . C313 C 0.9799(4) 0.5587(3) 0.30578(19) 0.0351(11) Uani 1 1 d . . . H31G H 1.0227 0.5604 0.2794 0.042 Uiso 1 1 calc R . . H31H H 1.0153 0.5112 0.3282 0.042 Uiso 1 1 calc R . . C314 C 0.9684(4) 0.6310(3) 0.3247(2) 0.0373(12) Uani 1 1 d . . . H31I H 1.0349 0.6321 0.3338 0.045 Uiso 1 1 calc R . . H31J H 0.9380 0.6793 0.3018 0.045 Uiso 1 1 calc R . . C315 C 0.8938(4) 0.6967(3) 0.3823(2) 0.0409(13) Uani 1 1 d . . . H31O H 0.8501 0.7450 0.3629 0.049 Uiso 1 1 calc R . . H31P H 0.9601 0.7043 0.3855 0.049 Uiso 1 1 calc R . . C316 C 0.8486(4) 0.6850(3) 0.42729(19) 0.0387(12) Uani 1 1 d . . . H31Q H 0.8921 0.6366 0.4468 0.046 Uiso 1 1 calc R . . H31R H 0.8429 0.7311 0.4413 0.046 Uiso 1 1 calc R . . C317 C 0.6993(4) 0.6759(3) 0.46314(18) 0.0350(11) Uani 1 1 d . . . H31K H 0.6880 0.7272 0.4728 0.042 Uiso 1 1 calc R . . H31L H 0.7405 0.6330 0.4866 0.042 Uiso 1 1 calc R . . C318 C 0.5999(4) 0.6625(3) 0.45721(19) 0.0382(12) Uani 1 1 d . . . H31M H 0.5651 0.6620 0.4859 0.046 Uiso 1 1 calc R . . H31N H 0.5579 0.7075 0.4351 0.046 Uiso 1 1 calc R . . K4 K 0.24706(7) 0.34162(6) 0.37334(4) 0.0261(2) Uani 1 1 d . . . N41 N 0.1293(3) 0.2377(2) 0.40662(16) 0.0348(10) Uani 1 1 d . . . N42 N 0.3789(3) 0.4347(3) 0.34248(18) 0.0404(11) Uani 1 1 d . . . O41 O 0.1072(3) 0.3862(2) 0.43955(12) 0.0345(8) Uani 1 1 d . . . O42 O 0.1897(3) 0.49662(19) 0.38694(12) 0.0340(8) Uani 1 1 d . . . O43 O 0.1241(3) 0.3142(2) 0.31239(13) 0.0413(9) Uani 1 1 d . . . O44 O 0.2859(3) 0.3689(2) 0.28041(13) 0.0415(9) Uani 1 1 d . . . O45 O 0.3516(3) 0.1795(2) 0.40417(16) 0.0506(11) Uani 1 1 d . . . O46 O 0.4316(3) 0.3005(2) 0.4189(2) 0.0766(18) Uani 1 1 d . . . C401 C 0.0853(4) 0.2572(3) 0.4486(2) 0.0450(14) Uani 1 1 d . . . H40A H 0.1388 0.2373 0.4722 0.054 Uiso 1 1 calc R . . H40B H 0.0352 0.2288 0.4572 0.054 Uiso 1 1 calc R . . C402 C 0.0354(4) 0.3442(4) 0.4471(2) 0.0447(14) Uani 1 1 d . . . H40C H -0.0167 0.3655 0.4230 0.054 Uiso 1 1 calc R . . H40D H 0.0024 0.3518 0.4758 0.054 Uiso 1 1 calc R . . C403 C 0.0604(4) 0.4698(3) 0.4338(2) 0.0443(14) Uani 1 1 d . . . H40E H 0.0225 0.4823 0.4607 0.053 Uiso 1 1 calc R . . H40F H 0.0124 0.4880 0.4080 0.053 Uiso 1 1 calc R . . C404 C 0.1368(5) 0.5121(3) 0.42609(19) 0.0424(13) Uani 1 1 d . . . H40G H 0.1037 0.5700 0.4230 0.051 Uiso 1 1 calc R . . H40H H 0.1845 0.4942 0.4520 0.051 Uiso 1 1 calc R . . C405 C 0.2600(4) 0.5402(3) 0.3774(2) 0.0407(13) Uani 1 1 d . . . H40I H 0.3064 0.5274 0.4034 0.049 Uiso 1 1 calc R . . H40J H 0.2239 0.5979 0.3718 0.049 Uiso 1 1 calc R . . C406 C 0.3184(5) 0.5197(3) 0.3375(2) 0.0435(14) Uani 1 1 d . . . H40K H 0.2712 0.5337 0.3116 0.052 Uiso 1 1 calc R . . H40L H 0.3639 0.5527 0.3307 0.052 Uiso 1 1 calc R . . C407 C 0.0494(4) 0.2482(4) 0.3735(2) 0.0526(16) Uani 1 1 d . . . H40M H -0.0040 0.2989 0.3741 0.063 Uiso 1 1 calc R . . H40N H 0.0193 0.2045 0.3821 0.063 Uiso 1 1 calc R . . C408 C 0.0869(5) 0.2489(4) 0.3264(2) 0.0561(17) Uani 1 1 d . . . H40O H 0.1408 0.1987 0.3255 0.067 Uiso 1 1 calc R . . H40P H 0.0314 0.2530 0.3060 0.067 Uiso 1 1 calc R . . C409 C 0.1515(4) 0.3208(4) 0.2670(2) 0.0527(17) Uani 1 1 d . . . H40Q H 0.0916 0.3315 0.2476 0.063 Uiso 1 1 calc R . . H40R H 0.2009 0.2704 0.2625 0.063 Uiso 1 1 calc R . . C410 C 0.1958(5) 0.3872(4) 0.2551(2) 0.0571(18) Uani 1 1 d . . . H41A H 0.2100 0.3955 0.2229 0.069 Uiso 1 1 calc R . . H41B H 0.1474 0.4369 0.2612 0.069 Uiso 1 1 calc R . . C411 C 0.3413(6) 0.4251(4) 0.2655(2) 0.063(2) Uani 1 1 d . . . H41C H 0.2944 0.4800 0.2598 0.075 Uiso 1 1 calc R . . H41D H 0.3743 0.4150 0.2371 0.075 Uiso 1 1 calc R . . C412 C 0.4182(5) 0.4171(4) 0.2998(3) 0.0584(19) Uani 1 1 d . . . H41E H 0.4645 0.3621 0.3049 0.070 Uiso 1 1 calc R . . H41F H 0.4579 0.4532 0.2879 0.070 Uiso 1 1 calc R . . C413 C 0.1946(5) 0.1541(3) 0.4148(2) 0.0465(14) Uani 1 1 d . . . H41G H 0.1597 0.1209 0.4346 0.056 Uiso 1 1 calc R . . H41H H 0.2050 0.1357 0.3861 0.056 Uiso 1 1 calc R . . C414 C 0.2934(5) 0.1417(3) 0.4354(2) 0.0501(15) Uani 1 1 d . . . H41I H 0.2844 0.1644 0.4627 0.060 Uiso 1 1 calc R . . H41J H 0.3291 0.0840 0.4438 0.060 Uiso 1 1 calc R . . C415 C 0.4505(6) 0.1663(4) 0.4203(4) 0.094(3) Uani 1 1 d . . . H41K H 0.4716 0.1137 0.4406 0.113 Uiso 1 1 calc R . . H41L H 0.4953 0.1629 0.3945 0.113 Uiso 1 1 calc R . . C416 C 0.4661(8) 0.2178(5) 0.4412(4) 0.119(5) Uani 1 1 d . . . H41M H 0.5392 0.2032 0.4474 0.143 Uiso 1 1 calc R . . H41N H 0.4333 0.2129 0.4704 0.143 Uiso 1 1 calc R . . C417 C 0.5065(5) 0.3280(4) 0.3939(3) 0.078(3) Uani 1 1 d . . . H41O H 0.5286 0.2988 0.3693 0.093 Uiso 1 1 calc R . . H41P H 0.5655 0.3188 0.4135 0.093 Uiso 1 1 calc R . . C418 C 0.4617(4) 0.4150(4) 0.3755(3) 0.062(2) Uani 1 1 d . . . H41Q H 0.4364 0.4425 0.4006 0.074 Uiso 1 1 calc R . . H41R H 0.5152 0.4360 0.3614 0.074 Uiso 1 1 calc R . . K5 K 0.66572(7) 1.03251(6) 0.33349(3) 0.0267(2) Uani 1 1 d . . . N51 N 0.5367(3) 0.9275(3) 0.35732(16) 0.0405(11) Uani 1 1 d . . . N52 N 0.7898(3) 1.1450(2) 0.30621(15) 0.0341(10) Uani 1 1 d . . . O51 O 0.4663(2) 1.0876(2) 0.29707(13) 0.0365(8) Uani 1 1 d . . . O52 O 0.5739(3) 1.1976(2) 0.28341(12) 0.0384(9) Uani 1 1 d . . . O53 O 0.7219(3) 0.8804(2) 0.31120(12) 0.0369(8) Uani 1 1 d . . . O54 O 0.8266(2) 0.9914(2) 0.27760(12) 0.0314(7) Uani 1 1 d . . . O55 O 0.6276(3) 0.9864(2) 0.42353(12) 0.0366(8) Uani 1 1 d . . . O56 O 0.7557(3) 1.0782(2) 0.39640(12) 0.0416(9) Uani 1 1 d . . . C501 C 0.4462(4) 0.9605(4) 0.3278(2) 0.0482(15) Uani 1 1 d . . . H50A H 0.3955 0.9347 0.3403 0.058 Uiso 1 1 calc R . . H50B H 0.4639 0.9467 0.2982 0.058 Uiso 1 1 calc R . . C502 C 0.3998(4) 1.0495(4) 0.3217(2) 0.0514(16) Uani 1 1 d . . . H50C H 0.3345 1.0663 0.3053 0.062 Uiso 1 1 calc R . . H50D H 0.3879 1.0651 0.3512 0.062 Uiso 1 1 calc R . . C503 C 0.4189(4) 1.1698(3) 0.2843(2) 0.0445(14) Uani 1 1 d . . . H50E H 0.4015 1.1936 0.3112 0.053 Uiso 1 1 calc R . . H50F H 0.3561 1.1796 0.2671 0.053 Uiso 1 1 calc R . . C504 C 0.4877(4) 1.2070(3) 0.25637(19) 0.0378(12) Uani 1 1 d . . . H50G H 0.5086 1.1810 0.2304 0.045 Uiso 1 1 calc R . . H50H H 0.4530 1.2642 0.2451 0.045 Uiso 1 1 calc R . . C505 C 0.6408(5) 1.2348(3) 0.2593(2) 0.0437(14) Uani 1 1 d . . . H50I H 0.6051 1.2916 0.2474 0.052 Uiso 1 1 calc R . . H50J H 0.6676 1.2088 0.2339 0.052 Uiso 1 1 calc R . . C506 C 0.7252(5) 1.2275(3) 0.2906(2) 0.0444(14) Uani 1 1 d . . . H50K H 0.7672 1.2594 0.2752 0.053 Uiso 1 1 calc R . . H50L H 0.6965 1.2502 0.3168 0.053 Uiso 1 1 calc R . . C507 C 0.5890(5) 0.8461(4) 0.3519(2) 0.0501(15) Uani 1 1 d . . . H50M H 0.5390 0.8175 0.3517 0.060 Uiso 1 1 calc R . . H50N H 0.6351 0.8185 0.3779 0.060 Uiso 1 1 calc R . . C508 C 0.6482(5) 0.8417(3) 0.3098(2) 0.0481(15) Uani 1 1 d . . . H50O H 0.6808 0.7854 0.3076 0.058 Uiso 1 1 calc R . . H50P H 0.6030 0.8681 0.2833 0.058 Uiso 1 1 calc R . . C509 C 0.7895(4) 0.8708(3) 0.27559(19) 0.0398(13) Uani 1 1 d . . . H50Q H 0.7532 0.8976 0.2468 0.048 Uiso 1 1 calc R . . H50R H 0.8196 0.8136 0.2750 0.048 Uiso 1 1 calc R . . C510 C 0.8696(4) 0.9062(3) 0.2822(2) 0.0423(13) Uani 1 1 d . . . H51A H 0.9013 0.8830 0.3123 0.051 Uiso 1 1 calc R . . H51B H 0.9220 0.8941 0.2599 0.051 Uiso 1 1 calc R . . C511 C 0.9034(4) 1.0275(4) 0.2792(2) 0.0462(14) Uani 1 1 d . . . H51C H 0.9533 1.0130 0.2562 0.055 Uiso 1 1 calc R . . H51D H 0.9383 1.0086 0.3088 0.055 Uiso 1 1 calc R . . C512 C 0.8562(5) 1.1158(4) 0.2711(2) 0.0465(14) Uani 1 1 d . . . H51E H 0.9102 1.1411 0.2677 0.056 Uiso 1 1 calc R . . H51F H 0.8172 1.1328 0.2425 0.056 Uiso 1 1 calc R . . C513 C 0.5093(5) 0.9257(5) 0.4042(2) 0.0538(17) Uani 1 1 d . . . H51G H 0.4826 0.8806 0.4146 0.065 Uiso 1 1 calc R . . H51H H 0.4552 0.9753 0.4063 0.065 Uiso 1 1 calc R . . C514 C 0.5969(5) 0.9174(4) 0.4349(2) 0.0503(15) Uani 1 1 d . . . H51I H 0.5762 0.9105 0.4663 0.060 Uiso 1 1 calc R . . H51J H 0.6534 0.8699 0.4316 0.060 Uiso 1 1 calc R . . C515 C 0.7141(4) 0.9804(4) 0.45008(18) 0.0425(13) Uani 1 1 d . . . H51K H 0.7729 0.9383 0.4425 0.051 Uiso 1 1 calc R . . H51L H 0.7010 0.9653 0.4821 0.051 Uiso 1 1 calc R . . C516 C 0.7360(4) 1.0569(4) 0.44175(19) 0.0428(13) Uani 1 1 d . . . H51M H 0.6779 1.0987 0.4501 0.051 Uiso 1 1 calc R . . H51N H 0.7949 1.0522 0.4603 0.051 Uiso 1 1 calc R . . C517 C 0.7931(5) 1.1445(3) 0.3880(2) 0.0438(14) Uani 1 1 d . . . H51O H 0.8378 1.1419 0.4130 0.053 Uiso 1 1 calc R . . H51P H 0.7371 1.1948 0.3847 0.053 Uiso 1 1 calc R . . C518 C 0.8503(4) 1.1406(3) 0.34558(19) 0.0403(13) Uani 1 1 d . . . H51Q H 0.8797 1.1849 0.3395 0.048 Uiso 1 1 calc R . . H51R H 0.9065 1.0902 0.3501 0.048 Uiso 1 1 calc R . . C1 C 0.3325(11) 0.2460(9) 0.1485(5) 0.147(5) Uani 1 1 d . . . H1A H 0.2792 0.2825 0.1625 0.220 Uiso 1 1 calc R . . H1B H 0.3592 0.1955 0.1697 0.220 Uiso 1 1 calc R . . H1C H 0.3050 0.2364 0.1219 0.220 Uiso 1 1 calc R . . C2 C 0.4070(9) 0.2786(7) 0.1368(3) 0.100(3) Uani 1 1 d . . . C3 C 0.3977(9) 0.3551(6) 0.1451(3) 0.093(4) Uani 1 1 d . . . H3 H 0.3406 0.3844 0.1590 0.111 Uiso 1 1 calc R . . C4 C 0.4739(11) 0.3837(9) 0.1323(4) 0.116(4) Uani 1 1 d . . . H4 H 0.4685 0.4347 0.1380 0.140 Uiso 1 1 calc R . . C5 C 0.5575(11) 0.3476(8) 0.1122(4) 0.116(4) Uani 1 1 d . . . H5 H 0.6076 0.3728 0.1037 0.139 Uiso 1 1 calc R . . C6 C 0.5681(11) 0.2711(6) 0.1042(4) 0.111(4) Uani 1 1 d . . . H6 H 0.6267 0.2427 0.0909 0.133 Uiso 1 1 calc R . . C7 C 0.4902(8) 0.2378(6) 0.1164(3) 0.084(3) Uani 1 1 d . . . H7 H 0.4950 0.1869 0.1106 0.101 Uiso 1 1 calc R . . N1S N 0.0915(10) 0.0171(8) 0.1910(5) 0.188(6) Uani 1 1 d D . . H1S1 H 0.0690 -0.0256 0.1927 0.282 Uiso 0.67 1 calc PR . . H1S2 H 0.1128 0.0306 0.1629 0.282 Uiso 0.67 1 calc PR . . H1S3 H 0.0409 0.0589 0.1974 0.282 Uiso 0.67 1 calc PR . . C1S C 0.1755(7) -0.0031(5) 0.2233(3) 0.076(2) Uani 1 1 d D . . H1S4 H 0.2322 -0.0480 0.2170 0.091 Uiso 1 1 calc R . . H1S5 H 0.1541 -0.0167 0.2543 0.091 Uiso 1 1 calc R . . C2S C 0.2049(12) 0.0768(10) 0.2156(6) 0.247(14) Uani 1 1 d D . . H2S1 H 0.2735 0.0678 0.2272 0.297 Uiso 1 1 calc R . . H2S2 H 0.1988 0.1031 0.1837 0.297 Uiso 1 1 calc R . . N2S N 0.1354(8) 0.1175(7) 0.2396(3) 0.145(4) Uani 1 1 d D . . H2S3 H 0.1432 0.1661 0.2386 0.217 Uiso 0.67 1 calc PR . . H2S4 H 0.1417 0.0906 0.2684 0.217 Uiso 0.67 1 calc PR . . H2S5 H 0.0735 0.1237 0.2284 0.217 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 Ge1A 