Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Alexander Rothenberger' _publ_contact_author_address ; Department of Inorganic Chemistry University of Karlsruhe Geb. 30.45 Kaiserstrasse 12 Karlsruhe 76131 GERMANY ; _publ_contact_author_email ROTHENBERGER@CHEMIE.UNI-KARLSRUHE.DE _publ_section_title ; Reactivity of a heterocyclic As-Se compound with metal salts: Syntheses and structures of the first copper complexes and of alkali metal salts containing As-Se anions ; loop_ _publ_author_name 'Alexander Rothenberger' 'Robert Langer' 'Lukasz Ponikiewskia' 'Weifeng Shi' 'Thomas Zell' data_1 _database_code_depnum_ccdc_archive 'CCDC 664248' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C140 H126 As6 Cl8 Cu8 P8 Se8' _chemical_formula_weight 3929.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.8226(7) _cell_length_b 20.8206(8) _cell_length_c 21.6135(9) _cell_angle_alpha 76.153(3) _cell_angle_beta 70.301(3) _cell_angle_gamma 69.693(3) _cell_volume 7406.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 49252 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 27.12 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3848 _exptl_absorpt_coefficient_mu 4.699 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3330 _exptl_absorpt_correction_T_max 0.4533 _exptl_absorpt_process_details 'stoe x-red32' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59429 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.10 _reflns_number_total 30240 _reflns_number_gt 18749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. # SQUEEZE RESULTS (APPEND TO CIF) #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons 1 0.031 0.490 0.107 10.9 0.4 2 0.094 0.676 0.713 7.1 0.3 3 0.198 -0.003 0.425 34.0 9.4 4 0.349 0.125 0.296 8.0 0.4 5 0.651 0.875 0.704 8.0 0.0 6 0.802 0.003 0.575 33.9 8.7 7 0.906 0.324 0.287 7.1 0.2 8 0.969 0.510 0.893 10.9 0.3 #_platon_squeeze_details Platon reports a 122.2 Ang^3 large solvent accesible void and unallocated electron density Electron Count / Cell = 20 No further reliable assigment to any particular solvent molecule can be made. ; _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^)+(0.0775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30240 _refine_ls_number_parameters 1255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Cu1 Cu 0.45204(6) 0.35128(6) 0.43707(5) 0.0361(2) Uani 1 1 d . . . Cu2 Cu 0.48773(6) 0.40270(6) 0.52405(6) 0.0371(2) Uani 1 1 d . . . Cu3 Cu 0.34057(6) 0.55033(5) 0.46206(5) 0.0327(2) Uani 1 1 d . . . Cu4 Cu 0.39870(6) 0.44574(5) 0.32616(5) 0.0329(2) Uani 1 1 d . A . Cu5 Cu 0.22716(6) 0.03459(6) -0.09042(5) 0.0345(2) Uani 1 1 d . . . Cu6 Cu 0.11909(6) -0.03752(6) -0.04151(5) 0.0337(2) Uani 1 1 d . . . Cu7 Cu 0.04821(6) 0.07143(5) 0.08833(5) 0.0303(2) Uani 1 1 d . . . Cu8 Cu 0.14751(6) 0.17834(5) -0.04838(5) 0.0304(2) Uani 1 1 d . . . As1 As 0.30376(5) 0.36943(5) 0.60529(4) 0.0357(2) Uani 1 1 d . . . As2 As 0.27925(5) 0.45629(5) 0.50757(4) 0.03154(19) Uani 1 1 d . . . As3 As 0.56880(5) 0.50076(5) 0.41585(4) 0.03204(19) Uani 1 1 d . . . As4 As 0.18837(5) 0.02285(4) 0.07653(4) 0.02852(18) Uani 1 1 d . . . As5 As 0.25955(5) -0.09929(4) 0.05793(4) 0.03159(18) Uani 1 1 d . . . As6 As -0.03278(5) 0.07837(5) -0.05928(4) 0.03109(18) Uani 1 1 d . . . Se1 Se 0.43573(5) 0.30865(5) 0.55580(4) 0.03578(19) Uani 1 1 d . . . Se2 Se 0.31825(5) 0.38748(4) 0.42248(4) 0.03246(18) Uani 1 1 d . . . Se3 Se 0.46287(5) 0.47525(4) 0.39832(4) 0.03202(18) Uani 1 1 d . . . Se4 Se 0.62724(5) 0.39341(5) 0.46987(4) 0.03349(19) Uani 1 1 d . . . Se5 Se 0.07302(4) 0.09575(4) -0.03355(4) 0.02970(17) Uani 1 1 d . . . Se6 Se 0.25597(5) -0.09015(4) -0.05255(4) 0.03209(18) Uani 1 1 d . . . Se7 Se 0.04639(5) -0.00645(5) -0.12780(4) 0.03231(18) Uani 1 1 d . . . Se8 Se 0.25815(4) 0.08444(4) -0.01593(4) 0.02875(17) Uani 1 1 d . . . P1 P 0.55062(13) 0.28103(12) 0.37220(12) 0.0345(5) Uani 1 1 d . . . P2 P 0.49594(12) 0.37725(12) 0.25502(11) 0.0327(5) Uani 1 1 d . . . P3 P 0.32305(12) 0.54735(12) 0.28598(11) 0.0318(5) Uani 1 1 d . . . P4 P 0.25806(12) 0.62706(12) 0.40723(11) 0.0322(5) Uani 1 1 d . . . P5 P 0.25035(12) 0.07457(12) -0.19725(10) 0.0307(4) Uani 1 1 d . . . P6 P 0.18726(12) 0.21970(11) -0.15631(10) 0.0308(5) Uani 1 1 d . . . P7 P 0.00686(12) 0.16293(11) 0.14237(10) 0.0298(4) Uani 1 1 d . . . P8 P 0.09574(12) 0.25290(11) 0.02644(11) 0.0317(5) Uani 1 1 d . . . C1 C 0.5283(4) 0.2055(3) 0.3618(4) 0.041(2) Uani 1 1 d G . . C2 C 0.4514(3) 0.2021(3) 0.3899(4) 0.058(3) Uani 1 1 d G . . H2 H 0.4126 0.2377 0.4138 0.070 Uiso 1 1 calc R . . C3 C 0.4311(3) 0.1465(4) 0.3830(5) 0.081(5) Uani 1 1 d G . . H3 H 0.3785 0.1442 0.4022 0.097 Uiso 1 1 calc R . . C4 C 0.4878(4) 0.0945(3) 0.3480(5) 0.061(3) Uani 1 1 d G . . H4 H 0.4740 0.0565 0.3433 0.074 Uiso 1 1 calc R . . C5 C 0.5648(4) 0.0980(3) 0.3199(4) 0.068(4) Uani 1 1 d G . . H5 H 0.6035 0.0624 0.2959 0.082 Uiso 1 1 calc R . . C6 C 0.5851(3) 0.1535(3) 0.3268(4) 0.072(4) Uani 1 1 d G . . H6 H 0.6377 0.1559 0.3076 0.086 Uiso 1 1 calc R . . C7 C 0.6455(2) 0.2426(3) 0.3925(3) 0.040(2) Uani 1 1 d G . . C8 C 0.6417(3) 0.2155(3) 0.4585(3) 0.046(2) Uani 1 1 d G . . H8 H 0.5922 0.2155 0.4899 0.056 Uiso 1 1 calc R . . C9 C 0.7104(3) 0.1885(4) 0.4786(2) 0.053(3) Uani 1 1 d G . . H9 H 0.7078 0.1701 0.5237 0.063 Uiso 1 1 calc R . . C10 C 0.7828(3) 0.1886(4) 0.4327(3) 0.048(2) Uani 1 1 d G . . H10 H 0.8298 0.1701 0.4464 0.057 Uiso 1 1 calc R . . C11 C 0.7866(2) 0.2156(3) 0.3666(3) 0.045(2) Uani 1 1 d G . . H11 H 0.8361 0.2157 0.3353 0.053 Uiso 1 1 calc R . . C12 C 0.7180(3) 0.2426(3) 0.3466(2) 0.041(2) Uani 1 1 d G . . H12 H 0.7205 0.2611 0.3014 0.049 Uiso 1 1 calc R . . C13 C 0.4705(4) 0.3148(3) 0.2267(3) 0.037(2) Uani 1 1 d G A . C14 C 0.3908(3) 0.3235(4) 0.2375(5) 0.075(4) Uani 1 1 d G . . H14 H 0.3522 0.3616 0.2579 0.090 Uiso 1 1 calc R A . C15 C 0.3675(4) 0.2764(6) 0.2185(6) 0.129(8) Uani 1 1 d G A . H15 H 0.3131 0.2823 0.2259 0.155 Uiso 1 1 calc R . . C16 C 0.4240(6) 0.2207(5) 0.1887(5) 0.095(5) Uani 1 1 d G . . H16 H 0.4081 0.1885 0.1758 0.114 Uiso 1 1 calc R A . C17 C 0.5037(5) 0.2120(4) 0.1779(5) 0.074(4) Uani 1 1 d G A . H17 H 0.5422 0.1739 0.1575 0.089 Uiso 1 1 calc R . . C18 C 0.5269(3) 0.2591(4) 0.1969(4) 0.060(3) Uani 1 1 d G . . H18 H 0.5814 0.2531 0.1895 0.072 Uiso 1 1 calc R A . C19 C 0.5500(7) 0.4221(7) 0.1767(5) 0.036(2) Uiso 0.50 1 d PG A 1 C20 C 0.6012(7) 0.4560(7) 0.1783(5) 0.021(3) Uiso 0.50 1 d PG A 1 H20 H 0.6115 0.4541 0.2189 0.026 Uiso 0.50 1 calc PR A 1 C21 C 0.6372(6) 0.4925(6) 0.1205(6) 0.033(4) Uiso 0.50 1 d PG A 1 H21 H 0.6722 0.5157 0.1216 0.039 Uiso 0.50 1 calc PR A 1 C22 C 0.6221(7) 0.4952(6) 0.0612(5) 0.031(3) Uiso 0.50 1 d PG A 1 H22 H 0.6467 0.5202 0.0217 0.037 Uiso 0.50 1 calc PR A 1 C23 C 0.5709(8) 0.4614(7) 0.0596(5) 0.053(4) Uiso 0.50 1 d PG A 1 H23 H 0.5605 0.4632 0.0190 0.064 Uiso 0.50 1 calc PR A 1 C24 C 0.5348(7) 0.4248(7) 0.1174(6) 0.047(3) Uiso 0.50 1 d PG A 1 H24 H 0.4998 0.4017 0.1163 0.056 Uiso 0.50 1 calc PR A 1 C19' C 0.5371(9) 0.4249(7) 0.1778(6) 0.036(2) Uiso 0.50 1 d PG A 2 C20' C 0.6047(9) 0.4437(9) 0.1674(7) 0.050(6) Uiso 0.50 1 d PG A 2 H20' H 0.6341 0.4264 0.1990 0.060 Uiso 0.50 1 calc PR A 2 C21' C 0.6291(8) 0.4879(9) 0.1108(8) 0.052(6) Uiso 0.50 1 d PG A 2 H21' H 0.6753 0.5008 0.1037 0.062 Uiso 0.50 1 calc PR A 2 C22' C 0.5860(9) 0.5133(8) 0.0645(7) 0.069(7) Uiso 0.50 1 d PG A 2 H22' H 0.6027 0.5435 0.0258 0.082 Uiso 0.50 1 calc PR A 2 C23' C 0.5185(8) 0.4945(8) 0.0749(6) 0.053(4) Uiso 0.50 1 d PG A 2 H23' H 0.4890 0.5118 0.0433 0.064 Uiso 0.50 1 calc PR A 2 C24' C 0.4940(7) 0.4503(7) 0.1316(7) 0.047(3) Uiso 0.50 1 d PG A 2 H24' H 0.4479 0.4374 0.1387 0.056 Uiso 0.50 1 calc PR A 2 C25 C 0.5800(5) 0.3259(4) 0.2874(4) 0.036(2) Uani 1 1 d . A . H25A H 0.6100 0.3567 0.2872 0.043 Uiso 1 1 calc R . . H25B H 0.6154 0.2912 0.2576 0.043 Uiso 1 1 calc R . . C26 C 0.2753(3) 0.5288(3) 0.2330(2) 0.0344(19) Uani 1 1 d G A . C27 C 0.2978(3) 0.5445(3) 0.1642(3) 0.046(2) Uani 1 1 d G . . H27 H 0.3373 0.5674 0.1431 0.055 Uiso 1 1 calc R A . C28 C 0.2625(4) 0.5266(4) 0.1264(2) 0.052(3) Uani 1 1 d G A . H28 H 0.2779 0.5373 0.0794 0.062 Uiso 1 1 calc R . . C29 C 0.2047(4) 0.4930(4) 0.1573(3) 0.049(2) Uani 1 1 d G . . H29 H 0.1806 0.4808 0.1314 0.058 Uiso 1 1 calc R A . C30 C 0.1822(3) 0.4774(3) 0.2260(3) 0.048(2) Uani 1 1 d G A . H30 H 0.1427 0.4544 0.2471 0.058 Uiso 1 1 calc R . . C31 C 0.2175(3) 0.4952(3) 0.2639(2) 0.038(2) Uani 1 1 d G . . H31 H 0.2021 0.4845 0.3108 0.046 Uiso 1 1 calc R A . C32 C 0.3671(3) 0.6144(2) 0.2334(3) 0.0321(18) Uani 1 1 d G A . C33 C 0.3227(2) 0.6771(3) 0.2071(3) 0.039(2) Uani 1 1 d G . . H33 H 0.2670 0.6871 0.2179 0.047 Uiso 1 1 calc R A . C34 C 0.3597(3) 0.7250(2) 0.1650(3) 0.044(2) Uani 1 1 d G A . H34 H 0.3293 0.7678 0.1469 0.053 Uiso 1 1 calc R . . C35 C 0.4411(3) 0.7104(3) 0.1492(3) 0.045(2) Uani 1 1 d G . . H35 H 0.4664 0.7431 0.1204 0.054 Uiso 1 1 calc R A . C36 C 0.4856(2) 0.6477(3) 0.1755(3) 0.042(2) Uani 1 1 d G A . H36 H 0.5412 0.6377 0.1647 0.051 Uiso 1 1 calc R . . C37 C 0.4485(3) 0.5998(2) 0.2176(3) 0.0360(19) Uani 1 1 d G . . H37 H 0.4789 0.5570 0.2357 0.043 Uiso 1 1 calc R A . C38 C 0.1591(2) 0.6620(3) 0.4627(3) 0.0352(19) Uani 1 1 d G A . C39 C 0.0890(3) 0.6627(3) 0.4540(3) 0.038(2) Uani 1 1 d G . . H39 H 0.0898 0.6460 0.4164 0.045 Uiso 1 1 calc R A . C40 C 0.0176(2) 0.6878(4) 0.5002(3) 0.049(2) Uani 1 1 d G A . H40 H -0.0303 0.6883 0.4942 0.058 Uiso 1 1 calc R . . C41 C 0.0164(2) 0.7122(4) 0.5551(3) 0.049(3) Uani 1 1 d G . . H41 H -0.0323 0.7294 0.5867 0.059 Uiso 1 1 calc R A . C42 C 0.0866(3) 0.7115(4) 0.5639(3) 0.049(3) Uani 1 1 d G A . H42 H 0.0857 0.7282 0.6014 0.058 Uiso 1 1 calc R . . C43 C 0.1579(2) 0.6864(3) 0.5177(3) 0.039(2) Uani 1 1 d G . . H43 H 0.2058 0.6859 0.5237 0.047 Uiso 1 1 calc R A . C44 C 0.2825(2) 0.7077(2) 0.36534(18) 0.0344(19) Uani 1 1 d G A . C45 C 0.2308(2) 0.7620(2) 0.3362(3) 0.049(2) Uani 1 1 d G . . H45 H 0.1824 0.7573 0.3361 0.058 Uiso 1 1 calc R A . C46 C 0.2497(3) 0.8234(2) 0.3073(3) 0.054(3) Uani 1 1 d G A . H46 H 0.2144 0.8605 0.2874 0.064 Uiso 1 1 calc R . . C47 C 0.3205(3) 0.8304(2) 0.3075(3) 0.053(3) Uani 1 1 d G . . H47 H 0.3334 0.8723 0.2878 0.063 Uiso 1 1 calc R A . C48 C 0.3722(3) 0.7760(3) 0.3366(3) 0.045(2) Uani 1 1 d G A . H48 H 0.4206 0.7808 0.3368 0.054 Uiso 1 1 calc R . . C49 C 0.3533(3) 0.7147(2) 0.3655(3) 0.037(2) Uani 1 1 d G . . H49 H 0.3886 0.6776 0.3854 0.044 Uiso 1 1 calc R A . C50 C 0.2348(4) 0.5954(3) 0.3451(4) 0.0321(18) Uani 1 1 d G A . H50A H 0.2008 0.5649 0.3688 0.039 Uiso 1 1 calc R . . H50B H 0.2044 0.6355 0.3199 0.039 Uiso 1 1 calc R . . C51 C 0.2472(3) 0.3076(3) 0.6001(3) 0.040(2) Uani 1 1 d G . . C52 C 0.2823(3) 0.2526(3) 0.5634(3) 0.045(2) Uani 1 1 d G . . H52 H 0.3366 0.2425 0.5397 0.054 Uiso 1 1 calc R . . C53 C 0.2378(4) 0.2123(3) 0.5615(3) 0.057(3) Uani 1 1 d G . . H53 H 0.2618 0.1747 0.5364 0.068 Uiso 1 1 calc R . . C54 C 0.1582(4) 0.2271(4) 0.5961(4) 0.065(3) Uani 1 1 d G . . H54 H 0.1278 0.1996 0.5948 0.078 Uiso 1 1 calc R . . C55 C 0.1232(3) 0.2822(4) 0.6328(4) 0.060(3) Uani 1 1 d G . . H55 H 0.0688 0.2923 0.6565 0.072 Uiso 1 1 calc R . . C56 C 0.1676(3) 0.3224(3) 0.6347(3) 0.053(3) Uani 1 1 d G . . H56 H 0.1437 0.3600 0.6598 0.063 Uiso 1 1 calc R . . C57 C 0.1642(2) 0.4756(3) 0.5410(3) 0.037(2) Uani 1 1 d G . . C58 C 0.1225(3) 0.4427(3) 0.5232(3) 0.043(2) Uani 1 1 d G . . H58 H 0.1490 0.4126 0.4904 0.052 Uiso 1 1 calc R . . C59 C 0.0422(3) 0.4538(4) 0.5536(3) 0.048(2) Uani 1 1 d G . . H59 H 0.0137 0.4313 0.5415 0.057 Uiso 1 1 calc R . . C60 C 0.0035(2) 0.4978(4) 0.6017(3) 0.055(3) Uani 1 1 d G . . H60 H -0.0514 0.5054 0.6224 0.065 Uiso 1 1 calc R . . C61 C 0.0452(3) 0.5307(3) 0.6194(3) 0.052(3) Uani 1 1 d G . . H61 H 0.0187 0.5608 0.6523 0.062 Uiso 1 1 calc R . . C62 C 0.1255(3) 0.5196(3) 0.5890(3) 0.044(2) Uani 1 1 d G . . H62 H 0.1540 0.5421 0.6012 0.053 Uiso 1 1 calc R . . C63 C 0.6442(3) 0.5039(3) 0.3273(2) 0.037(2) Uani 1 1 d G . . C64 C 0.7139(3) 0.4512(3) 0.3099(3) 0.046(2) Uani 1 1 d G . . H64 H 0.7244 0.4100 0.3401 0.055 Uiso 1 1 calc R . . C65 C 0.7683(3) 0.4589(3) 0.2485(3) 0.049(2) Uani 1 1 d G . . H65 H 0.8160 0.4228 0.2367 0.058 Uiso 1 1 calc R . . C66 C 0.7530(3) 0.5192(3) 0.2044(2) 0.053(3) Uani 1 1 d G . . H66 H 0.7901 0.5244 0.1624 0.064 Uiso 1 1 calc R . . C67 C 0.6833(4) 0.5719(3) 0.2217(3) 0.047(2) Uani 1 1 d G . . H67 H 0.6728 0.6132 0.1915 0.057 Uiso 1 1 calc R . . C68 C 0.6289(3) 0.5643(3) 0.2831(3) 0.041(2) Uani 1 1 d G . . H68 H 0.5813 0.6003 0.2949 0.049 Uiso 1 1 calc R . . C69 C 0.3534(2) 0.0747(3) -0.2410(3) 0.0343(19) Uani 1 1 d G . . C70 C 0.4076(3) 0.0532(3) -0.2042(2) 0.043(2) Uani 1 1 d G . . H70 H 0.3915 0.0382 -0.1579 0.051 Uiso 1 1 calc R . . C71 C 0.4853(3) 0.0536(4) -0.2351(3) 0.053(3) Uani 1 1 d G . . H71 H 0.5223 0.0389 -0.2099 0.064 Uiso 1 1 calc R . . C72 C 0.5088(2) 0.0756(4) -0.3029(3) 0.059(3) Uani 1 1 d G . . H72 H 0.5619 0.0759 -0.3240 0.071 Uiso 1 1 calc R . . C73 C 0.4547(3) 0.0972(4) -0.3397(2) 0.051(3) Uani 1 1 d G . . H73 H 0.4707 0.1122 -0.3860 0.062 Uiso 1 1 calc R . . C74 C 0.3770(3) 0.0967(3) -0.3088(3) 0.040(2) Uani 1 1 d G . . H74 H 0.3400 0.1115 -0.3339 0.048 Uiso 1 1 calc R . . C75 C 0.2282(3) 0.0300(3) -0.2495(3) 0.0347(19) Uani 1 1 d G . . C76 C 0.2085(4) 0.0626(2) -0.3081(3) 0.045(2) Uani 1 1 d G . . H76 H 0.2037 0.1104 -0.3217 0.054 Uiso 1 1 calc R . . C77 C 0.1959(4) 0.0252(3) -0.3467(3) 0.051(3) Uani 1 1 d G . . H77 H 0.1825 0.0474 -0.3867 0.062 Uiso 1 1 calc R . . C78 C 0.2030(4) -0.0449(3) -0.3267(3) 0.051(3) Uani 1 1 d G . . H78 H 0.1944 -0.0704 -0.3531 0.061 Uiso 1 1 calc R . . C79 C 0.2227(4) -0.0775(2) -0.2681(3) 0.047(2) Uani 1 1 d G . . H79 H 0.2275 -0.1253 -0.2544 0.056 Uiso 1 1 calc R . . C80 C 0.2352(4) -0.0401(3) -0.2295(2) 0.043(2) Uani 1 1 d G . . H80 H 0.2487 -0.0623 -0.1894 0.051 Uiso 1 1 calc R . . C81 C 0.2853(2) 0.2312(3) -0.1810(2) 0.0310(18) Uani 1 1 d G . . C82 C 0.3170(3) 0.2286(3) -0.13061(18) 0.0342(18) Uani 1 1 d G . . H82 H 0.2874 0.2221 -0.0855 0.041 Uiso 1 1 calc R . . C83 C 0.3922(3) 0.2355(3) -0.1462(2) 0.038(2) Uani 1 1 d G . . H83 H 0.4139 0.2338 -0.1118 0.046 Uiso 1 1 calc R . . C84 C 0.4356(2) 0.2450(3) -0.2122(3) 0.040(2) Uani 1 1 d G . . H84 H 0.4870 0.2498 -0.2228 0.048 Uiso 1 1 calc R . . C85 C 0.4039(3) 0.2476(3) -0.26255(19) 0.040(2) Uani 1 1 d G . . H85 H 0.4336 0.2541 -0.3076 0.048 Uiso 1 1 calc R . . C86 C 0.3288(3) 0.2407(3) -0.2469(2) 0.0358(19) Uani 1 1 d G . . H86 H 0.3071 0.2424 -0.2814 0.043 Uiso 1 1 calc R . . C87 C 0.1254(3) 0.3045(2) -0.1847(3) 0.037(2) Uani 1 1 d G . . C88 C 0.1513(3) 0.3630(3) -0.2026(4) 0.051(3) Uani 1 1 d G . . H88 H 0.2035 0.3591 -0.2036 0.062 Uiso 1 1 calc R . . C89 C 0.1010(3) 0.4272(2) -0.2191(4) 0.064(3) Uani 1 1 d G . . H89 H 0.1187 0.4672 -0.2313 0.077 Uiso 1 1 calc R . . C90 C 0.0247(3) 0.4329(3) -0.2177(4) 0.055(3) Uani 1 1 d G . . H90 H -0.0098 0.4768 -0.2289 0.066 Uiso 1 1 calc R . . C91 C -0.0013(3) 0.3744(3) -0.1998(4) 0.056(3) Uani 1 1 d G . . H91 H -0.0535 0.3783 -0.1988 0.067 Uiso 1 1 calc R . . C92 C 0.0491(3) 0.3102(3) -0.1833(4) 0.051(3) Uani 1 1 d G . . H92 H 0.0313 0.2702 -0.1711 0.061 Uiso 1 1 calc R . . C93 C 0.1924(5) 0.1651(4) -0.2146(4) 0.0308(17) Uani 1 1 d . . . H93A H 0.1383 0.1666 -0.2116 0.037 Uiso 1 1 calc R . . H93B H 0.2165 0.1842 -0.2604 0.037 Uiso 1 1 calc R . . C94 C 0.0003(3) 0.1402(3) 0.2320(2) 0.0340(19) Uani 1 1 d G . . C95 C -0.0266(3) 0.0834(3) 0.2651(3) 0.039(2) Uani 1 1 d G . . H95 H -0.0436 0.0602 0.2424 0.047 Uiso 1 1 calc R . . C96 C -0.0287(4) 0.0606(3) 0.3315(3) 0.047(2) Uani 1 1 d G . . H96 H -0.0471 0.0218 0.3541 0.057 Uiso 1 1 calc R . . C97 C -0.0039(4) 0.0945(3) 0.3647(2) 0.045(2) Uani 1 1 d G . . H97 H -0.0054 0.0789 0.4100 0.054 Uiso 1 1 calc R . . C98 C 0.0229(4) 0.1513(3) 0.3316(3) 0.043(2) Uani 1 1 d G . . H98 H 0.0399 0.1745 0.3543 0.052 Uiso 1 1 calc R . . C99 C 0.0251(4) 0.1741(3) 0.2653(3) 0.045(2) Uani 1 1 d G . . H99 H 0.0434 0.2129 0.2427 0.054 Uiso 1 1 calc R . . C100 C -0.0927(2) 0.2184(3) 0.1398(3) 