#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Jones, Cameron ' 'Junk, Peter C.' 'Steed, Jonathan W.' 'Thomas, Ryan C.' 'Williams, Thomas C.' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry University of Wales P.O. Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK data_compound 20 _database_code_CSD 165257 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H52 Cl O2 P2 Pt Sb' _chemical_formula_weight 882.97 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' '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 18.6340(10) _cell_length_b 10.1279(5) _cell_length_c 18.8286(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.568(3) _cell_angle_gamma 90.00 _cell_volume 3552.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 4.885 _exptl_absorpt_correction_type Scalepack _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 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o frames 90s' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27862 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8093 _reflns_number_gt 6438 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _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^)+(0.0000P)^2^+2.8662P] 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 SHELXL _refine_ls_extinction_coef 0.00138(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8093 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Pt1 Pt 0.772479(10) 0.702238(19) 0.029564(11) 0.01301(7) Uani 1 1 d . . . Sb1 Sb 0.775550(18) 0.83664(3) -0.088225(18) 0.01451(9) Uani 1 1 d . . . Cl1 Cl 0.77178(8) 0.55728(13) 0.13106(7) 0.0271(3) Uani 1 1 d . . . P1 P 0.80665(7) 0.87542(13) 0.10487(7) 0.0155(3) Uani 1 1 d . . . P2 P 0.74533(7) 0.50887(12) -0.03385(7) 0.0140(3) Uani 1 1 d . . . O1 O 0.70301(19) 1.1090(3) -0.0675(2) 0.0224(9) Uani 1 1 d . . . O2 O 0.8816(2) 1.0685(4) -0.0432(2) 0.0280(9) Uani 1 1 d . . . C1 C 0.6896(3) 0.9918(5) -0.0776(3) 0.0146(11) Uani 1 1 d . . . C2 C 0.8713(3) 0.9793(5) -0.0850(3) 0.0185(12) Uani 1 1 d . . . C3 C 0.6151(3) 0.9448(5) -0.0982(3) 0.0149(11) Uani 1 1 d . . . C4 C 0.5714(3) 0.8837(5) -0.0476(3) 0.0178(11) Uani 1 1 d . . . C5 C 0.5040(3) 0.8361(5) -0.0701(3) 0.0221(12) Uani 1 1 d . . . H5 H 0.4743 0.7948 -0.0365 0.026 Uiso 1 1 calc R . . C6 C 0.4791(3) 0.8476(5) -0.1407(3) 0.0219(12) Uani 1 1 d . . . C7 C 0.5227(3) 0.9108(5) -0.1894(3) 0.0232(13) Uani 1 1 d . . . H7 H 0.5058 0.9211 -0.2371 0.028 Uiso 1 1 calc R . . C8 C 0.5909(3) 0.9595(5) -0.1696(3) 0.0207(12) Uani 1 1 d . . . C9 C 0.5948(3) 0.8738(5) 0.0292(3) 0.0228(13) Uani 1 1 d . . . H9A H 0.5592 0.8233 0.0552 0.027 Uiso 1 1 calc R . . H9B H 0.5991 0.9626 0.0495 0.027 Uiso 1 1 calc R . . H9C H 0.6414 0.8290 0.0329 0.027 Uiso 1 1 calc R . . C10 C 0.4071(3) 0.7924(6) -0.1643(3) 0.0307(14) Uani 1 1 d . . . H10A H 0.4142 0.7118 -0.1921 0.037 Uiso 1 1 calc R . . H10B H 0.3813 0.8578 -0.1937 0.037 Uiso 1 1 calc R . . H10C H 0.3790 0.7717 -0.1225 0.037 Uiso 1 1 calc R . . C11 C 0.6364(3) 1.0287(6) -0.2236(3) 0.0270(14) Uani 1 1 d . . . H11A H 0.6312 1.1245 -0.2185 0.032 Uiso 1 1 calc R . . H11B H 0.6207 1.0022 -0.2716 0.032 Uiso 1 1 calc R . . H11C H 0.6869 1.0042 -0.2156 0.032 Uiso 1 1 calc R . . C12 C 0.9176(3) 0.9591(5) -0.1486(3) 0.0175(11) Uani 1 1 d . . . C13 C 0.9659(3) 0.8518(5) -0.1522(3) 0.0242(13) Uani 1 1 d . . . C14 C 1.0056(3) 0.8349(6) -0.2127(3) 0.0259(14) Uani 1 1 d . . . H14 H 1.0364 0.7605 -0.2158 0.031 Uiso 1 1 calc R . . C15 C 1.0016(3) 0.9243(6) -0.2693(3) 0.0296(14) Uani 1 1 d . . . C16 C 0.9550(3) 1.0325(6) -0.2645(3) 0.0224(12) Uani 1 1 d . . . H16 H 0.9523 1.0948 -0.3022 0.027 Uiso 1 1 calc R . . C17 C 0.9122(3) 1.0502(5) -0.2053(3) 0.0185(12) Uani 1 1 d . . . C18 C 0.9756(3) 0.7590(6) -0.0888(4) 0.0347(16) Uani 1 1 d . . . H18A H 1.0142 0.7922 -0.0571 0.042 Uiso 1 1 calc R . . H18B H 0.9881 0.6706 -0.1056 0.042 Uiso 1 1 calc R . . H18C H 0.9308 0.7546 -0.0628 0.042 Uiso 1 1 calc R . . C19 C 1.0481(4) 0.9082(8) -0.3342(4) 0.0479(19) Uani 1 1 d . . . H19A H 1.0931 0.9569 -0.3267 0.057 Uiso 1 1 calc R . . H19B H 1.0224 0.9429 -0.3763 0.057 Uiso 1 1 calc R . . H19C H 1.0587 0.8144 -0.3413 0.057 Uiso 1 1 calc