0.0267(3) 0.0421(3) 0.0290(3) -0.0051(2) -0.0001(2) -0.0059(2) Ge2A 0.0281(3) 0.0436(3) 0.0254(3) -0.0062(2) 0.0082(2) -0.0115(2) Ge3A 0.0439(3) 0.0378(3) 0.0288(3) -0.0094(2) 0.0050(2) -0.0227(2) Ge4A 0.0347(3) 0.0340(3) 0.0244(3) -0.0056(2) 0.0067(2) -0.0143(2) Ge5A 0.0472(3) 0.0404(3) 0.0347(3) -0.0171(3) 0.0045(2) -0.0182(3) Ge6A 0.0564(4) 0.0347(3) 0.0344(3) 0.0021(2) 0.0099(3) -0.0080(3) Ge7A 0.0337(3) 0.0445(3) 0.0334(3) -0.0078(3) 0.0087(2) 0.0002(2) Ge8A 0.0401(3) 0.0832(5) 0.0418(4) -0.0242(3) 0.0116(3) -0.0390(3) Ge9A 0.0300(3) 0.0659(4) 0.0243(3) -0.0129(3) -0.0018(2) -0.0076(3) Ge1B 0.0335(3) 0.0320(3) 0.0361(3) 0.0003(2) -0.0094(2) -0.0062(2) Ge2B 0.0228(2) 0.0280(2) 0.0341(3) -0.0051(2) 0.0066(2) -0.0078(2) Ge3B 0.0379(3) 0.0253(2) 0.0302(3) -0.0057(2) -0.0032(2) -0.0173(2) Ge4B 0.0426(3) 0.0330(3) 0.0243(3) -0.0092(2) 0.0076(2) -0.0200(2) Ge5B 0.0508(3) 0.0231(2) 0.0333(3) -0.0089(2) 0.0066(2) -0.0176(2) Ge6B 0.0409(3) 0.0244(2) 0.0262(3) -0.0011(2) -0.0012(2) -0.0063(2) Ge7B 0.0329(3) 0.0389(3) 0.0292(3) -0.0156(2) 0.0028(2) -0.0017(2) Ge8B 0.0347(3) 0.0698(4) 0.0444(3) -0.0307(3) 0.0141(3) -0.0341(3) Ge9B 0.0311(3) 0.0389(3) 0.0250(3) -0.0157(2) 0.0026(2) -0.0127(2) Hg1 0.03330(11) 0.04027(11) 0.02834(11) -0.01705(8) 0.00321(8) -0.00850(8) Hg2 0.03067(14) 0.04972(17) 0.03220(15) -0.02257(13) 0.00343(11) -0.00964(12) K1 0.0304(5) 0.0349(5) 0.0298(6) -0.0063(4) 0.0018(4) -0.0112(4) N11 0.041(3) 0.059(3) 0.031(2) -0.001(2) 0.003(2) -0.021(2) N12 0.032(2) 0.055(3) 0.034(2) -0.014(2) 0.0065(19) -0.017(2) O11 0.039(2) 0.052(2) 0.030(2) -0.0036(17) -0.0040(16) -0.0182(18) O12 0.0352(19) 0.050(2) 0.033(2) -0.0167(17) 0.0049(15) -0.0129(17) O13 0.072(3) 0.049(3) 0.137(6) 0.026(3) 0.067(4) 0.011(3) O14 0.036(2) 0.057(3) 0.070(3) 0.018(2) 0.009(2) -0.010(2) O15 0.043(2) 0.039(2) 0.032(2) 0.0035(16) -0.0029(16) -0.0057(17) O16 0.036(2) 0.059(2) 0.038(2) -0.0130(19) -0.0049(17) -0.0053(18) C101 0.057(4) 0.085(5) 0.041(4) 0.000(3) 0.002(3) -0.047(4) C102 0.046(3) 0.074(4) 0.040(3) -0.007(3) 0.002(3) -0.036(3) C103 0.039(3) 0.055(3) 0.034(3) -0.013(3) -0.006(2) -0.014(3) C104 0.042(3) 0.047(3) 0.034(3) -0.014(2) -0.007(2) -0.013(3) C105 0.038(3) 0.054(3) 0.032(3) -0.017(3) 0.006(2) -0.009(3) C106 0.040(3) 0.059(4) 0.037(3) -0.012(3) 0.012(2) -0.016(3) C107 0.028(3) 0.081(5) 0.043(4) -0.001(3) 0.011(2) -0.011(3) C108 0.037(3) 0.060(4) 0.063(4) -0.005(3) 0.012(3) -0.002(3) C109 0.053(4) 0.117(6) 0.126(7) 0.043(6) 0.030(5) 0.010(4) C110 0.040(3) 0.038(3) 0.065(4) 0.001(3) 0.001(3) -0.008(2) C111 0.060(4) 0.049(3) 0.052(4) -0.014(3) 0.018(3) -0.034(3) C112 0.047(4) 0.073(4) 0.052(4) -0.020(3) 0.015(3) -0.036(3) C113 0.052(4) 0.068(4) 0.033(3) 0.006(3) 0.005(3) -0.029(3) C114 0.069(4) 0.052(4) 0.036(3) 0.011(3) -0.003(3) -0.030(3) C115 0.059(4) 0.037(3) 0.033(3) -0.003(2) -0.008(3) 0.005(3) C116 0.039(3) 0.059(4) 0.042(3) -0.012(3) -0.013(3) 0.010(3) C117 0.026(3) 0.071(4) 0.055(4) -0.020(3) -0.004(3) -0.007(3) C118 0.026(3) 0.073(4) 0.049(4) -0.019(3) 0.005(2) -0.014(3) K2 0.0362(6) 0.0449(6) 0.0292(6) -0.0072(5) -0.0001(5) -0.0141(5) N21 0.117(6) 0.085(5) 0.045(4) -0.026(3) -0.033(4) 0.051(4) N22 0.150(7) 0.047(3) 0.056(4) 0.002(3) -0.053(4) -0.024(4) O21 0.047(3) 0.140(5) 0.093(4) -0.091(4) 0.015(3) -0.025(3) O22 0.121(5) 0.110(4) 0.039(3) -0.016(3) 0.019(3) -0.084(4) O23 0.105(4) 0.036(2) 0.091(4) -0.001(3) 0.037(3) -0.016(3) O24 0.046(3) 0.056(3) 0.105(4) -0.041(3) -0.008(3) -0.018(2) O25 0.071(3) 0.069(3) 0.047(3) -0.030(2) -0.021(2) 0.004(2) O26 0.114(4) 0.060(3) 0.041(3) -0.004(2) -0.008(3) -0.047(3) C201 0.092(7) 0.112(8) 0.140(10) -0.084(7) -0.067(7) 0.054(6) C202 0.049(5) 0.119(8) 0.147(10) -0.097(7) -0.012(5) 0.028(5) C203 0.075(6) 0.154(10) 0.103(7) -0.089(8) 0.051(5) -0.069(6) C204 0.117(8) 0.180(11) 0.075(6) -0.088(7) 0.072(6) -0.117(8) C205 0.210(14) 0.144(10) 0.039(5) 0.004(5) -0.007(6) -0.135(11) C206 0.230(15) 0.068(6) 0.043(5) 0.019(4) -0.058(7) -0.051(8) C207 0.191(12) 0.044(5) 0.058(5) 0.005(4) 0.004(6) 0.040(6) C208 0.215(14) 0.044(5) 0.097(8) 0.008(5) 0.065(9) 0.006(7) C209 0.117(9) 0.062(6) 0.219(15) -0.058(8) 0.108(10) -0.063(6) C210 0.064(5) 0.081(6) 0.190(12) -0.082(8) 0.034(7) -0.045(5) C211 0.053(4) 0.117(7) 0.102(7) -0.055(6) -0.040(5) 0.000(5) C212 0.145(10) 0.076(6) 0.093(7) -0.040(5) -0.073(7) 0.040(6) C213 0.271(16) 0.088(7) 0.053(5) -0.036(5) -0.080(8) 0.087(9) C214 0.145(9) 0.124(8) 0.093(7) -0.081(7) -0.086(7) 0.066(7) C215 0.072(5) 0.104(6) 0.038(4) -0.032(4) 0.008(3) -0.045(5) C216 0.115(6) 0.042(3) 0.043(4) -0.010(3) 0.002(4) -0.046(4) C217 0.200(12) 0.034(4) 0.088(7) -0.011(4) -0.052(7) -0.021(5) C218 0.290(17) 0.039(4) 0.084(7) 0.008(4) -0.088(9) -0.047(7) K3 0.0249(5) 0.0244(5) 0.0267(5) -0.0039(4) 0.0013(4) -0.0094(4) N31 0.030(2) 0.034(2) 0.033(2) -0.0101(18) 0.0048(17) -0.0133(18) N32 0.037(2) 0.031(2) 0.025(2) -0.0042(17) 0.0046(17) -0.0160(18) O31 0.0260(17) 0.053(2) 0.0292(19) -0.0033(16) -0.0014(14) -0.0160(16) O32 0.0242(17) 0.0344(18) 0.039(2) -0.0073(16) -0.0005(14) -0.0058(14) O33 0.0309(18) 0.0307(18) 0.053(2) -0.0120(17) 0.0087(16) -0.0159(15) O34 0.051(2) 0.0282(18) 0.046(2) 0.0016(17) 0.0096(18) -0.0146(17) O35 0.0282(17) 0.0325(18) 0.040(2) -0.0146(15) 0.0062(15) -0.0167(14) O36 0.0309(18) 0.0385(19) 0.0317(19) -0.0123(15) 0.0038(14) -0.0182(15) C301 0.033(3) 0.052(3) 0.031(3) 0.001(2) 0.007(2) -0.016(2) C302 0.040(3) 0.063(4) 0.026(3) 0.002(3) -0.002(2) -0.021(3) C303 0.025(3) 0.061(4) 0.038(3) -0.001(3) -0.011(2) -0.019(2) C304 0.023(2) 0.041(3) 0.043(3) -0.005(2) -0.006(2) -0.009(2) C305 0.023(2) 0.038(3) 0.053(3) -0.019(3) 0.005(2) -0.008(2) C306 0.040(3) 0.046(3) 0.046(3) -0.018(3) 0.019(2) -0.026(3) C307 0.041(3) 0.043(3) 0.053(4) -0.027(3) 0.015(3) -0.015(3) C308 0.055(4) 0.044(3) 0.063(4) -0.030(3) 0.010(3) -0.025(3) C309 0.035(3) 0.034(3) 0.085(5) -0.022(3) 0.015(3) -0.019(2) C310 0.027(3) 0.023(2) 0.072(4) -0.002(3) 0.008(3) -0.012(2) C311 0.067(4) 0.039(3) 0.036(3) 0.008(3) 0.003(3) -0.024(3) C312 0.068(4) 0.051(3) 0.027(3) 0.000(3) -0.001(3) -0.025(3) C313 0.025(2) 0.039(3) 0.039(3) -0.008(2) 0.005(2) -0.005(2) C314 0.026(2) 0.038(3) 0.050(3) -0.005(2) 0.009(2) -0.016(2) C315 0.033(3) 0.049(3) 0.053(4) -0.021(3) 0.009(2) -0.026(2) C316 0.034(3) 0.048(3) 0.044(3) -0.019(3) 0.003(2) -0.020(2) C317 0.043(3) 0.039(3) 0.031(3) -0.014(2) 0.006(2) -0.021(2) C318 0.046(3) 0.041(3) 0.038(3) -0.020(2) 0.018(2) -0.022(2) K4 0.0236(5) 0.0240(5) 0.0316(5) -0.0047(4) -0.0009(4) -0.0090(4) N41 0.035(2) 0.032(2) 0.045(3) -0.0111(19) 0.0081(19) -0.0190(19) N42 0.034(2) 0.030(2) 0.063(3) -0.013(2) 0.007(2) -0.0168(19) O41 0.0301(18) 0.0336(18) 0.041(2) -0.0113(16) 0.0037(15) -0.0101(15) O42 0.041(2) 0.0257(17) 0.037(2) -0.0121(15) -0.0002(16) -0.0098(15) O43 0.0323(19) 0.056(2) 0.038(2) -0.0185(18) -0.0024(16) -0.0100(17) O44 0.048(2) 0.0301(19) 0.041(2) -0.0030(16) 0.0052(18) -0.0083(17) O45 0.040(2) 0.0268(19) 0.078(3) 0.0048(19) -0.010(2) -0.0081(17) O46 0.050(3) 0.034(2) 0.137(5) 0.011(3) -0.049(3) -0.013(2) C401 0.044(3) 0.046(3) 0.054(4) -0.015(3) 0.022(3) -0.026(3) C402 0.028(3) 0.055(3) 0.061(4) -0.021(3) 0.016(3) -0.022(3) C403 0.047(3) 0.039(3) 0.038(3) -0.011(2) 0.006(3) 0.001(3) C404 0.059(4) 0.033(3) 0.033(3) -0.013(2) -0.002(3) -0.006(3) C405 0.048(3) 0.024(2) 0.053(4) -0.012(2) 0.000(3) -0.013(2) C406 0.056(4) 0.024(2) 0.056(4) -0.008(2) 0.009(3) -0.020(2) C407 0.036(3) 0.064(4) 0.072(5) -0.024(3) 0.005(3) -0.030(3) C408 0.048(4) 0.068(4) 0.063(4) -0.031(4) -0.013(3) -0.021(3) C409 0.032(3) 0.085(5) 0.041(3) -0.031(3) -0.006(2) -0.005(3) C410 0.045(3) 0.074(4) 0.032(3) -0.005(3) 0.001(3) 0.009(3) C411 0.102(6) 0.036(3) 0.057(4) -0.012(3) 0.030(4) -0.033(4) C412 0.060(4) 0.043(3) 0.087(5) -0.026(3) 0.038(4) -0.031(3) C413 0.062(4) 0.034(3) 0.052(4) -0.010(3) 0.012(3) -0.028(3) C414 0.065(4) 0.025(3) 0.053(4) -0.002(3) -0.001(3) -0.005(3) C415 0.050(4) 0.037(4) 0.183(10) -0.003(5) -0.049(5) -0.002(3) C416 0.106(7) 0.049(4) 0.187(11) 0.006(6) -0.114(8) -0.010(5) C417 0.036(4) 0.060(4) 0.134(8) -0.026(5) -0.029(4) -0.005(3) C418 0.031(3) 0.054(4) 0.111(6) -0.021(4) -0.004(3) -0.024(3) K5 0.0273(5) 0.0273(5) 0.0275(5) -0.0064(4) 0.0007(4) -0.0108(4) N51 0.036(2) 0.051(3) 0.039(3) 0.002(2) -0.004(2) -0.027(2) N52 0.036(2) 0.033(2) 0.037(2) -0.0022(19) -0.0054(19) -0.0176(19) O51 0.0223(17) 0.0365(19) 0.046(2) -0.0050(17) -0.0006(15) -0.0047(14) O52 0.040(2) 0.0340(19) 0.036(2) 0.0028(16) -0.0145(16) -0.0082(16) O53 0.047(2) 0.0292(18) 0.038(2) -0.0086(16) 0.0027(17) -0.0157(16) O54 0.0198(16) 0.0342(18) 0.039(2) -0.0112(15) -0.0002(14) -0.0048(14) O55 0.0309(18) 0.042(2) 0.035(2) -0.0011(16) -0.0060(15) -0.0125(16) O56 0.058(2) 0.044(2) 0.031(2) -0.0039(17) -0.0076(17) -0.0281(19) C501 0.042(3) 0.060(4) 0.050(4) 0.000(3) -0.002(3) -0.032(3) C502 0.027(3) 0.076(4) 0.053(4) -0.006(3) 0.005(3) -0.024(3) C503 0.030(3) 0.050(3) 0.046(3) -0.016(3) -0.006(2) 0.003(2) C504 0.037(3) 0.032(3) 0.038(3) -0.008(2) -0.015(2) 0.002(2) C505 0.056(4) 0.029(3) 0.043(3) 0.003(2) -0.010(3) -0.014(3) C506 0.057(4) 0.030(3) 0.050(4) 0.002(2) -0.008(3) -0.023(3) C507 0.059(4) 0.043(3) 0.055(4) 0.003(3) -0.003(3) -0.033(3) C508 0.068(4) 0.035(3) 0.048(4) -0.011(3) -0.003(3) -0.023(3) C509 0.052(3) 0.026(3) 0.036(3) -0.011(2) 0.001(2) -0.001(2) C510 0.031(3) 0.040(3) 0.043(3) -0.010(2) 0.000(2) 0.009(2) C511 0.024(3) 0.064(4) 0.057(4) -0.022(3) 0.005(2) -0.017(3) C512 0.048(3) 0.060(4) 0.045(3) -0.007(3) 0.006(3) -0.038(3) C513 0.048(3) 0.078(4) 0.044(4) 0.000(3) 0.003(3) -0.042(3) C514 0.062(4) 0.061(4) 0.033(3) -0.001(3) 0.002(3) -0.031(3) C515 0.040(3) 0.058(4) 0.027(3) -0.001(3) -0.007(2) -0.016(3) C516 0.044(3) 0.055(3) 0.032(3) -0.012(3) -0.004(2) -0.015(3) C517 0.057(4) 0.035(3) 0.046(3) -0.011(3) -0.012(3) -0.022(3) C518 0.041(3) 0.041(3) 0.045(3) -0.005(3) -0.013(2) -0.023(2) C1 0.123(11) 0.159(13) 0.130(12) 0.012(10) -0.023(9) -0.025(10) C2 0.101(8) 0.107(8) 0.064(6) 0.009(6) -0.021(6) -0.007(7) C3 0.113(8) 0.075(6) 0.055(5) -0.033(4) -0.031(5) 0.037(5) C4 0.111(9) 0.156(12) 0.096(9) -0.052(8) -0.031(7) -0.040(9) C5 0.140(11) 0.139(11) 0.078(7) -0.023(7) -0.028(7) -0.051(9) C6 0.173(12) 0.083(7) 0.074(7) -0.002(5) -0.042(7) -0.039(8) C7 