0.0348(19) Uani 1 1 d G . . C101 C -0.1294(3) 0.2795(3) 0.1676(3) 0.041(2) Uani 1 1 d G . . H101 H -0.1034 0.2941 0.1901 0.050 Uiso 1 1 calc R . . C102 C -0.2042(3) 0.3193(3) 0.1625(3) 0.047(2) Uani 1 1 d G . . H102 H -0.2293 0.3611 0.1815 0.057 Uiso 1 1 calc R . . C103 C -0.2423(2) 0.2980(3) 0.1296(3) 0.044(2) Uani 1 1 d G . . H103 H -0.2934 0.3252 0.1261 0.053 Uiso 1 1 calc R . . C104 C -0.2056(3) 0.2369(3) 0.1018(3) 0.042(2) Uani 1 1 d G . . H104 H -0.2316 0.2224 0.0793 0.050 Uiso 1 1 calc R . . C105 C -0.1308(3) 0.1971(2) 0.1069(3) 0.0371(19) Uani 1 1 d G . . H105 H -0.1057 0.1554 0.0879 0.045 Uiso 1 1 calc R . . C106 C 0.1752(3) 0.2897(3) 0.0187(3) 0.038(2) Uani 1 1 d G . . C107 C 0.2368(3) 0.2496(3) 0.0457(3) 0.044(2) Uani 1 1 d G . . H107 H 0.2344 0.2065 0.0723 0.053 Uiso 1 1 calc R . . C108 C 0.3020(3) 0.2726(4) 0.0337(3) 0.057(3) Uani 1 1 d G . . H108 H 0.3441 0.2451 0.0521 0.069 Uiso 1 1 calc R . . C109 C 0.3055(3) 0.3357(4) -0.0052(4) 0.057(3) Uani 1 1 d G . . H109 H 0.3500 0.3514 -0.0134 0.069 Uiso 1 1 calc R . . C110 C 0.2439(4) 0.3758(3) -0.0322(3) 0.051(3) Uani 1 1 d G . . H110 H 0.2463 0.4189 -0.0588 0.061 Uiso 1 1 calc R . . C111 C 0.1787(3) 0.3528(3) -0.0202(3) 0.047(2) Uani 1 1 d G . . H111 H 0.1366 0.3803 -0.0386 0.056 Uiso 1 1 calc R . . C112 C 0.0102(3) 0.3275(3) 0.0195(3) 0.0356(19) Uani 1 1 d G . . C113 C -0.0081(3) 0.3867(3) 0.0477(3) 0.045(2) Uani 1 1 d G . . H113 H 0.0252 0.3900 0.0708 0.054 Uiso 1 1 calc R . . C114 C -0.0751(4) 0.4411(3) 0.0422(4) 0.055(3) Uani 1 1 d G . . H114 H -0.0876 0.4815 0.0615 0.067 Uiso 1 1 calc R . . C115 C -0.1238(3) 0.4363(3) 0.0084(4) 0.071(4) Uani 1 1 d G . . H115 H -0.1696 0.4734 0.0046 0.085 Uiso 1 1 calc R . . C116 C -0.1055(4) 0.3771(4) -0.0199(4) 0.063(3) Uani 1 1 d G . . H116 H -0.1388 0.3738 -0.0429 0.076 Uiso 1 1 calc R . . C117 C -0.0385(4) 0.3227(3) -0.0143(3) 0.051(2) Uani 1 1 d G . . H117 H -0.0260 0.2823 -0.0336 0.061 Uiso 1 1 calc R . . C118 C 0.0694(4) 0.2208(4) 0.1164(4) 0.0306(17) Uani 1 1 d . . . H11A H 0.1187 0.1961 0.1294 0.037 Uiso 1 1 calc R . . H11B H 0.0418 0.2611 0.1409 0.037 Uiso 1 1 calc R . . C119 C 0.2260(3) 0.0286(3) 0.1495(2) 0.0337(18) Uani 1 1 d G . . C120 C 0.1840(3) 0.0094(3) 0.2138(3) 0.038(2) Uani 1 1 d G . . H120 H 0.1405 -0.0073 0.2212 0.046 Uiso 1 1 calc R . . C121 C 0.2057(4) 0.0146(4) 0.2675(2) 0.056(3) Uani 1 1 d G . . H121 H 0.1770 0.0015 0.3114 0.067 Uiso 1 1 calc R . . C122 C 0.2695(4) 0.0391(4) 0.2567(3) 0.053(3) Uani 1 1 d G . . H122 H 0.2843 0.0427 0.2934 0.064 Uiso 1 1 calc R . . C123 C 0.3115(3) 0.0584(4) 0.1924(3) 0.054(3) Uani 1 1 d G . . H123 H 0.3550 0.0751 0.1850 0.065 Uiso 1 1 calc R . . C124 C 0.2898(3) 0.0531(3) 0.1388(2) 0.041(2) Uani 1 1 d G . . H124 H 0.3185 0.0663 0.0948 0.049 Uiso 1 1 calc R . . C125 C 0.3678(3) -0.0952(3) 0.0420(3) 0.040(2) Uani 1 1 d G . . C126 C 0.3926(3) -0.1038(3) 0.0979(2) 0.043(2) Uani 1 1 d G . . H126 H 0.3578 -0.1105 0.1409 0.051 Uiso 1 1 calc R . . C127 C 0.4683(4) -0.1026(4) 0.0910(3) 0.051(3) Uani 1 1 d G . . H127 H 0.4853 -0.1085 0.1292 0.061 Uiso 1 1 calc R . . C128 C 0.5192(3) -0.0928(4) 0.0281(4) 0.057(3) Uani 1 1 d G . . H128 H 0.5709 -0.0920 0.0233 0.069 Uiso 1 1 calc R . . C129 C 0.4944(3) -0.0843(4) -0.0279(3) 0.052(3) Uani 1 1 d G . . H129 H 0.5291 -0.0776 -0.0709 0.063 Uiso 1 1 calc R . . C130 C 0.4187(3) -0.0854(4) -0.0209(2) 0.043(2) Uani 1 1 d G . . H130 H 0.4017 -0.0796 -0.0592 0.052 Uiso 1 1 calc R . . C131 C -0.0642(4) 0.1604(3) -0.1222(3) 0.038(2) Uani 1 1 d G . . C132 C -0.1214(4) 0.2181(3) -0.0964(3) 0.047(2) Uani 1 1 d G . . H132 H -0.1431 0.2172 -0.0498 0.056 Uiso 1 1 calc R . . C133 C -0.1466(4) 0.2773(3) -0.1389(4) 0.062(3) Uani 1 1 d G . . H133 H -0.1857 0.3167 -0.1213 0.074 Uiso 1 1 calc R . . C134 C -0.1147(5) 0.2787(3) -0.2071(4) 0.071(4) Uani 1 1 d G . . H134 H -0.1320 0.3191 -0.2362 0.085 Uiso 1 1 calc R . . C135 C -0.0576(5) 0.2209(4) -0.2329(2) 0.073(4) Uani 1 1 d G . . H135 H -0.0358 0.2219 -0.2796 0.088 Uiso 1 1 calc R . . C136 C -0.0323(4) 0.1618(3) -0.1905(3) 0.051(3) Uani 1 1 d G . . H136 H 0.0067 0.1223 -0.2081 0.061 Uiso 1 1 calc R . . C137 C 0.2324(9) 0.2682(7) 0.3955(7) 0.078(4) Uiso 1 1 d . . . H13A H 0.2313 0.2766 0.4391 0.093 Uiso 1 1 calc R . . H13B H 0.2866 0.2636 0.3659 0.093 Uiso 1 1 calc R . . Cl1 Cl 0.2098(2) 0.1905(2) 0.40595(19) 0.0827(10) Uiso 1 1 d . . . Cl2 Cl 0.1678(2) 0.3384(2) 0.36253(18) 0.0765(9) Uiso 1 1 d . . . C138 C 0.5950(9) 0.2697(9) 0.0096(9) 0.092(5) Uiso 1 1 d . . . H13C H 0.5990 0.2389 0.0519 0.111 Uiso 1 1 calc R . . H13D H 0.6080 0.2400 -0.0246 0.111 Uiso 1 1 calc R . . Cl3 Cl 0.6628(3) 0.3133(3) -0.0127(3) 0.1177(15) Uiso 1 1 d . . . Cl4 Cl 0.4978(3) 0.3223(2) 0.0198(2) 0.0998(12) Uiso 1 1 d . . . C139 C 0.1671(10) 0.3212(9) 0.1917(9) 0.099(5) Uiso 1 1 d . . . H13E H 0.1847 0.3280 0.1426 0.119 Uiso 1 1 calc R . . H13F H 0.1944 0.3444 0.2074 0.119 Uiso 1 1 calc R . . Cl5 Cl 0.0644(3) 0.3612(3) 0.2180(3) 0.1228(16) Uiso 1 1 d . . . Cl6 Cl 0.1954(3) 0.2322(2) 0.2204(2) 0.0994(12) Uiso 1 1 d . . . C140 C 0.6083(13) 0.0372(11) 0.4753(11) 0.128(7) Uiso 1 1 d . . . H14A H 0.6375 0.0621 0.4353 0.153 Uiso 1 1 calc R . . H14B H 0.5536 0.0676 0.4892 0.153 Uiso 1 1 calc R . . Cl7 Cl 0.6064(4) -0.0388(4) 0.4552(3) 0.143(2) Uiso 1 1 d . . . Cl8 Cl 0.6512(4) 0.0210(3) 0.5365(3) 0.1396(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0296(5) 0.0348(6) 0.0355(5) -0.0042(5) -0.0053(4) -0.0035(5) Cu2 0.0309(5) 0.0323(6) 0.0438(6) -0.0062(5) -0.0071(5) -0.0068(5) Cu3 0.0279(5) 0.0298(6) 0.0362(5) -0.0017(4) -0.0099(4) -0.0044(4) Cu4 0.0299(5) 0.0293(6) 0.0305(5) -0.0004(4) -0.0057(4) -0.0031(4) Cu5 0.0366(5) 0.0320(6) 0.0331(5) 0.0008(4) -0.0089(4) -0.0123(5) Cu6 0.0247(5) 0.0359(6) 0.0382(5) -0.0004(5) -0.0089(4) -0.0092(4) Cu7 0.0249(4) 0.0294(5) 0.0343(5) -0.0020(4) -0.0077(4) -0.0075(4) Cu8 0.0265(5) 0.0261(5) 0.0319(5) -0.0001(4) -0.0044(4) -0.0057(4) As1 0.0326(4) 0.0357(5) 0.0318(4) 0.0003(4) -0.0054(4) -0.0082(4) As2 0.0265(4) 0.0292(5) 0.0323(4) -0.0006(4) -0.0047(3) -0.0061(4) As3 0.0273(4) 0.0296(5) 0.0341(4) -0.0036(4) -0.0068(3) -0.0043(4) As4 0.0235(4) 0.0266(4) 0.0326(4) 0.0010(3) -0.0085(3) -0.0065(3) As5 0.0281(4) 0.0256(4) 0.0390(4) 0.0025(4) -0.0124(4) -0.0071(3) As6 0.0257(4) 0.0309(5) 0.0346(4) 0.0012(4) -0.0089(3) -0.0091(4) Se1 0.0334(4) 0.0304(5) 0.0356(4) 0.0027(4) -0.0070(4) -0.0071(4) Se2 0.0291(4) 0.0305(5) 0.0318(4) -0.0009(3) -0.0049(3) -0.0072(4) Se3 0.0268(4) 0.0306(5) 0.0350(4) -0.0033(4) -0.0077(3) -0.0056(3) Se4 0.0293(4) 0.0300(5) 0.0359(4) -0.0039(4) -0.0096(3) -0.0022(3) Se5 0.0254(4) 0.0286(4) 0.0334(4) 0.0011(3) -0.0092(3) -0.0084(3) Se6 0.0268(4) 0.0273(4) 0.0401(4) -0.0026(4) -0.0111(3) -0.0050(3) Se7 0.0271(4) 0.0351(5) 0.0335(4) -0.0020(4) -0.0071(3) -0.0107(4) Se8 0.0229(3) 0.0253(4) 0.0345(4) 0.0002(3) -0.0072(3) -0.0065(3) P1 0.0279(10) 0.0275(11) 0.0401(12) -0.0022(10) -0.0054(9) -0.0041(9) P2 0.0278(10) 0.0287(11) 0.0347(11) -0.0029(9) -0.0033(9) -0.0062(9) P3 0.0292(10) 0.0297(12) 0.0307(10) 0.0003(9) -0.0065(9) -0.0063(9) P4 0.0257(9) 0.0280(11) 0.0379(11) -0.0032(9) -0.0085(9) -0.0032(9) P5 0.0273(10) 0.0302(11) 0.0300(10) -0.0029(9) -0.0048(8) -0.0069(9) P6 0.0273(10) 0.0276(11) 0.0306(10) 0.0033(9) -0.0069(9) -0.0058(9) P7 0.0256(9) 0.0291(11) 0.0308(10) -0.0028(9) -0.0046(8) -0.0071(9) P8 0.0279(10) 0.0265(11) 0.0348(11) -0.0007(9) -0.0048(9) -0.0071(9) C1 0.044(5) 0.028(5) 0.041(5) 0.002(4) -0.008(4) -0.008(4) C2 0.034(5) 0.035(6) 0.090(8) -0.012(6) 0.000(5) -0.006(4) C3 0.041(6) 0.053(7) 0.138(13) -0.027(8) 0.003(7) -0.019(6) C4 0.058(6) 0.039(6) 0.088(8) -0.007(6) -0.018(6) -0.020(5) C5 0.066(7) 0.042(6) 0.086(9) -0.018(6) -0.005(7) -0.012(6) C6 0.057(7) 0.044(6) 0.110(10) -0.036(7) 0.012(7) -0.026(6) C7 0.035(4) 0.025(5) 0.052(5) -0.005(4) -0.010(4) -0.002(4) C8 0.030(4) 0.042(6) 0.052(6) -0.009(5) -0.006(4) 0.004(4) C9 0.045(5) 0.052(7) 0.056(6) -0.012(5) -0.020(5) 0.000(5) C10 0.033(4) 0.046(6) 0.062(6) -0.017(5) -0.015(5) 0.000(4) C11 0.027(4) 0.044(6) 0.058(6) -0.012(5) -0.005(4) -0.007(4) C12 0.034(4) 0.033(5) 0.055(6) -0.011(4) -0.009(4) -0.008(4) C13 0.035(4) 0.036(5) 0.040(5) -0.002(4) -0.009(4) -0.014(4) C14 0.051(6) 0.084(10) 0.104(10) -0.042(8) -0.017(7) -0.023(7) C15 0.083(11) 0.169(19) 0.175(19) -0.107(16) 0.012(12) -0.075(12) C16 0.125(13) 0.100(12) 0.089(10) -0.030(9) -0.014(10) -0.074(11) C17 0.087(9) 0.053(7) 0.091(9) -0.035(7) -0.017(8) -0.021(7) C18 0.056(6) 0.068(8) 0.062(7) -0.028(6) -0.010(6) -0.018(6) C25 0.033(4) 0.029(4) 0.041(5) -0.007(4) 0.001(4) -0.013(4) C26 0.032(4) 0.024(4) 0.041(5) -0.003(4) -0.011(4) 0.000(4) C27 0.057(6) 0.042(6) 0.035(5) 0.000(4) -0.011(4) -0.014(5) C28 0.067(7) 0.053(7) 0.034(5) -0.003(5) -0.021(5) -0.011(6) C29 0.050(6) 0.054(7) 0.048(6) -0.008(5) -0.027(5) -0.010(5) C30 0.044(5) 0.051(6) 0.053(6) -0.005(5) -0.015(5) -0.016(5) C31 0.038(4) 0.039(5) 0.039(5) -0.002(4) -0.013(4) -0.010(4) C32 0.033(4) 0.028(5) 0.036(4) 0.000(4) -0.012(4) -0.010(4) C33 0.032(4) 0.030(5) 0.047(5) 0.010(4) -0.016(4) -0.004(4) C34 0.044(5) 0.042(6) 0.046(5) 0.003(4) -0.011(4) -0.020(5) C35 0.047(5) 0.043(6) 0.041(5) -0.001(4) -0.001(4) -0.022(5) C36 0.030(4) 0.035(5) 0.049(5) 0.001(4) -0.004(4) -0.006(4) C37 0.030(4) 0.029(5) 0.039(5) -0.003(4) -0.004(4) -0.004(4) C38 0.028(4) 0.032(5) 0.042(5) -0.012(4) -0.002(4) -0.009(4) C39 0.025(4) 0.044(6) 0.043(5) -0.003(4) -0.013(4) -0.008(4) C40 0.031(4) 0.047(6) 0.068(7) -0.016(5) -0.014(5) -0.006(4) C41 0.032(4) 0.050(6) 0.059(6) -0.022(5) -0.003(4) -0.006(4) C42 0.033(5) 0.058(7) 0.058(6) -0.025(5) -0.007(4) -0.011(5) C43 0.033(4) 0.043(5) 0.039(5) -0.013(4) -0.003(4) -0.010(4) C44 0.029(4) 0.030(5) 0.042(5) -0.009(4) -0.007(4) -0.005(4) C45 0.046(5) 0.036(6) 0.063(6) 0.005(5) -0.018(5) -0.016(5) C46 0.056(6) 0.032(6) 0.070(7) 0.005(5) -0.029(6) -0.006(5) C47 0.059(6) 0.037(6) 0.057(6) -0.009(5) -0.002(5) -0.019(5) C48 0.034(4) 0.037(5) 0.048(5) 0.000(4) 0.004(4) -0.011(4) C49 0.033(4) 0.044(5) 0.029(4) -0.004(4) -0.002(4) -0.012(4) C50 0.032(4) 0.029(5) 0.035(4) 0.000(4) -0.014(4) -0.006(4) C51 0.039(5) 0.040(5) 0.034(4) 0.006(4) -0.007(4) -0.013(4) C52 0.050(5) 0.043(6) 0.041(5) 0.011(4) -0.018(4) -0.019(5) C53 0.071(7) 0.045(6) 0.059(6) 0.013(5) -0.028(6) -0.027(6) C54 0.081(8) 0.062(8) 0.065(7) 0.031(6) -0.041(7) -0.044(7) C55 0.042(5) 0.062(8) 0.067(7) 0.019(6) -0.021(5) -0.017(6) C56 0.051(6) 0.051(7) 0.050(6) 0.010(5) -0.016(5) -0.018(5) C57 0.037(4) 0.037(5) 0.028(4) 0.004(4) -0.006(4) -0.008(4) C58 0.036(5) 0.048(6) 0.041(5) -0.001(4) -0.007(4) -0.014(4) C59 0.038(5) 0.055(7) 0.049(6) -0.001(5) -0.011(4) -0.017(5) C60 0.028(4) 0.061(7) 0.066(7) -0.004(6) -0.005(5) -0.013(5) C61 0.047(5) 0.051(6) 0.051(6) -0.010(5) -0.005(5) -0.013(5) C62 0.039(5) 0.050(6) 0.037(5) 0.002(4) -0.008(4) -0.014(5) C63 0.031(4) 0.037(5) 0.044(5) -0.005(4) -0.008(4) -0.014(4) C64 0.035(5) 0.040(6) 0.054(6) -0.008(5) -0.010(4) -0.004(4) C65 0.035(5) 0.047(6) 0.047(5) -0.008(5) -0.002(4) 0.001(4) C66 0.043(5) 0.066(7) 0.043(5) -0.009(5) 0.006(5) -0.023(5) C67 0.047(5) 0.044(6) 0.040(5) 0.002(4) -0.011(4) -0.006(5) C68 0.032(4) 0.046(6) 0.041(5) -0.010(4) -0.005(4) -0.009(4) C69 0.028(4) 0.029(5) 0.042(5) -0.006(4) -0.010(4) -0.002(4) C70 0.031(4) 0.041(6) 0.053(6) -0.011(5) -0.015(4) 0.000(4) C71 0.027(4) 0.056(7) 0.076(7) -0.032(6) -0.009(5) -0.004(4) C72 0.029(5) 0.064(7) 0.080(8) -0.035(6) 0.008(5) -0.016(5) C73 0.045(5) 0.057(7) 0.052(6) -0.014(5) 0.005(5) -0.027(5) C74 0.033(4) 0.043(5) 0.044(5) -0.011(4) -0.004(4) -0.015(4) C75 0.024(4) 0.034(5) 0.038(4) -0.003(4) -0.003(3) -0.007(4) C76 0.048(5) 0.041(6) 0.047(5) -0.007(4) -0.014(5) -0.012(5) C77 0.055(6) 0.064(7) 0.045(5) -0.010(5) -0.022(5) -0.019(6) C78 0.046(5) 0.056(7) 0.050(6) -0.022(5) -0.007(5) -0.012(5) C79 0.042(5) 0.039(6) 0.058(6) -0.014(5) -0.005(5) -0.014(5) C80 0.035(4) 0.042(6) 0.046(5) -0.006(4) -0.006(4) -0.010(4) C81 0.027(4) 0.024(4) 0.034(4) 0.001(3) -0.005(3) -0.004(3) C82 0.033(4) 0.029(5) 0.033(4) 0.000(4) -0.007(4) -0.006(4) C83 0.033(4) 0.036(5) 0.044(5) -0.001(4) -0.011(4) -0.011(4) C84 0.034(4) 0.037(5) 0.042(5) -0.005(4) -0.003(4) -0.008(4) C85 0.030(4) 0.038(5) 0.043(5) -0.006(4) -0.002(4) -0.007(4) C86 0.031(4) 0.037(5) 0.034(4) -0.001(4) -0.005(4) -0.010(4) C87 0.032(4) 0.032(5) 0.038(5) -0.002(4) -0.007(4) -0.003(4) C88 0.030(4) 0.036(6) 0.076(7) 0.008(5) -0.014(5) -0.008(4) C89 0.042(5) 0.037(6) 0.095(9) 0.014(6) -0.020(6) -0.003(5) C90 0.037(5) 0.031(5) 0.080(8) 0.012(5) -0.017(5) 0.000(4) C91 0.030(5) 0.047(6) 0.076(7) 0.006(6) -0.013(5) -0.006(5) C92 0.042(5) 0.039(6) 0.064(6) 0.008(5) -0.013(5) -0.014(5) C93 0.027(4) 0.034(5) 0.029(4) 0.000(3) -0.006(3) -0.010(4) C94 0.023(4) 0.043(5) 0.030(4) -0.006(4) -0.003(3) -0.007(4) C95 0.033(4) 0.045(6) 0.038(5) -0.004(4) -0.010(4) -0.010(4) C96 0.046(5) 0.051(6) 0.037(5) 0.015(4) -0.013(4) -0.018(5) C97 0.038(5) 0.053(6) 0.035(5) -0.005(4) -0.009(4) -0.005(5) C98 0.038(5) 0.052(6) 0.038(5) -0.018(4) -0.006(4) -0.008(4) C99 0.050(5) 0.040(6) 0.040(5) -0.004(4) -0.011(4) -0.010(5) C100 0.034(4) 0.034(5) 0.031(4) 0.002(4) -0.010(4) -0.007(4) C101 0.033(4) 0.044(6) 0.043(5) -0.007(4) -0.006(4) -0.009(4) C102 0.031(4) 0.040(6) 0.059(6) -0.014(5) -0.005(4) 0.001(4) C103 0.027(4) 0.047(6) 0.050(5) -0.011(5) -0.005(4) -0.003(4) C104 0.038(5) 0.041(6) 0.048(5) -0.003(4) -0.016(4) -0.011(4) C105 0.037(4) 0.030(5) 0.042(5) -0.006(4) -0.015(4) -0.003(4) C106 0.031(4) 0.042(5) 0.036(4) -0.011(4) 0.005(4) -0.017(4) C107 0.040(5) 0.058(6) 0.037(5) 0.001(4) -0.006(4) -0.025(5) C108 0.041(5) 0.076(8) 0.061(7) -0.007(6) -0.014(5) -0.025(6) C109 0.049(6) 0.065(7) 0.068(7) -0.018(6) 0.001(5) -0.040(6) C110 0.052(6) 0.038(6) 0.054(6) -0.007(5) 0.006(5) -0.023(5) C111 0.036(5) 0.043(6) 0.053(6) -0.009(5) 0.000(4) -0.011(4) C112 0.030(4) 0.023(4) 0.037(4) 0.003(4) -0.004(4) 0.002(4) C113 0.035(4) 0.037(5) 0.055(6) -0.006(5) -0.007(4) -0.005(4) C114 0.057(6) 0.032(6) 0.058(6) -0.007(5) -0.003(5) -0.001(5) C115 0.054(7) 0.052(8) 0.073(8) -0.004(7) -0.018(6) 0.022(6) C116 0.054(6) 0.060(8) 0.061(7) -0.001(6) -0.031(6) 0.011(6) C117 0.053(6) 0.039(6) 0.053(6) 0.000(5) -0.027(5) 0.003(5) C118 0.019(3) 0.031(5) 0.039(4) -0.004(4) -0.009(3) -0.005(3) C119 0.026(4) 0.025(4) 0.045(5) -0.004(4) -0.012(4) 0.000(3) C120 0.033(4) 0.042(5) 0.035(4) -0.004(4) -0.009(4) -0.005(4) C121 0.058(6) 0.056(7) 0.040(5) -0.011(5) -0.013(5) 0.001(6) C122 0.056(6) 0.049(7) 0.051(6) -0.008(5) -0.033(5) 0.006(5) C123 0.065(7) 0.048(7) 0.066(7) -0.009(5) -0.041(6) -0.013(6) C124 0.041(5) 0.040(6) 0.041(5) -0.003(4) -0.018(4) -0.009(4) C125 0.039(5) 0.022(4) 0.059(6) -0.002(4) -0.022(4) -0.003(4) C126 0.047(5) 0.031(5) 0.053(6) -0.005(4) -0.027(5) -0.002(4) C127 0.046(5) 0.045(6) 0.072(7) -0.021(5) -0.031(5) -0.003(5) C128 0.034(5) 0.046(6) 0.100(9) -0.009(6) -0.031(6) -0.011(5) C129 0.031(5) 0.049(6) 0.077(7) -0.001(6) -0.019(5) -0.013(5) C130 0.035(4) 0.047(6) 0.051(5) -0.011(5) -0.006(4) -0.019(4) C131 0.032(4) 0.027(5) 0.049(5) 0.007(4) -0.019(4) -0.004(4) C132 0.044(5) 0.035(5) 0.057(6) 0.001(5) -0.016(5) -0.007(4) C133 0.045(6) 0.043(7) 0.100(10) 0.012(6) -0.038(6) -0.012(5) C134 0.058(7) 0.074(10) 0.092(10) 0.027(8) -0.056(7) -0.026(7) C135 0.077(9) 0.075(10) 0.065(8) 0.027(7) -0.036(7) -0.029(8) C136 0.053(6) 0.051(7) 0.042(5) 0.008(5) -0.014(5) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P1 2.212(2) . ? Cu1 Se1 2.4565(14) . ? Cu1 Se2 2.4726(14) . ? Cu1 Se3 2.5730(14) . ? Cu1 Cu2 2.7285(16) . ? Cu1 Cu4 2.9356(16) . ? Cu2 Se1 2.3447(13) . ? Cu2 As3 2.3860(14) 2_666 ? Cu2 Se4 2.4468(13) . ? Cu2 Se3 2.8787(15) . ? Cu3 P4 2.232(3) . ? Cu3 Se4 2.4132(14) 2_666 ? Cu3 As2 2.4523(13) . ? Cu3 Se3 2.4568(13) . ? Cu4 P2 2.256(2) . ? Cu4 P3 2.263(3) . ? Cu4 Se2 2.4576(12) . ? Cu4 Se3 2.5520(14) . ? Cu5 P5 2.206(2) . ? Cu5 Se8 2.4213(13) . ? Cu5 Se6 2.4522(14) . ? Cu5 Se5 2.7075(13) . ? Cu5 Cu6 2.7239(14) . ? Cu5 Cu8 3.0495(15) . ? Cu6 Se6 2.3763(13) . ? Cu6 As6 2.4072(12) 2 ? Cu6 Se7 2.5097(14) . ? Cu6 Se5 2.6342(14) . ? Cu7 P7 2.241(2) . ? Cu7 Se7 2.4133(12) 2 ? Cu7 As4 2.4221(12) . ? Cu7 Se5 2.4718(13) . ? Cu8 P6 2.248(2) . ? Cu8 P8 2.250(2) . ? Cu8 Se5 2.4762(12) . ? Cu8 Se8 2.4806(13) . ? As1 C51 1.976(5) . ? As1 Se1 2.3645(12) . ? As1 As2 2.4887(13) . ? As2 C57 1.963(4) . ? As2 Se2 2.3653(12) . ? As3 C63 1.964(4) . ? As3 Se4 2.3407(13) . ? As3 Cu2 2.3861(14) 2_666 ? As3 Se3 2.3960(12) . ? As4 C119 1.977(4) . ? As4 Se8 2.3527(11) . ? As4 As5 2.4870(12) . ? As5 C125 1.977(4) . ? As5 Se6 2.3717(13) . ? As6 C131 1.961(5) . ? As6 Se7 2.3388(12) . ? As6 Se5 2.3978(11) . ? As6 Cu6 2.4071(12) 2 ? Se4 Cu3 2.4131(14) 2_666 ? Se7 Cu7 2.4135(12) 2 ? P1 C1 1.840(5) . ? P1 C7 1.841(5) . ? P1 C25 1.842(9) . ? P2 C19' 1.800(11) . ? P2 C13 1.818(5) . ? P2 C25 1.830(10) . ? P2 C19 1.874(9) . ? P3 C32 1.827(4) . ? P3 C26 1.848(5) . ? P3 C50 1.850(7) . ? P4 C44 1.839(4) . ? P4 C38 1.846(4) . ? P4 C50 1.857(6) . ? P5 C93 1.842(9) . ? P5 C75 1.844(5) . ? P5 C69 1.851(4) . ? P6 C81 1.825(4) . ? P6 C87 1.840(5) . ? P6 C93 1.848(8) . ? P7 C118 1.836(8) . ? P7 C100 1.840(4) . ? P7 C94 1.853(5) . ? P8 C112 1.829(5) . ? P8 C106 1.850(4) . ? P8 C118 1.852(9) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C19' C20' 1.3900 . ? C19' C24' 1.3900 . ? C20' C21' 1.3900 . ? C21' C22' 1.3900 . ? C22' C23' 1.3900 . ? C23' C24' 1.3900 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C57 C58 1.3900 . ? C57 C62 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C75 C76 1.3900 . ? C75 C80 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? C87 C88 1.3900 . ? C87 C92 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? C91 C92 1.3900 . ? C94 C95 1.3900 . ? C94 C99 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C100 C101 1.3900 . ? C100 C105 1.3900 . ? C101 C102 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C106 C107 1.3900 . ? C106 C111 1.3900 . ? C107 C108 1.3900 . ? C108 C109 1.3900 . ? C109 C110 1.3900 . ? C110 C111 1.3900 . ? C112 C113 1.3900 . ? C112 C117 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C115 C116 1.3900 . ? C116 C117 1.3900 . ? C119 C120 1.3900 . ? C119 C124 1.3900 . ? C120 C121 1.3900 . ? C121 C122 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C125 C126 1.3900 . ? C125 C130 1.3900 . ? C126 C127 1.3900 . ? C127 C128 1.3900 . ? C128 C129 1.3900 . ? C129 C130 1.3900 . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C135 C136 1.3900 . ? C137 Cl2 1.725(16) . ? C137 Cl1 1.758(14) . ? C138 Cl3 1.693(16) . ? C138 Cl4 1.747(17) . ? C139 Cl6 1.759(18) . ? C139 Cl5 1.766(18) . ? C140 Cl8 1.68(2) . ? C140 Cl7 1.75(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu1 Se1 113.14(8) . . ? P1 Cu1 Se2 119.81(8) . . ? Se1 Cu1 Se2 105.52(5) . . ? P1 Cu1 Se3 109.05(7) . . ? Se1 Cu1 Se3 116.44(5) . . ? Se2 Cu1 Se3 91.47(5) . . ? P1 Cu1 Cu2 117.28(8) . . ? Se1 Cu1 Cu2 53.46(4) . . ? Se2 Cu1 Cu2 122.72(5) . . ? Se3 Cu1 Cu2 65.70(4) . . ? P1 Cu1 Cu4 93.96(8) . . ? Se1 Cu1 Cu4 152.43(5) . . ? Se2 Cu1 Cu4 53.22(3) . . ? Se3 Cu1 Cu4 54.72(4) . . ? Cu2 Cu1 Cu4 119.12(5) . . ? Se1 Cu2 As3 121.42(5) . 2_666 ? Se1 Cu2 Se4 123.94(5) . . ? As3 Cu2 Se4 108.52(5) 2_666 . ? Se1 Cu2 Cu1 57.32(4) . . ? As3 Cu2 Cu1 137.62(6) 2_666 . ? Se4 Cu2 Cu1 101.21(5) . . ? Se1 Cu2 Se3 109.47(5) . . ? As3 Cu2 Se3 97.93(5) 2_666 . ? Se4 Cu2 Se3 85.51(4) . . ? Cu1 Cu2 Se3 54.55(4) . . ? P4 Cu3 Se4 110.55(7) . 2_666 ? P4 Cu3 As2 102.76(7) . . ? Se4 Cu3 As2 122.87(5) 2_666 . ? P4 Cu3 Se3 118.34(7) . . ? Se4 Cu3 Se3 109.02(5) 2_666 . ? As2 Cu3 Se3 92.98(4) . . ? P2 Cu4 P3 119.57(9) . . ? P2 Cu4 Se2 116.33(7) . . ? P3 Cu4 Se2 110.86(7) . . ? P2 Cu4 Se3 107.10(7) . . ? P3 Cu4 Se3 106.41(7) . . ? Se2 Cu4 Se3 92.32(4) . . ? P2 Cu4 Cu1 89.36(7) . . ? P3 Cu4 Cu1 150.56(7) . . ? Se2 Cu4 Cu1 53.69(4) . . ? Se3 Cu4 Cu1 55.39(4) . . ? P5 Cu5 Se8 120.90(7) . . ? P5 Cu5 Se6 120.61(8) . . ? Se8 Cu5 Se6 106.98(5) . . ? P5 Cu5 Se5 106.63(7) . . ? Se8 Cu5 Se5 87.52(4) . . ? Se6 Cu5 Se5 108.53(4) . . ? P5 Cu5 Cu6 115.79(7) . . ? Se8 Cu5 Cu6 119.94(5) . . ? Se6 Cu5 Cu6 54.35(4) . . ? Se5 Cu5 Cu6 58.02(3) . . ? P5 Cu5 Cu8 93.52(7) . . ? Se8 Cu5 Cu8 52.41(3) . . ? Se6 Cu5 Cu8 145.38(5) . . ? Se5 Cu5 Cu8 50.52(3) . . ? Cu6 Cu5 Cu8 107.82(4) . . ? Se6 Cu6 As6 114.99(5) . 2 ? Se6 Cu6 Se7 128.94(5) . . ? As6 Cu6 Se7 105.53(4) 2 . ? Se6 Cu6 Se5 113.43(5) . . ? As6 Cu6 Se5 100.95(4) 2 . ? Se7 Cu6 Se5 86.51(4) . . ? Se6 Cu6 Cu5 56.99(4) . . ? As6 Cu6 Cu5 143.35(5) 2 . ? Se7 Cu6 Cu5 104.59(5) . . ? Se5 Cu6 Cu5 60.68(4) . . ? P7 Cu7 Se7 110.81(6) . 2 ? P7 Cu7 As4 106.63(7) . . ? Se7 Cu7 As4 125.24(5) 2 . ? P7 Cu7 Se5 116.69(7) . . ? Se7 Cu7 Se5 105.80(5) 2 . ? As4 Cu7 Se5 90.81(4) . . ? P6 Cu8 P8 118.48(9) . . ? P6 Cu8 Se5 110.33(7) . . ? P8 Cu8 Se5 115.22(7) . . ? P6 Cu8 Se8 109.61(7) . . ? P8 Cu8 Se8 108.14(8) . . ? Se5 Cu8 Se8 91.59(4) . . ? P6 Cu8 Cu5 86.57(7) . . ? P8 Cu8 Cu5 153.41(8) . . ? Se5 Cu8 Cu5 57.56(3) . . ? Se8 Cu8 Cu5 50.66(3) . . ? C51 As1 Se1 100.91(18) . . ? C51 As1 As2 98.0(2) . . ? Se1 As1 As2 98.20(4) . . ? C57 As2 Se2 105.21(17) . . ? C57 As2 Cu3 121.14(19) . . ? Se2 As2 Cu3 107.12(4) . . ? C57 As2 As1 93.7(2) . . ? Se2 As2 As1 103.12(4) . . ? Cu3 As2 As1 124.00(5) . . ? C63 As3 Se4 102.65(17) . . ? C63 As3 Cu2 122.10(18) . 2_666 ? Se4 As3 Cu2 118.02(5) . 2_666 ? C63 As3 Se3 103.58(19) . . ? Se4 As3 Se3 100.01(4) . . ? Cu2 As3 Se3 107.48(5) 2_666 . ? C119 As4 Se8 103.03(16) . . ? C119 As4 Cu7 116.82(17) . . ? Se8 As4 Cu7 109.54(5) . . ? C119 As4 As5 100.73(19) . . ? Se8 As4 As5 102.32(4) . . ? Cu7 As4 As5 121.98(4) . . ? C125 As5 Se6 100.59(17) . . ? C125 As5 As4 97.74(19) . . ? Se6 As5 As4 98.77(4) . . ? C131 As6 Se7 103.31(18) . . ? C131 As6 Se5 103.84(19) . . ? Se7 As6 Se5 96.21(4) . . ? C131 As6 Cu6 125.85(18) . 2 ? Se7 As6 Cu6 114.15(5) . 2 ? Se5 As6 Cu6 109.12(5) . 2 ? Cu2 Se1 As1 97.51(5) . . ? Cu2 Se1 Cu1 69.22(4) . . ? As1 Se1 Cu1 102.99(5) . . ? As2 Se2 Cu4 104.79(4) . . ? As2 Se2 Cu1 86.52(4) . . ? Cu4 Se2 Cu1 73.09(4) . . ? As3 Se3 Cu3 106.10(4) . . ? As3 Se3 Cu4 152.61(5) . . ? Cu3 Se3 Cu4 95.76(4) . . ? As3 Se3 Cu1 117.79(5) . . ? Cu3 Se3 Cu1 106.00(4) . . ? Cu4 Se3 Cu1 69.89(4) . . ? As3 Se3 Cu2 70.56(4) . . ? Cu3 Se3 Cu2 86.82(4) . . ? Cu4 Se3 Cu2 128.07(4) . . ? Cu1 Se3 Cu2 59.75(4) . . ? As3 Se4 Cu3 90.69(4) . 2_666 ? As3 Se4 Cu2 79.80(4) . . ? Cu3 Se4 Cu2 103.07(5) 2_666 . ? As6 Se5 Cu7 107.52(4) . . ? As6 Se5 Cu8 144.76(5) . . ? Cu7 Se5 Cu8 94.47(4) . . ? As6 Se5 Cu6 76.08(4) . . ? Cu7 Se5 Cu6 90.76(4) . . ? Cu8 Se5 Cu6 132.02(4) . . ? As6 Se5 Cu5 123.26(4) . . ? Cu7 Se5 Cu5 108.61(4) . . ? Cu8 Se5 Cu5 71.91(4) . . ? Cu6 Se5 Cu5 61.30(3) . . ? As5 Se6 Cu6 100.94(4) . . ? As5 Se6 Cu5 103.14(5) . . ? Cu6 Se6 Cu5 68.67(4) . . ? As6 Se7 Cu7 93.05(4) . 2 ? As6 Se7 Cu6 79.61(4) . . ? Cu7 Se7 Cu6 106.05(5) 2 . ? As4 Se8 Cu5 90.71(4) . . ? As4 Se8 Cu8 100.66(4) . . ? Cu5 Se8 Cu8 76.93(4) . . ? C1 P1 C7 103.1(3) . . ? C1 P1 C25 104.9(4) . . ? C7 P1 C25 102.1(3) . . ? C1 P1 Cu1 114.7(2) . . ? C7 P1 Cu1 119.3(2) . . ? C25 P1 Cu1 111.1(3) . . ? C19' P2 C13 101.8(5) . . ? C19' P2 C25 105.1(5) . . ? C13 P2 C25 104.5(4) . . ? C19' P2 C19 6.6(8) . . ? C13 P2 C19 104.0(5) . . ? C25 P2 C19 98.6(5) . . ? C19' P2 Cu4 113.1(5) . . ? C13 P2 Cu4 117.4(2) . . ? C25 P2 Cu4 113.5(3) . . ? C19 P2 Cu4 116.5(4) . . ? C32 P3 C26 103.4(3) . . ? C32 P3 C50 103.7(2) . . ? C26 P3 C50 99.9(3) . . ? C32 P3 Cu4 120.79(19) . . ? C26 P3 Cu4 108.1(2) . . ? C50 P3 Cu4 118.1(2) . . ? C44 P4 C38 100.4(3) . . ? C44 P4 C50 105.7(3) . . ? C38 P4 C50 102.0(3) . . ? C44 P4 Cu3 116.92(17) . . ? C38 P4 Cu3 112.5(2) . . ? C50 P4 Cu3 117.0(2) . . ? C93 P5 C75 102.8(3) . . ? C93 P5 C69 103.8(3) . . ? C75 P5 C69 103.0(3) . . ? C93 P5 Cu5 113.3(3) . . ? C75 P5 Cu5 116.8(2) . . ? C69 P5 Cu5 115.5(2) . . ? C81 P6 C87 103.8(3) . . ? C81 P6 C93 104.9(3) . . ? C87 P6 C93 102.2(4) . . ? C81 P6 Cu8 113.2(2) . . ? C87 P6 Cu8 116.4(2) . . ? C93 P6 Cu8 114.9(3) . . ? C118 P7 C100 106.0(3) . . ? C118 P7 C94 100.8(3) . . ? C100 P7 C94 104.3(3) . . ? C118 P7 Cu7 117.0(3) . . ? C100 P7 Cu7 113.1(2) . . ? C94 P7 Cu7 114.1(2) . . ? C112 P8 C106 105.2(3) . . ? C112 P8 C118 102.1(3) . . ? C106 P8 C118 101.2(3) . . ? C112 P8 Cu8 120.1(2) . . ? C106 P8 Cu8 105.5(2) . . ? C118 P8 Cu8 120.3(3) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 117.6(3) . . ? C6 C1 P1 122.4(3) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 116.3(3) . . ? C12 C7 P1 123.6(3) . . ? C7 C8 C9 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 P2 117.3(4) . . ? C18 C13 P2 122.7(4) . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 120.6(7) . . ? C24 C19 P2 119.3(7) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ? C20' C19' C24' 120.0 . . ? C20' C19' P2 121.5(8) . . ? C24' C19' P2 118.0(8) . . ? C21' C20' C19' 120.0 . . ? C22' C21' C20' 120.0 . . ? C23' C22' C21' 120.0 . . ? C22' C23' C24' 120.0 . . ? C23' C24' C19' 120.0 . . ? P2 C25 P1 113.1(4) . . ? C27 C26 C31 120.0 . . ? C27 C26 P3 122.2(3) . . ? C31 C26 P3 117.7(3) . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C31 120.0 . . ? C30 C31 C26 120.0 . . ? C33 C32 C37 120.0 . . ? C33 C32 P3 122.4(3) . . ? C37 C32 P3 117.5(3) . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 C32 120.0 . . ? C39 C38 C43 120.0 . . ? C39 C38 P4 124.6(3) . . ? C43 C38 P4 115.4(3) . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C38 120.0 . . ? C45 C44 C49 120.0 . . ? C45 C44 P4 121.5(2) . . ? C49 C44 P4 118.5(2) . . ? C44 C45 C46 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? P3 C50 P4 113.7(4) . . ? C52 C51 C56 120.0 . . ? C52 C51 As1 123.7(3) . . ? C56 C51 As1 116.3(3) . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C55 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C58 C57 C62 120.0 . . ? C58 C57 As2 123.0(3) . . ? C62 C57 As2 116.8(3) . . ? C59 C58 C57 120.0 . . ? C58 C59 C60 120.0 . . ? C61 C60 C59 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C57 120.0 . . ? C64 C63 C68 120.0 . . ? C64 C63 As3 122.5(3) . . ? C68 C63 As3 117.3(3) . . ? C65 C64 C63 120.0 . . ? C66 C65 C64 120.0 . . ? C67 C66 C65 120.0 . . ? C66 C67 C68 120.0 . . ? C67 C68 C63 120.0 . . ? C70 C69 C74 120.0 . . ? C70 C69 P5 118.3(3) . . ? C74 C69 P5 121.7(3) . . ? C69 C70 C71 120.0 . . ? C72 C71 C70 120.0 . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C69 120.0 . . ? C76 C75 C80 120.0 . . ? C76 C75 P5 122.9(3) . . ? C80 C75 P5 117.0(3) . . ? C77 C76 C75 120.0 . . ? C76 C77 C78 120.0 . . ? C79 C78 C77 120.0 . . ? C80 C79 C78 120.0 . . ? C79 C80 C75 120.0 . . ? C82 C81 C86 120.0 . . ? C82 C81 P6 117.3(3) . . ? C86 C81 P6 122.7(3) . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C85 C84 C83 120.0 . . ? C84 C85 C86 120.0 . . ? C85 C86 C81 120.0 . . ? C88 C87 C92 120.0 . . ? C88 C87 P6 121.4(3) . . ? C92 C87 P6 118.4(3) . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C91 C90 C89 120.0 . . ? C92 C91 C90 120.0 . . ? C91 C92 C87 120.0 . . ? P5 C93 P6 112.4(4) . . ? C95 C94 C99 120.0 . . ? C95 C94 P7 116.6(3) . . ? C99 C94 P7 123.3(3) . . ? C96 C95 C94 120.0 . . ? C97 C96 C95 120.0 . . ? C96 C97 C98 120.0 . . ? C99 C98 C97 120.0 . . ? C98 C99 C94 120.0 . . ? C101 C100 C105 120.0 . . ? C101 C100 P7 123.5(3) . . ? C105 C100 P7 116.5(3) . . ? C102 C101 C100 120.0 . . ? C103 C102 C101 120.0 . . ? C104 C103 C102 120.0 . . ? C103 C104 C105 120.0 . . ? C104 C105 C100 120.0 . . ? C107 C106 C111 120.0 . . ? C107 C106 P8 118.9(3) . . ? C111 C106 P8 120.7(3) . . ? C108 C107 C106 120.0 . . ? C109 C108 C107 120.0 . . ? C108 C109 C110 120.0 . . ? C111 C110 C109 120.0 . . ? C110 C111 C106 120.0 . . ? C113 C112 C117 120.0 . . ? C113 C112 P8 122.7(4) . . ? C117 C112 P8 117.3(4) . . ? C114 C113 C112 120.0 . . ? C115 C114 C113 120.0 . . ? C114 C115 C116 120.0 . . ? C117 C116 C115 120.0 . . ? C116 C117 C112 120.0 . . ? P7 C118 P8 115.1(4) . . ? C120 C119 C124 120.0 . . ? C120 C119 As4 117.1(3) . . ? C124 C119 As4 122.8(3) . . ? C119 C120 C121 120.0 . . ? C122 C121 C120 120.0 . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C123 C124 C119 120.0 . . ? C126 C125 C130 120.0 . . ? C126 C125 As5 116.4(3) . . ? C130 C125 As5 123.6(3) . . ? C127 C126 C125 120.0 . . ? C128 C127 C126 120.0 . . ? C127 C128 C129 120.0 . . ? C130 C129 C128 120.0 . . ? C129 C130 C125 120.0 . . ? C132 C131 C136 120.0 . . ? C132 C131 As6 117.7(3) . . ? C136 C131 As6 122.3(3) . . ? C131 C132 C133 120.0 . . ? C134 C133 C132 120.0 . . ? C135 C134 C133 120.0 . . ? C134 C135 C136 120.0 . . ? C135 C136 C131 120.0 . . ? Cl2 C137 Cl1 112.7(8) . . ? Cl3 C138 Cl4 114.5(10) . . ? Cl6 C139 Cl5 113.8(10) . . ? Cl8 C140 Cl7 112.1(13) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 3.566 _refine_diff_density_min -1.922 _refine_diff_density_rms 0.163 data_2 _database_code_depnum_ccdc_archive 'CCDC 664249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H104 As4 Cu4 O3 P4 Se4' _chemical_formula_weight 2443.47 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 24.736(5) _cell_length_b 15.659(3) _cell_length_c 26.355(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.85(3) _cell_angle_gamma 90.00 _cell_volume 9820(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2591 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.14 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4880 _exptl_absorpt_coefficient_mu 3.792 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53681 _diffrn_reflns_av_R_equivalents 0.2432 _diffrn_reflns_av_sigmaI/netI 0.2910 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17285 _reflns_number_gt 6831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Crystals were of poor quality. Delu was applied to restrain the thermal parameters of c73 to c78. # SQUEEZE RESULTS (APPEND TO CIF) #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons 1 0.025 0.024 0.519 8.6 0.8 2 0.475 0.024 0.981 7.8 0.5 3 0.750 0.178 0.250 220.3 67.5 4 0.250 0.150 0.250 22.2 5.1 5 0.250 0.822 0.750 220.3 61.0 6 0.750 0.850 0.750 22.1 5.0 7 0.530 0.971 0.023 6.8 0.9 8 0.970 0.971 0.477 6.1 0.5 #_platon_squeeze_details Electron Count per Cell 141 Solvent Accessible Void Vol 518.2 Ang3 correction was made for 1 thf molecule ; _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^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17285 _refine_ls_number_parameters 857 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.2359 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.2131 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.38036(8) -0.06519(12) 0.40997(7) 0.0369(5) Uani 1 1 d . . . As2 As 0.44302(8) 0.05716(11) 0.43675(7) 0.0342(5) Uani 1 1 d . . . As3 As 0.49996(8) 0.38655(11) 0.03970(7) 0.0328(4) Uani 1 1 d . . . As4 As 0.57596(9) 0.41773(12) 0.12009(8) 0.0406(5) Uani 1 1 d . . . Se1 Se 0.41633(8) -0.14123(12) 0.48930(8) 0.0372(5) Uani 1 1 d . . . Se2 Se 0.42299(8) 0.10632(11) 0.51411(7) 0.0352(4) Uani 1 1 d . . . Se3 Se 0.42694(8) 0.47403(11) 0.05143(8) 0.0348(5) Uani 1 1 d . . . Se4 Se 0.57821(8) 0.56582(12) 0.10335(8) 0.0409(5) Uani 1 1 d . . . Cu1 Cu 0.49154(10) -0.18252(14) 0.45398(9) 0.0377(6) Uani 1 1 d . . . Cu2 Cu 0.54195(10) 0.02862(14) 0.44436(9) 0.0380(6) Uani 1 1 d . . . Cu3 Cu 0.37482(9) 0.47021(14) -0.03820(9) 0.0396(6) Uani 1 1 d . . . Cu4 Cu 0.51816(9) 0.39843(13) -0.04809(9) 0.0338(5) Uani 1 1 d . . . P1 P 0.4934(2) -0.2961(3) 0.4040(2) 0.0357(12) Uani 1 1 d . . . P2 P 0.5644(2) 0.0566(3) 0.36918(19) 0.0367(12) Uani 1 1 d . . . P3 P 0.2826(2) 0.4785(3) -0.0515(2) 0.0416(13) Uani 1 1 d . . . P4 P 0.5495(2) 0.2750(3) -0.07228(19) 0.0340(12) Uani 1 1 d . . . C1 C 0.4276(4) -0.3488(6) 0.3664(4) 0.030(4) Uani 1 1 d G . . C2 C 0.3771(5) -0.3063(5) 0.3612(5) 0.041(5) Uani 1 1 d G . . H2A H 0.3770 -0.2506 0.3755 0.050 Uiso 1 1 calc R . . C3 C 0.3267(4) -0.3454(7) 0.3352(5) 0.051(5) Uani 1 1 d G . . H3A H 0.2921 -0.3164 0.3316 0.062 Uiso 1 1 calc R . . C4 C 0.3268(4) -0.4269(7) 0.3144(4) 0.052(6) Uani 1 1 d G . . H4A H 0.2924 -0.4536 0.2966 0.062 Uiso 1 1 calc R . . C5 C 0.3774(5) -0.4694(6) 0.3196(4) 0.039(5) Uani 1 1 d G . . H5A H 0.3775 -0.5251 0.3053 0.047 