R . . C20 C 0.8593(3) 1.1647(5) -0.2032(3) 0.0204(12) Uani 1 1 d . . . H20A H 0.8122 1.1318 -0.1897 0.024 Uiso 1 1 calc R . . H20B H 0.8554 1.2059 -0.2503 0.024 Uiso 1 1 calc R . . H20C H 0.8764 1.2301 -0.1683 0.024 Uiso 1 1 calc R . . C21 C 0.7786(3) 0.8527(5) 0.1963(3) 0.0198(12) Uani 1 1 d . . . H21A H 0.7970 0.7667 0.2141 0.024 Uiso 1 1 calc R . . H21B H 0.8006 0.9228 0.2264 0.024 Uiso 1 1 calc R . . C22 C 0.6975(3) 0.8564(6) 0.2043(3) 0.0245(13) Uani 1 1 d . . . H22A H 0.6794 0.9444 0.1916 0.029 Uiso 1 1 calc R . . H22B H 0.6859 0.8367 0.2536 0.029 Uiso 1 1 calc R . . H22C H 0.6750 0.7905 0.1728 0.029 Uiso 1 1 calc R . . C23 C 0.7752(3) 1.0435(5) 0.0851(3) 0.0163(11) Uani 1 1 d . . . H23A H 0.7941 1.0703 0.0386 0.020 Uiso 1 1 calc R . . H23B H 0.7222 1.0417 0.0802 0.020 Uiso 1 1 calc R . . C24 C 0.7966(3) 1.1496(5) 0.1404(3) 0.0230(13) Uani 1 1 d . . . H24A H 0.7731 1.1308 0.1853 0.028 Uiso 1 1 calc R . . H24B H 0.7815 1.2366 0.1229 0.028 Uiso 1 1 calc R . . H24C H 0.8488 1.1488 0.1483 0.028 Uiso 1 1 calc R . . C25 C 0.9048(3) 0.8868(5) 0.1119(3) 0.0215(12) Uani 1 1 d . . . H25A H 0.9227 0.9285 0.0682 0.026 Uiso 1 1 calc R . . H25B H 0.9183 0.9449 0.1524 0.026 Uiso 1 1 calc R . . C26 C 0.9418(3) 0.7533(6) 0.1223(3) 0.0297(14) Uani 1 1 d . . . H26A H 0.9221 0.7085 0.1636 0.036 Uiso 1 1 calc R . . H26B H 0.9935 0.7669 0.1302 0.036 Uiso 1 1 calc R . . H26C H 0.9337 0.6989 0.0798 0.036 Uiso 1 1 calc R . . C27 C 0.8170(3) 0.3872(5) -0.0222(3) 0.0213(12) Uani 1 1 d . . . H27A H 0.8210 0.3627 0.0286 0.026 Uiso 1 1 calc R . . H27B H 0.8035 0.3066 -0.0493 0.026 Uiso 1 1 calc R . . C28 C 0.8908(3) 0.4341(5) -0.0464(3) 0.0242(13) Uani 1 1 d . . . H28A H 0.9006 0.3957 -0.0929 0.029 Uiso 1 1 calc R . . H28B H 0.9279 0.4059 -0.0118 0.029 Uiso 1 1 calc R . . H28C H 0.8909 0.5306 -0.0500 0.029 Uiso 1 1 calc R . . C29 C 0.6670(3) 0.4229(5) -0.0003(3) 0.0182(11) Uani 1 1 d . . . H29A H 0.6646 0.3336 -0.0216 0.022 Uiso 1 1 calc R . . H29B H 0.6731 0.4122 0.0518 0.022 Uiso 1 1 calc R . . C30 C 0.5964(3) 0.4944(6) -0.0163(3) 0.0285(14) Uani 1 1 d . . . H30A H 0.6016 0.5881 -0.0041 0.034 Uiso 1 1 calc R . . H30B H 0.5584 0.4553 0.0119 0.034 Uiso 1 1 calc R . . H30C H 0.5837 0.4859 -0.0669 0.034 Uiso 1 1 calc R . . C31 C 0.7266(3) 0.5154(5) -0.1300(3) 0.0182(11) Uani 1 1 d . . . H31A H 0.6877 0.5803 -0.1391 0.022 Uiso 1 1 calc R . . H31B H 0.7700 0.5488 -0.1533 0.022 Uiso 1 1 calc R . . C32 C 0.7048(3) 0.3845(5) -0.1654(3) 0.0216(12) Uani 1 1 d . . . H32A H 0.7476 0.3303 -0.1721 0.026 Uiso 1 1 calc R . . H32B H 0.6813 0.4024 -0.2116 0.026 Uiso 1 1 calc R . . H32C H 0.6714 0.3373 -0.1350 0.026 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 Pt1 0.01493(11) 0.01089(10) 0.01313(11) 0.00012(8) -0.00094(7) 0.00027(8) Sb1 0.01650(18) 0.01215(17) 0.01489(18) 0.00084(14) 0.00068(14) -0.00155(14) Cl1 0.0451(9) 0.0182(7) 0.0176(7) 0.0032(6) -0.0027(6) -0.0015(6) P1 0.0170(7) 0.0155(7) 0.0138(7) 0.0002(6) -0.0029(6) 0.0007(5) P2 0.0160(7) 0.0106(6) 0.0154(7) 0.0017(6) 0.0012(6) 0.0012(5) O1 0.025(2) 0.0129(19) 0.029(2) 0.0004(17) -0.0070(18) -0.0009(16) O2 0.030(2) 0.024(2) 0.030(2) -0.0075(19) 0.0076(19) -0.0086(18) C1 0.017(3) 0.018(3) 0.009(2) 0.001(2) 0.002(2) -0.001(2) C2 0.016(3) 0.018(3) 0.021(3) 0.007(2) 0.004(2) -0.001(2) C3 0.015(3) 0.007(2) 0.022(3) -0.006(2) 0.000(2) 0.000(2) C4 0.023(3) 0.013(2) 0.017(3) 0.000(2) 0.003(2) 0.003(2) C5 0.015(3) 0.024(3) 0.027(3) 0.003(3) 0.005(2) -0.003(2) C6 0.012(3) 0.022(3) 0.031(3) -0.008(3) -0.003(2) 0.001(2) C7 0.015(3) 0.030(3) 0.025(3) -0.010(3) -0.005(2) 0.000(2) C8 0.023(3) 0.022(3) 0.017(3) -0.004(2) -0.002(2) -0.001(2) C9 0.023(3) 0.024(3) 0.022(3) 0.002(2) 0.002(2) 0.001(2) C10 0.027(3) 0.031(3) 0.034(4) -0.003(3) -0.004(3) -0.007(3) C11 0.033(3) 0.031(3) 0.016(3) 0.005(3) -0.002(3) -0.010(3) C12 0.014(3) 0.016(3) 0.023(3) -0.004(2) 0.003(2) -0.003(2) C13 0.016(3) 0.021(3) 0.035(4) -0.002(3) 0.001(3) -0.003(2) C14 0.008(2) 0.028(3) 0.042(4) -0.016(3) 0.000(2) 0.003(2) C15 0.015(3) 0.050(4) 0.024(3) -0.015(3) 0.002(2) 0.004(3) C16 0.018(3) 0.033(3) 0.017(3) 0.002(2) 0.000(2) -0.002(2) C17 0.014(3) 0.023(3) 0.019(3) -0.003(2) 