0.104(7) 0.074(5) 0.041(4) -0.014(4) -0.016(4) 0.024(5) N1S 0.162(12) 0.180(12) 0.235(16) -0.070(11) -0.033(11) -0.049(10) C1S 0.083(6) 0.062(5) 0.091(7) -0.017(4) -0.009(5) -0.030(4) C2S 0.137(13) 0.41(3) 0.131(14) -0.142(18) 0.024(11) 0.068(17) N2S 0.131(9) 0.186(11) 0.095(7) 0.032(7) 0.007(6) -0.052(8) _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 Ge1A Ge4A 2.5425(10) . ? Ge1A Ge3A 2.5485(11) . ? Ge1A Ge5A 2.6029(11) . ? Ge1A Ge2A 2.6099(12) . ? Ge2A Ge5A 2.6092(11) . ? Ge2A Ge6A 2.6115(13) . ? Ge2A Ge9A 2.6593(10) . ? Ge2A Ge3A 2.9380(11) . ? Ge3A Ge6A 2.5526(13) . ? Ge3A Ge4A 2.7048(10) . ? Ge3A Ge7A 2.7946(11) . ? Ge3A Hg1 2.9056(10) . ? Ge4A Ge8A 2.5386(11) . ? Ge4A Ge7A 2.7171(14) . ? Ge4A Hg1 2.7594(9) . ? Ge4A Ge5A 3.0688(11) . ? Ge5A Ge8A 2.6321(12) . ? Ge5A Ge9A 2.6332(14) . ? Ge6A Ge7A 2.5679(12) . ? Ge6A Ge9A 2.6031(11) . ? Ge7A Ge8A 2.5723(11) . ? Ge7A Ge9A 2.8890(11) . ? Ge7A Hg1 3.1806(11) . ? Ge8A Ge9A 2.5918(12) . ? Ge1B Ge4B 2.5574(11) . ? Ge1B Ge3B 2.5691(12) . ? Ge1B Ge2B 2.5758(10) . ? Ge1B Ge5B 2.6111(10) . ? Ge2B Ge9B 2.5876(10) . ? Ge2B Ge6B 2.6192(13) . ? Ge2B Ge5B 2.7614(11) . ? Ge2B Ge3B 2.7729(11) . ? Ge3B Ge6B 2.5810(11) . ? Ge3B Ge7B 2.6708(10) . ? Ge3B Ge4B 2.8299(11) . ? Ge4B Ge8B 2.5758(11) . ? Ge4B Ge7B 2.6862(14) . ? Ge4B Ge5B 2.7645(11) . ? Ge4B Hg2 3.1250(12) . ? Ge5B Ge9B 2.6005(13) . ? Ge5B Ge8B 2.6614(13) . ? Ge6B Ge7B 2.5592(11) . ? Ge6B Ge9B 2.5935(9) . ? Ge7B Ge8B 2.5380(10) . ? Ge7B Hg2 2.5712(8) . ? Ge7B Ge9B 3.1853(12) . ? Ge8B Ge9B 2.5783(11) . ? Ge9B Hg1 2.6078(9) . ? Hg2 Ge7B 2.5712(8) 2_576 ? Hg2 Ge4B 3.1250(11) 2_576 ? N11 C101 1.465(8) . ? N11 C107 1.465(8) . ? N11 C113 1.468(7) . ? N12 C118 1.473(7) . ? N12 C106 1.475(7) . ? N12 C112 1.478(8) . ? O11 C103 1.415(7) . ? O11 C102 1.423(7) . ? O12 C104 1.421(6) . ? O12 C105 1.435(6) . ? O13 C109 1.195(10) . ? O13 C108 1.407(8) . ? O14 C110 1.420(7) . ? O14 C111 1.435(7) . ? O15 C115 1.417(7) . ? O15 C114 1.432(7) . ? O16 C116 1.414(7) . ? O16 C117 1.424(7) . ? C101 C102 1.505(9) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.481(8) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.494(8) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.522(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.422(10) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.482(9) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.498(9) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.474(9) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.514(9) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? N21 C201 1.465(14) . ? N21 C213 1.468(10) . ? N21 C207 1.477(15) . ? N22 C212 1.442(14) . ? N22 C218 1.489(10) . ? N22 C206 1.496(14) . ? O21 C203 1.399(10) . ? O21 C202 1.456(13) . ? O22 C205 1.344(12) . ? O22 C204 1.489(12) . ? O23 C208 1.405(12) . ? O23 C209 1.448(13) . ? O24 C211 1.415(10) . ? O24 C210 1.431(10) . ? O25 C214 1.420(9) . ? O25 C215 1.428(9) . ? O26 C217 1.407(11) . ? O26 C216 1.443(8) . ? C201 C202 1.497(14) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.457(15) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.519(17) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.472(17) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.454(16) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.531(14) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.483(17) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.474(11) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.535(14) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? N31 C301 1.463(7) . ? N31 C307 1.465(7) . ? N31 C313 1.485(6) . ? N32 C306 1.464(7) . ? N32 C312 1.480(7) . ? N32 C318 1.481(6) . ? O31 C302 1.417(7) . ? O31 C303 1.424(6) . ? O32 C305 1.423(6) . ? O32 C304 1.440(6) . ? O33 C308 1.400(7) . ? O33 C309 1.429(6) . ? O34 C310 1.420(6) . ? O34 C311 1.421(7) . ? O35 C315 1.418(6) . ? O35 C314 1.435(6) . ? O36 C317 1.426(6) . ? O36 C316 1.437(6) . ? C301 C302 1.508(7) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.485(8) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.510(8) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.515(8) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.470(9) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.495(9) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.490(8) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.497(8) . ? C315 H31O 0.9900 . ? C315 H31P 0.9900 . ? C316 H31Q 0.9900 . ? C316 H31R 0.9900 . ? C317 C318 1.507(7) . ? C317 H31K 0.9900 . ? C317 H31L 0.9900 . ? C318 H31M 0.9900 . ? C318 H31N 0.9900 . ? N41 C401 1.464(7) . ? N41 C413 1.478(7) . ? N41 C407 1.479(8) . ? N42 C412 1.454(8) . ? N42 C418 1.476(8) . ? N42 C406 1.486(7) . ? O41 C402 1.421(6) . ? O41 C403 1.423(6) . ? O42 C404 1.415(7) . ? O42 C405 1.428(6) . ? O43 C408 1.416(8) . ? O43 C409 1.420(7) . ? O44 C410 1.420(7) . ? O44 C411 1.453(7) . ? O45 C415 1.420(8) . ? O45 C414 1.439(7) . ? O46 C417 1.429(10) . ? O46 C416 1.449(9) . ? C401 C402 1.499(8) . ? C401 H40A 0.9900 . ? C401 H40B 0.9900 . ? C402 H40C 0.9900 . ? C402 H40D 0.9900 . ? C403 C404 1.483(8) . ? C403 H40E 0.9900 . ? C403 H40F 0.9900 . ? C404 H40G 0.9900 . ? C404 H40H 0.9900 . ? C405 C406 1.489(8) . ? C405 H40I 0.9900 . ? C405 H40J 0.9900 . ? C406 H40K 0.9900 . ? C406 H40L 0.9900 . ? C407 C408 1.514(9) . ? C407 H40M 0.9900 . ? C407 H40N 0.9900 . ? C408 H40O 0.9900 . ? C408 H40P 0.9900 . ? C409 C410 1.489(10) . ? C409 H40Q 0.9900 . ? C409 H40R 0.9900 . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 C412 1.487(11) . ? C411 H41C 0.9900 . ? C411 H41D 0.9900 . ? C412 H41E 0.9900 . ? C412 H41F 0.9900 . ? C413 C414 1.473(9) . ? C413 H41G 0.9900 . ? C413 H41H 0.9900 . ? C414 H41I 0.9900 . ? C414 H41J 0.9900 . ? C415 C416 1.301(12) . ? C415 H41K 0.9900 . ? C415 H41L 0.9900 . ? C416 H41M 0.9900 . ? C416 H41N 0.9900 . ? C417 C418 1.497(10) . ? C417 H41O 0.9900 . ? C417 H41P 0.9900 . ? C418 H41Q 0.9900 . ? C418 H41R 0.9900 . ? N51 C507 1.464(8) . ? N51 C513 1.467(8) . ? N51 C501 1.476(7) . ? N52 C512 1.467(8) . ? N52 C518 1.472(7) . ? N52 C506 1.476(7) . ? O51 C503 1.404(7) . ? O51 C502 1.430(7) . ? O52 C505 1.420(7) . ? O52 C504 1.435(6) . ? O53 C509 1.419(7) . ? O53 C508 1.420(7) . ? O54 C511 1.425(6) . ? O54 C510 1.446(6) . ? O55 C514 1.414(7) . ? O55 C515 1.446(6) . ? O56 C516 1.405(7) . ? O56 C517 1.423(6) . ? C501 C502 1.510(9) . ? C501 H50A 0.9900 . ? C501 H50B 0.9900 . ? C502 H50C 0.9900 . ? C502 H50D 0.9900 . ? C503 C504 1.492(8) . ? C503 H50E 0.9900 . ? C503 H50F 0.9900 . ? C504 H50G 0.9900 . ? C504 H50H 0.9900 . ? C505 C506 1.504(8) . ? C505 H50I 0.9900 . ? C505 H50J 0.9900 . ? C506 H50K 0.9900 . ? C506 H50L 0.9900 . ? C507 C508 1.510(9) . ? C507 H50M 0.9900 . ? C507 H50N 0.9900 . ? C508 H50O 0.9900 . ? C508 H50P 0.9900 . ? C509 C510 1.489(8) . ? C509 H50Q 0.9900 . ? C509 H50R 0.9900 . ? C510 H51A 0.9900 . ? C510 H51B 0.9900 . ? C511 C512 1.495(9) . ? C511 H51C 0.9900 . ? C511 H51D 0.9900 . ? C512 H51E 0.9900 . ? C512 H51F 0.9900 . ? C513 C514 1.524(8) . ? C513 H51G 0.9900 . ? C513 H51H 0.9900 . ? C514 H51I 0.9900 . ? C514 H51J 0.9900 . ? C515 C516 1.476(8) . ? C515 H51K 0.9900 . ? C515 H51L 0.9900 . ? C516 H51M 0.9900 . ? C516 H51N 0.9900 . ? C517 C518 1.504(9) . ? C517 H51O 0.9900 . ? C517 H51P 0.9900 . ? C518 H51Q 0.9900 . ? C518 H51R 0.9900 . ? C1 C2 1.354(16) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.374(14) . ? C2 C3 1.419(15) . ? C3 C4 1.337(16) . ? C3 H3 0.9500 . ? C4 C5 1.346(16) . ? C4 H4 0.9500 . ? C5 C6 1.409(15) . ? C5 H5 0.9500 . ? C6 C7 1.408(15) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? N1S C1S 1.473(12) . ? N1S H1S1 0.9100 . ? N1S H1S2 0.9100 . ? N1S H1S3 0.9100 . ? C1S C2S 1.589(17) . ? C1S H1S4 0.9900 . ? C1S H1S5 0.9900 . ? C2S N2S 1.322(12) . ? 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 Ge4A Ge1A Ge3A 64.19(4) . . ? Ge4A Ge1A Ge5A 73.22(3) . . ? Ge3A Ge1A Ge5A 102.72(4) . . ? Ge4A Ge1A Ge2A 101.64(4) . . ? Ge3A Ge1A Ge2A 69.43(4) . . ? Ge5A Ge1A Ge2A 60.07(3) . . ? Ge5A Ge2A Ge1A 59.83(3) . . ? Ge5A Ge2A Ge6A 108.37(3) . . ? Ge1A Ge2A Ge6A 106.24(4) . . ? Ge5A Ge2A Ge9A 59.97(4) . . ? Ge1A Ge2A Ge9A 105.49(4) . . ? Ge6A Ge2A Ge9A 59.18(3) . . ? Ge5A Ge2A Ge3A 92.81(3) . . ? Ge1A Ge2A Ge3A 54.30(3) . . ? Ge6A Ge2A Ge3A 54.39(4) . . ? Ge9A Ge2A Ge3A 90.22(4) . . ? Ge1A Ge3A Ge6A 109.92(4) . . ? Ge1A Ge3A Ge4A 57.80(3) . . ? Ge6A Ge3A Ge4A 106.23(4) . . ? Ge1A Ge3A Ge7A 105.23(4) . . ? Ge6A Ge3A Ge7A 57.19(4) . . ? Ge4A Ge3A Ge7A 59.19(3) . . ? Ge1A Ge3A Hg1 106.80(4) . . ? Ge6A Ge3A Hg1 119.48(3) . . ? Ge4A Ge3A Hg1 58.79(3) . . ? Ge7A Ge3A Hg1 67.80(3) . . ? Ge1A Ge3A Ge2A 56.27(3) . . ? Ge6A Ge3A Ge2A 56.28(3) . . ? Ge4A Ge3A Ge2A 90.02(3) . . ? Ge7A Ge3A Ge2A 88.72(4) . . ? Hg1 Ge3A Ge2A 147.32(2) . . ? Ge8A Ge4A Ge1A 107.89(3) . . ? Ge8A Ge4A Ge3A 108.09(4) . . ? Ge1A Ge4A Ge3A 58.01(3) . . ? Ge8A Ge4A Ge7A 58.49(4) . . ? Ge1A Ge4A Ge7A 107.69(4) . . ? Ge3A Ge4A Ge7A 62.05(3) . . ? Ge8A Ge4A Hg1 122.89(4) . . ? Ge1A Ge4A Hg1 111.48(3) . . ? Ge3A Ge4A Hg1 64.24(3) . . ? Ge7A Ge4A Hg1 71.00(3) . . ? Ge8A Ge4A Ge5A 55.01(3) . . ? Ge1A Ge4A Ge5A 54.30(3) . . ? Ge3A Ge4A Ge5A 88.13(3) . . ? Ge7A Ge4A Ge5A 88.58(4) . . ? Hg1 Ge4A Ge5A 150.90(3) . . ? Ge1A Ge5A Ge2A 60.10(3) . . ? Ge1A Ge5A Ge8A 103.38(3) . . ? Ge2A Ge5A Ge8A 107.13(4) . . ? Ge1A Ge5A Ge9A 106.45(4) . . ? Ge2A Ge5A Ge9A 60.96(3) . . ? Ge8A Ge5A Ge9A 58.98(4) . . ? Ge1A Ge5A Ge4A 52.49(3) . . ? Ge2A Ge5A Ge4A 89.03(3) . . ? Ge8A Ge5A Ge4A 52.20(3) . . ? Ge9A Ge5A Ge4A 87.53(4) . . ? Ge3A Ge6A Ge7A 66.15(3) . . ? Ge3A Ge6A Ge9A 100.72(4) . . ? Ge7A Ge6A Ge9A 67.93(3) . . ? Ge3A Ge6A Ge2A 69.34(4) . . ? Ge7A Ge6A Ge2A 101.44(4) . . ? Ge9A Ge6A Ge2A 61.32(3) . . ? Ge6A Ge7A Ge8A 109.95(4) . . ? Ge6A Ge7A Ge4A 105.44(4) . . ? Ge8A Ge7A Ge4A 57.28(3) . . ? Ge6A Ge7A Ge3A 56.66(3) . . ? Ge8A Ge7A Ge3A 104.49(4) . . ? Ge4A Ge7A Ge3A 58.76(3) . . ? Ge6A Ge7A Ge9A 56.61(3) . . ? Ge8A Ge7A Ge9A 56.30(3) . . ? Ge4A Ge7A Ge9A 89.73(4) . . ? Ge3A Ge7A Ge9A 88.61(4) . . ? Ge6A Ge7A Hg1 109.85(3) . . ? Ge8A Ge7A Hg1 107.55(4) . . ? Ge4A Ge7A Hg1 55.12(3) . . ? Ge3A Ge7A Hg1 57.76(3) . . ? Ge9A Ge7A Hg1 139.65(3) . . ? Ge4A Ge8A Ge7A 64.23(4) . . ? Ge4A