Uiso 1 1 calc R . . C6 C 0.4278(4) -0.4303(7) 0.3456(4) 0.046(5) Uani 1 1 d G . . H6A H 0.4624 -0.4594 0.3491 0.055 Uiso 1 1 calc R . . C7 C 0.5329(5) -0.2814(7) 0.3548(4) 0.028(4) Uani 1 1 d G . . C8 C 0.5881(5) -0.2532(8) 0.3729(3) 0.048(5) Uani 1 1 d G . . H8A H 0.6053 -0.2485 0.4097 0.057 Uiso 1 1 calc R . . C9 C 0.6181(4) -0.2319(8) 0.3371(5) 0.052(6) Uani 1 1 d G . . H9A H 0.6558 -0.2127 0.3495 0.063 Uiso 1 1 calc R . . C10 C 0.5929(5) -0.2388(8) 0.2833(5) 0.055(6) Uani 1 1 d G . . H10A H 0.6134 -0.2243 0.2589 0.066 Uiso 1 1 calc R . . C11 C 0.5377(5) -0.2670(8) 0.2652(3) 0.040(5) Uani 1 1 d G . . H11A H 0.5205 -0.2717 0.2283 0.048 Uiso 1 1 calc R . . C12 C 0.5077(4) -0.2883(7) 0.3009(4) 0.042(5) Uani 1 1 d G . . H12A H 0.4699 -0.3075 0.2885 0.051 Uiso 1 1 calc R . . C13 C 0.5333(5) -0.3793(6) 0.4468(4) 0.036(4) Uani 1 1 d G . . C14 C 0.5643(5) -0.4418(8) 0.4299(4) 0.044(5) Uani 1 1 d G . . H14A H 0.5658 -0.4426 0.3942 0.053 Uiso 1 1 calc R . . C15 C 0.5932(5) -0.5031(7) 0.4651(6) 0.062(7) Uani 1 1 d G . . H15A H 0.6144 -0.5459 0.4535 0.075 Uiso 1 1 calc R . . C16 C 0.5910(5) -0.5020(7) 0.5172(5) 0.054(6) Uani 1 1 d G . . H16A H 0.6107 -0.5439 0.5413 0.065 Uiso 1 1 calc R . . C17 C 0.5600(5) -0.4395(8) 0.5341(4) 0.045(5) Uani 1 1 d G . . H17A H 0.5585 -0.4387 0.5698 0.054 Uiso 1 1 calc R . . C18 C 0.5311(5) -0.3781(6) 0.4989(4) 0.038(5) Uani 1 1 d G . . H18A H 0.5099 -0.3354 0.5105 0.046 Uiso 1 1 calc R . . C19 C 0.5763(6) 0.1716(6) 0.3615(6) 0.049(5) Uani 1 1 d G . . C20 C 0.5410(5) 0.2272(8) 0.3785(5) 0.052(6) Uani 1 1 d G . . H20A H 0.5130 0.2053 0.3934 0.063 Uiso 1 1 calc R . . C21 C 0.5468(6) 0.3149(7) 0.3736(6) 0.055(6) Uani 1 1 d G . . H21A H 0.5227 0.3529 0.3852 0.066 Uiso 1 1 calc R . . C22 C 0.5878(7) 0.3470(6) 0.3518(6) 0.064(7) Uani 1 1 d G . . H22A H 0.5918 0.4069 0.3485 0.077 Uiso 1 1 calc R . . C23 C 0.6231(6) 0.2914(9) 0.3349(6) 0.070(7) Uani 1 1 d G . . H23A H 0.6511 0.3133 0.3200 0.084 Uiso 1 1 calc R . . C24 C 0.6173(6) 0.2037(9) 0.3397(6) 0.054(6) Uani 1 1 d G . . H24A H 0.6414 0.1657 0.3281 0.065 Uiso 1 1 calc R . . C25 C 0.6304(4) 0.0102(7) 0.3633(5) 0.035(5) Uani 1 1 d G . . C26 C 0.6744(5) 0.0042(9) 0.4091(4) 0.054(6) Uani 1 1 d G . . H26A H 0.6691 0.0216 0.4419 0.065 Uiso 1 1 calc R . . C27 C 0.7263(5) -0.0272(9) 0.4067(5) 0.071(7) Uani 1 1 d G . . H27A H 0.7564 -0.0313 0.4380 0.085 Uiso 1 1 calc R . . C28 C 0.7340(4) -0.0526(8) 0.3587(6) 0.067(8) Uani 1 1 d G . . H28A H 0.7695 -0.0740 0.3571 0.080 Uiso 1 1 calc R . . C29 C 0.6900(6) -0.0466(8) 0.3129(5) 0.057(6) Uani 1 1 d G . . H29A H 0.6953 -0.0640 0.2801 0.068 Uiso 1 1 calc R . . C30 C 0.6381(5) -0.0152(8) 0.3153(4) 0.036(5) Uani 1 1 d G . . H30A H 0.6080 -0.0111 0.2840 0.043 Uiso 1 1 calc R . . C31 C 0.5138(4) 0.0274(7) 0.3070(4) 0.035(4) Uani 1 1 d G . . C32 C 0.4975(5) 0.0839(6) 0.2649(5) 0.047(5) Uani 1 1 d G . . H32A H 0.5149 0.1383 0.2668 0.057 Uiso 1 1 calc R . . C33 C 0.4558(6) 0.0607(8) 0.2200(4) 0.061(6) Uani 1 1 d G . . H33A H 0.4446 0.0994 0.1912 0.073 Uiso 1 1 calc R . . C34 C 0.4303(5) -0.0189(9) 0.2171(4) 0.057(6) Uani 1 1 d G . . H34A H 0.4018 -0.0347 0.1864 0.069 Uiso 1 1 calc R . . C35 C 0.4466(5) -0.0754(7) 0.2592(5) 0.046(5) Uani 1 1 d G . . H35A H 0.4292 -0.1299 0.2573 0.055 Uiso 1 1 calc R . . C36 C 0.4883(5) -0.0523(7) 0.3041(4) 0.044(5) Uani 1 1 d G . . H36A H 0.4995 -0.0909 0.3329 0.053 Uiso 1 1 calc R . . C37 C 0.4054(6) 0.1419(6) 0.3832(4) 0.042(5) Uani 1 1 d G . . C38 C 0.3947(6) 0.1207(6) 0.3301(5) 0.042(5) Uani 1 1 d G . . H38A H 0.4016 0.0643 0.3202 0.050 Uiso 1 1 calc R . . C39 C 0.3738(6) 0.1820(7) 0.2916(4) 0.061(7) Uani 1 1 d G . . H39A H 0.3664 0.1675 0.2554 0.074 Uiso 1 1 calc R . . C40 C 0.3636(7) 0.2645(7) 0.3062(4) 0.065(7) Uani 1 1 d G . . H40A H 0.3494 0.3064 0.2799 0.078 Uiso 1 1 calc R . . C41 C 0.3744(6) 0.2857(6) 0.3592(5) 0.061(7) Uani 1 1 d G . . H41A H 0.3675 0.3421 0.3692 0.074 Uiso 1 1 calc R . . C42 C 0.3953(6) 0.2244(7) 0.3977(4) 0.060(6) Uani 1 1 d G . . H42A H 0.4026 0.2389 0.4340 0.072 Uiso 1 1 calc R . . C43 C 0.3076(4) -0.0261(8) 0.4199(5) 0.050(6) Uani 1 1 d G . . C44 C 0.2781(5) 0.0390(7) 0.3884(5) 0.053(6) Uani 1 1 d G . . H44A H 0.2955 0.0710 0.3665 0.064 Uiso 1 1 calc R . . C45 C 0.2232(5) 0.0572(8) 0.3888(5) 0.067(7) Uani 1 1 d G . . H45A H 0.2031 0.1017 0.3672 0.080 Uiso 1 1 calc R . . C46 C 0.1978(4) 0.0104(9) 0.4207(6) 0.064(7) Uani 1 1 d G . . H46A H 0.1603 0.0228 0.4210 0.077 Uiso 1 1 calc R . . C47 C 0.2273(5) -0.0547(8) 0.4523(5) 0.058(6) Uani 1 1 d G . . H47A H 0.2100 -0.0867 0.4742 0.070 Uiso 1 1 calc R . . C48 C 0.2822(5) -0.0729(7) 0.4519(5) 0.044(5) Uani 1 1 d G . . H48A H 0.3024 -0.1174 0.4735 0.052 Uiso 1 1 calc R . . C49 C 0.2599(5) 0.3775(7) -0.0282(5) 0.037(5) Uani 1 1 d G . . C50 C 0.2867(5) 0.3041(9) -0.0384(6) 0.058(6) Uani 1 1 d G . . H50A H 0.3164 0.3083 -0.0547 0.070 Uiso 1 1 calc R . . C51 C 0.2701(7) 0.2246(7) -0.0246(7) 0.100(10) Uani 1 1 d G . . H51A H 0.2885 0.1744 -0.0316 0.120 Uiso 1 1 calc R . . C52 C 0.2267(7) 0.2185(7) -0.0007(6) 0.055(6) Uani 1 1 d G . . H52A H 0.2153 0.1641 0.0087 0.066 Uiso 1 1 calc R . . C53 C 0.1998(5) 0.2919(9) 0.0095(5) 0.063(7) Uani 1 1 d G . . H53A H 0.1701 0.2877 0.0258 0.076 Uiso 1 1 calc R . . C54 C 0.2164(5) 0.3714(7) -0.0043(5) 0.038(5) Uani 1 1 d G . . H54A H 0.1981 0.4216 0.0027 0.046 Uiso 1 1 calc R . . C55 C 0.2365(5) 0.4909(9) -0.1185(4) 0.046(5) Uani 1 1 d G . . C56 C 0.1870(6) 0.4443(8) -0.1357(5) 0.047(5) Uani 1 1 d G . . H56A H 0.1772 0.4037 -0.1129 0.056 Uiso 1 1 calc R . . C57 C 0.1520(5) 0.4571(9) -0.1862(6) 0.066(7) Uani 1 1 d G . . H57A H 0.1182 0.4252 -0.1979 0.080 Uiso 1 1 calc R . . C58 C 0.1664(7) 0.5164(11) -0.2195(4) 0.088(10) Uani 1 1 d G . . H58A H 0.1425 0.5251 -0.2540 0.105 Uiso 1 1 calc R . . C59 C 0.2159(7) 0.5630(9) -0.2022(5) 0.074(8) Uani 1 1 d G . . H59A H 0.2258 0.6036 -0.2250 0.088 Uiso 1 1 calc R . . C60 C 0.2509(5) 0.5503(9) -0.1517(6) 0.058(6) Uani 1 1 d G . . H60A H 0.2847 0.5821 -0.1400 0.070 Uiso 1 1 calc R . . C61 C 0.2570(5) 0.5622(7) -0.0144(5) 0.047(5) Uani 1 1 d G . . C62 C 0.2787(5) 0.5654(7) 0.0401(5) 0.043(5) Uani 1 1 d G . . H62A H 0.3063 0.5252 0.0575 0.052 Uiso 1 1 calc R . . C63 C 0.2601(6) 0.6275(8) 0.0691(4) 0.053(6) Uani 1 1 d G . . H63A H 0.2749 0.6296 0.1063 0.064 Uiso 1 1 calc R . . C64 C 0.2197(6) 0.6863(7) 0.0436(6) 0.061(6) Uani 1 1 d G . . H64A H 0.2070 0.7287 0.0634 0.073 Uiso 1 1 calc R . . C65 C 0.1979(5) 0.6831(7) -0.0109(6) 0.060(6) Uani 1 1 d G . . H65A H 0.1703 0.7233 -0.0284 0.072 Uiso 1 1 calc R . . C66 C 0.2166(5) 0.6211(9) -0.0399(4) 0.046(5) Uani 1 1 d G . . H66A H 0.2017 0.6189 -0.0772 0.055 Uiso 1 1 calc R . . C67 C 0.5970(5) 0.2113(7) -0.0191(4) 0.038(5) Uani 1 1 d G . . C68 C 0.6401(6) 0.2577(6) 0.0144(6) 0.051(6) Uani 1 1 d G . . H68A H 0.6450 0.3164 0.0076 0.061 Uiso 1 1 calc R . . C69 C 0.6761(5) 0.2183(9) 0.0579(5) 0.076(8) Uani 1 1 d G . . H69A H 0.7056 0.2501 0.0808 0.092 Uiso 1 1 calc R . . C70 C 0.6690(6) 0.1325(10) 0.0680(5) 0.064(7) Uani 1 1 d G . . H70A H 0.6937 0.1056 0.0977 0.077 Uiso 1 1 calc R . . C71 C 0.6259(6) 0.0861(6) 0.0345(6) 0.057(6) Uani 1 1 d G . . H71A H 0.6211 0.0274 0.0413 0.068 Uiso 1 1 calc R . . C72 C 0.5899(5) 0.1255(7) -0.0091(5) 0.046(5) Uani 1 1 d G . . H72A H 0.5604 0.0937 -0.0320 0.055 Uiso 1 1 calc R . . C73 C 0.4931(4) 0.1989(7) -0.1015(5) 0.043(5) Uani 1 1 d GU . . C74 C 0.4475(5) 0.1988(7) -0.0802(4) 0.051(5) Uani 1 1 d GU . . H74A H 0.4468 0.2368 -0.0523 0.062 Uiso 1 1 calc R . . C75 C 0.4030(4) 0.1430(8) -0.0998(5) 0.050(5) Uani 1 1 d GU . . H75A H 0.3718 0.1429 -0.0852 0.060 Uiso 1 1 calc R . . C76 C 0.4040(5) 0.0874(7) -0.1406(5) 0.060(6) Uani 1 1 d GU . . H76A H 0.3735 0.0493 -0.1539 0.072 Uiso 1 1 calc R . . C77 C 0.4495(5) 0.0875(7) -0.1619(4) 0.048(5) Uani 1 1 d GU . . H77A H 0.4502 0.0495 -0.1898 0.057 Uiso 1 1 calc R . . C78 C 0.4941(4) 0.1433(8) -0.1424(5) 0.052(5) Uani 1 1 d GU . . H78A H 0.5252 0.1434 -0.1569 0.062 Uiso 1 1 calc R . . C79 C 0.5916(5) 0.2801(8) -0.1202(4) 0.034(4) Uani 1 1 d G . . C80 C 0.6283(5) 0.2148(6) -0.1243(4) 0.039(5) Uani 1 1 d G . . H80A H 0.6325 0.1665 -0.1018 0.047 Uiso 1 1 calc R . . C81 C 0.6588(5) 0.2203(7) -0.1613(5) 0.040(5) Uani 1 1 d G . . H81A H 0.6839 0.1757 -0.1641 0.048 Uiso 1 1 calc R . . C82 C 0.6527(5) 0.2910(8) -0.1943(4) 0.053(6) Uani 1 1 d G . . H82A H 0.6736 0.2947 -0.2195 0.063 Uiso 1 1 calc R . . C83 C 0.6160(5) 0.3562(7) -0.1902(5) 0.050(5) Uani 1 1 d G . . H83A H 0.6118 0.4046 -0.2127 0.060 Uiso 1 1 calc R . . C84 C 0.5855(5) 0.3508(7) -0.1532(5) 0.043(5) Uani 1 1 d G . . H84A H 0.5604 0.3954 -0.1504 0.052 Uiso 1 1 calc R . . C85 C 0.4766(5) 0.2720(5) 0.0585(5) 0.033(4) Uani 1 1 d G . . C86 C 0.4210(5) 0.2531(7) 0.0561(6) 0.057(6) Uani 1 1 d G . . H86A H 0.3933 0.2966 0.0476 0.068 Uiso 1 1 calc R . . C87 C 0.4061(4) 0.1705(8) 0.0661(6) 0.069(7) Uani 1 1 d G . . H87A H 0.3681 0.1576 0.0644 0.082 Uiso 1 1 calc R . . C88 C 0.4467(6) 0.1068(6) 0.0785(5) 0.057(6) Uani 1 1 d G . . H88A H 0.4365 0.0504 0.0853 0.068 Uiso 1 1 calc R . . C89 C 0.5023(5) 0.1257(6) 0.0809(5) 0.045(5) Uani 1 1 d G . . H89A H 0.5300 0.0822 0.0894 0.054 Uiso 1 1 calc R . . C90 C 0.5172(4) 0.2083(7) 0.0709(5) 0.041(5) Uani 1 1 d G . . H90A H 0.5552 0.2212 0.0725 0.050 Uiso 1 1 calc R . . C91 C 0.5326(5) 0.4148(7) 0.1737(4) 0.042(5) Uani 1 1 d G . . C92 C 0.5226(6) 0.4880(6) 0.1996(5) 0.045(5) Uani 1 1 d G . . H92A H 0.5349 0.5420 0.1907 0.055 Uiso 1 1 calc R . . C93 C 0.4944(6) 0.4821(8) 0.2384(5) 0.064(7) Uani 1 1 d G . . H93A H 0.4875 0.5321 0.2561 0.077 Uiso 1 1 calc R . . C94 C 0.4764(6) 0.4031(10) 0.2515(5) 0.071(7) Uani 1 1 d G . . H94A H 0.4571 0.3991 0.2780 0.085 Uiso 1 1 calc R . . C95 C 0.4865(6) 0.3299(7) 0.2256(5) 0.058(6) Uani 1 1 d G . . H95A H 0.4741 0.2759 0.2345 0.069 Uiso 1 1 calc R . . C96 C 0.5146(6) 0.3358(6) 0.1867(5) 0.056(6) Uani 1 1 d G . . H96A H 0.5215 0.2858 0.1691 0.068 Uiso 1 1 calc R . . O1 O 0.2500 0.200(2) 0.7500 0.138(12) Uiso 1 2 d S . . C97 C 0.2783(18) 0.246(2) 0.7943(16) 0.148(14) Uiso 1 1 d . . . H97A H 0.3182 0.2284 0.8063 0.178 Uiso 1 1 calc R . . H97B H 0.2607 0.2374 0.8235 0.178 Uiso 1 1 calc R . . C98 C 0.2729(12) 0.3341(17) 0.7762(10) 0.093(9) Uiso 1 1 d . . . H98A H 0.3089 0.3549 0.7711 0.112 Uiso 1 1 calc R . . H98B H 0.2622 0.3714 0.8022 0.112 Uiso 1 1 calc R . . O2 O 0.7500 0.1914(13) 0.7500 0.065(6) Uiso 1 2 d S . . C99 C 0.7056(10) 0.1361(13) 0.7195(9) 0.061(6) Uiso 1 1 d . . . H99A H 0.7044 0.1383 0.6816 0.073 Uiso 1 1 calc R . . H99B H 0.6687 0.1547 0.7233 0.073 Uiso 1 1 calc R . . C100 C 0.7190(9) 0.0445(14) 0.7410(10) 0.075(7) Uiso 1 1 d . . . H10C H 0.7025 0.0332 0.7706 0.090 Uiso 1 1 calc R . . H10D H 0.7049 0.0014 0.7130 0.090 Uiso 1 1 calc R . . O3 O 0.2735(13) 0.2869(19) 0.1657(12) 0.192(12) Uiso 1 1 d D . . C101 C 0.3291(14) 0.2904(19) 0.1507(14) 0.120(11) Uiso 1 1 d D . . H10E H 0.3605 0.2669 0.1790 0.144 Uiso 1 1 calc R . . H10F H 0.3265 0.2593 0.1174 0.144 Uiso 1 1 calc R . . C102 C 0.3351(16) 0.380(2) 0.1445(17) 0.166(16) Uiso 1 1 d D . . H10G H 0.3753 0.3955 0.1511 0.199 Uiso 1 1 calc R . . H10H H 0.3150 0.3981 0.1081 0.199 Uiso 1 1 calc R . . C103 C 0.3126(16) 0.4206(19) 0.1802(15) 0.150(14) Uiso 1 1 d D . . H10I H 0.3045 0.4811 0.1700 0.180 Uiso 1 1 calc R . . H10J H 0.3396 0.4191 0.2157 0.180 Uiso 1 1 calc R . . C104 C 0.2626(13) 0.3784(18) 0.1812(12) 0.105(10) Uiso 1 1 d D . . H10K H 0.2297 0.4036 0.1555 0.127 Uiso 1 1 calc R . . H10L H 0.2566 0.3802 0.2168 0.127 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 As1 0.0369(11) 0.0389(10) 0.0331(11) -0.0054(9) 0.0067(9) 0.0023(9) As2 0.0333(11) 0.0325(10) 0.0368(11) -0.0016(9) 0.0097(9) 0.0006(9) As3 0.0296(11) 0.0328(10) 0.0371(11) -0.0031(9) 0.0109(9) -0.0003(9) As4 0.0368(12) 0.0390(11) 0.0444(12) -0.0019(9) 0.0083(10) 0.0061(9) Se1 0.0368(12) 0.0364(10) 0.0386(11) -0.0042(9) 0.0106(9) -0.0049(9) Se2 0.0344(11) 0.0360(10) 0.0355(11) -0.0028(9) 0.0100(9) -0.0006(9) Se3 0.0318(11) 0.0347(10) 0.0413(11) -0.0027(9) 0.0159(9) 0.0003(9) Se4 0.0348(11) 0.0416(11) 0.0462(12) -0.0044(9) 0.0106(9) -0.0014(9) Cu1 0.0406(14) 0.0344(12) 0.0374(14) -0.0057(10) 0.0096(12) -0.0023(11) Cu2 0.0413(14) 0.0400(13) 0.0343(13) -0.0009(11) 0.0127(11) 0.0016(11) Cu3 0.0286(13) 0.0405(13) 0.0504(15) 0.0003(11) 0.0118(11) 0.0018(11) Cu4 0.0304(13) 0.0315(12) 0.0409(13) -0.0013(10) 0.0124(11) 0.0034(10) P1 0.036(3) 0.035(3) 0.037(3) -0.001(2) 0.011(2) 0.005(2) P2 0.038(3) 0.039(3) 0.033(3) 0.001(2) 0.011(2) -0.007(2) P3 0.028(3) 0.046(3) 0.051(3) -0.002(3) 0.010(3) 0.000(2) P4 0.032(3) 0.035(3) 0.036(3) 0.001(2) 0.011(2) 0.005(2) C1 0.046(12) 0.022(9) 0.027(10) 0.005(7) 0.019(9) -0.007(8) C2 0.043(13) 0.032(10) 0.047(12) 0.002(9) 0.011(10) -0.014(9) C3 0.033(12) 0.062(14) 0.055(14) -0.006(11) 0.005(11) -0.008(10) C4 0.083(17) 0.035(11) 0.030(11) 0.025(9) 0.005(11) -0.020(11) C5 0.050(12) 0.038(10) 0.018(9) -0.015(8) -0.012(9) -0.005(10) C6 0.070(15) 0.049(12) 0.016(9) -0.010(9) 0.008(10) -0.027(11) C7 0.052(12) 0.020(8) 0.007(8) -0.001(7) 0.001(8) 0.012(8) C8 0.036(12) 0.068(14) 0.032(12) -0.015(10) -0.004(10) -0.021(11) C9 0.070(17) 0.047(12) 0.047(14) 0.000(10) 0.028(13) 0.012(11) C10 0.072(17) 0.039(12) 0.070(17) 0.021(11) 0.046(14) -0.005(11) C11 0.034(12) 0.041(11) 0.041(12) 0.000(9) 0.002(10) -0.008(9) C12 0.046(13) 0.038(11) 0.046(13) 0.020(9) 0.018(11) 0.004(9) C13 0.027(10) 0.032(10) 0.042(12) -0.009(9) 0.000(9) -0.003(8) C14 0.037(11) 0.039(11) 0.050(12) 0.005(10) 0.001(10) 0.002(9) C15 0.032(12) 0.068(15) 0.078(18) -0.008(13) -0.001(12) -0.009(11) C16 0.046(13) 0.022(10) 0.082(18) -0.001(10) -0.002(13) 0.011(9) C17 0.066(14) 0.037(11) 0.025(10) -0.001(9) 0.000(10) -0.015(10) C18 0.034(11) 0.049(11) 0.020(10) 0.006(8) -0.011(8) -0.005(9) C19 0.048(14) 0.054(13) 0.050(13) -0.007(10) 0.023(11) -0.004(11) C20 0.065(16) 0.049(12) 0.041(13) 0.025(10) 0.010(12) 0.004(11) C21 0.071(17) 0.037(12) 0.057(15) 0.007(11) 0.016(13) -0.001(11) C22 0.082(19) 0.052(14) 0.052(15) 0.010(12) 0.008(14) -0.021(13) C23 0.067(18) 0.059(15) 0.078(18) -0.012(13) 0.010(15) -0.018(13) C24 0.049(14) 0.065(15) 0.050(14) -0.011(11) 0.017(11) -0.014(11) C25 0.030(11) 0.023(9) 0.054(13) -0.014(9) 0.013(10) -0.014(8) C26 0.038(13) 0.058(13) 0.065(16) 0.011(11) 0.013(12) -0.011(11) C27 0.049(14) 0.12(2) 0.040(14) 0.009(14) 0.010(12) 0.027(15) C28 0.063(16) 0.036(12) 0.13(2) 0.021(13) 0.076(17) 0.012(11) C29 0.064(15) 0.069(15) 0.035(12) -0.005(11) 0.011(11) -0.016(13) C30 0.051(13) 0.036(10) 0.031(11) 0.004(8) 0.030(10) 0.005(9) C31 0.031(10) 0.033(10) 0.041(12) -0.014(9) 0.008(9) -0.017(9) C32 0.069(15) 0.056(13) 0.027(11) 0.008(9) 0.028(11) -0.013(11) C33 0.072(17) 0.069(15) 0.047(14) -0.002(12) 0.022(13) 0.001(13) C34 0.047(13) 0.084(17) 0.041(13) -0.036(12) 0.012(11) -0.002(13) C35 0.054(14) 0.029(10) 0.062(14) -0.004(10) 0.028(12) -0.002(10) C36 0.024(10) 0.070(14) 0.037(11) -0.013(10) 0.006(9) 0.001(10) C37 0.063(14) 0.032(10) 0.033(11) 0.002(8) 0.017(10) 0.018(10) C38 0.059(14) 0.032(10) 0.036(11) -0.006(9) 0.015(10) 0.015(9) C39 0.092(19) 0.028(11) 0.059(15) 0.006(10) 0.011(14) 0.016(11) C40 0.089(19) 0.038(12) 0.057(16) 0.002(11) 0.003(14) 0.003(12) C41 0.080(18) 0.054(13) 0.041(13) 0.013(11) 0.001(12) 0.032(12) C42 0.067(16) 0.040(12) 0.067(16) 0.025(11) 0.009(13) 0.003(11) C43 0.063(14) 0.041(11) 0.047(13) -0.035(10) 0.018(11) 0.007(11) C44 0.035(12) 0.040(12) 0.070(15) -0.005(11) -0.012(11) 0.007(10) C45 0.076(18) 0.058(14) 0.063(16) -0.003(12) 0.013(14) 0.032(13) C46 0.055(15) 0.063(15) 0.072(17) 0.015(13) 0.012(13) -0.021(13) C47 0.033(12) 0.082(16) 0.066(15) -0.003(13) 0.025(11) -0.018(12) C48 0.059(14) 0.029(10) 0.057(13) -0.015(9) 0.040(12) 0.003(10) C49 0.029(11) 0.045(12) 0.036(11) -0.014(9) 0.007(9) -0.013(9) C50 0.047(14) 0.051(13) 0.082(18) -0.009(12) 0.027(13) -0.010(11) C51 0.07(2) 0.08(2) 0.15(3) -0.01(2) 0.04(2) -0.013(16) C52 0.045(14) 0.025(10) 0.073(16) 0.019(10) -0.021(12) -0.011(10) C53 0.070(17) 0.093(18) 0.031(12) 0.017(12) 0.019(12) -0.012(15) C54 