0.001(2) -0.006(2) C18 0.020(3) 0.028(3) 0.056(4) 0.008(3) 0.008(3) 0.005(3) C19 0.036(4) 0.080(6) 0.027(4) -0.012(4) 0.007(3) 0.016(4) C20 0.017(3) 0.021(3) 0.024(3) 0.000(2) 0.005(2) -0.001(2) C21 0.035(3) 0.015(3) 0.010(3) -0.003(2) -0.002(2) 0.001(2) C22 0.029(3) 0.026(3) 0.019(3) 0.000(3) 0.000(3) 0.001(3) C23 0.017(3) 0.013(2) 0.020(3) 0.002(2) 0.003(2) 0.002(2) C24 0.027(3) 0.018(3) 0.024(3) -0.004(2) -0.005(3) 0.002(2) C25 0.019(3) 0.021(3) 0.024(3) 0.000(2) -0.005(2) 0.000(2) C26 0.025(3) 0.029(3) 0.034(4) -0.004(3) -0.005(3) 0.003(3) C27 0.023(3) 0.018(3) 0.023(3) 0.000(2) -0.001(2) 0.003(2) C28 0.015(3) 0.024(3) 0.033(3) 0.002(3) 0.002(2) 0.004(2) C29 0.019(3) 0.019(3) 0.017(3) -0.002(2) 0.005(2) -0.006(2) C30 0.020(3) 0.028(3) 0.037(4) -0.002(3) 0.007(3) -0.002(3) C31 0.018(3) 0.017(3) 0.020(3) 0.001(2) 0.002(2) -0.001(2) C32 0.027(3) 0.022(3) 0.016(3) -0.006(2) -0.002(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.3330(14) . ? Pt1 P2 2.3418(13) . ? Pt1 Cl1 2.4101(13) . ? Pt1 Sb1 2.6042(4) . ? Sb1 C1 2.257(5) . ? Sb1 C2 2.295(5) . ? P1 C21 1.828(5) . ? P1 C23 1.835(5) . ? P1 C25 1.835(5) . ? P2 C27 1.827(5) . ? P2 C29 1.827(5) . ? P2 C31 1.835(5) . ? O1 C1 1.227(6) . ? O2 C2 1.210(6) . ? C1 C3 1.509(7) . ? C2 C12 1.508(7) . ? C3 C4 1.413(7) . ? C3 C8 1.415(7) . ? C4 C5 1.399(7) . ? C4 C9 1.502(7) . ? C5 C6 1.401(8) . ? C6 C7 1.395(8) . ? C6 C10 1.509(7) . ? C7 C8 1.404(7) . ? C8 C11 1.513(7) . ? C12 C17 1.413(7) . ? C12 C13 1.414(7) . ? C13 C14 1.386(8) . ? C13 C18 1.526(8) . ? C14 C15 1.399(9) . ? C15 C16 1.402(8) . ? C15 C19 1.527(8) . ? C16 C17 1.399(7) . ? C17 C20 1.524(7) . ? C21 C22 1.524(8) . ? C23 C24 1.541(7) . ? C25 C26 1.528(7) . ? C27 C28 1.535(7) . ? C29 C30 1.525(7) . ? C31 C32 1.534(7) . ? 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 Pt1 P2 171.96(5) . . ? P1 Pt1 Cl1 89.05(5) . . ? P2 Pt1 Cl1 83.63(5) . . ? P1 Pt1 Sb1 96.47(4) . . ? P2 Pt1 Sb1 90.71(3) . . ? Cl1 Pt1 Sb1 173.92(3) . . ? C1 Sb1 C2 96.46(18) . . ? C1 Sb1 Pt1 104.83(13) . . ? C2 Sb1 Pt1 109.99(14) . . ? C21 P1 C23 102.1(2) . . ? C21 P1 C25 104.5(3) . . ? C23 P1 C25 105.6(2) . . ? C21 P1 Pt1 113.42(18) . . ? C23 P1 Pt1 119.60(18) . . ? C25 P1 Pt1 110.25(18) . . ? C27 P2 C29 103.0(2) . . ? C27 P2 C31 105.1(3) . . ? C29 P2 C31 103.1(2) . . ? C27 P2 Pt1 110.87(18) . . ? C29 P2 Pt1 112.68(18) . . ? C31 P2 Pt1 120.35(17) . . ? O1 C1 C3 121.8(4) . . ? O1 C1 Sb1 123.1(4) . . ? C3 C1 Sb1 114.1(3) . . ? O2 C2 C12 122.2(5) . . ? O2 C2 Sb1 126.6(4) . . ? C12 C2 Sb1 110.8(4) . . ? C4 C3 C8 120.8(5) . . ? C4 C3 C1 120.5(5) . . ? C8 C3 C1 118.6(5) . . ? C5 C4 C3 118.4(5) . . ? C5 C4 C9 120.2(5) . . ? C3 C4 C9 121.3(5) . . ? C4 C5 C6 122.0(5) . . ? C7 C6 C5 118.5(5) . . ? C7 C6 C10 120.4(5) . . ? C5 C6 C10 121.1(5) . . ? C6 C7 C8 121.7(5) . . ? C7 C8 C3 118.5(5) . . ? C7 C8 C11 120.3(5) . . ? C3 C8 C11 121.1(5) . . ? C17 C12 C13 119.8(5) . . ? C17 C12 C2 118.8(4) . . ? C13 C12 C2 121.4(5) . . ? C14 C13 C12 119.2(5) . . ? C14 C13 C18 120.8(5) . . ? C12 C13 C18 119.9(5) . . ? C13 C14 C15 121.9(5) . . ? C14 C15 C16 118.5(5) . . ? C14 C15 C19 121.4(6) . . ? C16 C15 C19 120.1(6) . . ? C17 C16 C15 121.2(5) . . ? C16 C17 C12 119.3(5) . . ? C16 C17 C20 120.1(5) . . ? C12 C17 C20 120.6(5) . . ? C22 C21 P1 113.5(4) . . ? C24 C23 P1 115.8(4) . . ? C26 C25 P1 113.5(4) . . ? C28 C27 P2 114.4(4) . . ? C30 C29 P2 113.5(4) . . ? C32 C31 P2 116.0(4) . . ? 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 P1 Pt1 Sb1 C1 -63.81(14) . . . . ? P2 Pt1 Sb1 C1 119.82(14) . . . . ? Cl1 Pt1 Sb1 C1 141.2(4) . . . . ? P1 Pt1 Sb1 C2 38.91(15) . . . . ? P2 Pt1 Sb1 C2 -137.46(15) . . . . ? Cl1 Pt1 Sb1 C2 -116.1(4) . . . . ? P2 Pt1 P1 C21 -50.2(4) . . . . ? Cl1 Pt1 P1 C21 -25.9(2) . . . . ? Sb1 Pt1 P1 C21 156.6(2) . . . . ? P2 Pt1 P1 C23 -170.9(3) . . . . ? Cl1 Pt1 P1 C23 -146.5(2) . . . . ? Sb1 Pt1 P1 C23 36.0(2) . . . . ? P2 Pt1 P1 C25 66.5(4) . . . . ? Cl1 Pt1 P1 C25 90.8(2) . . . . ? Sb1 Pt1 P1 C25 -86.6(2) . . . . ? P1 Pt1 P2 C27 -36.8(4) . . . . ? Cl1 Pt1 P2 C27 -61.3(2) . . . . ? Sb1 Pt1 P2 C27 116.5(2) . . . . ? P1 Pt1 P2 C29 78.1(4) . . . . ? Cl1 Pt1 P2 C29 53.64(19) . . . . ? Sb1 Pt1 