Ge8A Ge9A 100.91(3) . . ? Ge7A Ge8A Ge9A 68.03(3) . . ? Ge4A Ge8A Ge5A 72.79(3) . . ? Ge7A Ge8A Ge5A 102.11(4) . . ? Ge9A Ge8A Ge5A 60.53(4) . . ? Ge8A Ge9A Ge6A 108.24(3) . . ? Ge8A Ge9A Ge5A 60.49(4) . . ? Ge6A Ge9A Ge5A 107.90(3) . . ? Ge8A Ge9A Ge2A 106.84(4) . . ? Ge6A Ge9A Ge2A 59.49(3) . . ? Ge5A Ge9A Ge2A 59.07(3) . . ? Ge8A Ge9A Ge7A 55.66(3) . . ? Ge6A Ge9A Ge7A 55.46(3) . . ? Ge5A Ge9A Ge7A 94.17(4) . . ? Ge2A Ge9A Ge7A 92.45(4) . . ? Ge4B Ge1B Ge3B 67.01(4) . . ? Ge4B Ge1B Ge2B 98.97(4) . . ? Ge3B Ge1B Ge2B 65.22(4) . . ? Ge4B Ge1B Ge5B 64.66(3) . . ? Ge3B Ge1B Ge5B 99.92(4) . . ? Ge2B Ge1B Ge5B 64.33(3) . . ? Ge1B Ge2B Ge9B 108.11(4) . . ? Ge1B Ge2B Ge6B 110.91(4) . . ? Ge9B Ge2B Ge6B 59.74(3) . . ? Ge1B Ge2B Ge5B 58.46(3) . . ? Ge9B Ge2B Ge5B 58.07(3) . . ? Ge6B Ge2B Ge5B 104.93(3) . . ? Ge1B Ge2B Ge3B 57.27(3) . . ? Ge9B Ge2B Ge3B 95.04(3) . . ? Ge6B Ge2B Ge3B 57.11(3) . . ? Ge5B Ge2B Ge3B 91.56(3) . . ? Ge1B Ge3B Ge6B 112.38(4) . . ? Ge1B Ge3B Ge7B 107.62(4) . . ? Ge6B Ge3B Ge7B 58.30(3) . . ? Ge1B Ge3B Ge2B 57.50(3) . . ? Ge6B Ge3B Ge2B 58.45(3) . . ? Ge7B Ge3B Ge2B 93.95(4) . . ? Ge1B Ge3B Ge4B 56.30(3) . . ? Ge6B Ge3B Ge4B 103.33(3) . . ? Ge7B Ge3B Ge4B 58.38(3) . . ? Ge2B Ge3B Ge4B 88.30(3) . . ? Ge1B Ge4B Ge8B 113.90(3) . . ? Ge1B Ge4B Ge7B 107.50(4) . . ? Ge8B Ge4B Ge7B 57.63(3) . . ? Ge1B Ge4B Ge5B 58.61(3) . . ? Ge8B Ge4B Ge5B 59.66(3) . . ? Ge7B Ge4B Ge5B 95.00(3) . . ? Ge1B Ge4B Ge3B 56.69(3) . . ? Ge8B Ge4B Ge3B 103.38(3) . . ? Ge7B Ge4B Ge3B 57.85(3) . . ? Ge5B Ge4B Ge3B 90.29(3) . . ? Ge1B Ge4B Hg2 125.55(3) . . ? Ge8B Ge4B Hg2 95.79(4) . . ? Ge7B Ge4B Hg2 51.85(3) . . ? Ge5B Ge4B Hg2 146.85(3) . . ? Ge3B Ge4B Hg2 73.10(3) . . ? Ge9B Ge5B Ge1B 106.66(3) . . ? Ge9B Ge5B Ge8B 58.67(4) . . ? Ge1B Ge5B Ge8B 109.38(3) . . ? Ge9B Ge5B Ge2B 57.61(3) . . ? Ge1B Ge5B Ge2B 57.22(3) . . ? Ge8B Ge5B Ge2B 102.69(4) . . ? Ge9B Ge5B Ge4B 94.10(3) . . ? Ge1B Ge5B Ge4B 56.73(3) . . ? Ge8B Ge5B Ge4B 56.64(3) . . ? Ge2B Ge5B Ge4B 89.86(3) . . ? Ge7B Ge6B Ge3B 62.61(3) . . ? Ge7B Ge6B Ge9B 76.37(4) . . ? Ge3B Ge6B Ge9B 99.71(4) . . ? Ge7B Ge6B Ge2B 100.45(4) . . ? Ge3B Ge6B Ge2B 64.44(4) . . ? Ge9B Ge6B Ge2B 59.52(3) . . ? Ge8B Ge7B Ge6B 104.18(4) . . ? Ge8B Ge7B Hg2 112.39(4) . . ? Ge6B Ge7B Hg2 135.78(3) . . ? Ge8B Ge7B Ge3B 109.12(4) . . ? Ge6B Ge7B Ge3B 59.10(3) . . ? Hg2 Ge7B Ge3B 85.35(4) . . ? Ge8B Ge7B Ge4B 59.00(3) . . ? Ge6B Ge7B Ge4B 108.10(4) . . ? Hg2 Ge7B Ge4B 72.90(3) . . ? Ge3B Ge7B Ge4B 63.77(4) . . ? Ge8B Ge7B Ge9B 52.07(3) . . ? Ge6B Ge7B Ge9B 52.30(3) . . ? Hg2 Ge7B Ge9B 156.43(3) . . ? Ge3B Ge7B Ge9B 84.49(3) . . ? Ge4B Ge7B Ge9B 83.52(3) . . ? Ge7B Ge8B Ge4B 63.37(4) . . ? Ge7B Ge8B Ge9B 77.00(4) . . ? Ge4B Ge8B Ge9B 99.31(3) . . ? Ge7B Ge8B Ge5B 101.21(3) . . ? Ge4B Ge8B Ge5B 63.70(3) . . ? Ge9B Ge8B Ge5B 59.49(4) . . ? Ge8B Ge9B Ge2B 110.14(3) . . ? Ge8B Ge9B Ge6B 102.08(4) . . ? Ge2B Ge9B Ge6B 60.73(3) . . ? Ge8B Ge9B Ge5B 61.84(3) . . ? Ge2B Ge9B Ge5B 64.32(4) . . ? Ge6B Ge9B Ge5B 110.50(3) . . ? Ge8B Ge9B Hg1 135.21(3) . . ? Ge2B Ge9B Hg1 101.05(3) . . ? Ge6B Ge9B Hg1 121.29(3) . . ? Ge5B Ge9B Hg1 107.77(3) . . ? Ge8B Ge9B Ge7B 50.93(3) . . ? Ge2B Ge9B Ge7B 86.52(3) . . ? Ge6B Ge9B Ge7B 51.33(3) . . ? Ge5B Ge9B Ge7B 87.38(3) . . ? Hg1 Ge9B Ge7B 164.79(3) . . ? Ge9B Hg1 Ge4A 157.76(2) . . ? Ge9B Hg1 Ge3A 143.68(2) . . ? Ge4A Hg1 Ge3A 56.97(3) . . ? Ge9B Hg1 Ge7A 138.25(2) . . ? Ge4A Hg1 Ge7A 53.88(3) . . ? Ge3A Hg1 Ge7A 54.44(2) . . ? Ge7B Hg2 Ge7B 180.000(7) . 2_576 ? Ge7B Hg2 Ge4B 124.76(3) . 2_576 ? Ge7B Hg2 Ge4B 55.24(3) 2_576 2_576 ? Ge7B Hg2 Ge4B 55.24(3) . . ? Ge7B Hg2 Ge4B 124.76(3) 2_576 . ? Ge4B Hg2 Ge4B 180.000(18) 2_576 . ? C101 N11 C107 109.6(5) . . ? C101 N11 C113 110.8(5) . . ? C107 N11 C113 110.8(5) . . ? C118 N12 C106 109.2(4) . . ? C118 N12 C112 110.2(5) . . ? C106 N12 C112 110.3(5) . . ? C103 O11 C102 110.9(4) . . ? C104 O12 C105 112.4(4) . . ? C109 O13 C108 122.5(6) . . ? C110 O14 C111 114.2(5) . . ? C115 O15 C114 112.9(5) . . ? C116 O16 C117 111.9(5) . . ? N11 C101 C102 114.0(5) . . ? N11 C101 H10A 108.7 . . ? C102 C101 H10A 108.7 . . ? N11 C101 H10B 108.7 . . ? C102 C101 H10B 108.7 . . ? H10A C101 H10B 107.6 . . ? O11 C102 C101 107.9(5) . . ? 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(4) . . ? 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 109.5(5) . . ? O12 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O12 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 108.5(4) . . ? O12 C105 H10I 110.0 . . ? C106 C105 H10I 110.0 . . ? O12 C105 H10J 110.0 . . ? C106 C105 H10J 110.0 . . ? H10I C105 H10J 108.4 . . ? N12 C106 C105 114.0(5) . . ? N12 C106 H10K 108.8 . . ? C105 C106 H10K 108.8 . . ? N12 C106 H10L 108.8 . . ? C105 C106 H10L 108.8 . . ? H10K C106 H10L 107.7 . . ? N11 C107 C108 114.9(5) . . ? N11 C107 H10M 108.5 . . ? C108 C107 H10M 108.5 . . ? N11 C107 H10N 108.5 . . ? C108 C107 H10N 108.5 . . ? H10M C107 H10N 107.5 . . ? O13 C108 C107 112.1(6) . . ? O13 C108 H10O 109.2 . . ? C107 C108 H10O 109.2 . . ? O13 C108 H10P 109.2 . . ? C107 C108 H10P 109.2 . . ? H10O C108 H10P 107.9 . . ? O13 C109 C110 126.5(7) . . ? O13 C109 H10Q 105.7 . . ? C110 C109 H10Q 105.7 . . ? O13 C109 H10R 105.7 . . ? C110 C109 H10R 105.7 . . ? H10Q C109 H10R 106.1 . . ? O14 C110 C109 111.7(6) . . ? O14 C110 H11A 109.3 . . ? C109 C110 H11A 109.3 . . ? O14 C110 H11B 109.3 . . ? C109 C110 H11B 109.3 . . ? H11A C110 H11B 107.9 . . ? O14 C111 C112 109.7(5) . . ? O14 C111 H11C 109.7 . . ? C112 C111 H11C 109.7 . . ? O14 C111 H11D 109.7 . . ? C112 C111 H11D 109.7 . . ? H11C C111 H11D 108.2 . . ? N12 C112 C111 114.8(5) . . ? N12 C112 H11E 108.6 . . ? C111 C112 H11E 108.6 . . ? N12 C112 H11F 108.6 . . ? C111 C112 H11F 108.6 . . ? H11E C112 H11F 107.5 . . ? N11 C113 C114 114.0(5) . . ? N11 C113 H11G 108.7 . . ? C114 C113 H11G 108.7 . . ? N11 C113 H11H 108.7 . . ? C114 C113 H11H 108.7 . . ? H11G C113 H11H 107.6 . . ? O15 C114 C113 110.1(5) . . ? O15 C114 H11I 109.6 . . ? C113 C114 H11I 109.6 . . ? O15 C114 H11J 109.6 . . ? C113 C114 H11J 109.6 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 110.2(5) . . ? O15 C115 H11K 109.6 . . ? C116 C115 H11K 109.6 . . ? O15 C115 H11L 109.6 . . ? C116 C115 H11L 109.6 . . ? H11K C115 H11L 108.1 . . ? O16 C116 C115 109.6(5) . . ? 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 110.2(5) . . ? O16 C117 H11O 109.6 . . ? C118 C117 H11O 109.6 . . ? O16 C117 H11P 109.6 . . ? C118 C117 H11P 109.6 . . ? H11O C117 H11P 108.1 . . ? N12 C118 C117 113.2(5) . . ? N12 C118 H11Q 108.9 . . ? C117 C118 H11Q 108.9 . . ? N12 C118 H11R 108.9 . . ? C117 C118 H11R 108.9 . . ? H11Q C118 H11R 107.8 . . ? C201 N21 C213 109.8(9) . . ? C201 N21 C207 111.0(8) . . ? C213 N21 C207 112.1(10) . . ? C212 N22 C218 110.4(9) . . ? C212 N22 C206 111.7(8) . . ? C218 N22 C206 107.8(8) . . ? C203 O21 C202 108.7(7) . . ? C205 O22 C204 112.6(8) . . ? C208 O23 C209 111.8(9) . . ? C211 O24 C210 109.8(7) . . ? C214 O25 C215 111.3(7) . . ? C217 O26 C216 110.7(7) . . ? N21 C201 C202 113.6(7) . . ? 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 107.6(7) . . ? O21 C202 H20C 110.2 . . ? C201 C202 H20C 110.2 . . ? O21 C202 H20D 110.2 . . ? C201 C202 H20D 110.2 . . ? H20C C202 H20D 108.5 . . ? O21 C203 C204 106.8(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 . . ? C203 C204 O22 110.5(6) . . ? C203 C204 H20G 109.5 . . ? O22 C204 H20G 109.5 . . ? C203 C204 H20H 109.5 . . ? O22 C204 H20H 109.5 . . ? H20G C204 H20H 108.1 . . ? O22 C205 C206 109.2(8) . . ? O22 C205 H20I 109.8 . . ? C206 C205 H20I 109.8 . . ? O22 C205 H20J 109.8 . . ? C206 C205 H20J 109.8 . . ? H20I C205 H20J 108.3 . . ? N22 C206 C205 114.9(8) . . ? N22 C206 H20K 108.6 . . ? C205 C206 H20K 108.6 . . ? N22 C206 H20L 108.6 . . ? C205 C206 H20L 108.6 . . ? H20K C206 H20L 107.5 . . ? C208 C207 N21 112.0(7) . . ? C208 C207 H20M 109.2 . . ? N21 C207 H20M 109.2 . . ? C208 C207 H20N 109.2 . . ? N21 C207 H20N 109.2 . . ? H20M C207 H20N 107.9 . . ? 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 109.6(7) . . ? O23 C209 H20Q 109.8 . . ? C210 C209 H20Q 109.8 . . ? O23 C209 H20R 109.8 . . ? C210 C209 H20R 109.8 . . ? H20Q C209 H20R 108.2 . . ? O24 C210 C209 109.4(8) . . ? O24 C210 H21A 109.8 . . ? C209 C210 H21A 109.8 . . ? O24 C210 H21B 109.8 . . ? C209 C210 H21B 109.8 . . ? H21A C210 H21B 108.2 . . ? O24 C211 C212 108.8(6) . . ? 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 . . ? N22 C212 C211 114.6(7) . . ? N22 C212 H21E 108.6 . . ? C211 C212 H21E 108.6 . . ? N22 C212 H21F 108.6 . . ? C211 C212 H21F 108.6 . . ? H21E C212 H21F 107.6 . . ? N21 C213 C214 116.8(10) . . ? N21 C213 H21G 108.1 . . ? C214 C213 H21G 108.1 . . ? N21 C213 H21H 108.1 . . ? C214 C213 H21H 108.1 . . ? H21G C213 H21H 107.3 . . ? O25 C214 C213 108.8(8) . . ? 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 108.2(5) . . ? O25 C215 H21K 110.1 . . ? C216 C215 H21K 110.1 . . ? O25 C215 H21L 110.1 . . ? C216 C215 H21L 110.1 . . ? H21K C215 H21L 108.4 . . ? O26 C216 C215 108.2(6) . . ? 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 107.6(9) . . ? O26 C217 H21O 110.2 . . ? C218 C217 H21O 110.2 . . ? O26 C217 H21P 110.2 . . ? C218 C217 H21P 110.2 . . ? H21O C217 H21P 108.5 . . ? N22 C218 C217 111.8(8) . . ? N22 C218 H21Q 109.3 . . ? C217 C218 H21Q 109.3 . . ? N22 C218 H21R 109.3 . . ? C217 C218 H21R 109.3 . . ? H21Q C218 H21R 107.9 . . ? C301 N31 C307 112.3(5) . . ? C301 N31 C313 110.4(4) . . ? C307 N31 C313 109.5(4) . . ? C306 N32 C312 111.4(4) . . ? C306 N32 C318 110.4(4) . . ? C312 N32 C318 109.1(4) . . ? C302 O31 C303 112.3(4) . . ? C305 O32 C304 110.3(4) . . ? C308 O33 C309 111.7(4) . . ? C310 O34 C311 113.2(4) . . ? C315 O35 C314 111.2(4) . . ? C317 O36 C316 111.4(4) . . ? N31 C301 C302 114.3(4) . . ? N31 C301 H30A 108.7 . . ? C302 C301 H30A 108.7 . . ? N31 C301 H30B 108.7 . . ? C302 C301 H30B 108.7 . . ? H30A C301 H30B 107.6 . . ? O31 C302 C301 110.0(4) . . ? O31 C302 H30C 109.7 . . ? C301 C302 H30C 109.7 . . ? O31 C302 H30D 109.7 . . ? C301 C302 H30D 109.7 . . ? H30C C302 H30D 108.2 . . ? O31 C303 C304 109.3(4) . . ? O31 C303 H30E 109.8 . . ? C304 C303 H30E 109.8 . . ? O31 C303 H30F 109.8 . . ? C304 C303 H30F 109.8 . . ? H30E C303 H30F 108.3 . . ? O32 C304 C303 109.3(4) . . ? 