0.011(9) 0.041(11) 0.056(13) 0.017(9) -0.002(9) 0.002(8) C55 0.023(11) 0.073(14) 0.036(12) 0.004(10) 0.000(9) 0.025(10) C56 0.056(14) 0.055(12) 0.029(11) 0.010(10) 0.011(10) 0.005(11) C57 0.080(18) 0.049(14) 0.060(16) -0.012(12) 0.003(14) 0.030(13) C58 0.066(18) 0.11(2) 0.069(19) -0.017(18) -0.006(15) 0.064(18) C59 0.10(2) 0.11(2) 0.017(11) 0.018(13) 0.023(12) 0.036(18) C60 0.058(15) 0.066(15) 0.064(16) -0.002(12) 0.038(13) 0.012(12) C61 0.012(9) 0.063(13) 0.064(14) -0.015(12) 0.005(9) -0.001(10) C62 0.038(11) 0.037(10) 0.038(11) -0.007(9) -0.017(9) -0.009(9) C63 0.059(15) 0.029(11) 0.073(16) -0.019(10) 0.022(13) 0.000(10) C64 0.053(15) 0.039(12) 0.10(2) -0.019(13) 0.031(14) 0.000(11) C65 0.038(13) 0.057(14) 0.082(18) 0.023(13) 0.011(13) -0.020(11) C66 0.032(12) 0.046(12) 0.060(14) -0.018(11) 0.013(11) -0.009(10) C67 0.034(11) 0.053(12) 0.033(11) 0.008(9) 0.023(10) 0.019(10) C68 0.049(14) 0.043(12) 0.068(16) -0.010(11) 0.030(13) 0.003(11) C69 0.050(16) 0.086(19) 0.09(2) 0.022(16) 0.020(15) -0.004(14) C70 0.058(16) 0.062(15) 0.069(17) 0.017(13) 0.014(13) 0.022(13) C71 0.074(17) 0.043(12) 0.051(14) 0.012(11) 0.014(12) 0.029(12) C72 0.063(15) 0.018(9) 0.071(15) -0.003(9) 0.044(13) 0.010(9) C73 0.013(9) 0.039(10) 0.066(14) -0.015(8) -0.005(8) -0.008(8) C74 0.053(13) 0.038(11) 0.065(14) -0.001(9) 0.021(10) -0.024(9) C75 0.023(10) 0.067(13) 0.058(13) -0.010(9) 0.005(9) -0.009(8) C76 0.056(12) 0.027(10) 0.091(17) -0.011(9) 0.010(11) -0.016(10) C77 0.057(12) 0.037(11) 0.040(11) -0.012(8) -0.003(9) -0.006(9) C78 0.031(10) 0.056(12) 0.056(13) -0.020(9) -0.010(9) 0.001(8) C79 0.041(12) 0.043(11) 0.023(10) -0.001(8) 0.014(9) -0.001(9) C80 0.024(11) 0.054(12) 0.039(12) -0.029(9) 0.011(9) -0.006(9) C81 0.043(12) 0.055(12) 0.020(10) -0.010(9) 0.004(9) -0.007(10) C82 0.043(14) 0.066(14) 0.056(14) -0.008(12) 0.025(11) -0.022(11) C83 0.024(11) 0.057(13) 0.060(14) 0.007(11) -0.004(10) -0.005(10) C84 0.014(10) 0.069(14) 0.048(13) -0.005(11) 0.010(9) 0.003(9) C85 0.057(13) 0.031(10) 0.016(9) 0.000(7) 0.019(9) 0.006(9) C86 0.061(16) 0.049(13) 0.069(16) 0.000(11) 0.032(14) -0.011(12) C87 0.043(14) 0.034(12) 0.14(2) 0.002(13) 0.037(15) -0.011(10) C88 0.082(18) 0.044(12) 0.047(13) -0.007(11) 0.022(13) -0.008(13) C89 0.052(14) 0.055(13) 0.033(11) 0.006(9) 0.022(10) 0.009(11) C90 0.073(15) 0.026(10) 0.026(11) -0.004(8) 0.014(10) 0.008(10) C91 0.028(11) 0.027(10) 0.059(13) 0.007(9) -0.011(9) 0.015(8) C92 0.065(14) 0.042(11) 0.033(12) 0.004(9) 0.021(11) 0.034(11) C93 0.100(19) 0.067(15) 0.028(12) -0.005(11) 0.020(13) 0.004(14) C94 0.088(19) 0.084(18) 0.057(15) 0.011(14) 0.047(14) 0.014(15) C95 0.069(17) 0.064(15) 0.036(12) -0.016(11) 0.009(12) -0.007(13) C96 0.081(18) 0.027(11) 0.061(15) 0.013(10) 0.020(13) 0.008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C43 1.985(9) . ? As1 Se1 2.359(3) . ? As1 As2 2.444(3) . ? As2 C37 1.975(8) . ? As2 Se2 2.355(3) . ? As2 Cu2 2.441(3) . ? As3 C85 1.988(9) . ? As3 Se3 2.354(3) . ? As3 As4 2.467(3) . ? As3 Cu4 2.482(3) . ? As4 C91 1.994(9) . ? As4 Se4 2.364(3) . ? Se1 Cu1 2.386(3) . ? Se1 Cu2 2.499(3) 3_656 ? Se2 Cu1 2.373(3) 3_656 ? Se2 Cu2 2.428(3) 3_656 ? Se3 Cu3 2.363(3) . ? Se3 Cu4 2.430(3) 3_665 ? Se4 Cu3 2.389(3) 3_665 ? Se4 Cu4 2.494(3) 3_665 ? Cu1 P1 2.221(5) . ? Cu1 Se2 2.373(3) 3_656 ? Cu2 P2 2.242(5) . ? Cu2 Se2 2.428(3) 3_656 ? Cu2 Se1 2.499(3) 3_656 ? Cu3 P3 2.216(5) . ? Cu3 Se4 2.389(3) 3_665 ? Cu4 P4 2.239(5) . ? Cu4 Se3 2.430(3) 3_665 ? Cu4 Se4 2.494(3) 3_665 ? P1 C13 1.827(9) . ? P1 C7 1.839(10) . ? P1 C1 1.851(9) . ? P2 C31 1.828(10) . ? P2 C25 1.831(10) . ? P2 C19 1.844(11) . ? P3 C55 1.830(11) . ? P3 C49 1.839(10) . ? P3 C61 1.848(10) . ? P4 C73 1.837(9) . ? P4 C79 1.846(10) . ? P4 C67 1.855(10) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C68 C69 1.3900 . ? C69 C70 1.3900 . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C85 C86 1.3900 . ? C85 C90 1.3900 . ? C86 C87 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? O1 C97 1.39(4) . ? O1 C97 1.39(4) 2_556 ? C97 C98 1.46(4) . ? C98 C98 1.53(5) 2_556 ? O2 C99 1.46(2) 2_656 ? O2 C99 1.46(2) . ? C99 C100 1.54(3) . ? C100 C100 1.48(4) 2_656 ? O3 C101 1.53(3) . ? O3 C104 1.53(3) . ? C101 C102 1.43(3) . ? C102 C103 1.37(5) . ? C103 C104 1.41(3) . ? 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 C43 As1 Se1 100.0(4) . . ? C43 As1 As2 104.3(4) . . ? Se1 As1 As2 94.81(9) . . ? C37 As2 Se2 103.3(4) . . ? C37 As2 Cu2 116.6(4) . . ? Se2 As2 Cu2 115.59(11) . . ? C37 As2 As1 100.5(4) . . ? Se2 As2 As1 103.86(10) . . ? Cu2 As2 As1 114.99(10) . . ? C85 As3 Se3 101.9(4) . . ? C85 As3 As4 99.8(4) . . ? Se3 As3 As4 101.78(9) . . ? C85 As3 Cu4 116.0(3) . . ? Se3 As3 Cu4 114.83(10) . . ? As4 As3 Cu4 119.74(10) . . ? C91 As4 Se4 101.5(3) . . ? C91 As4 As3 100.0(4) . . ? Se4 As4 As3 94.88(9) . . ? As1 Se1 Cu1 86.36(10) . . ? As1 Se1 Cu2 104.34(10) . 3_656 ? Cu1 Se1 Cu2 104.31(10) . 3_656 ? As2 Se2 Cu1 95.36(10) . 3_656 ? As2 Se2 Cu2 88.41(9) . 3_656 ? Cu1 Se2 Cu2 95.97(11) 3_656 3_656 ? As3 Se3 Cu3 94.74(10) . . ? As3 Se3 Cu4 90.97(9) . 3_665 ? Cu3 Se3 Cu4 98.18(10) . 3_665 ? As4 Se4 Cu3 86.75(10) . 3_665 ? As4 Se4 Cu4 105.18(10) . 3_665 ? Cu3 Se4 Cu4 102.02(10) 3_665 3_665 ? P1 Cu1 Se2 116.89(17) . 3_656 ? P1 Cu1 Se1 126.36(17) . . ? Se2 Cu1 Se1 116.09(11) 3_656 . ? P2 Cu2 Se2 115.12(16) . 3_656 ? P2 Cu2 As2 112.10(17) . . ? Se2 Cu2 As2 115.02(11) 3_656 . ? P2 Cu2 Se1 109.00(16) . 3_656 ? Se2 Cu2 Se1 105.68(11) 3_656 3_656 ? As2 Cu2 Se1 98.12(10) . 3_656 ? P3 Cu3 Se3 114.46(18) . . ? P3 Cu3 Se4 125.59(18) . 3_665 ? Se3 Cu3 Se4 119.01(11) . 3_665 ? P4 Cu4 Se3 117.29(16) . 3_665 ? P4 Cu4 As3 111.47(16) . . ? Se3 Cu4 As3 109.93(10) 3_665 . ? P4 Cu4 Se4 112.19(16) . 3_665 ? Se3 Cu4 Se4 104.40(10) 3_665 3_665 ? As3 Cu4 Se4 99.99(10) . 3_665 ? C13 P1 C7 102.9(6) . . ? C13 P1 C1 105.1(6) . . ? C7 P1 C1 103.7(5) . . ? C13 P1 Cu1 107.4(4) . . ? C7 P1 Cu1 114.8(4) . . ? C1 P1 Cu1 121.2(4) . . ? C31 P2 C25 103.5(6) . . ? C31 P2 C19 103.7(6) . . ? C25 P2 C19 101.9(6) . . ? C31 P2 Cu2 118.0(4) . . ? C25 P2 Cu2 116.0(5) . . ? C19 P2 Cu2 111.9(5) . . ? C55 P3 C49 104.3(6) . . ? C55 P3 C61 102.8(6) . . ? C49 P3 C61 104.7(6) . . ? C55 P3 Cu3 120.2(5) . . ? C49 P3 Cu3 106.9(5) . . ? C61 P3 Cu3 116.4(4) . . ? C73 P4 C79 104.3(6) . . ? C73 P4 C67 102.7(6) . . ? C79 P4 C67 100.5(6) . . ? C73 P4 Cu4 113.4(5) . . ? C79 P4 Cu4 117.5(4) . . ? C67 P4 Cu4 116.5(4) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 118.3(6) . . ? C6 C1 P1 121.6(6) . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 117.3(7) . . ? C12 C7 P1 122.3(7) . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 123.9(7) . . ? C18 C13 P1 116.1(7) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 116.4(8) . . ? C24 C19 P2 123.6(8) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 P2 117.3(7) . . ? C30 C25 P2 122.6(7) . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 122.3(7) . . ? C36 C31 P2 117.6(7) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 As2 118.8(6) . . ? C42 C37 As2 120.8(6) . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 As1 119.6(7) . . ? C48 C43 As1 119.6(7) . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C47 C48 C43 120.0 . . ? C50 C49 C54 120.0 . . ? C50 C49 P3 116.2(8) . . ? C54 C49 P3 123.7(8) . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C49 120.0 . . ? C56 C55 C60 120.0 . . ? C56 C55 P3 121.3(9) . . ? C60 C55 P3 118.6(9) . . ? C55 C56 C57 120.0 . . ? C56 C57 C58 120.0 . . ? C57 C58 C59 120.0 . . ? C58 C59 C60 120.0 . . ? C59 C60 C55 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 P3 118.7(8) . . ? C66 C61 P3 121.3(8) . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C65 C64 C63 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? C68 C67 C72 120.0 . . ? C68 C67 P4 114.6(8) . . ? C72 C67 P4 125.2(8) . . ? C67 C68 C69 120.0 . . ? C70 C69 C68 120.0 . . ? C71 C70 C69 120.0 . . ? C70 C71 C72 120.0 . . ? C71 C72 C67 120.0 . . ? C74 C73 C78 120.0 . . ? C74 C73 P4 116.0(7) . . ? C78 C73 P4 124.0(7) . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C77 C76 C75 120.0 . . ? C76 C77 C78 120.0 . . ? C77 C78 C73 120.0 . . ? C80 C79 C84 120.0 . . ? C80 C79 P4 121.5(7) . . ? C84 C79 P4 118.5(7) . . ? C81 C80 C79 120.0 . . ? C80 C81 C82 120.0 . . ? C83 C82 C81 120.0 . . ? C82 C83 C84 120.0 . . ? C83 C84 C79 120.0 . . ? C86 C85 C90 120.0 . . ? C86 C85 As3 122.1(7) . . ? C90 C85 As3 117.7(7) . . ? C87 C86 C85 120.0 . . ? C86 C87 C88 120.0 . . ? C89 C88 C87 120.0 . . ? C90 C89 C88 120.0 . . ? C89 C90 C85 120.0 . . ? C92 C91 C96 120.0 . . ? C92 C91 As4 122.1(6) . . ? C96 C91 As4 117.8(6) . . ? C91 C92 C93 120.0 . . ? C94 C93 C92 120.0 . . ? C93 C94 C95 120.0 . . ? C96 C95 C94 120.0 . . ? C95 C96 C91 120.0 . . ? C97 O1 C97 118(4) . 2_556 ? O1 C97 C98 104(3) . . ? C97 C98 C98 106(2) . 2_556 ? C99 O2 C99 107(2) 2_656 . ? O2 C99 C100 107.2(18) . . ? C100 C100 C99 102.6(14) 2_656 . ? C101 O3 C104 106(3) . . ? C102 C101 O3 101(2) . . ? C103 C102 C101 107(2) . . ? C102 C103 C104 108.7(18) . . ? C103 C104 O3 102(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.895 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.156 data_3 _database_code_depnum_ccdc_archive 'CCDC 664250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 As K2 O15 Se3' _chemical_formula_weight 1130.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9580(18) _cell_length_b 28.590(6) _cell_length_c 19.330(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.29(3) _cell_angle_gamma 90.00 _cell_volume 4885.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6222 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 27.02 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 3.160 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19956 _diffrn_reflns_av_R_equivalents 0.1763 _diffrn_reflns_av_sigmaI/netI 0.3471 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.06 _reflns_number_total 9299 _reflns_number_gt 3247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0041P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9299 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2149 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 0.774 _refine_ls_restrained_S_all 0.774 _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 As1 As 0.53040(11) 0.77148(5) 0.19612(4) 0.0212(3) Uani 1 1 d . . . Se1 Se 0.63895(12) 0.76812(5) 0.31219(5) 0.0265(3) Uani 1 1 d . . . Se2 Se 0.29285(12) 0.80285(5) 0.18138(5) 0.0307(3) Uani 1 1 d . . . Se3 Se 0.55159(12) 0.70248(5) 0.13875(5) 0.0284(3) Uani 1 1 d . . . K1 K 0.4195(3) 0.86012(10) 0.34125(10) 0.0275(6) Uani 1 1 d . . . K2 K 0.8011(3) 0.66501(9) 0.28314(10) 0.0269(6) Uani 1 1 d . . . O1 O 0.7098(9) 0.8957(4) 0.4073(4) 0.042(3) Uani 1 1 d . . . O2 O 0.5569(9) 0.8396(3) 0.4907(3) 0.038(2) Uani 1 1 d . . . O3 O 0.2579(9) 0.8123(4) 0.4333(4) 0.048(3) Uani 1 1 d . . . O4 O 0.0870(9) 0.8734(4) 0.3351(4) 0.042(2) Uani 1 1 d . . . O5 O 0.2488(10) 0.9337(4) 0.2591(4) 0.045(3) Uani 1 1 d . . . O6 O 0.5455(9) 0.9571(3) 0.3119(3) 0.035(2) Uani 1 1 d . . . O7 O 0.6727(9) 0.5750(3) 0.2063(4) 0.041(3) Uani 1 1 d . . . O8 O 0.9337(9) 0.6201(3) 0.1732(3) 0.034(2) Uani 1 1 d . . . O9 O 1.1346(8) 0.6620(3) 0.2806(3) 0.033(2) Uani 1 1 d . . . O10 O 1.0274(7) 0.6962(3) 0.4011(3) 0.032(2) Uani 1 1 d . . . O11 O 0.7596(8) 0.6550(3) 0.4312(3) 0.033(2) Uani 1 1 d . . . O12 O 0.5594(9) 0.6119(3) 0.3232(4) 0.038(2) Uani 1 1 d . . . O13 O 0.8035(9) 0.5145(3) 0.9896(4) 0.038(2) Uani 1 1 d . . . O14 O 1.3305(13) 0.4649(5) 0.4398(5) 0.075(4) Uani 1 1 d . . . O15 O 1.057(2) 0.5285(8) 0.4052(7) 0.196(12) Uani 1 1 d . . . C1 C 0.6613(11) 0.8151(4) 0.1545(4) 0.022(3) Uani 1 1 d . . . C2 C 0.6128(13) 0.8617(5) 0.1421(5) 0.030(3) Uani 1 1 d . . . H2A H 0.5198 0.8723 0.1542 0.036 Uiso 1 1 calc R . . C3 C 0.7047(15) 0.8916(5) 0.1116(5) 0.039(4) Uani 1 1 d . . . H3A H 0.6734 0.9231 0.1031 0.047 Uiso 1 1 calc R . . C4 C 0.8408(16) 0.8774(6) 0.0930(5) 0.047(4) Uani 1 1 d . . . H4A H 0.9031 0.8986 0.0726 0.056 Uiso 1 1 calc R . . C5 C 0.8821(14) 0.8311(5) 0.1052(5) 0.037(3) Uani 1 1 d . . . H5A H 0.9737 0.8202 0.0920 0.044 Uiso 1 1 calc R . . C6 C 0.7945(11) 0.8006(5) 0.1358(4) 0.027(3) Uani 1 1 d . . . H6A H 0.8266 0.7691 0.1441 0.032 Uiso 1 1 calc R . . C7 C 0.7704(13) 0.8855(6) 0.4772(7) 0.049(5) Uani 1 1 d . . . H7A H 0.7360 0.9088 0.5090 0.059 Uiso 1 1 calc R . . H7B H 0.8823 0.8861 0.4838 0.059 Uiso 1 1 calc R . . C8 C 0.7152(14) 0.8373(6) 0.4927(6) 0.059(5) Uani 1 1 d . . . H8A H 0.7396 0.8147 0.4573 0.071 Uiso 1 1 calc R . . H8B H 0.7653 0.8268 0.5395 0.071 Uiso 1 1 calc R . . C9 C 0.4949(18) 0.7956(6) 0.5060(6) 0.056(4) Uani 1 1 d . . . H9A H 0.5421 0.7848 0.5532 0.067 Uiso 1 1 calc R . . H9B H 0.5153 0.7719 0.4713 0.067 Uiso 1 1 calc R . . C10 C 0.3302(19) 0.8012(7) 0.5033(5) 0.064(5) Uani 1 1 d . . . H10A H 0.2870 0.7719 0.5188 0.077 Uiso 1 1 calc R . . H10B H 0.3107 0.8265 0.5355 0.077 Uiso 1 1 calc R . . C11 C 0.1012(16) 0.8188(7) 0.4265(8) 0.064(5) Uani 1 1 d . . . H11A H 0.0798 0.8452 0.4567 0.077 Uiso 1 1 calc R . . H11B H 0.0537 0.7903 0.4423 0.077 Uiso 1 1 calc R . . C12 C 0.0358(15) 0.8289(7) 0.3531(8) 0.065(5) Uani 1 1 d . . . H12A H 0.0676 0.8047 0.3219 0.078 Uiso 1 1 calc R . . H12B H -0.0760 0.8287 0.3475 0.078 Uiso 1 1 calc R . . C13 C 0.0351(14) 0.8844(6) 0.2640(7) 0.051(5) Uani 1 1 d . . . H13A H -0.0767 0.8831 0.2543 0.061 Uiso 1 1 calc R . . H13B H 0.0752 0.8615 0.2334 0.061 Uiso 1 1 calc R . . C14 C 0.0885(15) 0.9332(6) 0.2491(6) 0.051(4) Uani 1 1 d . . . H14A H 0.0474 0.9422 0.2003 0.062 Uiso 1 1 calc R . . H14B H 0.0517 0.9560 0.2810 0.062 Uiso 1 1 calc R . . C15 C 0.3061(17) 0.9768(6) 0.2458(7) 0.052(4) Uani 1 1 d . . . H15A H 0.2873 0.9994 0.2823 0.063 Uiso 1 1 calc R . . H15B H 0.2551 0.9885 0.1998 0.063 Uiso 1 1 calc R . . C16 C 0.4724(17) 0.9727(6) 0.2455(6) 0.051(4) Uani 1 1 d . . . H16A H 0.4911 0.9503 0.2088 0.061 Uiso 1 1 calc R . . H16B H 0.5137 1.0035 0.2346 0.061 Uiso 1 1 calc R . . C17 C 0.7001(14) 0.9480(6) 0.3111(6) 0.049(4) Uani 1 1 d . . . H17A H 0.7487 0.9757 0.2935 0.059 Uiso 1 1 calc R . . H17B H 0.7107 0.9213 0.2796 0.059 Uiso 1 1 calc R . . C18 C 0.7757(14) 0.9366(6) 0.3846(6) 0.047(4) Uani 1 1 d . . . H18A H 0.8854 0.9317 0.3855 0.056 Uiso 1 1 calc R . . H18B H 0.7626 0.9629 0.4164 0.056 Uiso 1 1 calc R . . C19 C 0.7041(15) 0.5802(4) 0.1350(5) 0.037(4) Uani 1 1 d . . . H19A H 0.6583 0.5540 0.1056 0.044 Uiso 1 1 calc R . . H19B H 0.6591 0.6098 0.1145 0.044 Uiso 1 1 calc R . . C20 C 0.8665(14) 0.5808(5) 0.1362(5) 0.035(3) Uani 1 1 d . . . H20A H 0.9114 0.5519 0.1587 0.043 Uiso 1 1 calc R . . H20B H 0.8879 0.5816 0.0875 0.043 Uiso 1 1 calc R . . C21 C 1.0916(12) 0.6236(5) 0.1714(5) 0.036(4) Uani 1 1 d . . . H21A H 1.1090 0.6250 0.1221 0.044 Uiso 1 1 calc R . . H21B H 1.1443 0.5957 0.1936 0.044 Uiso 1 1 calc R . . C22 C 1.1540(13) 0.6670(6) 0.2097(5) 0.041(4) Uani 1 1 d . . . H22A H 1.2626 0.6706 0.2066 0.049 Uiso 1 1 calc R . . H22B H 1.0993 0.6950 0.1889 0.049 Uiso 1 1 calc R . . C23 C 1.2062(13) 0.6989(5) 0.3215(5) 0.038(3) Uani 1 1 d . . . H23A H 1.1619 0.7292 0.3039 0.046 Uiso 1 1 calc R . . H23B H 1.3155 0.6993 0.3187 0.046 Uiso 1 1 calc R . . C24 C 1.1839(12) 0.6917(5) 0.3961(5) 0.041(4) Uani 1 1 d . . . H24A H 1.2203 0.6603 0.4122 0.049 Uiso 1 1 calc R . . H24B H 1.2431 0.7152 0.4266 0.049 Uiso 1 1 calc R . . C25 C 0.9968(13) 0.6903(5) 0.4708(4) 0.034(3) Uani 1 1 d . . . H25A H 1.0486 0.7150 0.5015 0.041 Uiso 1 1 calc R . . H25B H 1.0357 0.6596 0.4894 0.041 Uiso 1 1 calc R . . C26 C 0.8315(13) 0.6928(5) 0.4706(5) 0.035(3) Uani 1 1 d . . . H26A H 0.8105 0.6914 0.5193 0.042 Uiso 1 1 calc R . . H26B H 0.7916 0.7228 0.4497 0.042 Uiso 1 1 calc R . . C27 C 0.6030(13) 0.6558(5) 0.4280(6) 0.039(3) Uani 1 1 d . . . H27A H 0.5603 0.6835 0.4009 0.047 Uiso 1 1 calc R . . H27B H 0.5781 0.6582 0.4759 0.047 Uiso 1 1 calc R . . C28 C 0.5351(14) 0.6119(5) 0.3934(5) 0.038(3) Uani 1 1 d . . . H28A H 0.5832 0.5841 0.4181 0.046 Uiso 1 1 calc R . . H28B H 0.4253 0.6108 0.3952 0.046 Uiso 1 1 calc R . . C29 C 0.4927(15) 