P2 C29 -128.59(19) . . . . ? P1 Pt1 P2 C31 -159.9(4) . . . . ? Cl1 Pt1 P2 C31 175.6(2) . . . . ? Sb1 Pt1 P2 C31 -6.6(2) . . . . ? C2 Sb1 C1 O1 -5.2(4) . . . . ? Pt1 Sb1 C1 O1 107.5(4) . . . . ? C2 Sb1 C1 C3 163.2(4) . . . . ? Pt1 Sb1 C1 C3 -84.0(3) . . . . ? C1 Sb1 C2 O2 46.9(5) . . . . ? Pt1 Sb1 C2 O2 -61.4(5) . . . . ? C1 Sb1 C2 C12 -126.1(3) . . . . ? Pt1 Sb1 C2 C12 125.5(3) . . . . ? O1 C1 C3 C4 -103.5(6) . . . . ? Sb1 C1 C3 C4 87.9(5) . . . . ? O1 C1 C3 C8 78.4(6) . . . . ? Sb1 C1 C3 C8 -90.2(5) . . . . ? C8 C3 C4 C5 1.0(7) . . . . ? C1 C3 C4 C5 -177.0(5) . . . . ? C8 C3 C4 C9 -176.7(5) . . . . ? C1 C3 C4 C9 5.2(7) . . . . ? C3 C4 C5 C6 -0.1(8) . . . . ? C9 C4 C5 C6 177.7(5) . . . . ? C4 C5 C6 C7 -1.2(8) . . . . ? C4 C5 C6 C10 178.3(5) . . . . ? C5 C6 C7 C8 1.6(8) . . . . ? C10 C6 C7 C8 -178.0(5) . . . . ? C6 C7 C8 C3 -0.7(8) . . . . ? C6 C7 C8 C11 -179.4(5) . . . . ? C4 C3 C8 C7 -0.7(7) . . . . ? C1 C3 C8 C7 177.4(5) . . . . ? C4 C3 C8 C11 178.1(5) . . . . ? C1 C3 C8 C11 -3.9(7) . . . . ? O2 C2 C12 C17 -70.6(7) . . . . ? Sb1 C2 C12 C17 102.8(4) . . . . ? O2 C2 C12 C13 109.2(6) . . . . ? Sb1 C2 C12 C13 -77.4(5) . . . . ? C17 C12 C13 C14 -2.3(8) . . . . ? C2 C12 C13 C14 177.9(5) . . . . ? C17 C12 C13 C18 175.6(5) . . . . ? C2 C12 C13 C18 -4.2(8) . . . . ? C12 C13 C14 C15 2.8(8) . . . . ? C18 C13 C14 C15 -175.1(5) . . . . ? C13 C14 C15 C16 -1.1(8) . . . . ? C13 C14 C15 C19 177.1(6) . . . . ? C14 C15 C16 C17 -1.1(8) . . . . ? C19 C15 C16 C17 -179.4(5) . . . . ? C15 C16 C17 C12 1.6(8) . . . . ? C15 C16 C17 C20 -176.9(5) . . . . ? C13 C12 C17 C16 0.1(7) . . . . ? C2 C12 C17 C16 180.0(5) . . . . ? C13 C12 C17 C20 178.6(5) . . . . ? C2 C12 C17 C20 -1.6(7) . . . . ? C23 P1 C21 C22 63.6(4) . . . . ? C25 P1 C21 C22 173.4(4) . . . . ? Pt1 P1 C21 C22 -66.5(4) . . . . ? C21 P1 C23 C24 50.1(4) . . . . ? C25 P1 C23 C24 -58.9(5) . . . . ? Pt1 P1 C23 C24 176.2(3) . . . . ? C21 P1 C25 C26 77.5(5) . . . . ? C23 P1 C25 C26 -175.2(4) . . . . ? Pt1 P1 C25 C26 -44.7(5) . . . . ? C29 P2 C27 C28 -179.8(4) . . . . ? C31 P2 C27 C28 72.5(4) . . . . ? Pt1 P2 C27 C28 -59.0(4) . . . . ? C27 P2 C29 C30 -169.5(4) . . . . ? C31 P2 C29 C30 -60.3(4) . . . . ? Pt1 P2 C29 C30 70.9(4) . . . . ? C27 P2 C31 C32 57.9(4) . . . . ? C29 P2 C31 C32 -49.7(4) . . . . ? Pt1 P2 C31 C32 -176.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.247 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.175 data_compound 8 _database_code_CSD 165258 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H25 As Fe O4' _chemical_formula_weight 532.23 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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(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 11.0904(10) _cell_length_b 15.1249(9) _cell_length_c 15.130(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.150(10) _cell_angle_gamma 90.00 _cell_volume 2425.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cut needle _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-Turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4732 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.21 _reflns_number_total 4362 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0559P)^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 4362 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.014 _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 0.43070(4) 0.81989(3) -0.00438(3) 0.04996(15) Uani 1 1 d . . . Fe1 Fe 0.25948(5) 0.78344(4) 0.05556(4) 0.04657(18) Uani 1 1 d . . . O1 O 0.3854(3) 0.7735(2) -0.1920(2) 0.0740(9) Uani 1 1 d . . . O2 O 0.4759(3) 0.6349(2) 0.0145(2) 0.0741(9) Uani 1 1 d . . . O3 O 0.1865(3) 0.6235(2) -0.0528(2) 0.0854(10) Uani 1 1 d . . . O4 O 0.0740(3) 0.8920(2) -0.0743(2) 0.0898(11) Uani 1 1 d . . . C1 C 0.3673(4) 0.8309(3) -0.1423(3) 0.0517(10) Uani 1 1 d . . . C2 C 0.5143(4) 0.7017(3) -0.0114(3) 0.0546(11) Uani 1 1 d . . . C3 C 0.3025(3) 0.9144(3) -0.1820(3) 0.0476(10) Uani 1 1 d . . . C4 C 0.2998(4) 0.9874(3) -0.1284(3) 0.0573(11) Uani 1 1 d . . . H4 H 0.3406 0.9861 -0.0652 0.069 Uiso 1 1 calc R . . C5 C 0.2363(4) 1.0628(3) -0.1686(4) 0.0694(13) Uani 1 1 d . . . H5 H 0.2340 