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 110.3(4) . . ? O32 C305 H30I 109.6 . . ? C306 C305 H30I 109.6 . . ? O32 C305 H30J 109.6 . . ? C306 C305 H30J 109.6 . . ? H30I C305 H30J 108.1 . . ? N32 C306 C305 113.8(4) . . ? 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 114.1(4) . . ? 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 109.5(5) . . ? O33 C308 H30O 109.8 . . ? C307 C308 H30O 109.8 . . ? O33 C308 H30P 109.8 . . ? C307 C308 H30P 109.8 . . ? H30O C308 H30P 108.2 . . ? O33 C309 C310 111.1(5) . . ? O33 C309 H30Q 109.4 . . ? C310 C309 H30Q 109.4 . . ? O33 C309 H30R 109.4 . . ? C310 C309 H30R 109.4 . . ? H30Q C309 H30R 108.0 . . ? O34 C310 C309 109.0(4) . . ? 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 109.3(4) . . ? 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 114.7(5) . . ? N32 C312 H31E 108.6 . . ? C311 C312 H31E 108.6 . . ? N32 C312 H31F 108.6 . . ? C311 C312 H31F 108.6 . . ? H31E C312 H31F 107.6 . . ? N31 C313 C314 114.2(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 109.2(4) . . ? O35 C314 H31I 109.8 . . ? C313 C314 H31I 109.8 . . ? O35 C314 H31J 109.8 . . ? C313 C314 H31J 109.8 . . ? H31I C314 H31J 108.3 . . ? O35 C315 C316 110.2(4) . . ? O35 C315 H31O 109.6 . . ? C316 C315 H31O 109.6 . . ? O35 C315 H31P 109.6 . . ? C316 C315 H31P 109.6 . . ? H31O C315 H31P 108.1 . . ? O36 C316 C315 109.1(4) . . ? O36 C316 H31Q 109.9 . . ? C315 C316 H31Q 109.9 . . ? O36 C316 H31R 109.9 . . ? C315 C316 H31R 109.9 . . ? H31Q C316 H31R 108.3 . . ? O36 C317 C318 109.9(4) . . ? O36 C317 H31K 109.7 . . ? C318 C317 H31K 109.7 . . ? O36 C317 H31L 109.7 . . ? C318 C317 H31L 109.7 . . ? H31K C317 H31L 108.2 . . ? N32 C318 C317 113.6(4) . . ? N32 C318 H31M 108.8 . . ? C317 C318 H31M 108.8 . . ? N32 C318 H31N 108.8 . . ? C317 C318 H31N 108.8 . . ? H31M C318 H31N 107.7 . . ? C401 N41 C413 109.4(5) . . ? C401 N41 C407 110.3(4) . . ? C413 N41 C407 109.3(5) . . ? C412 N42 C418 110.3(5) . . ? C412 N42 C406 110.6(5) . . ? C418 N42 C406 110.3(5) . . ? C402 O41 C403 111.4(4) . . ? C404 O42 C405 111.4(4) . . ? C408 O43 C409 111.3(5) . . ? C410 O44 C411 112.6(5) . . ? C415 O45 C414 113.3(6) . . ? C417 O46 C416 114.3(7) . . ? N41 C401 C402 114.7(5) . . ? N41 C401 H40A 108.6 . . ? C402 C401 H40A 108.6 . . ? N41 C401 H40B 108.6 . . ? C402 C401 H40B 108.6 . . ? H40A C401 H40B 107.6 . . ? O41 C402 C401 110.4(4) . . ? O41 C402 H40C 109.6 . . ? C401 C402 H40C 109.6 . . ? O41 C402 H40D 109.6 . . ? C401 C402 H40D 109.6 . . ? H40C C402 H40D 108.1 . . ? O41 C403 C404 110.3(5) . . ? O41 C403 H40E 109.6 . . ? C404 C403 H40E 109.6 . . ? O41 C403 H40F 109.6 . . ? C404 C403 H40F 109.6 . . ? H40E C403 H40F 108.1 . . ? O42 C404 C403 110.2(4) . . ? O42 C404 H40G 109.6 . . ? C403 C404 H40G 109.6 . . ? O42 C404 H40H 109.6 . . ? C403 C404 H40H 109.6 . . ? H40G C404 H40H 108.1 . . ? O42 C405 C406 110.4(4) . . ? O42 C405 H40I 109.6 . . ? C406 C405 H40I 109.6 . . ? O42 C405 H40J 109.6 . . ? C406 C405 H40J 109.6 . . ? H40I C405 H40J 108.1 . . ? N42 C406 C405 114.5(5) . . ? N42 C406 H40K 108.6 . . ? C405 C406 H40K 108.6 . . ? N42 C406 H40L 108.6 . . ? C405 C406 H40L 108.6 . . ? H40K C406 H40L 107.6 . . ? N41 C407 C408 113.1(5) . . ? N41 C407 H40M 109.0 . . ? C408 C407 H40M 109.0 . . ? N41 C407 H40N 109.0 . . ? C408 C407 H40N 109.0 . . ? H40M C407 H40N 107.8 . . ? O43 C408 C407 109.9(5) . . ? O43 C408 H40O 109.7 . . ? C407 C408 H40O 109.7 . . ? O43 C408 H40P 109.7 . . ? C407 C408 H40P 109.7 . . ? H40O C408 H40P 108.2 . . ? O43 C409 C410 108.7(5) . . ? O43 C409 H40Q 109.9 . . ? C410 C409 H40Q 109.9 . . ? O43 C409 H40R 109.9 . . ? C410 C409 H40R 109.9 . . ? H40Q C409 H40R 108.3 . . ? O44 C410 C409 109.9(5) . . ? O44 C410 H41A 109.7 . . ? C409 C410 H41A 109.7 . . ? O44 C410 H41B 109.7 . . ? C409 C410 H41B 109.7 . . ? H41A C410 H41B 108.2 . . ? O44 C411 C412 110.2(5) . . ? O44 C411 H41C 109.6 . . ? C412 C411 H41C 109.6 . . ? O44 C411 H41D 109.6 . . ? C412 C411 H41D 109.6 . . ? H41C C411 H41D 108.1 . . ? N42 C412 C411 115.2(5) . . ? N42 C412 H41E 108.5 . . ? C411 C412 H41E 108.5 . . ? N42 C412 H41F 108.5 . . ? C411 C412 H41F 108.5 . . ? H41E C412 H41F 107.5 . . ? C414 C413 N41 114.2(5) . . ? C414 C413 H41G 108.7 . . ? N41 C413 H41G 108.7 . . ? C414 C413 H41H 108.7 . . ? N41 C413 H41H 108.7 . . ? H41G C413 H41H 107.6 . . ? O45 C414 C413 109.6(5) . . ? O45 C414 H41I 109.8 . . ? C413 C414 H41I 109.8 . . ? O45 C414 H41J 109.8 . . ? C413 C414 H41J 109.8 . . ? H41I C414 H41J 108.2 . . ? C416 C415 O45 118.2(7) . . ? C416 C415 H41K 107.8 . . ? O45 C415 H41K 107.8 . . ? C416 C415 H41L 107.8 . . ? O45 C415 H41L 107.8 . . ? H41K C415 H41L 107.1 . . ? C415 C416 O46 116.8(8) . . ? C415 C416 H41M 108.1 . . ? O46 C416 H41M 108.1 . . ? C415 C416 H41N 108.1 . . ? O46 C416 H41N 108.1 . . ? H41M C416 H41N 107.3 . . ? O46 C417 C418 108.0(6) . . ? O46 C417 H41O 110.1 . . ? C418 C417 H41O 110.1 . . ? O46 C417 H41P 110.1 . . ? C418 C417 H41P 110.1 . . ? H41O C417 H41P 108.4 . . ? N42 C418 C417 114.5(5) . . ? N42 C418 H41Q 108.6 . . ? C417 C418 H41Q 108.6 . . ? N42 C418 H41R 108.6 . . ? C417 C418 H41R 108.6 . . ? H41Q C418 H41R 107.6 . . ? C507 N51 C513 108.5(5) . . ? C507 N51 C501 109.3(5) . . ? C513 N51 C501 110.5(5) . . ? C512 N52 C518 109.6(4) . . ? C512 N52 C506 111.3(5) . . ? C518 N52 C506 110.0(4) . . ? C503 O51 C502 110.6(4) . . ? C505 O52 C504 111.3(4) . . ? C509 O53 C508 112.4(4) . . ? C511 O54 C510 110.6(4) . . ? C514 O55 C515 111.8(4) . . ? C516 O56 C517 111.9(4) . . ? N51 C501 C502 114.4(5) . . ? N51 C501 H50A 108.7 . . ? C502 C501 H50A 108.7 . . ? N51 C501 H50B 108.7 . . ? C502 C501 H50B 108.7 . . ? H50A C501 H50B 107.6 . . ? O51 C502 C501 109.1(5) . . ? O51 C502 H50C 109.9 . . ? C501 C502 H50C 109.9 . . ? O51 C502 H50D 109.9 . . ? C501 C502 H50D 109.9 . . ? H50C C502 H50D 108.3 . . ? O51 C503 C504 109.3(4) . . ? O51 C503 H50E 109.8 . . ? C504 C503 H50E 109.8 . . ? O51 C503 H50F 109.8 . . ? C504 C503 H50F 109.8 . . ? H50E C503 H50F 108.3 . . ? O52 C504 C503 108.4(4) . . ? O52 C504 H50G 110.0 . . ? C503 C504 H50G 110.0 . . ? O52 C504 H50H 110.0 . . ? C503 C504 H50H 110.0 . . ? H50G C504 H50H 108.4 . . ? O52 C505 C506 108.2(5) . . ? O52 C505 H50I 110.1 . . ? C506 C505 H50I 110.1 . . ? O52 C505 H50J 110.1 . . ? C506 C505 H50J 110.1 . . ? H50I C505 H50J 108.4 . . ? N52 C506 C505 114.0(4) . . ? N52 C506 H50K 108.8 . . ? C505 C506 H50K 108.8 . . ? N52 C506 H50L 108.8 . . ? C505 C506 H50L 108.8 . . ? H50K C506 H50L 107.7 . . ? N51 C507 C508 113.6(5) . . ? 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 108.3(5) . . ? O53 C508 H50O 110.0 . . ? C507 C508 H50O 110.0 . . ? O53 C508 H50P 110.0 . . ? C507 C508 H50P 110.0 . . ? H50O C508 H50P 108.4 . . ? O53 C509 C510 108.7(4) . . ? O53 C509 H50Q 110.0 . . ? C510 C509 H50Q 110.0 . . ? O53 C509 H50R 110.0 . . ? C510 C509 H50R 110.0 . . ? H50Q C509 H50R 108.3 . . ? O54 C510 C509 109.6(4) . . ? O54 C510 H51A 109.7 . . ? C509 C510 H51A 109.7 . . ? O54 C510 H51B 109.7 . . ? C509 C510 H51B 109.7 . . ? H51A C510 H51B 108.2 . . ? O54 C511 C512 108.6(4) . . ? O54 C511 H51C 110.0 . . ? C512 C511 H51C 110.0 . . ? O54 C511 H51D 110.0 . . ? C512 C511 H51D 110.0 . . ? H51C C511 H51D 108.4 . . ? N52 C512 C511 114.7(5) . . ? N52 C512 H51E 108.6 . . ? C511 C512 H51E 108.6 . . ? N52 C512 H51F 108.6 . . ? C511 C512 H51F 108.6 . . ? H51E C512 H51F 107.6 . . ? N51 C513 C514 113.3(5) . . ? N51 C513 H51G 108.9 . . ? C514 C513 H51G 108.9 . . ? N51 C513 H51H 108.9 . . ? C514 C513 H51H 108.9 . . ? H51G C513 H51H 107.7 . . ? O55 C514 C513 109.2(5) . . ? O55 C514 H51I 109.8 . . ? C513 C514 H51I 109.8 . . ? O55 C514 H51J 109.8 . . ? C513 C514 H51J 109.8 . . ? H51I C514 H51J 108.3 . . ? O55 C515 C516 110.4(4) . . ? O55 C515 H51K 109.6 . . ? C516 C515 H51K 109.6 . . ? O55 C515 H51L 109.6 . . ? C516 C515 H51L 109.6 . . ? H51K C515 H51L 108.1 . . ? O56 C516 C515 109.9(5) . . ? 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 106.8(4) . . ? O56 C517 H51O 110.4 . . ? C518 C517 H51O 110.4 . . ? O56 C517 H51P 110.4 . . ? C518 C517 H51P 110.4 . . ? H51O C517 H51P 108.6 . . ? N52 C518 C517 114.5(5) . . ? N52 C518 H51Q 108.6 . . ? C517 C518 H51Q 108.6 . . ? N52 C518 H51R 108.6 . . ? C517 C518 H51R 108.6 . . ? H51Q C518 H51R 107.6 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C7 119.9(13) . . ? C1 C2 C3 119.4(13) . . ? C7 C2 C3 120.7(12) . . ? C4 C3 C2 116.1(11) . . ? C4 C3 H3 122.0 . . ? C2 C3 H3 122.0 . . ? C3 C4 C5 126.8(13) . . ? C3 C4 H4 116.6 . . ? C5 C4 H4 116.6 . . ? C4 C5 C6 117.6(14) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C7 C6 C5 118.6(13) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C2 C7 C6 120.2(11) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C1S N1S H1S1 109.5 . . ? C1S N1S H1S2 109.5 . . ? H1S1 N1S H1S2 109.5 . . ? C1S N1S H1S3 109.5 . . ? H1S1 N1S H1S3 109.5 . . ? H1S2 N1S H1S3 109.5 . . ? N1S C1S C2S 102.5(10) . . ? N1S C1S H1S4 111.3 . . ? C2S C1S H1S4 111.3 . . ? N1S C1S H1S5 111.3 . . ? C2S C1S H1S5 111.3 . . ? H1S4 C1S H1S5 109.2 . . ? N2S C2S C1S 99.1(13) . . ? N2S C2S H2S1 111.9 . . ? C1S C2S H2S1 111.9 . . ? N2S C2S H2S2 111.9 . . ? C1S C2S H2S2 111.9 . . ? H2S1 C2S H2S2 109.6 . . ? 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 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.804 _refine_diff_density_min -1.575 _refine_diff_density_rms 0.145 #===END data_[Hg(Ge9)]2- _database_code_depnum_ccdc_archive 'CCDC 693236' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)]2[Hg(Ge9)]*2py ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K-(2,2,2-crypt))2(Hg(Ge9))*2py _chemical_melting_point ? _chemical_formula_moiety '2(C18 H36 K N2 O6), Ge9 Hg, 2(C5 H5 N)' _chemical_formula_sum 'C46 H82 Ge9 Hg K2 N6 O12' _chemical_formula_weight 1843.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 14.30030(10) _cell_length_b 16.14560(10) _cell_length_c 28.9538(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.8634(3) _cell_angle_gamma 90.00 _cell_volume 6669.86(8) _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 'dark green-black' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 6.