0.5730(5) 0.2851(6) 0.043(4) Uani 1 1 d . . . H29A H 0.3830 0.5721 0.2870 0.051 Uiso 1 1 calc R . . H29B H 0.5387 0.5437 0.3061 0.051 Uiso 1 1 calc R . . C30 C 0.5177(14) 0.5768(5) 0.2089(6) 0.044(4) Uani 1 1 d . . . H30A H 0.4653 0.5508 0.1811 0.053 Uiso 1 1 calc R . . H30B H 0.4752 0.6066 0.1885 0.053 Uiso 1 1 calc R . . C31 C 0.7075(16) 0.5443(8) 0.9457(6) 0.082(8) Uani 1 1 d . . . H31A H 0.6027 0.5391 0.9525 0.124 Uiso 1 1 calc R . . H31B H 0.7167 0.5379 0.8967 0.124 Uiso 1 1 calc R . . H31C H 0.7356 0.5769 0.9569 0.124 Uiso 1 1 calc R . . C32 C 0.9517(12) 0.5169(5) 0.9760(5) 0.032(3) Uani 1 1 d . . . H32A H 0.9913 0.5491 0.9842 0.039 Uiso 1 1 calc R . . H32B H 0.9541 0.5086 0.9265 0.039 Uiso 1 1 calc R . . C33 C 1.2352(17) 0.4254(6) 0.4282(6) 0.060(5) Uani 1 1 d . . . H33A H 1.2835 0.4014 0.4031 0.090 Uiso 1 1 calc R . . H33B H 1.1385 0.4345 0.4003 0.090 Uiso 1 1 calc R . . H33C H 1.2176 0.4128 0.4734 0.090 Uiso 1 1 calc R . . C34 C 1.2817(19) 0.5000(7) 0.4816(7) 0.070(5) Uani 1 1 d . . . H34A H 1.3709 0.5181 0.5038 0.084 Uiso 1 1 calc R . . H34B H 1.2365 0.4850 0.5195 0.084 Uiso 1 1 calc R . . C35 C 1.167(2) 0.5337(9) 0.4420(9) 0.092(9) Uani 1 1 d . . . H35A H 1.1388 0.5543 0.4791 0.111 Uiso 1 1 calc R . . H35B H 1.2273 0.5535 0.4150 0.111 Uiso 1 1 calc R . . C36 C 0.964(3) 0.5649(8) 0.3734(9) 0.120(10) Uani 1 1 d . . . H36A H 0.9751 0.5924 0.4041 0.180 Uiso 1 1 calc R . . H36B H 0.8583 0.5547 0.3656 0.180 Uiso 1 1 calc R . . H36C H 0.9943 0.5730 0.3284 0.180 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 As1 0.0241(6) 0.0211(7) 0.0184(4) 0.0003(5) 0.0035(4) 0.0026(5) Se1 0.0322(6) 0.0265(8) 0.0196(4) -0.0016(5) 0.0008(5) 0.0036(6) Se2 0.0251(6) 0.0370(9) 0.0300(5) 0.0009(5) 0.0046(5) 0.0086(6) Se3 0.0340(6) 0.0242(8) 0.0270(5) -0.0067(5) 0.0052(5) 0.0002(6) K1 0.0262(13) 0.0285(18) 0.0286(11) 0.0003(10) 0.0065(10) 0.0024(11) K2 0.0285(13) 0.0256(16) 0.0261(10) 0.0006(10) 0.0029(10) 0.0029(11) O1 0.027(5) 0.047(8) 0.051(5) -0.010(4) -0.002(4) -0.010(4) O2 0.050(5) 0.029(6) 0.033(4) 0.000(4) 0.002(4) 0.005(4) O3 0.038(5) 0.054(9) 0.059(5) 0.000(5) 0.033(4) 0.001(5) O4 0.037(5) 0.030(7) 0.056(5) -0.020(4) 0.001(4) 0.000(4) O5 0.054(6) 0.051(8) 0.028(4) 0.002(4) -0.002(4) 0.019(5) O6 0.036(5) 0.038(7) 0.034(4) -0.003(4) 0.018(4) -0.005(4) O7 0.037(5) 0.042(7) 0.040(4) 0.001(4) -0.004(4) -0.001(4) O8 0.038(5) 0.029(6) 0.035(4) -0.005(4) 0.011(4) 0.014(4) O9 0.030(5) 0.036(7) 0.037(4) 0.004(4) 0.014(4) -0.009(4) O10 0.030(4) 0.045(6) 0.021(3) 0.000(4) 0.002(3) 0.007(4) O11 0.033(5) 0.044(7) 0.024(3) 0.005(3) 0.009(4) 0.004(4) O12 0.035(5) 0.039(7) 0.039(4) 0.006(4) 0.005(4) -0.014(4) O13 0.027(5) 0.044(7) 0.043(4) 0.016(4) 0.005(4) 0.003(4) O14 0.070(7) 0.063(11) 0.093(7) -0.019(7) 0.021(6) -0.001(7) O15 0.26(2) 0.19(2) 0.101(10) -0.082(11) -0.086(13) 0.169(18) C1 0.022(6) 0.027(8) 0.016(4) -0.002(4) -0.001(4) -0.003(5) C2 0.025(6) 0.036(9) 0.030(5) 0.004(5) 0.003(5) 0.005(6) C3 0.056(9) 0.026(9) 0.034(6) 0.013(5) -0.001(6) -0.010(7) C4 0.042(8) 0.076(13) 0.020(5) 0.004(6) -0.003(6) -0.016(8) C5 0.040(7) 0.041(10) 0.029(5) 0.007(5) 0.002(5) -0.011(7) C6 0.028(6) 0.035(8) 0.018(4) 0.011(5) 0.003(4) 0.002(6) C7 0.013(6) 0.065(14) 0.068(8) -0.022(8) -0.001(6) 0.001(7) C8 0.044(9) 0.078(15) 0.048(7) -0.021(8) -0.015(7) 0.028(9) C9 0.084(11) 0.051(12) 0.029(6) 0.006(6) -0.001(7) 0.004(10) C10 0.127(14) 0.043(12) 0.034(6) -0.017(6) 0.046(8) -0.027(11) C11 0.043(9) 0.046(14) 0.115(12) 0.005(9) 0.047(9) 0.001(8) C12 0.028(8) 0.045(14) 0.117(12) -0.026(10) 0.001(9) 0.008(8) C13 0.029(7) 0.048(12) 0.068(9) -0.028(8) -0.011(7) 0.011(7) C14 0.040(8) 0.084(14) 0.028(6) -0.007(7) -0.001(6) 0.034(9) C15 0.072(11) 0.043(12) 0.047(7) 0.010(6) 0.027(8) 0.025(9) C16 0.090(12) 0.033(11) 0.037(6) -0.013(6) 0.032(8) -0.001(8) C17 0.033(7) 0.056(13) 0.065(8) -0.027(7) 0.029(7) -0.016(8) C18 0.023(7) 0.055(13) 0.070(8) -0.028(8) 0.028(7) -0.015(7) C19 0.063(9) 0.015(8) 0.030(6) 0.000(5) -0.002(6) 0.019(6) C20 0.050(8) 0.020(8) 0.033(6) 0.000(5) -0.003(6) 0.002(6) C21 0.030(7) 0.066(12) 0.020(5) 0.008(5) 0.021(5) 0.005(7) C22 0.032(7) 0.070(12) 0.021(5) 0.008(6) 0.010(5) -0.005(7) C23 0.029(6) 0.040(9) 0.045(6) 0.000(6) 0.002(5) -0.005(7) C24 0.027(6) 0.052(10) 0.038(6) -0.023(6) -0.012(6) 0.004(6) C25 0.050(8) 0.036(9) 0.015(4) -0.002(5) -0.002(5) -0.005(6) C26 0.046(7) 0.037(10) 0.022(5) -0.014(5) 0.010(5) 0.000(7) C27 0.041(8) 0.042(11) 0.040(6) 0.004(6) 0.026(6) 0.015(7) C28 0.032(7) 0.043(11) 0.044(6) 0.011(6) 0.019(6) 0.000(6) C29 0.040(8) 0.029(10) 0.057(7) -0.005(6) 0.002(7) -0.016(7) C30 0.041(8) 0.041(10) 0.047(7) 0.002(6) -0.005(7) -0.017(7) C31 0.050(9) 0.15(2) 0.040(7) 0.012(9) -0.009(7) 0.046(11) C32 0.033(7) 0.037(9) 0.028(5) 0.003(5) 0.011(5) 0.008(6) C33 0.082(11) 0.066(14) 0.028(6) -0.003(6) -0.001(7) -0.031(10) C34 0.092(13) 0.057(15) 0.060(8) -0.016(8) 0.013(9) -0.027(11) C35 0.085(13) 0.12(2) 0.066(10) -0.039(11) 0.003(10) 0.062(14) C36 0.17(2) 0.10(2) 0.083(12) 0.002(12) -0.013(14) 0.085(18) _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 As1 C1 1.971(11) . ? As1 Se2 2.2843(16) . ? As1 Se3 2.2858(18) . ? As1 Se1 2.2988(13) . ? Se1 K2 3.373(3) . ? Se1 K1 3.384(3) . ? Se2 K1 3.519(2) . ? Se3 K2 3.452(2) . ? K1 O3 2.822(10) . ? K1 O1 2.890(7) . ? K1 O5 2.916(9) . ? K1 O4 2.986(9) . ? K1 O2 3.009(6) . ? K1 O6 3.081(10) . ? K2 O12 2.852(9) . ? K2 O8 2.897(8) . ? K2 O10 2.935(6) . ? K2 O11 2.958(7) . ? K2 O9 2.997(8) . ? K2 O7 3.100(9) . ? O1 C7 1.403(13) . ? O1 C18 1.412(18) . ? O2 C8 1.414(15) . ? O2 C9 1.425(18) . ? O3 C11 1.401(15) . ? O3 C10 1.438(13) . ? O4 C13 1.413(14) . ? O4 C12 1.41(2) . ? O5 C15 1.376(18) . ? O5 C14 1.418(16) . ? O6 C17 1.412(15) . ? O6 C16 1.415(13) . ? O7 C30 1.398(15) . ? O7 C19 1.458(14) . ? O8 C20 1.413(14) . ? O8 C21 1.424(13) . ? O9 C23 1.411(15) . ? O9 C22 1.414(12) . ? O10 C24 1.426(13) . ? O10 C25 1.427(12) . ? O11 C27 1.394(13) . ? O11 C26 1.417(14) . ? O12 C28 1.409(13) . ? O12 C29 1.413(14) . ? O13 C32 1.396(13) . ? O13 C31 1.398(15) . ? O14 C34 1.40(2) . ? O14 C33 1.411(19) . ? O15 C35 1.127(17) . ? O15 C36 1.41(2) . ? C1 C6 1.366(14) . ? C1 C2 1.410(16) . ? C2 C3 1.382(16) . ? C3 C4 1.387(18) . ? C4 C5 1.39(2) . ? C5 C6 1.369(16) . ? C7 C8 1.51(2) . ? C9 C10 1.477(19) . ? C11 C12 1.474(18) . ? C13 C14 1.52(2) . ? C15 C16 1.495(19) . ? C17 C18 1.507(16) . ? C19 C20 1.452(18) . ? C21 C22 1.505(19) . ? C23 C24 1.501(15) . ? C25 C26 1.481(16) . ? C27 C28 1.505(18) . ? C29 C30 1.529(17) . ? C32 C32 1.51(2) 3_767 ? C34 C35 1.53(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 Se2 107.7(3) . . ? C1 As1 Se3 104.3(3) . . ? Se2 As1 Se3 115.27(6) . . ? C1 As1 Se1 103.8(2) . . ? Se2 As1 Se1 112.14(6) . . ? Se3 As1 Se1 112.48(7) . . ? As1 Se1 K2 89.98(6) . . ? As1 Se1 K1 87.94(6) . . ? K2 Se1 K1 169.75(7) . . ? As1 Se2 K1 84.91(6) . . ? As1 Se3 K2 88.24(6) . . ? O3 K1 O1 114.1(3) . . ? O3 K1 O5 114.6(3) . . ? O1 K1 O5 110.0(3) . . ? O3 K1 O4 58.5(3) . . ? O1 K1 O4 142.5(3) . . ? O5 K1 O4 56.9(3) . . ? O3 K1 O2 58.1(2) . . ? O1 K1 O2 56.3(3) . . ? O5 K1 O2 139.5(3) . . ? O4 K1 O2 108.3(2) . . ? O3 K1 O6 142.5(3) . . ? O1 K1 O6 55.6(2) . . ? O5 K1 O6 54.9(3) . . ? O4 K1 O6 105.7(3) . . ? O2 K1 O6 104.3(2) . . ? O3 K1 Se1 95.7(2) . . ? O1 K1 Se1 80.9(2) . . ? O5 K1 Se1 137.56(18) . . ? O4 K1 Se1 134.0(2) . . ? O2 K1 Se1 81.32(18) . . ? O6 K1 Se1 115.42(19) . . ? O3 K1 Se2 101.7(2) . . ? O1 K1 Se2 133.7(2) . . ? O5 K1 Se2 77.95(17) . . ? O4 K1 Se2 81.14(16) . . ? O2 K1 Se2 140.9(2) . . ? O6 K1 Se2 109.44(14) . . ? Se1 K1 Se2 66.81(6) . . ? O12 K2 O8 112.5(3) . . ? O12 K2 O10 114.2(2) . . ? O8 K2 O10 113.0(2) . . ? O12 K2 O11 57.7(2) . . ? O8 K2 O11 142.8(2) . . ? O10 K2 O11 57.1(2) . . ? O12 K2 O9 142.3(3) . . ? O8 K2 O9 56.4(2) . . ? O10 K2 O9 57.1(2) . . ? O11 K2 O9 107.1(2) . . ? O12 K2 O7 56.6(3) . . ? O8 K2 O7 56.3(2) . . ? O10 K2 O7 141.4(2) . . ? O11 K2 O7 106.8(2) . . ? O9 K2 O7 105.2(2) . . ? O12 K2 Se1 93.1(2) . . ? O8 K2 Se1 138.43(18) . . ? O10 K2 Se1 82.37(18) . . ? O11 K2 Se1 78.41(18) . . ? O9 K2 Se1 119.0(2) . . ? O7 K2 Se1 132.01(17) . . ? O12 K2 Se3 87.94(15) . . ? O8 K2 Se3 80.39(14) . . ? O10 K2 Se3 144.1(2) . . ? O11 K2 Se3 130.25(17) . . ? O9 K2 Se3 120.83(15) . . ? O7 K2 Se3 74.24(15) . . ? Se1 K2 Se3 67.88(5) . . ? C7 O1 C18 110.7(9) . . ? C7 O1 K1 122.2(8) . . ? C18 O1 K1 123.1(6) . . ? C8 O2 C9 112.1(12) . . ? C8 O2 K1 106.7(7) . . ? C9 O2 K1 105.0(5) . . ? C11 O3 C10 114.2(11) . . ? C11 O3 K1 119.0(9) . . ? C10 O3 K1 120.0(8) . . ? C13 O4 C12 111.8(10) . . ? C13 O4 K1 103.7(7) . . ? C12 O4 K1 103.7(8) . . ? C15 O5 C14 112.6(11) . . ? C15 O5 K1 124.7(7) . . ? C14 O5 K1 119.8(8) . . ? C17 O6 C16 111.1(10) . . ? C17 O6 K1 102.9(8) . . ? C16 O6 K1 108.7(7) . . ? C30 O7 C19 112.0(8) . . ? C30 O7 K2 104.2(7) . . ? C19 O7 K2 104.7(7) . . ? C20 O8 C21 112.8(10) . . ? C20 O8 K2 122.2(7) . . ? C21 O8 K2 120.9(6) . . ? C23 O9 C22 110.6(10) . . ? C23 O9 K2 109.4(7) . . ? C22 O9 K2 106.9(6) . . ? C24 O10 C25 113.3(7) . . ? C24 O10 K2 118.9(5) . . ? C25 O10 K2 118.9(6) . . ? C27 O11 C26 112.1(10) . . ? C27 O11 K2 103.8(6) . . ? C26 O11 K2 109.2(7) . . ? C28 O12 C29 112.6(10) . . ? C28 O12 K2 120.3(7) . . ? C29 O12 K2 123.6(7) . . ? C32 O13 C31 111.5(10) . . ? C34 O14 C33 115.3(13) . . ? C35 O15 C36 125(2) . . ? C6 C1 C2 120.0(11) . . ? C6 C1 As1 121.2(9) . . ? C2 C1 As1 118.7(9) . . ? C3 C2 C1 117.9(12) . . ? C2 C3 C4 122.6(14) . . ? C5 C4 C3 117.2(13) . . ? C6 C5 C4 121.8(14) . . ? C1 C6 C5 120.4(13) . . ? O1 C7 C8 107.0(10) . . ? O2 C8 C7 108.2(12) . . ? O2 C9 C10 108.4(14) . . ? O3 C10 C9 110.7(10) . . ? O3 C11 C12 110.6(13) . . ? O4 C12 C11 108.6(11) . . ? O4 C13 C14 109.0(9) . . ? O5 C14 C13 109.1(11) . . ? O5 C15 C16 109.4(13) . . ? O6 C16 C15 109.6(11) . . ? O6 C17 C18 108.8(10) . . ? O1 C18 C17 108.9(9) . . ? C20 C19 O7 109.4(8) . . ? O8 C20 C19 111.1(11) . . ? O8 C21 C22 109.7(11) . . ? O9 C22 C21 107.5(11) . . ? O9 C23 C24 108.6(11) . . ? O10 C24 C23 109.8(8) . . ? O10 C25 C26 109.6(7) . . ? O11 C26 C25 109.3(10) . . ? O11 C27 C28 109.6(11) . . ? O12 C28 C27 108.2(11) . . ? O12 C29 C30 109.3(11) . . ? O7 C30 C29 109.5(9) . . ? O13 C32 C32 108.7(13) . 3_767 ? O14 C34 C35 114.3(12) . . ? O15 C35 C34 133(2) . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 0.617 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.118 data_4 _database_code_depnum_ccdc_archive 'CCDC 664251' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H162.67 As6 Na12 O31 Se18' _chemical_formula_weight 4031.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 32.3388(19) _cell_length_b 32.3388(19) _cell_length_c 12.6601(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11466.1(11) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15876 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 26.98 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5894 _exptl_absorpt_coefficient_mu 5.677 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15805 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4952 _reflns_number_gt 3564 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. # SQUEEZE RESULTS (APPEND TO CIF) #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons 1 0.000 0.000 -0.003 553.8 56.5 2 0.333 0.667 0.671 554.7 56.4 3 0.667 0.333 0.337 554.7 56.4 #_platon_squeeze_details three molecules of thf and one molecule of hexane are disordered around a three-fold axis. attempts to refine disordered thf as noncoordinating 15-cr-5 failed. Total Potential Solvent Accessible Void Vol 1667.4 Ang3 Electron Count / Cell = 169 correction for unallocated electron density was made using the squeeze option in the programme Platon by a.l. spek 2006. ; _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^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4952 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.797 _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 As1 As 0.489805(19) 0.118735(19) 0.96765(4) 0.02292(13) Uani 1 1 d . . . Se1 Se 0.419649(19) 0.11047(2) 0.90470(4) 0.02606(14) Uani 1 1 d . . . Se2 Se 0.50624(2) 0.065054(19) 0.88956(4) 0.02670(14) Uani 1 1 d . . . Se3 Se 0.55177(2) 0.19601(2) 0.95219(4) 0.02776(14) Uani 1 1 d . . . Na1 Na 0.46200(8) 0.08873(8) 0.69747(15) 0.0279(5) Uani 1 1 d . . . Na2 Na 0.47976(8) 0.21249(8) 0.83423(17) 0.0312(5) Uani 1 1 d . . . O1 O 0.54671(15) 0.13135(14) 0.6300(3) 0.0305(9) Uani 1 1 d . . . O2 O 0.48204(14) 0.03427(14) 0.5936(3) 0.0309(9) Uani 1 1 d . . . O3 O 0.39244(15) 0.01108(16) 0.6470(3) 0.0370(9) Uani 1 1 d . . . O4 O 0.40943(15) 0.09908(15) 0.5785(3) 0.0342(9) Uani 1 1 d . . . O5 O 0.49360(14) 0.17804(15) 0.6629(3) 0.0306(9) Uani 1 1 d . . . C1 C 0.4815(2) 0.1034(2) 1.1194(4) 0.0273(11) Uani 1 1 d . . . C2 C 0.4609(2) 0.0568(2) 1.1508(5) 0.0398(15) Uani 1 1 d . . . H2A H 0.4517 0.0322 1.0998 0.048 Uiso 1 1 calc R . . C3 C 0.4534(2) 0.0455(3) 1.2587(5) 0.0495(18) Uani 1 1 d . . . H3A H 0.4380 0.0131 1.2809 0.059 Uiso 1 1 calc R . . C4 C 0.4686(3) 0.0817(3) 1.3322(5) 0.054(2) Uani 1 1 d . . . H4A H 0.4644 0.0743 1.4054 0.064 Uiso 1 1 calc R . . C5 C 0.4897(3) 0.1284(3) 1.3000(5) 0.0484(18) Uani 1 1 d . . . H5A H 0.4995 0.1531 1.3509 0.058 Uiso 1 1 calc R . . C6 C 0.4967(3) 0.1394(3) 1.1937(4) 0.0385(14) Uani 1 1 d . . . H6A H 0.5119 0.1718 1.1716 0.046 Uiso 1 1 calc R . . C7 C 0.5439(2) 0.2032(2) 0.6453(4) 0.0313(12) Uani 1 1 d . . . H7A H 0.5604 0.2109 0.7144 0.038 Uiso 1 1 calc R . . H7B H 0.5529 0.2337 0.6093 0.038 Uiso 1 1 calc R . . C8 C 0.5608(2) 0.1759(2) 0.5803(4) 0.0331(13) Uani 1 1 d . . . H8A H 0.5468 0.1705 0.5086 0.040 Uiso 1 1 calc R . . H8B H 0.5960 0.1945 0.5736 0.040 Uiso 1 1 calc R . . C9 C 0.5584(2) 0.1013(2) 0.5686(4) 0.0299(12) Uani 1 1 d . . . H9A H 0.5931 0.1133 0.5725 0.036 Uiso 1 1 calc R . . H9B H 0.5498 0.1017 0.4937 0.036 Uiso 1 1 calc R . . C10 C 0.5316(2) 0.0521(2) 0.6106(4) 0.0282(12) Uani 1 1 d . . . H10A H 0.5417 0.0315 0.5740 0.034 Uiso 1 1 calc R . . H10B H 0.5380 0.0520 0.6870 0.034 Uiso 1 1 calc R . . C11 C 0.4524(2) -0.0103(2) 0.6447(5) 0.0337(13) Uani 1 1 d . . . H11A H 0.4567 -0.0066 0.7222 0.040 Uiso 1 1 calc R . . H11B H 0.4608 -0.0343 0.6209 0.040 Uiso 1 1 calc R . . C12 C 0.4014(2) -0.0260(2) 0.6159(5) 0.0391(14) Uani 1 1 d . . . H12A H 0.3966 -0.0315 0.5388 0.047 Uiso 1 1 calc R . . H12B H 0.3793 -0.0560 0.6529 0.047 Uiso 1 1 calc R . . C13 C 0.3593(2) 0.0151(2) 0.5784(5) 0.0424(15) Uani 1 1 d . . . H13A H 0.3264 -0.0115 0.5912 0.051 Uiso 1 1 calc R . . H13B H 0.3676 0.0140 0.5036 0.051 Uiso 1 1 calc R . . C14 C 0.3622(2) 0.0618(2) 0.6018(5) 0.0388(14) Uani 1 1 d . . . H14A H 0.3388 0.0654 0.5581 0.047 Uiso 1 1 calc R . . H14B H 0.3548 0.0632 0.6771 0.047 Uiso 1 1 calc R . . C15 C 0.4152(2) 0.1458(2) 0.5910(5) 0.0352(13) Uani 1 1 d . . . H15A H 0.4043 0.1488 0.6620 0.042 Uiso 1 1 calc R . . H15B H 0.3958 0.1508 0.5377 0.042 Uiso 1 1 calc R . . C16 C 0.4667(2) 0.1823(2) 0.5773(4) 0.0318(12) Uani 1 1 d . . . H16A H 0.4785 0.1772 0.5091 0.038 Uiso 1 1 calc R . . H16B H 0.4707 0.2146 0.5769 0.038 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 As1 0.0247(3) 0.0263(3) 0.0201(2) -0.00137(19) -0.00115(19) 0.0145(2) Se1 0.0251(3) 0.0286(3) 0.0270(3) -0.0016(2) -0.0022(2) 0.0152(2) Se2 0.0268(3) 0.0279(3) 0.0281(3) -0.0031(2) -0.0009(2) 0.0157(2) Se3 0.0278(3) 0.0267(3) 0.0289(3) -0.0017(2) -0.0027(2) 0.0136(2) Na1 0.0298(12) 0.0303(12) 0.0256(10) -0.0030(8) -0.0022(8) 0.0166(10) Na2 0.0316(12) 0.0302(12) 0.0313(11) 0.0031(9) -0.0013(9) 0.0150(10) O1 0.037(2) 0.028(2) 0.0269(18) -0.0007(15) 0.0038(16) 0.0172(18) O2 0.028(2) 0.034(2) 0.0303(19) -0.0041(16) -0.0047(16) 0.0148(18) O3 0.035(2) 0.039(2) 0.041(2) -0.0088(18) -0.0042(18) 0.021(2) O4 0.035(2) 0.033(2) 0.040(2) -0.0080(17) -0.0048(17) 0.0204(19) O5 0.030(2) 0.033(2) 0.0299(19) 0.0010(16) -0.0019(16) 0.0170(18) C1 0.028(3) 0.038(3) 0.022(2) 0.002(2) -0.001(2) 0.020(3) C2 0.034(3) 0.044(4) 0.029(3) 0.001(3) -0.007(2) 0.011(3) C3 0.034(4) 0.064(5) 0.037(3) 0.016(3) -0.004(3) 0.014(3) C4 0.041(4) 0.102(7) 0.022(3) 0.019(3) 0.008(3) 0.039(4) C5 0.056(4) 0.074(5) 0.026(3) -0.007(3) -0.005(3) 0.040(4) C6 0.052(4) 0.050(4) 0.027(3) -0.002(3) -0.002(3) 0.035(3) C7 0.031(3) 0.032(3) 0.028(3) 0.002(2) 0.000(2) 0.013(3) C8 0.032(3) 0.035(3) 0.031(3) 0.002(2) 0.002(2) 0.016(3) C9 0.029(3) 0.038(3) 0.029(3) -0.002(2) 0.003(2) 0.021(3) C10 0.030(3) 0.036(3) 0.025(2) -0.006(2) -0.004(2) 0.021(3) C11 0.033(3) 0.030(3) 0.035(3) -0.006(2) -0.002(2) 0.013(3) C12 0.031(3) 0.034(3) 0.048(3) -0.010(3) -0.002(3) 0.013(3) C13 0.032(3) 0.039(4) 0.052(4) -0.009(3) -0.012(3) 0.015(3) C14 0.021(3) 0.046(4) 0.050(4) -0.007(3) -0.008(3) 0.018(3) C15 0.043(4) 0.039(3) 0.031(3) -0.015(2) -0.011(2) 0.026(3) C16 0.040(3) 0.030(3) 0.027(3) -0.003(2) -0.007(2) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 1.969(5) . ? As1 Se2 2.2795(8) . ? As1 Se1 2.2907(8) . ? As1 Se3 2.3001(8) . ? As1 Na1 3.546(2) . ? Se1 Na2 3.008(2) . ? Se1 Na1 3.196(2) . ? Se2 Na2 2.955(2) 18_546 ? Se2 Na1 3.105(2) . ? Se3 Na2 3.030(2) . ? Se3 Na2 3.146(2) 18_546 ? Na1 O4 2.416(5) . ? Na1 O3 2.475(5) . ? Na1 O1 2.521(5) . ? Na1 O2 2.528(4) . ? Na1 O5 2.574(5) . ? Na1 Na2 4.129(3) . ? Na2 O5 2.578(4) . ? Na2 Se2 2.954(2) 17_556 ? Na2 O1 2.999(4) 17_556 ? Na2 Se3 3.146(2) 17_556 ? O1 C8 1.423(7) . ? O1 C9 1.434(7) . ? O1 Na2 2.999(4) 18_546 ? O2 C10 1.422(7) . ? O2 C11 1.426(7) . ? O3 C12 1.422(8) . ? O3 C13 1.437(8) . ? O4 C14 1.425(8) . ? O4 C15 1.434(7) . ? O5 C7 1.426(7) . ? O5 C16 1.438(7) . ? C1 C2 1.366(9) . ? C1 C6 1.383(8) . ? C2 C3 1.403(9) . ? C2 H2A 0.9500 . ? C3 C4 1.381(12) . ? C3 H3A 0.9500 . ? C4 C5 1.370(12) . ? C4 H4A 0.9500 . ? C5 C6 1.382(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.494(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.481(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.508(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.493(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.493(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 Se2 106.59(17) . . ? C1 As1 Se1 107.93(16) . . ? Se2 As1 Se1 110.77(3) . . ? C1 As1 Se3 106.97(17) . . ? Se2 As1 Se3 112.48(3) . . ? Se1 As1 Se3 111.79(3) . . ? C1 As1 Na1 152.65(18) . . ? Se2 As1 Na1 59.81(4) . . ? Se1 As1 Na1 62.07(4) . . ? Se3 As1 Na1 100.32(4) . . ? As1 Se1 Na2 85.18(5) . . ? As1 Se1 Na1 78.64(4) . . ? Na2 Se1 Na1 83.38(6) . . ? As1 Se2 Na2 87.60(5) . 