1.1118 -0.1319 0.083 Uiso 1 1 calc R . . C6 C 0.1769(5) 1.0663(3) -0.2616(4) 0.0817(15) Uani 1 1 d . . . H6 H 0.1344 1.1173 -0.2880 0.098 Uiso 1 1 calc R . . C7 C 0.1805(4) 0.9949(4) -0.3151(4) 0.0778(14) Uani 1 1 d . . . H7 H 0.1401 0.9973 -0.3784 0.093 Uiso 1 1 calc R . . C8 C 0.2434(4) 0.9183(3) -0.2770(3) 0.0637(12) Uani 1 1 d . . . H8 H 0.2461 0.8701 -0.3145 0.076 Uiso 1 1 calc R . . C9 C 0.6304(4) 0.7008(3) -0.0408(3) 0.0586(12) Uani 1 1 d . . . C10 C 0.6877(4) 0.7781(4) -0.0564(3) 0.0781(15) Uani 1 1 d . . . H10 H 0.6521 0.8326 -0.0502 0.094 Uiso 1 1 calc R . . C11 C 0.7999(5) 0.7740(5) -0.0816(4) 0.0956(19) Uani 1 1 d . . . H11 H 0.8379 0.8257 -0.0934 0.115 Uiso 1 1 calc R . . C12 C 0.8530(5) 0.6934(5) -0.0887(4) 0.101(2) Uani 1 1 d . . . H12 H 0.9275 0.6909 -0.1049 0.121 Uiso 1 1 calc R . . C13 C 0.7990(6) 0.6182(5) -0.0726(4) 0.103(2) Uani 1 1 d . . . H13 H 0.8364 0.5642 -0.0777 0.124 Uiso 1 1 calc R . . C14 C 0.6863(5) 0.6206(4) -0.0482(3) 0.0838(16) Uani 1 1 d . . . H14 H 0.6493 0.5682 -0.0370 0.101 Uiso 1 1 calc R . . C15 C 0.3961(4) 0.7827(3) 0.1899(3) 0.0552(11) Uani 1 1 d . . . C16 C 0.3136(4) 0.7094(3) 0.1800(3) 0.0559(11) Uani 1 1 d . . . C17 C 0.1892(4) 0.7431(4) 0.1632(3) 0.0632(12) Uani 1 1 d . . . C18 C 0.1949(4) 0.8363(3) 0.1622(3) 0.0648(13) Uani 1 1 d . . . C19 C 0.3237(4) 0.8609(3) 0.1758(3) 0.0598(11) Uani 1 1 d . . . C20 C 0.5377(4) 0.7774(3) 0.2185(3) 0.0739(14) Uani 1 1 d . . . H20A H 0.5679 0.7561 0.2809 0.111 Uiso 1 1 calc R . . H20B H 0.5719 0.8351 0.2148 0.111 Uiso 1 1 calc R . . H20C H 0.5636 0.7377 0.1781 0.111 Uiso 1 1 calc R . . C21 C 0.3542(5) 0.6146(3) 0.1931(3) 0.0793(15) Uani 1 1 d . . . H21A H 0.2856 0.5773 0.1602 0.119 Uiso 1 1 calc R . . H21B H 0.3781 0.6002 0.2578 0.119 Uiso 1 1 calc R . . H21C H 0.4248 0.6056 0.1697 0.119 Uiso 1 1 calc R . . C22 C 0.0729(5) 0.6877(4) 0.1579(4) 0.098(2) Uani 1 1 d . . . H22A H 0.0718 0.6725 0.2192 0.146 Uiso 1 1 calc R . . H22B H 0.0748 0.6347 0.1234 0.146 Uiso 1 1 calc R . . H22C H -0.0016 0.7210 0.1276 0.146 Uiso 1 1 calc R . . C23 C 0.0856(5) 0.8982(4) 0.1540(4) 0.110(2) Uani 1 1 d . . . H23A H 0.0994 0.9521 0.1250 0.165 Uiso 1 1 calc R . . H23B H 0.0788 0.9108 0.2146 0.165 Uiso 1 1 calc R . . H23C H 0.0091 0.8709 0.1173 0.165 Uiso 1 1 calc R . . C24 C 0.3751(5) 0.9538(3) 0.1858(4) 0.0949(17) Uani 1 1 d . . . H24A H 0.4047 0.9692 0.2501 0.142 Uiso 1 1 calc R . . H24B H 0.3096 0.9941 0.1543 0.142 Uiso 1 1 calc R . . H24C H 0.4437 0.9574 0.1593 0.142 Uiso 1 1 calc R . . C25 C 0.2202(4) 0.6868(3) -0.0121(3) 0.0559(11) Uani 1 1 d . . . C26 C 0.1516(4) 0.8498(3) -0.0244(3) 0.0587(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0468(2) 0.0581(3) 0.0452(2) 0.0017(2) 0.01391(18) -0.0004(2) Fe1 0.0441(3) 0.0538(4) 0.0422(3) -0.0009(3) 0.0132(3) 0.0031(3) O1 0.100(3) 0.063(2) 0.0532(19) -0.0035(16) 0.0135(17) 0.0165(19) O2 0.073(2) 0.067(2) 0.094(2) 0.0163(19) 0.0427(19) 0.0145(18) O3 0.082(2) 0.083(3) 0.085(2) -0.031(2) 0.0143(19) -0.012(2) O4 0.061(2) 0.105(3) 0.099(3) 0.039(2) 0.0173(19) 0.021(2) C1 0.052(2) 0.056(3) 0.048(2) -0.002(2) 0.015(2) -0.006(2) C2 0.045(2) 0.072(3) 0.046(2) 0.008(2) 0.0137(19) 0.006(2) C3 0.048(2) 0.043(2) 0.050(2) 0.004(2) 0.0125(19) -0.0105(19) C4 0.060(3) 0.048(3) 0.063(3) 0.000(2) 0.016(2) -0.007(2) C5 0.074(3) 0.047(3) 0.091(4) 0.004(3) 0.030(3) -0.004(2) C6 0.076(4) 0.056(4) 0.105(5) 0.027(3) 0.014(3) 0.001(3) C7 0.081(3) 0.068(4) 0.071(3) 0.023(3) 0.000(3) -0.002(3) C8 0.066(3) 0.063(3) 0.057(3) 0.005(2) 0.010(2) -0.014(2) C9 0.050(3) 0.082(4) 0.042(2) 0.002(2) 0.009(2) 0.008(3) C10 0.056(3) 0.106(4) 0.076(3) 0.008(3) 0.025(3) 0.007(3) C11 0.059(3) 0.149(6) 0.079(4) 0.015(4) 0.021(3) -0.013(4) C12 0.056(3) 0.184(8) 0.065(4) -0.011(4) 0.022(3) 0.004(4) C13 0.079(4) 0.142(7) 0.097(4) -0.019(4) 0.039(3) 0.025(4) C14 0.073(3) 0.097(4) 0.087(4) -0.018(3) 0.033(3) 0.008(3) C15 0.051(3) 0.075(3) 0.037(2) -0.003(2) 0.0091(19) 0.001(2) C16 0.061(3) 0.064(3) 0.042(2) 0.002(2) 0.014(2) -0.005(2) C17 0.052(3) 0.095(4) 0.048(3) -0.004(2) 0.024(2) -0.011(3) C18 0.060(3) 0.084(4) 0.054(3) -0.009(2) 0.022(2) 0.011(3) C19 0.067(3) 0.063(3) 0.049(3) -0.015(2) 