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1125 _exptl_absorpt_correction_T_max 0.6258 _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25494 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0330 _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 -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13001 _reflns_number_gt 11358 _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^)+(0.0323P)^2^+16.2727P] 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 13001 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Hg1 Hg 0.483150(11) 0.799112(10) 0.247416(6) 0.03276(6) Uani 1 1 d . . . Ge1 Ge 0.54650(4) 0.52877(3) 0.133508(17) 0.04733(14) Uani 1 1 d . . . Ge2 Ge 0.44450(3) 0.44392(3) 0.186192(17) 0.03544(11) Uani 1 1 d . . . Ge3 Ge 0.42586(3) 0.61441(3) 0.176818(17) 0.03846(12) Uani 1 1 d . . . Ge4 Ge 0.61869(3) 0.63272(3) 0.192426(16) 0.03443(11) Uani 1 1 d . . . Ge5 Ge 0.63811(3) 0.46204(3) 0.203648(17) 0.03604(11) Uani 1 1 d . . . Ge6 Ge 0.37373(3) 0.53297(3) 0.249351(18) 0.03848(12) Uani 1 1 d . . . Ge7 Ge 0.50245(3) 0.64349(3) 0.259358(16) 0.03350(11) Uani 1 1 d . . . Ge8 Ge 0.65719(3) 0.56445(3) 0.272466(16) 0.03594(11) Uani 1 1 d . . . Ge9 Ge 0.52485(3) 0.45490(3) 0.272649(16) 0.03389(11) Uani 1 1 d . . . K1 K 1.02694(7) 0.82632(6) 0.29961(4) 0.0375(2) Uani 1 1 d . . . N11 N 0.8930(3) 0.8620(3) 0.21594(15) 0.0468(10) Uani 1 1 d . . . N12 N 1.1583(3) 0.7901(3) 0.38527(15) 0.0489(10) Uani 1 1 d . . . O11 O 0.8415(2) 0.7730(2) 0.29942(12) 0.0493(8) Uani 1 1 d . . . O12 O 0.9560(2) 0.7506(2) 0.38178(14) 0.0563(9) Uani 1 1 d . . . O13 O 1.0010(2) 0.99401(19) 0.26966(11) 0.0382(7) Uani 1 1 d . . . O14 O 1.1253(2) 0.95041(19) 0.34524(12) 0.0448(8) Uani 1 1 d . . . O15 O 1.0629(3) 0.7661(2) 0.21165(13) 0.0508(9) Uani 1 1 d . . . O16 O 1.1773(2) 0.7182(2) 0.29259(14) 0.0535(9) Uani 1 1 d . . . C101 C 0.8040(4) 0.8187(4) 0.2222(2) 0.0621(15) Uani 1 1 d . . . H10A H 0.8099 0.7606 0.2120 0.074 Uiso 1 1 calc R . . H10B H 0.7538 0.8451 0.2021 0.074 Uiso 1 1 calc R . . C102 C 0.7759(3) 0.8194(4) 0.2710(2) 0.0581(15) Uani 1 1 d . . . H10C H 0.7737 0.8771 0.2823 0.070 Uiso 1 1 calc R . . H10D H 0.7126 0.7950 0.2722 0.070 Uiso 1 1 calc R . . C103 C 0.8052(4) 0.7510(4) 0.3415(2) 0.0591(15) Uani 1 1 d . . . H10E H 0.7467 0.7188 0.3355 0.071 Uiso 1 1 calc R . . H10F H 0.7903 0.8015 0.3590 0.071 Uiso 1 1 calc R . . C104 C 0.8754(4) 0.7005(4) 0.3690(2) 0.0670(17) Uani 1 1 d . . . H10G H 0.8478 0.6794 0.3972 0.080 Uiso 1 1 calc R . . H10H H 0.8942 0.6524 0.3505 0.080 Uiso 1 1 calc R . . C105 C 1.0241(4) 0.7076(4) 0.4107(2) 0.0696(18) Uani 1 1 d . . . H10I H 1.0486 0.6597 0.3940 0.084 Uiso 1 1 calc R . . H10J H 0.9956 0.6869 0.4387 0.084 Uiso 1 1 calc R . . C106 C 1.1029(4) 0.7673(4) 0.4243(2) 0.0671(17) Uani 1 1 d . . . H10K H 1.0760 0.8182 0.4371 0.081 Uiso 1 1 calc R . . H10L H 1.1448 0.7418 0.4489 0.081 Uiso 1 1 calc R . . C107 C 0.8792(3) 0.9527(3) 0.2141(2) 0.0490(12) Uani 1 1 d . . . H10M H 0.8355 0.9687 0.2376 0.059 Uiso 1 1 calc R . . H10N H 0.8496 0.9677 0.1833 0.059 Uiso 1 1 calc R . . C108 C 0.9680(3) 1.0010(3) 0.22230(18) 0.0454(11) Uani 1 1 d . . . H10O H 1.0160 0.9794 0.2023 0.054 Uiso 1 1 calc R . . H10P H 0.9565 1.0599 0.2144 0.054 Uiso 1 1 calc R . . C109 C 1.0908(3) 1.0315(3) 0.27833(18) 0.0425(11) Uani 1 1 d . . . H10Q H 1.0898 1.0885 0.2657 0.051 Uiso 1 1 calc R . . H10R H 1.1386 0.9994 0.2628 0.051 Uiso 1 1 calc R . . C110 C 1.1153(4) 1.0337(3) 0.32922(19) 0.0463(12) Uani 1 1 d . . . H11A H 1.1747 1.0644 0.3358 0.056 Uiso 1 1 calc R . . H11B H 1.0653 1.0621 0.3452 0.056 Uiso 1 1 calc R . . C111 C 1.1634(4) 0.9441(3) 0.39162(19) 0.0509(13) Uani 1 1 d . . . H11C H 1.1125 0.9455 0.4131 0.061 Uiso 1 1 calc R . . H11D H 1.2061 0.9912 0.3990 0.061 Uiso 1 1 calc R . . C112 C 1.2162(4) 0.8640(3) 0.39694(19) 0.0509(13) Uani 1 1 d . . . H11E H 1.2694 0.8653 0.3768 0.061 Uiso 1 1 calc R . . H11F H 1.2424 0.8591 0.4293 0.061 Uiso 1 1 calc R . . C113 C 0.9325(4) 0.8335(3) 0.17312(19) 0.0535(13) Uani 1 1 d . . . H11G H 0.9753 0.8766 0.1624 0.064 Uiso 1 1 calc R . . H11H H 0.8811 0.8262 0.1488 0.064 Uiso 1 1 calc R . . C114 C 0.9853(4) 0.7534(3) 0.1793(2) 0.0601(15) Uani 1 1 d . . . H11I H 0.9438 0.7100 0.1908 0.072 Uiso 1 1 calc R . . H11J H 1.0074 0.7349 0.1493 0.072 Uiso 1 1 calc R . . C115 C 1.1277(5) 0.6989(3) 0.2131(2) 0.0620(17) Uani 1 1 d . . . H11K H 1.1504 0.6896 0.1819 0.074 Uiso 1 1 calc R . . H11L H 1.0968 0.6476 0.2229 0.074 Uiso 1 1 calc R . . C116 C 1.2076(4) 0.7197(4) 0.2464(2) 0.0654(18) Uani 1 1 d . . . H11M H 1.2588 0.6791 0.2435 0.078 Uiso 1 1 calc R . . H11N H 1.2319 0.7754 0.2394 0.078 Uiso 1 1 calc R . . C117 C 1.2543(4) 0.7273(3) 0.3257(2) 0.0620(16) Uani 1 1 d . . . H11O H 1.2846 0.7817 0.3217 0.074 Uiso 1 1 calc R . . H11P H 1.3013 0.6835 0.3212 0.074 Uiso 1 1 calc R . . C118 C 1.2198(4) 0.7209(3) 0.3731(2) 0.0604(16) Uani 1 1 d . . . H11Q H 1.1850 0.6682 0.3755 0.073 Uiso 1 1 calc R . . H11R H 1.2745 0.7189 0.3960 0.073 Uiso 1 1 calc R . . K2 K 0.64425(7) 0.82176(6) 0.00605(3) 0.0348(2) Uani 1 1 d . . . N21 N 0.5308(3) 0.6710(3) -0.02425(15) 0.0518(11) Uani 1 1 d . . . N22 N 0.7590(4) 0.9756(3) 0.03882(17) 0.0608(13) Uani 1 1 d . . . O21 O 0.5121(3) 0.7591(3) 0.05963(15) 0.0787(14) Uani 1 1 d . . . O22 O 0.6098(3) 0.8993(2) 0.08927(11) 0.0497(8) Uani 1 1 d . . . O23 O 0.5355(3) 0.8264(2) -0.07780(11) 0.0497(9) Uani 1 1 d . . . O24 O 0.6559(3) 0.9612(2) -0.05155(14) 0.0598(10) Uani 1 1 d . . . O25 O 0.7357(3) 0.6688(2) 0.00079(16) 0.0671(11) Uani 1 1 d . . . O26 O 0.8359(3) 0.8076(3) 0.03550(17) 0.0757(13) Uani 1 1 d . . . C201 C 0.4705(5) 0.6451(4) 0.0125(2) 0.0724(19) Uani 1 1 d . . . H20A H 0.4170 0.6130 -0.0016 0.087 Uiso 1 1 calc R . . H20B H 0.5068 0.6081 0.0343 0.087 Uiso 1 1 calc R . . C202 C 0.4345(5) 0.7144(5) 0.0384(3) 0.082(2) Uani 1 1 d . . . H20C H 0.3964 0.7513 0.0173 0.099 Uiso 1 1 calc R . . H20D H 0.3942 0.6936 0.0624 0.099 Uiso 1 1 calc R . . C203 C 0.4966(5) 0.7982(4) 0.1008(2) 0.0698(19) Uani 1 1 d . . . H20E H 0.4758 0.7568 0.1232 0.084 Uiso 1 1 calc R . . H20F H 0.4460 0.8395 0.0954 0.084 Uiso 1 1 calc R . . C204 C 0.5798(5) 0.8387(4) 0.12007(18) 0.0625(16) Uani 1 1 d . . . H20G H 0.5668 0.8652 0.1498 0.075 Uiso 1 1 calc R . . H20H H 0.6302 0.7973 0.1263 0.075 Uiso 1 1 calc R . . C205 C 0.6804(6) 0.9504(4) 0.1109(2) 0.076(2) Uani 1 1 d . . . H20I H 0.7344 0.9160 0.1224 0.092 Uiso 1 1 calc R . . H20J H 0.6556 0.9793 0.1376 0.092 Uiso 1 1 calc R . . C206 C 0.7115(6) 1.0125(4) 0.0767(2) 0.0756(19) Uani 1 1 d . . . H20K H 0.6561 1.0435 0.0637 0.091 Uiso 1 1 calc R . . H20L H 0.7543 1.0526 0.0930 0.091 Uiso 1 1 calc R . . C207 C 0.4727(4) 0.6928(4) -0.0666(2) 0.0610(15) Uani 1 1 d . . . H20M H 0.4151 0.7208 -0.0575 0.073 Uiso 1 1 calc R . . H20N H 0.4534 0.6411 -0.0830 0.073 Uiso 1 1 calc R . . C208 C 0.5203(5) 0.7476(4) -0.09908(18) 0.0614(15) Uani 1 1 d . . . H20O H 0.5809 0.7229 -0.1064 0.074 Uiso 1 1 calc R . . H20P H 0.4808 0.7538 -0.1283 0.074 Uiso 1 1 calc R . . C209 C 0.5680(4) 0.8852(4) -0.10916(17) 0.0576(14) Uani 1 1 d . . . H20Q H 0.5214 0.8911 -0.1358 0.069 Uiso 1 1 calc R . . H20R H 0.6274 0.8654 -0.1210 0.069 Uiso 1 1 calc R . . C210 C 0.5834(4) 0.9658(3) -0.0869(2) 0.0574(14) Uani 1 1 d . . . H21A H 0.5999 1.0071 -0.1102 0.069 Uiso 1 1 calc R . . H21B H 0.5249 0.9843 -0.0735 0.069 Uiso 1 1 calc R . . C211 C 0.6732(5) 1.0388(3) -0.0292(2) 0.0715(19) Uani 1 1 d . . . H21C H 0.6209 1.0526 -0.0099 0.086 Uiso 1 1 calc R . . H21D H 0.6779 1.0830 -0.0526 0.086 Uiso 1 1 calc R . . C212 C 0.7626(6) 1.0333(4) 0.0003(3) 0.082(2) Uani 1 1 d . . . H21E H 0.8134 1.0160 -0.0192 0.098 Uiso 1 1 calc R . . H21F H 0.7786 1.0890 0.0128 0.098 Uiso 1 1 calc R . . C213 C 0.5967(5) 0.6048(4) -0.0338(2) 0.0750(19) Uani 1 1 d . . . H21G H 0.6233 0.6155 -0.0639 0.090 Uiso 1 1 calc R . . H21H H 0.5626 0.5514 -0.0362 0.090 Uiso 1 1 calc R . . C214 C 0.6761(5) 0.5978(4) 0.0036(3) 0.077(2) Uani 1 1 d . . . H21I H 0.6504 0.5954 0.0345 0.092 Uiso 1 1 calc R . . H21J H 0.7124 0.5466 -0.0009 0.092 Uiso 1 1 calc R . . C215 C 0.8167(5) 0.6635(4) 0.0311(3) 0.089(2) Uani 1 1 d . . . H21K H 0.8494 0.6105 0.0261 0.106 Uiso 1 1 calc R . . H21L H 0.7992 0.6651 0.0635 0.106 Uiso 1 1 calc R . . C216 C 0.8785(5) 0.7325(5) 0.0225(4) 0.100(3) Uani 1 1 d . . . H21M H 0.9392 0.7251 0.0406 0.120 Uiso 1 1 calc R . . H21N H 0.8907 0.7344 -0.0108 0.120 Uiso 1 1 calc R . . C217 C 0.8894(5) 0.8801(5) 0.0250(3) 0.084(2) Uani 1 1 d . . . H21O H 0.8803 0.8935 -0.0083 0.101 Uiso 1 1 calc R . . H21P H 0.9569 0.8703 0.0328 0.101 Uiso 1 1 calc R . . C218 C 0.8550(5) 0.9497(4) 0.0534(2) 0.075(2) Uani 1 1 d . . . H21Q H 0.8571 0.9323 0.0863 0.090 Uiso 1 1 calc R . . H21R H 0.8976 0.9976 0.0512 0.090 Uiso 1 1 calc R . . N1S N 0.1073(4) 0.8683(4) 0.08035(19) 0.0719(15) Uani 1 1 d . . . C1S C 0.1611(5) 0.8029(5) 0.0878(3) 0.0763(19) Uani 1 1 d . . . H1S H 0.1495 0.7549 0.0692 0.092 Uiso 1 1 calc R . . C2S C 0.2349(5) 0.8016(6) 0.1221(3) 0.087(3) Uani 1 1 d . . . H2S H 0.2735 0.7541 0.1273 0.105 Uiso 1 1 calc R . . C3S C 0.2488(5) 0.8731(7) 0.1482(2) 0.090(3) Uani 1 1 d . . . H3S H 0.2978 0.8757 0.1720 0.108 Uiso 1 1 calc R . . C4S C 0.1922(5) 0.9389(6) 0.1395(3) 0.081(2) Uani 1 1 d . . . H4S H 0.2010 0.9885 0.1569 0.097 Uiso 1 1 calc R . . C5S C 0.1249(5) 0.9331(5) 0.1066(3) 0.0751(18) Uani 1 1 d . . . H5S H 0.0855 0.9800 0.1014 0.090 Uiso 1 1 calc R . . N1P N 0.1061(7) 0.4805(9) 0.1004(4) 0.202(6) Uani 1 1 d . . . C1P C 0.0616(6) 0.5035(10) 0.0593(4) 0.163(6) Uani 1 1 d . . . H1P H 0.0019 0.4812 0.0498 0.195 Uiso 1 1 calc R . . C2P C 0.1026(5) 0.5574(6) 0.0327(3) 0.091(2) Uani 1 1 d . . . H2P H 0.0696 0.5774 0.0054 0.109 Uiso 1 1 calc R . . C3P C 0.1874(5) 0.5833(4) 0.0435(2) 0.0785(19) Uani 1 1 d . . . H3P H 0.2168 0.6192 0.0229 0.094 Uiso 1 1 calc R . . C4P C 0.2355(5) 0.5595(5) 0.0843(3) 0.082(2) Uani 1 1 d . . . H4P H 0.2979 0.5779 0.0914 0.098 Uiso 1 1 calc R . . C5P C 0.1931(5) 0.5102(5) 0.1140(3) 0.085(2) Uani 1 1 d . . . H5P H 0.2226 0.4964 0.1434 0.102 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 Hg1 0.03748(10) 0.02002(9) 0.04108(10) 0.00305(7) 0.00486(7) -0.00043(6) Ge1 0.0718(4) 0.0441(3) 0.0267(2) -0.0038(2) 0.0076(2) -0.0089(3) Ge2 0.0439(3) 0.0206(2) 0.0412(3) -0.00341(19) -0.0015(2) -0.00402(18) Ge3 0.0443(3) 0.0258(2) 0.0438(3) 0.0085(2) -0.0084(2) 