18_546 ? As1 Se2 Na1 80.81(4) . . ? Na2 Se2 Na1 89.24(6) 18_546 . ? As1 Se3 Na2 84.51(5) . . ? As1 Se3 Na2 82.76(5) . 18_546 ? Na2 Se3 Na2 118.560(17) . 18_546 ? O4 Na1 O3 68.55(15) . . ? O4 Na1 O1 111.13(16) . . ? O3 Na1 O1 130.92(16) . . ? O4 Na1 O2 102.45(14) . . ? O3 Na1 O2 65.07(14) . . ? O1 Na1 O2 67.53(14) . . ? O4 Na1 O5 69.56(14) . . ? O3 Na1 O5 138.08(16) . . ? O1 Na1 O5 67.40(14) . . ? O2 Na1 O5 126.64(15) . . ? O4 Na1 Se2 164.80(13) . . ? O3 Na1 Se2 104.42(13) . . ? O1 Na1 Se2 83.77(11) . . ? O2 Na1 Se2 85.72(11) . . ? O5 Na1 Se2 115.88(11) . . ? O4 Na1 Se1 94.16(11) . . ? O3 Na1 Se1 99.38(12) . . ? O1 Na1 Se1 128.73(12) . . ? O2 Na1 Se1 150.15(12) . . ? O5 Na1 Se1 82.32(10) . . ? Se2 Na1 Se1 73.28(4) . . ? O4 Na1 As1 131.52(12) . . ? O3 Na1 As1 120.27(12) . . ? O1 Na1 As1 96.87(11) . . ? O2 Na1 As1 125.03(11) . . ? O5 Na1 As1 87.31(10) . . ? Se2 Na1 As1 39.38(3) . . ? Se1 Na1 As1 39.29(3) . . ? O4 Na1 Na2 83.89(11) . . ? O3 Na1 Na2 135.00(13) . . ? O1 Na1 Na2 91.47(11) . . ? O2 Na1 Na2 158.98(12) . . ? O5 Na1 Na2 36.77(9) . . ? Se2 Na1 Na2 93.02(6) . . ? Se1 Na1 Na2 46.36(4) . . ? As1 Na1 Na2 55.74(4) . . ? O5 Na2 Se2 102.41(11) . 17_556 ? O5 Na2 O1 178.56(15) . 17_556 ? Se2 Na2 O1 78.87(10) 17_556 17_556 ? O5 Na2 Se1 86.11(11) . . ? Se2 Na2 Se1 95.48(7) 17_556 . ? O1 Na2 Se1 93.13(10) 17_556 . ? O5 Na2 Se3 91.37(11) . . ? Se2 Na2 Se3 164.42(8) 17_556 . ? O1 Na2 Se3 87.28(9) 17_556 . ? Se1 Na2 Se3 78.04(5) . . ? O5 Na2 Se3 85.46(11) . 17_556 ? Se2 Na2 Se3 77.17(5) 17_556 17_556 ? O1 Na2 Se3 95.49(10) 17_556 17_556 ? Se1 Na2 Se3 167.34(8) . 17_556 ? Se3 Na2 Se3 111.58(7) . 17_556 ? O5 Na2 Na1 36.70(10) . . ? Se2 Na2 Na1 109.45(7) 17_556 . ? O1 Na2 Na1 142.30(11) 17_556 . ? Se1 Na2 Na1 50.26(5) . . ? Se3 Na2 Na1 77.45(6) . . ? Se3 Na2 Na1 122.15(7) 17_556 . ? C8 O1 C9 112.8(4) . . ? C8 O1 Na1 114.4(3) . . ? C9 O1 Na1 113.3(3) . . ? C8 O1 Na2 110.3(3) . 18_546 ? C9 O1 Na2 104.2(3) . 18_546 ? Na1 O1 Na2 100.58(13) . 18_546 ? C10 O2 C11 113.1(4) . . ? C10 O2 Na1 105.6(3) . . ? C11 O2 Na1 101.0(3) . . ? C12 O3 C13 112.7(5) . . ? C12 O3 Na1 117.5(3) . . ? C13 O3 Na1 113.9(4) . . ? C14 O4 C15 112.9(5) . . ? C14 O4 Na1 106.5(3) . . ? C15 O4 Na1 110.3(3) . . ? C7 O5 C16 113.6(4) . . ? C7 O5 Na1 111.5(3) . . ? C16 O5 Na1 108.4(3) . . ? C7 O5 Na2 106.3(3) . . ? C16 O5 Na2 110.4(3) . . ? Na1 O5 Na2 106.52(15) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 As1 119.4(4) . . ? C6 C1 As1 120.3(4) . . ? C1 C2 C3 119.7(6) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 119.5(7) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 120.2(6) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.2(7) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 120.0(7) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? O5 C7 C8 113.5(5) . . ? O5 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? O5 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O1 C8 C7 109.2(5) . . ? O1 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O1 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? O1 C9 C10 108.9(4) . . ? O1 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O1 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O2 C10 C9 108.4(4) . . ? O2 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O2 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? O2 C11 C12 107.4(5) . . ? O2 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O2 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O3 C12 C11 107.4(5) . . ? O3 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? O3 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? O3 C13 C14 107.4(5) . . ? O3 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? O3 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? O4 C14 C13 108.3(5) . . ? O4 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? O4 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? O4 C15 C16 109.1(5) . . ? O4 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O4 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O5 C16 C15 109.0(5) . . ? O5 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? O5 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 As1 Se1 Na2 123.53(19) . . . . ? Se2 As1 Se1 Na2 -120.13(5) . . . . ? Se3 As1 Se1 Na2 6.17(5) . . . . ? Na1 As1 Se1 Na2 -84.20(6) . . . . ? C1 As1 Se1 Na1 -152.26(19) . . . . ? Se2 As1 Se1 Na1 -35.93(5) . . . . ? Se3 As1 Se1 Na1 90.37(5) . . . . ? C1 As1 Se2 Na2 -116.36(18) . . . 18_546 ? Se1 As1 Se2 Na2 126.47(5) . . . 18_546 ? Se3 As1 Se2 Na2 0.56(5) . . . 18_546 ? Na1 As1 Se2 Na2 89.62(6) . . . 18_546 ? C1 As1 Se2 Na1 154.02(18) . . . . ? Se1 As1 Se2 Na1 36.85(5) . . . . ? Se3 As1 Se2 Na1 -89.06(5) . . . . ? C1 As1 Se3 Na2 -124.07(17) . . . . ? Se2 As1 Se3 Na2 119.23(5) . . . . ? Se1 As1 Se3 Na2 -6.13(5) . . . . ? Na1 As1 Se3 Na2 57.78(6) . . . . ? C1 As1 Se3 Na2 116.17(17) . . . 18_546 ? Se2 As1 Se3 Na2 -0.53(5) . . . 18_546 ? Se1 As1 Se3 Na2 -125.89(5) . . . 18_546 ? Na1 As1 Se3 Na2 -61.98(6) . . . 18_546 ? As1 Se2 Na1 O4 -60.1(5) . . . . ? Na2 Se2 Na1 O4 -147.8(5) 18_546 . . . ? As1 Se2 Na1 O3 -120.47(12) . . . . ? Na2 Se2 Na1 O3 151.84(12) 18_546 . . . ? As1 Se2 Na1 O1 108.82(10) . . . . ? Na2 Se2 Na1 O1 21.12(11) 18_546 . . . ? As1 Se2 Na1 O2 176.64(11) . . . . ? Na2 Se2 Na1 O2 88.95(11) 18_546 . . . ? As1 Se2 Na1 O5 47.68(12) . . . . ? Na2 Se2 Na1 O5 -40.01(13) 18_546 . . . ? As1 Se2 Na1 Se1 -24.81(3) . . . . ? Na2 Se2 Na1 Se1 -112.51(5) 18_546 . . . ? Na2 Se2 Na1 As1 -87.69(5) 18_546 . . . ? As1 Se2 Na1 Na2 17.67(4) . . . . ? Na2 Se2 Na1 Na2 -70.03(8) 18_546 . . . ? As1 Se1 Na1 O4 -163.87(12) . . . . ? Na2 Se1 Na1 O4 -77.48(12) . . . . ? As1 Se1 Na1 O3 127.21(12) . . . . ? Na2 Se1 Na1 O3 -146.40(13) . . . . ? As1 Se1 Na1 O1 -42.41(15) . . . . ? Na2 Se1 Na1 O1 43.98(15) . . . . ? As1 Se1 Na1 O2 72.0(2) . . . . ? Na2 Se1 Na1 O2 158.4(2) . . . . ? As1 Se1 Na1 O5 -95.16(10) . . . . ? Na2 Se1 Na1 O5 -8.77(10) . . . . ? As1 Se1 Na1 Se2 24.87(3) . . . . ? Na2 Se1 Na1 Se2 111.26(6) . . . . ? Na2 Se1 Na1 As1 86.39(5) . . . . ? As1 Se1 Na1 Na2 -86.39(5) . . . . ? C1 As1 Na1 O4 96.3(4) . . . . ? Se2 As1 Na1 O4 162.33(18) . . . . ? Se1 As1 Na1 O4 21.73(16) . . . . ? Se3 As1 Na1 O4 -87.57(17) . . . . ? C1 As1 Na1 O3 9.1(4) . . . . ? Se2 As1 Na1 O3 75.13(14) . . . . ? Se1 As1 Na1 O3 -65.47(14) . . . . ? Se3 As1 Na1 O3 -174.77(14) . . . . ? C1 As1 Na1 O1 -137.4(4) . . . . ? Se2 As1 Na1 O1 -71.40(11) . . . . ? Se1 As1 Na1 O1 148.00(12) . . . . ? Se3 As1 Na1 O1 38.70(11) . . . . ? C1 As1 Na1 O2 -70.1(4) . . . . ? Se2 As1 Na1 O2 -4.09(13) . . . . ? Se1 As1 Na1 O2 -144.69(15) . . . . ? Se3 As1 Na1 O2 106.01(14) . . . . ? C1 As1 Na1 O5 155.7(4) . . . . ? Se2 As1 Na1 O5 -138.24(11) . . . . ? Se1 As1 Na1 O5 81.15(10) . . . . ? Se3 As1 Na1 O5 -28.15(10) . . . . ? C1 As1 Na1 Se2 -66.0(4) . . . . ? Se1 As1 Na1 Se2 -140.60(5) . . . . ? Se3 As1 Na1 Se2 110.10(4) . . . . ? C1 As1 Na1 Se1 74.6(4) . . . . ? Se2 As1 Na1 Se1 140.60(5) . . . . ? Se3 As1 Na1 Se1 -109.30(3) . . . . ? C1 As1 Na1 Na2 135.5(4) . . . . ? Se2 As1 Na1 Na2 -158.49(6) . . . . ? Se1 As1 Na1 Na2 60.91(5) . . . . ? Se3 As1 Na1 Na2 -48.39(5) . . . . ? As1 Se1 Na2 O5 87.79(10) . . . . ? Na1 Se1 Na2 O5 8.70(10) . . . . ? As1 Se1 Na2 Se2 -170.10(5) . . . 17_556 ? Na1 Se1 Na2 Se2 110.81(6) . . . 17_556 ? As1 Se1 Na2 O1 -90.99(9) . . . 17_556 ? Na1 Se1 Na2 O1 -170.08(10) . . . 17_556 ? As1 Se1 Na2 Se3 -4.44(4) . . . . ? Na1 Se1 Na2 Se3 -83.53(5) . . . . ? As1 Se1 Na2 Se3 136.1(4) . . . 17_556 ? Na1 Se1 Na2 Se3 57.0(4) . . . 17_556 ? As1 Se1 Na2 Na1 79.09(4) . . . . ? As1 Se3 Na2 O5 -81.31(11) . . . . ? Na2 Se3 Na2 O5 -2.64(14) 18_546 . . . ? As1 Se3 Na2 Se2 71.1(3) . . . 17_556 ? Na2 Se3 Na2 Se2 149.7(3) 18_546 . . 17_556 ? As1 Se3 Na2 O1 98.20(9) . . . 17_556 ? Na2 Se3 Na2 O1 176.87(9) 18_546 . . 17_556 ? As1 Se3 Na2 Se1 4.43(4) . . . . ? Na2 Se3 Na2 Se1 83.09(8) 18_546 . . . ? As1 Se3 Na2 Se3 -166.97(7) . . . 17_556 ? Na2 Se3 Na2 Se3 -88.30(8) 18_546 . . 17_556 ? As1 Se3 Na2 Na1 -47.09(4) . . . . ? Na2 Se3 Na2 Na1 31.58(8) 18_546 . . . ? O4 Na1 Na2 O5 -63.67(19) . . . . ? O3 Na1 Na2 O5 -114.8(2) . . . . ? O1 Na1 Na2 O5 47.43(18) . . . . ? O2 Na1 Na2 O5 45.3(4) . . . . ? Se2 Na1 Na2 O5 131.27(17) . . . . ? Se1 Na1 Na2 O5 -165.38(17) . . . . ? As1 Na1 Na2 O5 144.74(17) . . . . ? O4 Na1 Na2 Se2 21.03(13) . . . 17_556 ? O3 Na1 Na2 Se2 -30.1(2) . . . 17_556 ? O1 Na1 Na2 Se2 132.13(11) . . . 17_556 ? O2 Na1 Na2 Se2 130.0(3) . . . 17_556 ? O5 Na1 Na2 Se2 84.70(16) . . . 17_556 ? Se2 Na1 Na2 Se2 -144.04(6) . . . 17_556 ? Se1 Na1 Na2 Se2 -80.68(7) . . . 17_556 ? As1 Na1 Na2 Se2 -130.56(7) . . . 17_556 ? O4 Na1 Na2 O1 118.0(2) . . . 17_556 ? O3 Na1 Na2 O1 66.9(3) . . . 17_556 ? O1 Na1 Na2 O1 -130.85(17) . . . 17_556 ? O2 Na1 Na2 O1 -132.9(3) . . . 17_556 ? O5 Na1 Na2 O1 -178.3(2) . . . 17_556 ? Se2 Na1 Na2 O1 -47.02(18) . . . 17_556 ? Se1 Na1 Na2 O1 16.34(16) . . . 17_556 ? As1 Na1 Na2 O1 -33.54(17) . . . 17_556 ? O4 Na1 Na2 Se1 101.71(12) . . . . ? O3 Na1 Na2 Se1 50.56(18) . . . . ? O1 Na1 Na2 Se1 -147.19(11) . . . . ? O2 Na1 Na2 Se1 -149.3(3) . . . . ? O5 Na1 Na2 Se1 165.38(17) . . . . ? Se2 Na1 Na2 Se1 -63.36(5) . . . . ? As1 Na1 Na2 Se1 -49.88(3) . . . . ? O4 Na1 Na2 Se3 -173.51(12) . . . . ? O3 Na1 Na2 Se3 135.34(18) . . . . ? O1 Na1 Na2 Se3 -62.41(10) . . . . ? O2 Na1 Na2 Se3 -64.5(3) . . . . ? O5 Na1 Na2 Se3 -109.84(17) . . . . ? Se2 Na1 Na2 Se3 21.42(5) . . . . ? Se1 Na1 Na2 Se3 84.78(5) . . . . ? As1 Na1 Na2 Se3 34.90(3) . . . . ? O4 Na1 Na2 Se3 -65.75(14) . . . 17_556 ? O3 Na1 Na2 Se3 -116.89(18) . . . 17_556 ? O1 Na1 Na2 Se3 45.35(13) . . . 17_556 ? O2 Na1 Na2 Se3 43.3(3) . . . 17_556 ? O5 Na1 Na2 Se3 -2.08(16) . . . 17_556 ? Se2 Na1 Na2 Se3 129.19(8) . . . 17_556 ? Se1 Na1 Na2 Se3 -167.45(10) . . . 17_556 ? As1 Na1 Na2 Se3 142.67(9) . . . 17_556 ? O4 Na1 O1 C8 37.5(4) . . . . ? O3 Na1 O1 C8 116.9(4) . . . . ? O2 Na1 O1 C8 132.7(4) . . . . ? O5 Na1 O1 C8 -18.0(3) . . . . ? Se2 Na1 O1 C8 -139.4(3) . . . . ? Se1 Na1 O1 C8 -76.7(4) . . . . ? As1 Na1 O1 C8 -102.2(3) . . . . ? Na2 Na1 O1 C8 -46.5(3) . . . . ? O4 Na1 O1 C9 -93.7(3) . . . . ? O3 Na1 O1 C9 -14.3(4) . . . . ? O2 Na1 O1 C9 1.5(3) . . . . ? O5 Na1 O1 C9 -149.2(4) . . . . ? Se2 Na1 O1 C9 89.4(3) . . . . ? Se1 Na1 O1 C9 152.1(3) . . . . ? As1 Na1 O1 C9 126.7(3) . . . . ? Na2 Na1 O1 C9 -177.7(3) . . . . ? O4 Na1 O1 Na2 155.72(14) . . . 18_546 ? O3 Na1 O1 Na2 -124.87(19) . . . 18_546 ? O2 Na1 O1 Na2 -109.11(15) . . . 18_546 ? O5 Na1 O1 Na2 100.23(14) . . . 18_546 ? Se2 Na1 O1 Na2 -21.17(10) . . . 18_546 ? Se1 Na1 O1 Na2 41.53(19) . . . 18_546 ? As1 Na1 O1 Na2 16.05(12) . . . 18_546 ? Na2 Na1 O1 Na2 71.71(11) . . . 18_546 ? O4 Na1 O2 C10 138.9(3) . . . . ? O3 Na1 O2 C10 -162.2(3) . . . . ? O1 Na1 O2 C10 30.9(3) . . . . ? O5 Na1 O2 C10 65.2(4) . . . . ? Se2 Na1 O2 C10 -54.1(3) . . . . ? Se1 Na1 O2 C10 -98.8(4) . . . . ? As1 Na1 O2 C10 -51.5(3) . . . . ? Na2 Na1 O2 C10 33.2(5) . . . . ? O4 Na1 O2 C11 -103.1(3) . . . . ? O3 Na1 O2 C11 -44.2(3) . . . . ? O1 Na1 O2 C11 148.9(3) . . . . ? O5 Na1 O2 C11 -176.8(3) . . . . ? Se2 Na1 O2 C11 63.9(3) . . . . ? Se1 Na1 O2 C11 19.2(4) . . . . ? As1 Na1 O2 C11 66.5(3) . . . . ? Na2 Na1 O2 C11 151.2(3) . . . . ? O4 Na1 O3 C12 133.4(4) . . . . ? O1 Na1 O3 C12 33.5(5) . . . . ? O2 Na1 O3 C12 17.4(4) . . . . ? O5 Na1 O3 C12 135.2(4) . . . . ? Se2 Na1 O3 C12 -60.8(4) . . . . ? Se1 Na1 O3 C12 -135.8(4) . . . . ? As1 Na1 O3 C12 -100.1(4) . . . . ? Na2 Na1 O3 C12 -170.3(4) . . . . ? O4 Na1 O3 C13 -1.5(4) . . . . ? O1 Na1 O3 C13 -101.4(4) . . . . ? O2 Na1 O3 C13 -117.5(4) . . . . ? O5 Na1 O3 C13 0.3(5) . . . . ? Se2 Na1 O3 C13 164.3(4) . . . . ? Se1 Na1 O3 C13 89.3(4) . . . . ? As1 Na1 O3 C13 125.0(4) . . . . ? Na2 Na1 O3 C13 54.8(5) . . . . ? O3 Na1 O4 C14 33.2(3) . . . . ? O1 Na1 O4 C14 160.2(3) . . . . ? O2 Na1 O4 C14 89.7(4) . . . . ? O5 Na1 O4 C14 -145.5(4) . . . . ? Se2 Na1 O4 C14 -31.6(7) . . . . ? Se1 Na1 O4 C14 -65.3(3) . . . . ? As1 Na1 O4 C14 -78.9(4) . . . . ? Na2 Na1 O4 C14 -110.6(3) . . . . ? O3 Na1 O4 C15 156.0(4) . . . . ? O1 Na1 O4 C15 -76.9(4) . . . . ? O2 Na1 O4 C15 -147.4(4) . . . . ? O5 Na1 O4 C15 -22.7(4) . . . . ? Se2 Na1 O4 C15 91.2(6) . . . . ? Se1 Na1 O4 C15 57.6(4) . . . . ? As1 Na1 O4 C15 44.0(4) . . . . ? Na2 Na1 O4 C15 12.3(4) . . . . ? O4 Na1 O5 C7 -136.5(3) . . . . ? O3 Na1 O5 C7 -138.4(3) . . . . ? O1 Na1 O5 C7 -11.6(3) . . . . ? O2 Na1 O5 C7 -45.9(4) . . . . ? Se2 Na1 O5 C7 59.0(3) . . . . ? Se1 Na1 O5 C7 126.1(3) . . . . ? As1 Na1 O5 C7 87.0(3) . . . . ? Na2 Na1 O5 C7 115.5(4) . . . . ? O4 Na1 O5 C16 -10.8(3) . . . . ? O3 Na1 O5 C16 -12.7(4) . . . . ? O1 Na1 O5 C16 114.1(3) . . . . ? O2 Na1 O5 C16 79.7(4) . . . . ? Se2 Na1 O5 C16 -175.3(3) . . . . ? Se1 Na1 O5 C16 -108.2(3) . . . . ? As1 Na1 O5 C16 -147.3(3) . . . . ? Na2 Na1 O5 C16 -118.8(4) . . . . ? O4 Na1 O5 Na2 108.00(18) . . . . ? O3 Na1 O5 Na2 106.1(2) . . . . ? O1 Na1 O5 Na2 -127.11(18) . . . . ? O2 Na1 O5 Na2 -161.46(16) . . . . ? Se2 Na1 O5 Na2 -56.54(17) . . . . ? Se1 Na1 O5 Na2 10.62(13) . . . . ? As1 Na1 O5 Na2 -28.53(13) . . . . ? Se2 Na2 O5 C7 135.0(3) 17_556 . . . ? O1 Na2 O5 C7 -72(7) 17_556 . . . ? Se1 Na2 O5 C7 -130.2(3) . . . . ? Se3 Na2 O5 C7 -52.3(3) . . . . ? Se3 Na2 O5 C7 59.3(3) 17_556 . . . ? Na1 Na2 O5 C7 -119.0(4) . . . . ? Se2 Na2 O5 C16 11.5(4) 17_556 . . . ? O1 Na2 O5 C16 164(7) 17_556 . . . ? Se1 Na2 O5 C16 106.2(3) . . . . ? Se3 Na2 O5 C16 -175.9(3) . . . . ? Se3 Na2 O5 C16 -64.3(3) 17_556 . . . ? Na1 Na2 O5 C16 117.4(4) . . . . ? Se2 Na2 O5 Na1 -105.98(13) 17_556 . . . ? O1 Na2 O5 Na1 47(7) 17_556 . . . ? Se1 Na2 O5 Na1 -11.22(13) . . . . ? Se3 Na2 O5 Na1 66.70(14) . . . . ? Se3 Na2 O5 Na1 178.24(13) 17_556 . . . ? Se2 As1 C1 C2 -35.1(5) . . . . ? Se1 As1 C1 C2 83.9(5) . . . . ? Se3 As1 C1 C2 -155.6(5) . . . . ? Na1 As1 C1 C2 20.4(7) . . . . ? Se2 As1 C1 C6 144.5(5) . . . . ? Se1 As1 C1 C6 -96.5(5) . . . . ? Se3 As1 C1 C6 24.0(5) . . . . ? Na1 As1 C1 C6 -160.0(4) . . . . ? C6 C1 C2 C3 2.6(10) . . . . ? As1 C1 C2 C3 -177.8(5) . . . . ? C1 C2 C3 C4 -2.5(10) . . . . ? C2 C3 C4 C5 1.8(11) . . . . ? C3 C4 C5 C6 -1.3(11) . . . . ? C4 C5 C6 C1 1.3(10) . . . . ? C2 C1 C6 C5 -2.0(10) . . . . ? As1 C1 C6 C5 178.4(5) . . . . ? C16 O5 C7 C8 -83.1(6) . . . . ? Na1 O5 C7 C8 39.6(5) . . . . ? Na2 O5 C7 C8 155.3(4) . . . . ? C9 O1 C8 C7 175.5(5) . . . . ? Na1 O1 C8 C7 44.1(5) . . . . ? Na2 O1 C8 C7 -68.4(5) 18_546 . . . ? O5 C7 C8 O1 -56.8(6) . . . . ? C8 O1 C9 C10 -165.0(5) . . . . ? Na1 O1 C9 C10 -33.0(5) . . . . ? Na2 O1 C9 C10 75.4(4) 18_546 . . . ? C11 O2 C10 C9 -171.3(4) . . . . ? Na1 O2 C10 C9 -61.8(4) . . . . ? O1 C9 C10 O2 65.6(5) . . . . ? C10 O2 C11 C12 -177.3(4) . . . . ? Na1 O2 C11 C12 70.3(4) . . . . ? C13 O3 C12 C11 147.4(5) . . . . ? Na1 O3 C12 C11 12.0(6) . . . . ? O2 C11 C12 O3 -56.8(6) . . . . ? C12 O3 C13 C14 -166.0(5) . . . . ? Na1 O3 C13 C14 -28.9(6) . . . . ? C15 O4 C14 C13 175.7(5) . . . . ? Na1 O4 C14 C13 -63.1(5) . . . . ? O3 C13 C14 O4 62.0(7) . . . . ? C14 O4 C15 C16 173.5(5) . . . . ? Na1 O4 C15 C16 54.5(5) . . . . ? C7 O5 C16 C15 166.2(5) . . . . ? Na1 O5 C16 C15 41.7(5) . . . . ? Na2 O5 C16 C15 -74.6(5) . . . . ? O4 C15 C16 O5 -66.