0.017(2) -0.001(3) C20 0.058(3) 0.104(4) 0.051(3) 0.004(3) 0.004(2) 0.002(3) C21 0.093(4) 0.076(4) 0.066(3) 0.022(3) 0.019(3) 0.005(3) C22 0.072(3) 0.153(6) 0.073(4) -0.003(3) 0.031(3) -0.033(4) C23 0.084(4) 0.139(6) 0.111(5) -0.029(4) 0.036(3) 0.038(4) C24 0.117(5) 0.070(4) 0.096(4) -0.024(3) 0.030(4) -0.011(3) C25 0.053(3) 0.065(3) 0.050(3) -0.003(2) 0.016(2) -0.001(2) C26 0.047(3) 0.069(3) 0.062(3) 0.007(2) 0.019(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 2.003(4) . ? As1 C2 2.030(4) . ? As1 Fe1 2.3974(7) . ? Fe1 C26 1.746(5) . ? Fe1 C25 1.764(5) . ? Fe1 C17 2.093(4) . ? Fe1 C19 2.104(4) . ? Fe1 C18 2.107(4) . ? Fe1 C16 2.120(4) . ? Fe1 C15 2.147(4) . ? O1 C1 1.203(5) . ? O2 C2 1.205(5) . ? O3 C25 1.140(5) . ? O4 C26 1.156(5) . ? C1 C3 1.489(5) . ? C2 C9 1.481(6) . ? C3 C4 1.376(5) . ? C3 C8 1.394(5) . ? C4 C5 1.383(6) . ? C5 C6 1.368(7) . ? C6 C7 1.357(7) . ? C7 C8 1.386(6) . ? C9 C14 1.382(6) . ? C9 C10 1.384(6) . ? C10 C11 1.406(7) . ? C11 C12 1.372(8) . ? C12 C13 1.340(8) . ? C13 C14 1.405(7) . ? C15 C19 1.409(6) . ? C15 C16 1.417(6) . ? C15 C20 1.503(5) . ? C16 C17 1.422(6) . ? C16 C21 1.498(6) . ? C17 C18 1.412(6) . ? C17 C22 1.520(6) . ? C18 C19 1.431(6) . ? C18 C23 1.506(6) . ? C19 C24 1.508(6) . ? 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 C2 92.54(17) . . ? C1 As1 Fe1 109.84(11) . . ? C2 As1 Fe1 104.00(13) . . ? C26 Fe1 C25 94.2(2) . . ? C26 Fe1 C17 111.74(19) . . ? C25 Fe1 C17 97.2(2) . . ? C26 Fe1 C19 105.5(2) . . ? C25 Fe1 C19 157.81(19) . . ? C17 Fe1 C19 66.31(18) . . ? C26 Fe1 C18 89.67(19) . . ? C25 Fe1 C18 132.7(2) . . ? C17 Fe1 C18 39.29(18) . . ? C19 Fe1 C18 39.75(16) . . ? C26 Fe1 C16 151.15(18) . . ? C25 Fe1 C16 91.97(18) . . ? C17 Fe1 C16 39.44(16) . . ? C19 Fe1 C16 65.85(17) . . ? C18 Fe1 C16 65.89(17) . . ? C26 Fe1 C15 143.8(2) . . ? C25 Fe1 C15 121.97(19) . . ? C17 Fe1 C15 65.33(16) . . ? C19 Fe1 C15 38.71(16) . . ? C18 Fe1 C15 65.25(16) . . ? C16 Fe1 C15 38.78(15) . . ? C26 Fe1 As1 93.63(13) . . ? C25 Fe1 As1 93.36(14) . . ? C17 Fe1 As1 151.59(12) . . ? C19 Fe1 As1 95.47(13) . . ? C18 Fe1 As1 133.53(14) . . ? C16 Fe1 As1 114.14(12) . . ? C15 Fe1 As1 86.73(11) . . ? O1 C1 C3 120.7(4) . . ? O1 C1 As1 121.2(3) . . ? C3 C1 As1 118.0(3) . . ? O2 C2 C9 120.7(4) . . ? O2 C2 As1 120.7(3) . . ? C9 C2 As1 118.3(3) . . ? C4 C3 C8 119.2(4) . . ? C4 C3 C1 122.3(4) . . ? C8 C3 C1 118.5(4) . . ? C3 C4 C5 120.0(4) . . ? C6 C5 C4 120.8(5) . . ? C7 C6 C5 119.5(5) . . ? C6 C7 C8 121.1(5) . . ? C7 C8 C3 119.4(5) . . ? C14 C9 C10 119.2(5) . . ? C14 C9 C2 118.9(4) . . ? C10 C9 C2 121.8(4) . . ? C9 C10 C11 119.8(5) . . ? C12 C11 C10 119.7(6) . . ? C13 C12 C11 121.0(6) . . ? C12 C13 C14 120.4(6) . . ? C9 C14 C13 119.9(6) . . ? C19 C15 C16 108.6(4) . . ? C19 C15 C20 126.0(4) . . ? C16 C15 C20 125.2(4) . . ? C19 C15 Fe1 69.0(2) . . ? C16 C15 Fe1 69.6(2) . . ? C20 C15 Fe1 131.2(3) . . ? C15 C16 C17 107.5(4) . . ? C15 C16 C21 125.2(4) . . ? C17 C16 C21 127.2(4) . . ? C15 C16 Fe1 71.6(2) . . ? C17 C16 Fe1 69.2(2) . . ? C21 C16 Fe1 128.2(3) . . ? C18 C17 C16 108.4(4) . . ? C18 C17 C22 126.1(5) . . ? C16 C17 C22 125.2(5) . . ? C18 C17 Fe1 70.9(2) . . ? C16 C17 Fe1 71.3(2) . . ? C22 C17 Fe1 128.6(3) . . ? C17 C18 C19 107.7(4) . . ? C17 C18 C23 125.7(4) . . ? C19 C18 C23 126.5(5) . . ? C17 C18 Fe1 69.8(2) . . ? C19 C18 Fe1 70.0(2) . . ? C23 C18 Fe1 128.3(3) . . ? C15 C19 C18 107.7(4) . . ? C15 C19 C24 125.8(4) . . ? C18 C19 C24 126.0(4) . . ? C15 C19 Fe1 72.3(2) . . ? C18 C19 Fe1 70.2(2) . . ? C24 C19 Fe1 128.8(3) . . ? O3 C25 Fe1 174.2(4) . . ? O4 C26 Fe1 175.2(4) . . ? 