0.00051(19) Ge4 0.0418(2) 0.0236(2) 0.0384(2) 0.00401(19) 0.00617(19) -0.00549(19) Ge5 0.0400(3) 0.0236(2) 0.0458(3) -0.0043(2) 0.0123(2) 0.00446(18) Ge6 0.0365(2) 0.0253(2) 0.0551(3) 0.0022(2) 0.0137(2) 0.00214(19) Ge7 0.0422(2) 0.0174(2) 0.0410(3) -0.00417(18) 0.00376(19) 0.00354(18) Ge8 0.0398(2) 0.0291(2) 0.0379(2) -0.0007(2) -0.00541(19) 0.00114(19) Ge9 0.0441(3) 0.0205(2) 0.0374(2) 0.00540(18) 0.00542(19) 0.00171(18) K1 0.0343(5) 0.0272(5) 0.0519(6) 0.0024(4) 0.0091(4) 0.0025(4) N11 0.043(2) 0.042(2) 0.055(2) -0.001(2) 0.0021(18) -0.0026(18) N12 0.041(2) 0.046(3) 0.060(3) 0.020(2) 0.0067(19) 0.0005(18) O11 0.0368(17) 0.053(2) 0.060(2) 0.0043(18) 0.0135(15) -0.0066(15) O12 0.047(2) 0.055(2) 0.068(2) 0.0172(19) 0.0112(17) -0.0082(17) O13 0.0359(16) 0.0286(16) 0.0501(18) 0.0023(14) 0.0038(13) 0.0003(13) O14 0.0447(18) 0.0295(17) 0.059(2) 0.0020(15) -0.0046(16) 0.0035(14) O15 0.062(2) 0.0306(18) 0.061(2) -0.0041(16) 0.0153(18) 0.0069(16) O16 0.0431(19) 0.040(2) 0.080(3) 0.0116(18) 0.0208(18) 0.0123(15) C101 0.046(3) 0.071(4) 0.067(4) 0.005(3) -0.010(3) -0.017(3) C102 0.031(2) 0.061(4) 0.082(4) 0.008(3) 0.003(2) -0.004(2) C103 0.045(3) 0.064(4) 0.069(4) 0.002(3) 0.014(3) -0.015(3) C104 0.062(4) 0.067(4) 0.074(4) 0.019(3) 0.019(3) -0.025(3) C105 0.064(4) 0.071(4) 0.074(4) 0.037(3) 0.008(3) -0.015(3) C106 0.062(4) 0.083(5) 0.056(3) 0.030(3) -0.001(3) -0.012(3) C107 0.040(3) 0.049(3) 0.057(3) 0.004(2) -0.003(2) 0.005(2) C108 0.050(3) 0.034(3) 0.052(3) 0.005(2) 0.004(2) 0.005(2) C109 0.038(2) 0.031(2) 0.059(3) 0.005(2) 0.008(2) -0.0037(19) C110 0.046(3) 0.030(3) 0.062(3) -0.003(2) -0.001(2) -0.001(2) C111 0.054(3) 0.048(3) 0.049(3) -0.004(2) -0.002(2) 0.004(2) C112 0.046(3) 0.052(3) 0.054(3) 0.015(3) -0.005(2) 0.004(2) C113 0.067(3) 0.043(3) 0.050(3) -0.005(2) 0.002(3) -0.005(3) C114 0.085(4) 0.039(3) 0.058(3) -0.010(3) 0.019(3) -0.009(3) C115 0.087(4) 0.030(3) 0.074(4) 0.007(3) 0.039(3) 0.017(3) C116 0.063(4) 0.040(3) 0.097(5) 0.017(3) 0.040(3) 0.025(3) C117 0.044(3) 0.032(3) 0.112(5) 0.008(3) 0.017(3) 0.011(2) C118 0.046(3) 0.038(3) 0.096(5) 0.023(3) -0.005(3) 0.003(2) K2 0.0457(5) 0.0294(5) 0.0289(4) 0.0007(4) 0.0000(4) -0.0032(4) N21 0.070(3) 0.035(2) 0.047(2) 0.0015(19) -0.013(2) -0.009(2) N22 0.081(3) 0.040(3) 0.059(3) 0.006(2) -0.008(2) -0.021(2) O21 0.089(3) 0.082(3) 0.068(3) -0.016(2) 0.032(2) -0.039(3) O22 0.076(2) 0.0408(19) 0.0324(17) 0.0001(15) 0.0057(16) 0.0012(17) O23 0.074(2) 0.044(2) 0.0299(16) 0.0009(15) -0.0029(16) -0.0042(17) O24 0.077(3) 0.043(2) 0.057(2) 0.0168(18) -0.008(2) -0.0030(18) O25 0.064(2) 0.047(2) 0.087(3) 0.006(2) -0.018(2) 0.0097(19) O26 0.058(3) 0.068(3) 0.097(3) -0.001(3) -0.022(2) -0.009(2) C201 0.080(4) 0.060(4) 0.075(4) 0.016(3) -0.012(3) -0.034(3) C202 0.084(5) 0.090(5) 0.075(4) 0.005(4) 0.022(4) -0.041(4) C203 0.080(4) 0.069(4) 0.064(4) 0.036(3) 0.028(3) 0.013(3) C204 0.107(5) 0.050(3) 0.032(3) 0.005(2) 0.020(3) 0.004(3) C205 0.123(6) 0.063(4) 0.043(3) -0.018(3) -0.001(3) -0.011(4) C206 0.114(6) 0.038(3) 0.073(4) -0.017(3) -0.005(4) -0.020(3) C207 0.074(4) 0.048(3) 0.058(3) -0.007(3) -0.021(3) -0.008(3) C208 0.087(4) 0.056(4) 0.039(3) -0.012(3) -0.012(3) 0.000(3) C209 0.072(4) 0.065(4) 0.035(3) 0.015(3) -0.001(2) 0.005(3) C210 0.071(4) 0.050(3) 0.051(3) 0.025(3) -0.004(3) 0.000(3) C211 0.101(5) 0.032(3) 0.080(4) 0.021(3) -0.007(4) -0.012(3) C212 0.114(6) 0.052(4) 0.077(4) 0.018(3) -0.013(4) -0.039(4) C213 0.101(5) 0.032(3) 0.088(5) -0.009(3) -0.028(4) -0.004(3) C214 0.105(5) 0.030(3) 0.090(5) 0.003(3) -0.027(4) 0.008(3) C215 0.075(5) 0.059(4) 0.127(7) 0.003(4) -0.036(4) 0.016(4) C216 0.056(4) 0.096(6) 0.144(8) 0.011(6) -0.021(4) 0.022(4) C217 0.054(4) 0.091(6) 0.106(6) 0.000(5) -0.012(4) -0.014(4) C218 0.077(4) 0.074(5) 0.070(4) 0.006(3) -0.025(3) -0.033(4) N1S 0.052(3) 0.086(4) 0.077(4) 0.001(3) -0.009(2) -0.009(3) C1S 0.075(5) 0.067(5) 0.089(5) -0.013(4) 0.017(4) -0.018(4) C2S 0.053(4) 0.100(6) 0.111(6) 0.052(5) 0.023(4) 0.008(4) C3S 0.052(4) 0.155(9) 0.060(4) 0.023(5) -0.012(3) -0.048(5) C4S 0.063(4) 0.109(6) 0.071(4) -0.014(4) 0.005(4) -0.029(4) C5S 0.059(4) 0.071(4) 0.096(5) 0.000(4) 0.013(4) -0.005(3) N1P 0.093(6) 0.326(16) 0.184(10) 0.133(11) -0.021(7) -0.043(8) C1P 0.048(4) 0.302(16) 0.131(8) 0.103(10) -0.040(5) -0.039(7) C2P 0.060(4) 0.131(7) 0.079(5) 0.013(5) -0.020(4) 0.016(4) C3P 0.099(5) 0.070(5) 0.065(4) 0.005(3) -0.007(4) -0.016(4) C4P 0.079(5) 0.079(5) 0.084(5) 0.006(4) -0.023(4) -0.024(4) C5P 0.064(4) 0.111(6) 0.076(5) 0.022(4) -0.018(3) -0.003(4) _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 Hg1 Ge7 2.5488(5) . ? Hg1 Ge9 2.5823(5) 2_655 ? Hg1 Ge2 3.1566(5) 2_655 ? Ge1 Ge4 2.5602(7) . ? Ge1 Ge2 2.5751(7) . ? Ge1 Ge5 2.5774(7) . ? Ge1 Ge3 2.5984(8) . ? Ge2 Ge6 2.5855(7) . ? Ge2 Ge9 2.6889(7) . ? Ge2 Ge3 2.7770(6) . ? Ge2 Ge5 2.7961(7) . ? Ge2 Hg1 3.1566(5) 2_645 ? Ge3 Ge7 2.6036(7) . ? Ge3 Ge6 2.6279(7) . ? Ge3 Ge4 2.7798(7) . ? Ge4 Ge8 2.5916(7) . ? Ge4 Ge7 2.6425(6) . ? Ge4 Ge5 2.7865(6) . ? Ge5 Ge8 2.5896(7) . ? Ge5 Ge9 2.6578(6) . ? Ge6 Ge9 2.5529(7) . ? Ge6 Ge7 2.5659(7) . ? Ge7 Ge8 2.5604(6) . ? Ge8 Ge9 2.5908(7) . ? Ge9 Hg1 2.5823(5) 2_645 ? K1 O14 2.736(3) . ? K1 O11 2.788(3) . ? K1 O16 2.788(3) . ? K1 O15 2.806(4) . ? K1 O13 2.860(3) . ? K1 O12 2.917(4) . ? K1 N11 3.041(4) . ? K1 N12 3.065(4) . ? K1 C109 3.502(5) . ? N11 C113 1.471(7) . ? N11 C101 1.472(6) . ? N11 C107 1.478(6) . ? N12 C106 1.469(7) . ? N12 C112 1.478(7) . ? N12 C118 1.478(7) . ? O11 C103 1.402(6) . ? O11 C102 1.420(6) . ? O12 C105 1.422(7) . ? O12 C104 1.436(7) . ? O13 C108 1.424(6) . ? O13 C109 1.427(5) . ? O14 C111 1.419(6) . ? O14 C110 1.427(6) . ? O15 C114 1.417(7) . ? O15 C115 1.426(6) . ? O16 C117 1.417(7) . ? O16 C116 1.434(7) . ? C101 C102 1.494(8) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.483(9) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.514(8) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.495(7) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.492(7) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.500(7) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.502(8) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.483(9) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.495(9) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? K2 O21 2.719(4) . ? K2 O22 2.788(3) . ? K2 O23 2.795(3) . ? K2 O25 2.803(4) . ? K2 O24 2.814(4) . ? K2 O26 2.824(4) . ? K2 N21 3.023(4) . ? K2 N22 3.090(4) . ? K2 C204 3.497(5) . ? N21 C213 1.464(8) . ? N21 C201 1.475(8) . ? N21 C207 1.476(7) . ? N22 C206 1.455(8) . ? N22 C212 1.455(8) . ? N22 C218 1.470(8) . ? O21 C203 1.380(8) . ? O21 C202 1.428(8) . ? O22 C204 1.409(6) . ? O22 C205 1.416(7) . ? O23 C209 1.414(6) . ? O23 C208 1.424(6) . ? O24 C210 1.408(7) . ? O24 C211 1.424(7) . ? O25 C215 1.408(7) . ? O25 C214 1.434(7) . ? O26 C216 1.420(9) . ? O26 C217 1.442(8) . ? C201 C202 1.461(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.438(9) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.498(9) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.490(9) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.463(8) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.492(10) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.518(8) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.453(11) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.495(10) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? N1S C5S 1.307(9) . ? N1S C1S 1.316(9) . ? C1S C2S 1.401(11) . ? C1S H1S 0.9500 . ? C2S C3S 1.386(11) . ? C2S H2S 0.9500 . ? C3S C4S 1.349(11) . ? C3S H3S 0.9500 . ? C4S C5S 1.312(10) . ? C4S H4S 0.9500 . ? C5S H5S 0.9500 . ? N1P C1P 1.364(13) . ? N1P C5P 1.366(11) . ? C1P C2P 1.323(12) . ? C1P H1P 0.9500 . ? C2P C3P 1.301(10) . ? C2P H2P 0.9500 . ? C3P C4P 1.381(9) . ? C3P H3P 0.9500 . ? C4P C5P 1.346(10) . ? C4P H4P 0.9500 . ? C5P H5P 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 Ge7 Hg1 Ge9 173.468(16) . 2_655 ? Ge7 Hg1 Ge2 128.281(15) . 2_655 ? Ge9 Hg1 Ge2 54.779(13) 2_655 2_655 ? Ge4 Ge1 Ge2 99.97(2) . . ? Ge4 Ge1 Ge5 65.689(19) . . ? Ge2 Ge1 Ge5 65.731(19) . . ? Ge4 Ge1 Ge3 65.207(19) . . ? Ge2 Ge1 Ge3 64.927(19) . . ? Ge5 Ge1 Ge3 99.26(2) . . ? Ge1 Ge2 Ge6 112.80(2) . . ? Ge1 Ge2 Ge9 107.03(2) . . ? Ge6 Ge2 Ge9 57.857(18) . . ? Ge1 Ge2 Ge3 57.943(19) . . ? Ge6 Ge2 Ge3 58.559(17) . . ? Ge9 Ge2 Ge3 93.316(19) . . ? Ge1 Ge2 Ge5 57.174(19) . . ? Ge6 Ge2 Ge5 104.12(2) . . ? Ge9 Ge2 Ge5 57.928(17) . . ? Ge3 Ge2 Ge5 90.076(18) . . ? Ge1 Ge2 Hg1 125.40(2) . 2_645 ? Ge6 Ge2 Hg1 96.259(18) . 2_645 ? Ge9 Ge2 Hg1 51.678(13) . 2_645 ? Ge3 Ge2 Hg1 144.99(2) . 2_645 ? Ge5 Ge2 Hg1 71.787(15) . 2_645 ? Ge1 Ge3 Ge7 106.68(2) . . ? Ge1 Ge3 Ge6 110.66(2) . . ? Ge7 Ge3 Ge6 58.741(18) . . ? Ge1 Ge3 Ge2 57.131(18) . . ? Ge7 Ge3 Ge2 93.288(19) . . ? Ge6 Ge3 Ge2 57.076(17) . . ? Ge1 Ge3 Ge4 56.734(19) . . ? Ge7 Ge3 Ge4 58.687(17) . . ? Ge6 Ge3 Ge4 104.77(2) . . ? Ge2 Ge3 Ge4 90.109(19) . . ? Ge1 Ge4 Ge8 111.65(2) . . ? Ge1 Ge4 Ge7 106.65(2) . . ? Ge8 Ge4 Ge7 58.563(17) . . ? Ge1 Ge4 Ge3 58.06(2) . . ? Ge8 Ge4 Ge3 104.41(2) . . ? Ge7 Ge4 Ge3 57.325(17) . . ? Ge1 Ge4 Ge5 57.452(19) . . ? Ge8 Ge4 Ge5 57.429(17) . . ? Ge7 Ge4 Ge5 92.422(19) . . ? Ge3 Ge4 Ge5 90.217(19) . . ? Ge1 Ge5 Ge8 111.16(2) . . ? Ge1 Ge5 Ge9 107.89(2) . . ? Ge8 Ge5 Ge9 59.154(18) . . ? Ge1 Ge5 Ge4 56.859(18) . . ? Ge8 Ge5 Ge4 57.502(17) . . ? Ge9 Ge5 Ge4 93.987(19) . . ? Ge1 Ge5 Ge2 57.094(19) . . ? Ge8 Ge5 Ge2 104.93(2) . . ? Ge9 Ge5 Ge2 59.014(17) . . ? Ge4 Ge5 Ge2 89.579(19) . . ? Ge9 Ge6 Ge7 74.069(19) . . ? Ge9 Ge6 Ge2 63.104(18) . . ? Ge7 Ge6 Ge2 98.89(2) . . ? Ge9 Ge6 Ge3 100.23(2) . . ? Ge7 Ge6 Ge3 60.156(18) . . ? Ge2 Ge6 Ge3 64.365(19) . . ? Hg1 Ge7 Ge8 126.58(2) . . ? Hg1 Ge7 Ge6 126.86(2) . . ? Ge8 Ge7 Ge6 106.05(2) . . ? Hg1 Ge7 Ge3 91.045(18) . . ? Ge8 Ge7 Ge3 110.62(2) . . ? Ge6 Ge7 Ge3 61.103(19) . . ? Hg1 Ge7 Ge4 91.897(18) . . ? Ge8 Ge7 Ge4 59.725(18) . . ? Ge6 Ge7 Ge4 110.69(2) . . ? Ge3 Ge7 Ge4 63.988(18) . . ? Ge7 Ge8 Ge5 99.15(2) . . ? Ge7 Ge8 Ge9 73.524(19) . . ? Ge5 Ge8 Ge9 61.736(18) . . ? Ge7 Ge8 Ge4 61.712(18) . . ? Ge5 Ge8 Ge4 65.069(19) . . ? Ge9 Ge8 Ge4 100.42(2) . . ? Ge6 Ge9 Hg1 113.43(2) . 