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.742 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.111 data_5 _database_code_depnum_ccdc_archive 'CCDC 664252' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H19 As Na2 O4 Se3' _chemical_formula_weight 561.03 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 19.9887(15) _cell_length_b 6.9605(8) _cell_length_c 14.3162(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.304(13) _cell_angle_gamma 90.00 _cell_volume 1868.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.08 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 7.717 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'stoe ipds 1 on schneider rotary anode' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12655 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.90 _reflns_number_total 3623 _reflns_number_gt 2686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe expose' _computing_cell_refinement 'stoe expose' _computing_data_reduction 'stoe expose' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3623 _refine_ls_number_parameters 188 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.31186(4) 0.30434(9) 0.77699(5) 0.01693(19) Uani 1 1 d . . . Na1 Na 0.50001(16) -0.0168(4) 0.8736(2) 0.0269(7) Uani 1 1 d . . . Na2 Na 0.69084(18) 0.1810(4) 1.0296(3) 0.0372(8) Uani 1 1 d . . . Se1 Se 0.33085(4) -0.02089(10) 0.78580(6) 0.0237(2) Uani 1 1 d . . . Se2 Se 0.34634(4) 0.45542(10) 0.65938(6) 0.0245(2) Uani 1 1 d . . . Se3 Se 0.35411(5) 0.44369(11) 0.93174(6) 0.0300(2) Uani 1 1 d . . . O1 O 0.5103(3) 0.2255(7) 1.0017(4) 0.0304(12) Uani 1 1 d . . . H1A H 0.5564 0.2918 1.0225 0.036 Uiso 1 1 calc R . . H1B H 0.4715 0.3197 0.9805 0.036 Uiso 1 1 calc R . . O2 O 0.5000 -0.2609(10) 0.7500 0.0303(17) Uani 1 2 d SD . . H2B H 0.467(3) -0.335(10) 0.716(6) 0.036 Uiso 1 1 d D . . O3 O 0.5000 0.2029(11) 0.7500 0.0287(17) Uani 1 2 d SD . . H3B H 0.541(2) 0.252(12) 0.774(7) 0.034 Uiso 1 1 d D . . O4 O 0.6292(3) -0.0538(8) 0.9247(4) 0.0329(13) Uani 1 1 d . . . H4B H 0.6427 -0.1785 0.9576 0.039 Uiso 1 1 calc R . . H4C H 0.6428 -0.0538 0.8652 0.039 Uiso 1 1 calc R . . O5 O 0.8062(4) 0.1114(11) 1.0514(6) 0.0582(19) Uani 1 1 d . . . C1 C 0.2088(4) 0.3515(11) 0.7358(6) 0.0277(16) Uani 1 1 d . . . C2 C 0.1626(5) 0.2042(14) 0.7360(8) 0.047(2) Uani 1 1 d . . . H2A H 0.1802 0.0800 0.7559 0.057 Uiso 1 1 calc R . . C3 C 0.0901(6) 0.2411(18) 0.7065(11) 0.069(4) Uani 1 1 d . . . H3A H 0.0582 0.1417 0.7063 0.083 Uiso 1 1 calc R . . C4 C 0.0648(5) 0.4234(19) 0.6775(10) 0.067(3) Uani 1 1 d . . . H4A H 0.0157 0.4484 0.6578 0.080 Uiso 1 1 calc R . . C5 C 0.1109(6) 0.5684(17) 0.6773(10) 0.064(3) Uani 1 1 d . . . H5A H 0.0931 0.6925 0.6574 0.077 Uiso 1 1 calc R . . C6 C 0.1828(5) 0.5341(13) 0.7057(9) 0.046(3) Uani 1 1 d . . . H6A H 0.2142 0.6341 0.7048 0.055 Uiso 1 1 calc R . . C7 C 0.8243(6) -0.051(2) 1.0100(10) 0.071(3) Uani 1 1 d . . . H7A H 0.7987 -0.0538 0.9379 0.085 Uiso 1 1 calc R . . H7B H 0.8122 -0.1671 1.0394 0.085 Uiso 1 1 calc R . . C8 C 0.9033(8) -0.041(3) 1.0319(17) 0.123(7) Uani 1 1 d . . . H8A H 0.9281 -0.1423 1.0787 0.148 Uiso 1 1 calc R . . H8B H 0.9143 -0.0548 0.9707 0.148 Uiso 1 1 calc R . . C9 C 0.9250(8) 0.154(3) 1.0771(14) 0.112(7) Uani 1 1 d . . . H9A H 0.9498 0.1438 1.1492 0.134 Uiso 1 1 calc R . . H9B H 0.9566 0.2175 1.0474 0.134 Uiso 1 1 calc R . . C10 C 0.8580(7) 0.260(2) 1.0549(10) 0.079(4) Uani 1 1 d . . . H10A H 0.8612 0.3544 1.1073 0.095 Uiso 1 1 calc R . . H10B H 0.8455 0.3272 0.9909 0.095 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 As1 0.0241(4) 0.0129(3) 0.0160(4) 0.0007(3) 0.0098(3) 0.0001(2) Na1 0.0389(17) 0.0244(14) 0.0202(16) 0.0027(12) 0.0140(13) 0.0008(12) Na2 0.0455(19) 0.0261(16) 0.042(2) -0.0007(14) 0.0171(16) 0.0026(14) Se1 0.0345(4) 0.0138(3) 0.0263(4) 0.0003(3) 0.0149(3) -0.0002(3) Se2 0.0365(4) 0.0186(3) 0.0238(4) 0.0032(3) 0.0172(3) -0.0012(3) Se3 0.0488(5) 0.0189(4) 0.0208(4) -0.0021(3) 0.0102(3) 0.0021(3) O1 0.042(3) 0.022(3) 0.030(3) 0.003(2) 0.016(3) 0.002(2) O2 0.039(5) 0.015(3) 0.032(5) 0.000 0.007(4) 0.000 O3 0.041(5) 0.024(4) 0.027(4) 0.000 0.019(4) 0.000 O4 0.047(3) 0.031(3) 0.026(3) 0.010(2) 0.020(3) -0.001(2) O5 0.049(4) 0.069(5) 0.060(5) 0.011(4) 0.023(4) 0.002(4) C1 0.023(4) 0.032(4) 0.030(4) 0.008(3) 0.011(3) 0.002(3) C2 0.029(4) 0.045(5) 0.064(7) 0.017(5) 0.012(4) -0.008(4) C3 0.036(5) 0.070(7) 0.094(10) 0.030(7) 0.014(6) -0.011(5) C4 0.025(5) 0.092(9) 0.081(9) 0.021(7) 0.015(5) 0.009(5) C5 0.045(6) 0.058(6) 0.093(10) 0.018(6) 0.028(6) 0.026(5) C6 0.030(5) 0.028(4) 0.075(7) 0.010(4) 0.012(5) 0.009(3) C7 0.063(7) 0.085(9) 0.061(8) -0.011(7) 0.018(6) 0.018(6) C8 0.056(9) 0.164(18) 0.139(17) -0.050(15) 0.019(9) 0.028(10) C9 0.058(9) 0.185(19) 0.096(12) -0.042(13) 0.031(8) -0.036(11) C10 0.070(8) 0.108(11) 0.053(7) 0.001(8) 0.013(6) -0.031(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 As1 C1 1.963(7) . ? As1 Se2 2.2850(10) . ? As1 Se1 2.2916(10) . ? As1 Se3 2.2942(11) . ? Na1 O3 2.339(6) . ? Na1 O1 2.366(6) 3_657 ? Na1 O4 2.441(6) . ? Na1 O1 2.447(6) . ? Na1 O2 2.453(6) . ? Na1 Se1 3.172(3) . ? Na1 Na1 3.539(6) 2_656 ? Na1 Na1 3.627(6) 3_657 ? Na1 Na2 3.940(5) . ? Na1 H3B 2.64(8) . ? Na2 O5 2.269(8) . ? Na2 O4 2.272(7) . ? Na2 Se3 2.878(3) 3_667 ? Na2 Se1 3.035(4) 3_657 ? Na2 Se2 3.182(4) 2_656 ? Se1 Na2 3.035(4) 3_657 ? Se2 Na2 3.182(4) 2_656 ? Se3 Na2 2.878(3) 3_667 ? O1 Na1 2.365(6) 3_657 ? O1 H1A 0.9800 . ? O1 H1B 0.9800 . ? O2 Na1 2.453(6) 2_656 ? O2 H2B 0.85(2) . ? O3 Na1 2.339(6) 2_656 ? O3 H3B 0.84(2) . ? O4 H4B 0.9800 . ? O4 H4C 0.9800 . ? O5 C7 1.383(14) . ? O5 C10 1.454(14) . ? C1 C2 1.380(12) . ? C1 C6 1.385(11) . ? C2 C3 1.387(14) . ? C2 H2A 0.9400 . ? C3 C4 1.375(17) . ? C3 H3A 0.9400 . ? C4 C5 1.366(16) . ? C4 H4A 0.9400 . ? C5 C6 1.373(13) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 C8 1.501(19) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.50(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.47(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 Se2 104.8(2) . . ? C1 As1 Se1 108.5(2) . . ? Se2 As1 Se1 114.12(4) . . ? C1 As1 Se3 102.4(2) . . ? Se2 As1 Se3 114.39(4) . . ? Se1 As1 Se3 111.47(4) . . ? O3 Na1 O1 174.6(2) . 3_657 ? O3 Na1 O4 91.03(16) . . ? O1 Na1 O4 94.0(2) 3_657 . ? O3 Na1 O1 95.4(2) . . ? O1 Na1 O1 82.2(2) 3_657 . ? O4 Na1 O1 92.5(2) . . ? O3 Na1 O2 84.7(2) . . ? O1 Na1 O2 98.1(2) 3_657 . ? O4 Na1 O2 83.01(17) . . ? O1 Na1 O2 175.50(19) . . ? O3 Na1 Se1 89.19(9) . . ? O1 Na1 Se1 86.21(16) 3_657 . ? O4 Na1 Se1 171.51(18) . . ? O1 Na1 Se1 95.95(16) . . ? O2 Na1 Se1 88.55(9) . . ? O3 Na1 Na1 40.83(15) . 2_656 ? O1 Na1 Na1 141.73(15) 3_657 2_656 ? O4 Na1 Na1 86.13(17) . 2_656 ? O1 Na1 Na1 136.07(14) . 2_656 ? O2 Na1 Na1 43.83(14) . 2_656 ? Se1 Na1 Na1 88.49(11) . 2_656 ? O3 Na1 Na1 135.5(2) . 3_657 ? O1 Na1 Na1 41.95(14) 3_657 3_657 ? O4 Na1 Na1 94.26(18) . 3_657 ? O1 Na1 Na1 40.25(14) . 3_657 ? O2 Na1 Na1 139.87(19) . 3_657 ? Se1 Na1 Na1 91.54(11) . 3_657 ? Na1 Na1 Na1 176.30(9) 2_656 3_657 ? O3 Na1 Na2 86.92(11) . . ? O1 Na1 Na2 96.15(17) 3_657 . ? O4 Na1 Na2 31.95(15) . . ? O1 Na1 Na2 61.41(16) . . ? O2 Na1 Na2 114.12(11) . . ? Se1 Na1 Na2 156.48(10) . . ? Na1 Na1 Na2 103.35(12) 2_656 . ? Na1 Na1 Na2 75.35(11) 3_657 . ? O3 Na1 H3B 18.2(11) . . ? O1 Na1 H3B 164.6(13) 3_657 . ? O4 Na1 H3B 75.1(14) . . ? O1 Na1 H3B 87.4(19) . . ? O2 Na1 H3B 91.4(19) . . ? Se1 Na1 H3B 106.2(12) . . ? Na1 Na1 H3B 49.9(18) 2_656 . ? Na1 Na1 H3B 126.7(18) 3_657 . ? Na2 Na1 H3B 68.8(11) . . ? O5 Na2 O4 103.3(3) . . ? O5 Na2 Se3 122.5(2) . 3_667 ? O4 Na2 Se3 130.2(2) . 3_667 ? O5 Na2 Se1 104.3(2) . 3_657 ? O4 Na2 Se1 95.90(18) . 3_657 ? Se3 Na2 Se1 90.99(10) 3_667 3_657 ? O5 Na2 Se2 99.9(2) . 2_656 ? O4 Na2 Se2 87.51(17) . 2_656 ? Se3 Na2 Se2 67.81(7) 3_667 2_656 ? Se1 Na2 Se2 154.04(12) 3_657 2_656 ? O5 Na2 Na1 137.8(3) . . ? O4 Na2 Na1 34.65(16) . . ? Se3 Na2 Na1 96.94(10) 3_667 . ? Se1 Na2 Na1 87.85(9) 3_657 . ? Se2 Na2 Na1 80.40(9) 2_656 . ? As1 Se1 Na2 109.86(7) . 3_657 ? As1 Se1 Na1 98.42(6) . . ? Na2 Se1 Na1 96.48(9) 3_657 . ? As1 Se2 Na2 108.00(7) . 2_656 ? As1 Se3 Na2 122.32(8) . 3_667 ? Na1 O1 Na1 97.8(2) 3_657 . ? Na1 O1 H1A 112.2 3_657 . ? Na1 O1 H1A 112.2 . . ? Na1 O1 H1B 112.2 3_657 . ? Na1 O1 H1B 112.2 . . ? H1A O1 H1B 109.8 . . ? Na1 O2 Na1 92.3(3) 2_656 . ? Na1 O2 H2B 101(6) 2_656 . ? Na1 O2 H2B 130(6) . . ? Na1 O3 Na1 98.3(3) 2_656 . ? Na1 O3 H3B 109(6) 2_656 . ? Na1 O3 H3B 102(7) . . ? Na2 O4 Na1 113.4(3) . . ? Na2 O4 H4B 108.9 . . ? Na1 O4 H4B 108.9 . . ? Na2 O4 H4C 108.9 . . ? Na1 O4 H4C 108.9 . . ? H4B O4 H4C 107.7 . . ? C7 O5 C10 108.0(10) . . ? C7 O5 Na2 121.4(7) . . ? C10 O5 Na2 122.0(8) . . ? C2 C1 C6 120.2(8) . . ? C2 C1 As1 120.6(6) . . ? C6 C1 As1 119.3(6) . . ? C1 C2 C3 119.5(9) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 119.9(10) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 120.4(9) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.5(10) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 119.6(9) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? O5 C7 C8 106.6(12) . . ? O5 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O5 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C9 C8 C7 105.0(13) . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8B 110.7 . . ? C7 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C10 C9 C8 104.9(12) . . ? C10 C9 H9A 110.8 . . ? C8 C9 H9A 110.8 . . ? C10 C9 H9B 110.8 . . ? C8 C9 H9B 110.8 . . ? H9A C9 H9B 108.8 . . ? O5 C10 C9 103.5(13) . . ? O5 C10 H10A 111.1 . . ? C9 C10 H10A 111.1 . . ? O5 C10 H10B 111.1 . . ? C9 C10 H10B 111.1 . . ? H10A C10 H10B 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Na1 Na2 O5 -91.5(4) . . . . ? O1 Na1 Na2 O5 93.1(4) 3_657 . . . ? O4 Na1 Na2 O5 5.5(4) . . . . ? O1 Na1 Na2 O5 170.7(4) . . . . ? O2 Na1 Na2 O5 -8.7(4) . . . . ? Se1 Na1 Na2 O5 -172.3(3) . . . . ? Na1 Na1 Na2 O5 -53.8(4) 2_656 . . . ? Na1 Na1 Na2 O5 129.8(4) 3_657 . . . ? O3 Na1 Na2 O4 -96.9(3) . . . . ? O1 Na1 Na2 O4 87.6(3) 3_657 . . . ? O1 Na1 Na2 O4 165.2(3) . . . . ? O2 Na1 Na2 O4 -14.2(3) . . . . ? Se1 Na1 Na2 O4 -177.7(4) . . . . ? Na1 Na1 Na2 O4 -59.2(3) 2_656 . . . ? Na1 Na1 Na2 O4 124.3(3) 3_657 . . . ? O3 Na1 Na2 Se3 68.74(16) . . . 3_667 ? O1 Na1 Na2 Se3 -106.75(17) 3_657 . . 3_667 ? O4 Na1 Na2 Se3 165.6(3) . . . 3_667 ? O1 Na1 Na2 Se3 -29.13(16) . . . 3_667 ? O2 Na1 Na2 Se3 151.49(17) . . . 3_667 ? Se1 Na1 Na2 Se3 -12.1(3) . . . 3_667 ? Na1 Na1 Na2 Se3 106.41(9) 2_656 . . 3_667 ? Na1 Na1 Na2 Se3 -70.02(12) 3_657 . . 3_667 ? O3 Na1 Na2 Se1 159.47(15) . . . 3_657 ? O1 Na1 Na2 Se1 -16.02(16) 3_657 . . 3_657 ? O4 Na1 Na2 Se1 -103.6(3) . . . 3_657 ? O1 Na1 Na2 Se1 61.61(16) . . . 3_657 ? O2 Na1 Na2 Se1 -117.77(17) . . . 3_657 ? Se1 Na1 Na2 Se1 78.6(3) . . . 3_657 ? Na1 Na1 Na2 Se1 -162.86(6) 2_656 . . 3_657 ? Na1 Na1 Na2 Se1 20.72(10) 3_657 . . 3_657 ? O3 Na1 Na2 Se2 2.72(15) . . . 2_656 ? O1 Na1 Na2 Se2 -172.77(16) 3_657 . . 2_656 ? O4 Na1 Na2 Se2 99.6(3) . . . 2_656 ? O1 Na1 Na2 Se2 -95.14(16) . . . 2_656 ? O2 Na1 Na2 Se2 85.48(17) . . . 2_656 ? Se1 Na1 Na2 Se2 -78.1(3) . . . 2_656 ? Na1 Na1 Na2 Se2 40.39(7) 2_656 . . 2_656 ? Na1 Na1 Na2 Se2 -136.03(11) 3_657 . . 2_656 ? C1 As1 Se1 Na2 -74.6(3) . . . 3_657 ? Se2 As1 Se1 Na2 169.00(8) . . . 3_657 ? Se3 As1 Se1 Na2 37.53(9) . . . 3_657 ? C1 As1 Se1 Na1 -174.6(3) . . . . ? Se2 As1 Se1 Na1 68.93(7) . . . . ? Se3 As1 Se1 Na1 -62.54(7) . . . . ? O3 Na1 Se1 As1 -49.53(16) . . . . ? O1 Na1 Se1 As1 127.56(15) 3_657 . . . ? O4 Na1 Se1 As1 -141.0(12) . . . . ? O1 Na1 Se1 As1 45.82(15) . . . . ? O2 Na1 Se1 As1 -134.21(14) . . . . ? Na1 Na1 Se1 As1 -90.37(3) 2_656 . . . ? Na1 Na1 Se1 As1 85.93(10) 3_657 . . . ? Na2 Na1 Se1 As1 30.8(3) . . . . ? O3 Na1 Se1 Na2 -160.78(16) . . . 3_657 ? O1 Na1 Se1 Na2 16.31(16) 3_657 . . 3_657 ? O4 Na1 Se1 Na2 107.7(12) . . . 3_657 ? O1 Na1 Se1 Na2 -65.43(16) . . . 3_657 ? O2 Na1 Se1 Na2 114.54(15) . . . 3_657 ? Na1 Na1 Se1 Na2 158.38(6) 2_656 . . 3_657 ? Na1 Na1 Se1 Na2 -25.32(12) 3_657 . . 3_657 ? Na2 Na1 Se1 Na2 -80.4(3) . . . 3_657 ? C1 As1 Se2 Na2 -80.9(3) . . . 2_656 ? Se1 As1 Se2 Na2 37.66(8) . . . 2_656 ? Se3 As1 Se2 Na2 167.70(7) . . . 2_656 ? C1 As1 Se3 Na2 -45.9(2) . . . 3_667 ? Se2 As1 Se3 Na2 66.85(10) . . . 3_667 ? Se1 As1 Se3 Na2 -161.81(9) . . . 3_667 ? O3 Na1 O1 Na1 175.1(2) . . . 3_657 ? O1 Na1 O1 Na1 0.0 3_657 . . 3_657 ? O4 Na1 O1 Na1 -93.7(2) . . . 3_657 ? O2 Na1 O1 Na1 -94(3) . . . 3_657 ? Se1 Na1 O1 Na1 85.34(18) . . . 3_657 ? Na1 Na1 O1 Na1 179.3(3) 2_656 . . 3_657 ? Na2 Na1 O1 Na1 -101.4(2) . . . 3_657 ? O3 Na1 O2 Na1 0.0 . . . 2_656 ? O1 Na1 O2 Na1 175.3(2) 3_657 . . 2_656 ? O4 Na1 O2 Na1 -91.70(15) . . . 2_656 ? O1 Na1 O2 Na1 -91(3) . . . 2_656 ? Se1 Na1 O2 Na1 89.32(8) . . . 2_656 ? Na1 Na1 O2 Na1 180.0(3) 3_657 . . 2_656 ? Na2 Na1 O2 Na1 -84.20(12) . . . 2_656 ? O1 Na1 O3 Na1 -121(2) 3_657 . . 2_656 ? O4 Na1 O3 Na1 82.89(16) . . . 2_656 ? O1 Na1 O3 Na1 175.48(19) . . . 2_656 ? O2 Na1 O3 Na1 0.0 . . . 2_656 ? Se1 Na1 O3 Na1 -88.62(8) . . . 2_656 ? Na1 Na1 O3 Na1 -180.0(3) 3_657 . . 2_656 ? Na2 Na1 O3 Na1 114.59(10) . . . 2_656 ? O5 Na2 O4 Na1 -176.2(3) . . . . ? Se3 Na2 O4 Na1 -18.8(4) 3_667 . . . ? Se1 Na2 O4 Na1 77.5(2) 3_657 . . . ? Se2 Na2 O4 Na1 -76.7(2) 2_656 . . . ? O3 Na1 O4 Na2 82.5(3) . . . . ? O1 Na1 O4 Na2 -95.3(3) 3_657 . . . ? O1 Na1 O4 Na2 -13.0(3) . . . . ? O2 Na1 O4 Na2 167.0(3) . . . . ? Se1 Na1 O4 Na2 173.9(10) . . . . ? Na1 Na1 O4 Na2 123.1(2) 2_656 . . . ? Na1 Na1 O4 Na2 -53.2(3) 3_657 . . . ? O4 Na2 O5 C7 -4.0(9) . . . . ? Se3 Na2 O5 C7 -163.7(8) 3_667 . . . ? Se1 Na2 O5 C7 95.7(9) 3_657 . . . ? Se2 Na2 O5 C7 -93.8(9) 2_656 . . . ? Na1 Na2 O5 C7 -7.2(10) . . . . ? O4 Na2 O5 C10 139.8(8) . . . . ? Se3 Na2 O5 C10 -19.8(9) 3_667 . . . ? Se1 Na2 O5 C10 -120.4(8) 3_657 . . . ? Se2 Na2 O5 C10 50.1(9) 2_656 . . . ? Na1 Na2 O5 C10 136.6(8) . . . . ? Se2 As1 C1 C2 134.8(8) . . . . ? Se1 As1 C1 C2 12.5(8) . . . . ? Se3 As1 C1 C2 -105.5(8) . . . . ? Se2 As1 C1 C6 -44.7(8) . . . . ? Se1 As1 C1 C6 -167.0(7) . . . . ? Se3 As1 C1 C6 75.0(8) . . . . ? C6 C1 C2 C3 -0.5(17) . . . . ? As1 C1 C2 C3 -179.9(9) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C2 C1 C6 C5 0.8(17) . . . . ? As1 C1 C6 C5 -179.7(9) . . . . ? C10 O5 C7 C8 26.8(16) . . . . ? Na2 O5 C7 C8 175.1(11) . . . . ? O5 C7 C8 C9 -7(2) . . . . ? C7 C8 C9 C10 -14(2) . . . . ? C7 O5 C10 C9 -36.0(14) . . . . ? Na2 O5 C10 C9 176.0(9) . . . . ? C8 C9 C10 O5 29.8(18) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.975 _refine_diff_density_min -1.780 _refine_diff_density_rms 0.212