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 Fe1 C26 -37.0(2) . . . . ? C2 As1 Fe1 C26 -134.98(19) . . . . ? C1 As1 Fe1 C25 57.37(19) . . . . ? C2 As1 Fe1 C25 -40.59(18) . . . . ? C1 As1 Fe1 C17 169.2(3) . . . . ? C2 As1 Fe1 C17 71.2(3) . . . . ? C1 As1 Fe1 C19 -143.01(19) . . . . ? C2 As1 Fe1 C19 119.02(18) . . . . ? C1 As1 Fe1 C18 -130.0(2) . . . . ? C2 As1 Fe1 C18 132.0(2) . . . . ? C1 As1 Fe1 C16 151.04(19) . . . . ? C2 As1 Fe1 C16 53.08(18) . . . . ? C1 As1 Fe1 C15 179.24(18) . . . . ? C2 As1 Fe1 C15 81.27(17) . . . . ? C2 As1 C1 O1 2.2(4) . . . . ? Fe1 As1 C1 O1 -103.7(3) . . . . ? C2 As1 C1 C3 -174.8(3) . . . . ? Fe1 As1 C1 C3 79.3(3) . . . . ? C1 As1 C2 O2 -113.0(4) . . . . ? Fe1 As1 C2 O2 -1.8(4) . . . . ? C1 As1 C2 C9 72.5(3) . . . . ? Fe1 As1 C2 C9 -176.3(3) . . . . ? O1 C1 C3 C4 -168.2(4) . . . . ? As1 C1 C3 C4 8.8(5) . . . . ? O1 C1 C3 C8 11.4(6) . . . . ? As1 C1 C3 C8 -171.6(3) . . . . ? C8 C3 C4 C5 1.5(6) . . . . ? C1 C3 C4 C5 -178.9(4) . . . . ? C3 C4 C5 C6 -0.7(7) . . . . ? C4 C5 C6 C7 -0.1(8) . . . . ? C5 C6 C7 C8 0.0(8) . . . . ? C6 C7 C8 C3 0.8(7) . . . . ? C4 C3 C8 C7 -1.6(6) . . . . ? C1 C3 C8 C7 178.8(4) . . . . ? O2 C2 C9 C14 7.2(6) . . . . ? As1 C2 C9 C14 -178.3(3) . . . . ? O2 C2 C9 C10 -169.4(4) . . . . ? As1 C2 C9 C10 5.1(5) . . . . ? C14 C9 C10 C11 1.5(7) . . . . ? C2 C9 C10 C11 178.1(4) . . . . ? C9 C10 C11 C12 -1.3(8) . . . . ? C10 C11 C12 C13 0.5(9) . . . . ? C11 C12 C13 C14 0.1(10) . . . . ? C10 C9 C14 C13 -0.9(7) . . . . ? C2 C9 C14 C13 -177.6(4) . . . . ? C12 C13 C14 C9 0.1(9) . . . . ? C26 Fe1 C15 C19 11.3(4) . . . . ? C25 Fe1 C15 C19 -165.1(3) . . . . ? C17 Fe1 C15 C19 -82.3(3) . . . . ? C18 Fe1 C15 C19 -38.9(3) . . . . ? C16 Fe1 C15 C19 -120.6(4) . . . . ? As1 Fe1 C15 C19 102.9(2) . . . . ? C26 Fe1 C15 C16 131.8(3) . . . . ? C25 Fe1 C15 C16 -44.6(3) . . . . ? C17 Fe1 C15 C16 38.3(3) . . . . ? C19 Fe1 C15 C16 120.6(4) . . . . ? C18 Fe1 C15 C16 81.7(3) . . . . ? As1 Fe1 C15 C16 -136.5(2) . . . . ? C26 Fe1 C15 C20 -108.8(5) . . . . ? C25 Fe1 C15 C20 74.8(5) . . . . ? C17 Fe1 C15 C20 157.7(5) . . . . ? C19 Fe1 C15 C20 -120.0(6) . . . . ? C18 Fe1 C15 C20 -158.9(5) . . . . ? C16 Fe1 C15 C20 119.4(6) . . . . ? As1 Fe1 C15 C20 -17.1(4) . . . . ? C19 C15 C16 C17 -2.2(5) . . . . ? C20 C15 C16 C17 173.1(4) . . . . ? Fe1 C15 C16 C17 -60.3(3) . . . . ? C19 C15 C16 C21 -177.7(4) . . . . ? C20 C15 C16 C21 -2.4(7) . . . . ? Fe1 C15 C16 C21 124.3(4) . . . . ? C19 C15 C16 Fe1 58.0(3) . . . . ? C20 C15 C16 Fe1 -126.7(4) . . . . ? C26 Fe1 C16 C15 -114.3(4) . . . . ? C25 Fe1 C16 C15 143.4(3) . . . . ? C17 Fe1 C16 C15 -117.7(4) . . . . ? C19 Fe1 C16 C15 -36.2(2) . . . . ? C18 Fe1 C16 C15 -79.9(3) . . . . ? As1 Fe1 C16 C15 48.9(3) . . . . ? C26 Fe1 C16 C17 3.4(5) . . . . ? C25 Fe1 C16 C17 -98.9(3) . . . . ? C19 Fe1 C16 C17 81.5(3) . . . . ? C18 Fe1 C16 C17 37.7(3) . . . . ? C15 Fe1 C16 C17 117.7(4) . . . . ? As1 Fe1 C16 C17 166.5(2) . . . . ? C26 Fe1 C16 C21 125.0(5) . . . . ? C25 Fe1 C16 C21 22.7(4) . . . . ? C17 Fe1 C16 C21 121.6(5) . . . . ? C19 Fe1 C16 C21 -156.9(5) . . . . ? C18 Fe1 C16 C21 159.4(5) . . . . ? C15 Fe1 C16 C21 -120.7(5) . . . . ? As1 Fe1 C16 C21 -71.9(4) . . . . ? C15 C16 C17 C18 0.3(5) . . . . ? C21 C16 C17 C18 175.6(4) . . . . ? Fe1 C16 C17 C18 -61.5(3) . . . . ? C15 C16 C17 C22 -173.6(4) . . . . ? C21 C16 C17 C22 1.8(7) . . . . ? Fe1 C16 C17 C22 124.6(4) . . . . ? C15 C16 C17 Fe1 61.8(3) . . . . ? C21 C16 C17 Fe1 -122.9(4) . . . . ? C26 Fe1 C17 C18 -60.2(3) . . . . ? C25 Fe1 C17 C18 -157.6(3) . . . . ? C19 Fe1 C17 C18 37.8(3) . . . . ? C16 Fe1 C17 C18 118.1(4) . . . . ? C15 Fe1 C17 C18 80.4(3) . . . . ? As1 Fe1 C17 C18 91.5(4) . . . . ? C26 Fe1 C17 C16 -178.2(3) . . . . ? C25 Fe1 C17 C16 84.3(3) . . . . ? C19 Fe1 C17 C16 -80.2(3) . . . . ? C18 Fe1 C17 C16 -118.1(4) . . . . ? C15 Fe1 C17 C16 -37.6(2) . . . . ? As1 Fe1 C17 C16 -26.6(5) . . . . ? C26 Fe1 C17 C22 61.2(5) . . . . ? C25 Fe1 C17 C22 -36.2(5) . . . . ? C19 Fe1 C17 C22 159.2(5) . . . . ? C18 Fe1 C17 C22 121.4(6) . . . . ? C16 Fe1 C17 C22 -120.5(6) . . . . ? C15 Fe1 C17 C22 -158.2(5) . . . . ? As1 Fe1 C17 C22 -147.1(3) . . . . ? C16 C17 C18 C19 1.7(5) . . . . ? C22 C17 C18 C19 175.5(4) . . . . ? Fe1 C17 C18 C19 -60.1(3) . . . . ? C16 C17 C18 C23 -174.9(4) . . . . ? C22 C17 C18 C23 -1.1(7) . . . . ? Fe1 C17 C18 C23 123.3(5) . . . . ? C16 C17 C18 Fe1 61.8(3) . . . . ? C22 C17 C18 Fe1 -124.4(4) . . . . ? C26 Fe1 C18 C17 126.3(3) . . . . ? C25 Fe1 C18 C17 30.9(4) . . . . ? C19 Fe1 C18 C17 -118.5(4) . . . . ? C16 Fe1 C18 C17 -37.9(2) . . . . ? C15 Fe1 C18 C17 -80.7(3) . . . . ? As1 Fe1 C18 C17 -139.0(2) . . . . ? C26 Fe1 C18 C19 -115.2(3) . . . . ? C25 Fe1 C18 C19 149.5(3) . . . . ? C17 Fe1 C18 C19 118.5(4) . . . . ? C16 Fe1 C18 C19 