2_645 ? Ge6 Ge9 Ge8 105.53(2) . . ? Hg1 Ge9 Ge8 133.30(2) 2_645 . ? Ge6 Ge9 Ge5 109.14(2) . . ? Hg1 Ge9 Ge5 83.864(17) 2_645 . ? Ge8 Ge9 Ge5 59.109(18) . . ? Ge6 Ge9 Ge2 59.039(19) . . ? Hg1 Ge9 Ge2 73.543(16) 2_645 . ? Ge8 Ge9 Ge2 108.03(2) . . ? Ge5 Ge9 Ge2 63.058(18) . . ? O14 K1 O11 133.23(11) . . ? O14 K1 O16 96.87(11) . . ? O11 K1 O16 123.03(11) . . ? O14 K1 O15 124.91(11) . . ? O11 K1 O15 97.11(11) . . ? O16 K1 O15 61.80(12) . . ? O14 K1 O13 60.34(9) . . ? O11 K1 O13 100.81(10) . . ? O16 K1 O13 130.97(10) . . ? O15 K1 O13 94.63(10) . . ? O14 K1 O12 96.25(11) . . ? O11 K1 O12 59.28(11) . . ? O16 K1 O12 96.28(11) . . ? O15 K1 O12 133.63(11) . . ? O13 K1 O12 126.81(11) . . ? O14 K1 N11 121.46(11) . . ? O11 K1 N11 60.56(11) . . ? O16 K1 N11 120.55(12) . . ? O15 K1 N11 59.11(11) . . ? O13 K1 N11 61.13(10) . . ? O12 K1 N11 119.60(11) . . ? O14 K1 N12 58.80(11) . . ? O11 K1 N12 118.29(11) . . ? O16 K1 N12 60.37(12) . . ? O15 K1 N12 121.90(12) . . ? O13 K1 N12 119.08(11) . . ? O12 K1 N12 59.21(11) . . ? N11 K1 N12 178.75(11) . . ? O14 K1 C109 42.33(11) . . ? O11 K1 C109 123.43(11) . . ? O16 K1 C109 111.58(11) . . ? O15 K1 C109 95.86(11) . . ? O13 K1 C109 23.22(10) . . ? O12 K1 C109 130.48(12) . . ? N11 K1 C109 80.71(12) . . ? N12 K1 C109 99.79(12) . . ? C113 N11 C101 109.9(4) . . ? C113 N11 C107 109.7(4) . . ? C101 N11 C107 111.1(4) . . ? C113 N11 K1 110.8(3) . . ? C101 N11 K1 108.4(3) . . ? C107 N11 K1 107.0(3) . . ? C106 N12 C112 110.4(5) . . ? C106 N12 C118 110.7(4) . . ? C112 N12 C118 109.4(4) . . ? C106 N12 K1 109.6(3) . . ? C112 N12 K1 109.5(3) . . ? C118 N12 K1 107.1(3) . . ? C103 O11 C102 111.7(4) . . ? C103 O11 K1 119.0(3) . . ? C102 O11 K1 115.4(3) . . ? C105 O12 C104 112.5(4) . . ? C105 O12 K1 115.0(3) . . ? C104 O12 K1 110.1(3) . . ? C108 O13 C109 111.8(4) . . ? C108 O13 K1 113.2(3) . . ? C109 O13 K1 104.6(2) . . ? C111 O14 C110 113.5(4) . . ? C111 O14 K1 123.8(3) . . ? C110 O14 K1 119.8(3) . . ? C114 O15 C115 112.8(4) . . ? C114 O15 K1 117.8(3) . . ? C115 O15 K1 113.3(3) . . ? C117 O16 C116 111.1(4) . . ? C117 O16 K1 117.0(3) . . ? C116 O16 K1 109.9(3) . . ? N11 C101 C102 113.8(5) . . ? N11 C101 H10A 108.8 . . ? C102 C101 H10A 108.8 . . ? N11 C101 H10B 108.8 . . ? C102 C101 H10B 108.8 . . ? H10A C101 H10B 107.7 . . ? O11 C102 C101 109.6(5) . . ? O11 C102 H10C 109.8 . . ? C101 C102 H10C 109.8 . . ? O11 C102 H10D 109.8 . . ? C101 C102 H10D 109.8 . . ? H10C C102 H10D 108.2 . . ? O11 C103 C104 109.2(5) . . ? O11 C103 H10E 109.8 . . ? C104 C103 H10E 109.8 . . ? O11 C103 H10F 109.8 . . ? C104 C103 H10F 109.8 . . ? H10E C103 H10F 108.3 . . ? O12 C104 C103 109.4(5) . . ? O12 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O12 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 108.1(5) . . ? O12 C105 H10I 110.1 . . ? C106 C105 H10I 110.1 . . ? O12 C105 H10J 110.1 . . ? C106 C105 H10J 110.1 . . ? H10I C105 H10J 108.4 . . ? N12 C106 C105 113.0(5) . . ? N12 C106 H10K 109.0 . . ? C105 C106 H10K 109.0 . . ? N12 C106 H10L 109.0 . . ? C105 C106 H10L 109.0 . . ? H10K C106 H10L 107.8 . . ? N11 C107 C108 113.7(4) . . ? N11 C107 H10M 108.8 . . ? C108 C107 H10M 108.8 . . ? N11 C107 H10N 108.8 . . ? C108 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? O13 C108 C107 109.6(4) . . ? 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(4) . . ? O13 C109 K1 52.2(2) . . ? C110 C109 K1 84.0(3) . . ? O13 C109 H10Q 109.8 . . ? C110 C109 H10Q 109.8 . . ? K1 C109 H10Q 161.2 . . ? O13 C109 H10R 109.8 . . ? C110 C109 H10R 109.8 . . ? K1 C109 H10R 77.3 . . ? H10Q C109 H10R 108.2 . . ? O14 C110 C109 108.1(4) . . ? O14 C110 H11A 110.1 . . ? C109 C110 H11A 110.1 . . ? O14 C110 H11B 110.1 . . ? C109 C110 H11B 110.1 . . ? H11A C110 H11B 108.4 . . ? O14 C111 C112 108.5(4) . . ? O14 C111 H11C 110.0 . . ? C112 C111 H11C 110.0 . . ? O14 C111 H11D 110.0 . . ? C112 C111 H11D 110.0 . . ? H11C C111 H11D 108.4 . . ? N12 C112 C111 113.7(4) . . ? N12 C112 H11E 108.8 . . ? C111 C112 H11E 108.8 . . ? N12 C112 H11F 108.8 . . ? C111 C112 H11F 108.8 . . ? H11E C112 H11F 107.7 . . ? N11 C113 C114 112.7(5) . . ? N11 C113 H11G 109.0 . . ? C114 C113 H11G 109.0 . . ? N11 C113 H11H 109.0 . . ? C114 C113 H11H 109.0 . . ? H11G C113 H11H 107.8 . . ? O15 C114 C113 108.6(4) . . ? O15 C114 H11I 110.0 . . ? C113 C114 H11I 110.0 . . ? O15 C114 H11J 110.0 . . ? C113 C114 H11J 110.0 . . ? H11I C114 H11J 108.3 . . ? O15 C115 C116 108.5(5) . . ? O15 C115 H11K 110.0 . . ? C116 C115 H11K 110.0 . . ? O15 C115 H11L 110.0 . . ? C116 C115 H11L 110.0 . . ? H11K C115 H11L 108.4 . . ? O16 C116 C115 109.6(5) . . ? 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 109.0(4) . . ? 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 113.9(4) . . ? N12 C118 H11Q 108.8 . . ? C117 C118 H11Q 108.8 . . ? N12 C118 H11R 108.8 . . ? C117 C118 H11R 108.8 . . ? H11Q C118 H11R 107.7 . . ? O21 K2 O22 60.26(12) . . ? O21 K2 O23 97.93(13) . . ? O22 K2 O23 128.19(11) . . ? O21 K2 O25 92.74(15) . . ? O22 K2 O25 123.54(12) . . ? O23 K2 O25 102.16(12) . . ? O21 K2 O24 135.00(15) . . ? O22 K2 O24 100.02(11) . . ? O23 K2 O24 61.02(11) . . ? O25 K2 O24 128.77(14) . . ? O21 K2 O26 119.67(16) . . ? O22 K2 O26 89.99(13) . . ? O23 K2 O26 137.44(13) . . ? O25 K2 O26 59.89(13) . . ? O24 K2 O26 98.55(13) . . ? O21 K2 N21 59.07(13) . . ? O22 K2 N21 119.31(12) . . ? O23 K2 N21 60.85(11) . . ? O25 K2 N21 61.18(12) . . ? O24 K2 N21 121.64(12) . . ? O26 K2 N21 120.89(13) . . ? O21 K2 N22 119.91(14) . . ? O22 K2 N22 59.67(13) . . ? O23 K2 N22 119.87(12) . . ? O25 K2 N22 119.01(13) . . ? O24 K2 N22 59.15(12) . . ? O26 K2 N22 59.22(14) . . ? N21 K2 N22 178.96(13) . . ? O21 K2 C204 41.70(14) . . ? O22 K2 C204 22.48(12) . . ? O23 K2 C204 130.64(14) . . ? O25 K2 C204 105.90(14) . . ? O24 K2 C204 121.78(13) . . ? O26 K2 C204 91.91(16) . . ? N21 K2 C204 99.60(14) . . ? N22 K2 C204 79.36(14) . . ? C213 N21 C201 110.1(5) . . ? C213 N21 C207 110.6(5) . . ? C201 N21 C207 110.1(5) . . ? C213 N21 K2 107.6(3) . . ? C201 N21 K2 110.3(3) . . ? C207 N21 K2 108.1(3) . . ? C206 N22 C212 110.9(5) . . ? C206 N22 C218 112.0(5) . . ? C212 N22 C218 108.8(5) . . ? C206 N22 K2 107.2(3) . . ? C212 N22 K2 109.0(3) . . ? C218 N22 K2 109.0(3) . . ? C203 O21 C202 115.9(5) . . ? C203 O21 K2 118.8(4) . . ? C202 O21 K2 119.5(4) . . ? C204 O22 C205 111.3(4) . . ? C204 O22 K2 108.4(3) . . ? C205 O22 K2 118.7(3) . . ? C209 O23 C208 111.7(4) . . ? C209 O23 K2 112.8(3) . . ? C208 O23 K2 114.3(3) . . ? C210 O24 C211 112.4(4) . . ? C210 O24 K2 113.7(3) . . ? C211 O24 K2 116.8(3) . . ? C215 O25 C214 112.6(5) . . ? C215 O25 K2 112.8(4) . . ? C214 O25 K2 114.8(4) . . ? C216 O26 C217 113.2(6) . . ? C216 O26 K2 114.5(4) . . ? C217 O26 K2 112.9(4) . . ? C202 C201 N21 113.4(5) . . ? C202 C201 H20A 108.9 . . ? N21 C201 H20A 108.9 . . ? C202 C201 H20B 108.9 . . ? N21 C201 H20B 108.9 . . ? H20A C201 H20B 107.7 . . ? O21 C202 C201 108.5(6) . . ? O21 C202 H20C 110.0 . . ? C201 C202 H20C 110.0 . . ? O21 C202 H20D 110.0 . . ? C201 C202 H20D 110.0 . . ? H20C C202 H20D 108.4 . . ? O21 C203 C204 111.5(5) . . ? O21 C203 H20E 109.3 . . ? C204 C203 H20E 109.3 . . ? O21 C203 H20F 109.3 . . ? C204 C203 H20F 109.3 . . ? H20E C203 H20F 108.0 . . ? O22 C204 C203 110.5(5) . . ? O22 C204 K2 49.2(2) . . ? C203 C204 K2 82.1(3) . . ? O22 C204 H20G 109.6 . . ? C203 C204 H20G 109.6 . . ? K2 C204 H20G 158.7 . . ? O22 C204 H20H 109.6 . . ? C203 C204 H20H 109.6 . . ? K2 C204 H20H 83.3 . . ? H20G C204 H20H 108.1 . . ? O22 C205 C206 109.5(5) . . ? 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 113.5(5) . . ? N22 C206 H20K 108.9 . . ? C205 C206 H20K 108.9 . . ? N22 C206 H20L 108.9 . . ? C205 C206 H20L 108.9 . . ? H20K C206 H20L 107.7 . . ? N21 C207 C208 114.2(5) . . ? 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 108.7(4) . . ? O23 C208 H20O 110.0 . . ? C207 C208 H20O 110.0 . . ? O23 C208 H20P 110.0 . . ? C207 C208 H20P 110.0 . . ? H20O C208 H20P 108.3 . . ? O23 C209 C210 111.1(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 110.8(5) . . ? O24 C210 H21A 109.5 . . ? C209 C210 H21A 109.5 . . ? O24 C210 H21B 109.5 . . ? C209 C210 H21B 109.5 . . ? H21A C210 H21B 108.1 . . ? O24 C211 C212 108.9(5) . . ? 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 . . ? N22 C212 C211 113.8(5) . . ? N22 C212 H21E 108.8 . . ? C211 C212 H21E 108.8 . . ? N22 C212 H21F 108.8 . . ? C211 C212 H21F 108.8 . . ? H21E C212 H21F 107.7 . . ? N21 C213 C214 112.3(5) . . ? N21 C213 H21G 109.1 . . ? C214 C213 H21G 109.1 . . ? N21 C213 H21H 109.1 . . ? C214 C213 H21H 109.1 . . ? H21G C213 H21H 107.9 . . ? O25 C214 C213 108.6(5) . . ? O25 C214 H21I 110.0 . . ? C213 C214 H21I 110.0 . . ? O25 C214 H21J 110.0 . . ? C213 C214 H21J 110.0 . . ? H21I C214 H21J 108.3 . . ? O25 C215 C216 109.4(6) . . ? O25 C215 H21K 109.8 . . ? C216 C215 H21K 109.8 . . ? O25 C215 H21L 109.8 . . ? C216 C215 H21L 109.8 . . ? H21K C215 H21L 108.2 . . ? O26 C216 C215 109.4(7) . . ? O26 C216 H21M 109.8 . . ? C215 C216 H21M 109.8 . . ? O26 C216 H21N 109.8 . . ? C215 C216 H21N 109.8 . . ? H21M C216 H21N 108.2 . . ? O26 C217 C218 107.2(6) . . ? O26 C217 H21O 110.3 . . ? C218 C217 H21O 110.3 . . ? O26 C217 H21P 110.3 . . ? C218 C217 H21P 110.3 . . ? H21O C217 H21P 108.5 . . ? N22 C218 C217 113.0(5) . . ? N22 C218 H21Q 109.0 . . ? C217 C218 H21Q 109.0 . . ? N22 C218 H21R 109.0 . . ? C217 C218 H21R 109.0 . . ? H21Q C218 H21R 107.8 . . ? C5S N1S C1S 117.4(6) . . ? N1S C1S C2S 122.2(7) . . ? N1S C1S H1S 118.9 . . ? C2S C1S H1S 118.9 . . ? C3S C2S C1S 116.6(7) . . ? C3S C2S H2S 121.7 . . ? C1S C2S H2S 121.7 . . ? C4S C3S C2S 119.5(6) . . ? C4S C3S H3S 120.2 . . ? C2S C3S H3S 120.2 . . ? C5S C4S C3S 118.7(8) . . ? C5S C4S H4S 120.6 . . ? C3S C4S H4S 120.6 . . ? N1S C5S C4S 125.6(8) . . ? N1S C5S H5S 117.2 . . ? C4S C5S H5S 117.2 . . ? C1P N1P C5P 121.2(9) . . ? C2P C1P N1P 119.2(8) . . ? C2P C1P H1P 120.4 . . ? N1P C1P H1P 120.4 . . ? C3P C2P C1P 120.9(7) . . ? C3P C2P H2P 119.5 . . ? C1P C2P H2P 119.5 . . ? C2P C3P C4P 121.2(7) . . ? C2P C3P H3P 119.4 . . ? C4P C3P H3P 119.4 . . ? C5P C4P C3P 119.4(7) . . ? C5P C4P H4P 120.3 . . ? C3P C4P H4P 120.3 . . ? C4P C5P N1P 117.7(7) . . ? C4P C5P H5P 121.1 . . ? N1P C5P H5P 121.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.537 _refine_diff_density_min -1.460 _refine_diff_density_rms 0.106