80.6(3) . . . . ? C15 Fe1 C18 C19 37.9(3) . . . . ? As1 Fe1 C18 C19 -20.5(3) . . . . ? C26 Fe1 C18 C23 6.1(5) . . . . ? C25 Fe1 C18 C23 -89.2(5) . . . . ? C17 Fe1 C18 C23 -120.2(6) . . . . ? C19 Fe1 C18 C23 121.3(6) . . . . ? C16 Fe1 C18 C23 -158.1(5) . . . . ? C15 Fe1 C18 C23 159.2(5) . . . . ? As1 Fe1 C18 C23 100.8(5) . . . . ? C16 C15 C19 C18 3.3(4) . . . . ? C20 C15 C19 C18 -172.0(4) . . . . ? Fe1 C15 C19 C18 61.7(3) . . . . ? C16 C15 C19 C24 176.0(4) . . . . ? C20 C15 C19 C24 0.8(7) . . . . ? Fe1 C15 C19 C24 -125.6(5) . . . . ? C16 C15 C19 Fe1 -58.4(3) . . . . ? C20 C15 C19 Fe1 126.4(4) . . . . ? C17 C18 C19 C15 -3.1(5) . . . . ? C23 C18 C19 C15 173.5(4) . . . . ? Fe1 C18 C19 C15 -63.0(3) . . . . ? C17 C18 C19 C24 -175.8(4) . . . . ? C23 C18 C19 C24 0.8(7) . . . . ? Fe1 C18 C19 C24 124.2(5) . . . . ? C17 C18 C19 Fe1 59.9(3) . . . . ? C23 C18 C19 Fe1 -123.5(5) . . . . ? C26 Fe1 C19 C15 -173.1(3) . . . . ? C25 Fe1 C19 C15 35.2(6) . . . . ? C17 Fe1 C19 C15 79.5(3) . . . . ? C18 Fe1 C19 C15 117.0(4) . . . . ? C16 Fe1 C19 C15 36.2(2) . . . . ? As1 Fe1 C19 C15 -77.8(2) . . . . ? C26 Fe1 C19 C18 69.9(3) . . . . ? C25 Fe1 C19 C18 -81.8(6) . . . . ? C17 Fe1 C19 C18 -37.4(3) . . . . ? C16 Fe1 C19 C18 -80.7(3) . . . . ? C15 Fe1 C19 C18 -117.0(4) . . . . ? As1 Fe1 C19 C18 165.2(3) . . . . ? C26 Fe1 C19 C24 -51.0(5) . . . . ? C25 Fe1 C19 C24 157.3(5) . . . . ? C17 Fe1 C19 C24 -158.3(5) . . . . ? C18 Fe1 C19 C24 -120.9(6) . . . . ? C16 Fe1 C19 C24 158.4(5) . . . . ? C15 Fe1 C19 C24 122.2(5) . . . . ? As1 Fe1 C19 C24 44.3(4) . . . . ? C26 Fe1 C25 O3 -83(4) . . . . ? C17 Fe1 C25 O3 30(4) . . . . ? C19 Fe1 C25 O3 70(4) . . . . ? C18 Fe1 C25 O3 11(4) . . . . ? C16 Fe1 C25 O3 69(4) . . . . ? C15 Fe1 C25 O3 95(4) . . . . ? As1 Fe1 C25 O3 -176(4) . . . . ? C25 Fe1 C26 O4 88(5) . . . . ? C17 Fe1 C26 O4 -11(5) . . . . ? C19 Fe1 C26 O4 -82(5) . . . . ? C18 Fe1 C26 O4 -45(5) . . . . ? C16 Fe1 C26 O4 -14(6) . . . . ? C15 Fe1 C26 O4 -89(5) . . . . ? As1 Fe1 C26 O4 -178(100) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.654 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.067 data_compound 11 _database_code_CSD 165259 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H46 As2 Fe O6' _chemical_formula_weight 636.30 _chemical_melting_point ? _chemical_compound_source ? 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.971(2) _cell_length_b 15.347(3) _cell_length_c 18.694(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.61(3) _cell_angle_gamma 90.00 _cell_volume 3144.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method ? _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.599 _exptl_absorpt_correction_type Difabs _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.57 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4-turbo _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6207 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.22 _reflns_number_total 5649 _reflns_number_observed 4234 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+3.3737P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5649 _refine_ls_number_parameters 312 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_obs 0.0482 _refine_ls_wR_factor_all 0.1398 _refine_ls_wR_factor_obs 0.1304 _refine_ls_goodness_of_fit_all 1.097 _refine_ls_goodness_of_fit_obs 1.192 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.230 _refine_ls_shift/esd_max -0.014 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.36787(5) 0.80008(4) 0.02908(3) 0.0315(2) Uani 1 d . . As1 As 0.06672(5) 0.66432(4) 0.02365(3) 0.0520(2) Uani 1 d . . As2 As 0.49045(4) 0.83490(3) 0.22329(2) 0.0394(2) Uani 1 d . . O1 O 0.3159(3) 0.6851(2) 0.0711(2) 0.0463(8) Uani 1 d . . O2 O 0.2087(3) 0.8048(2) -0.0280(2) 0.0357(7) Uani 1 d . . O3 O 0.5377(3) 0.7968(2) 0.0779(2) 0.0371(7) Uani 1 d . . O4 O 0.3126(3) 0.8724(2) 0.1130(2) 0.0405(8) Uani 1 d . . O5 O 0.4553(3) 0.7490(3) -0.0647(2) 0.0599(11) Uani 1 d . . O6 O 0.4145(3) 0.9166(2) -0.0328(2) 0.0492(9) Uani 1 d . . C1 C 0.2179(5) 0.6428(3) 0.0751(3) 0.0433(12) Uani 1 d . . C2 C 0.1082(4) 0.7659(3) -0.0286(2) 0.0328(10) Uani 1 d . . C3 C 0.2243(6) 0.5651(3) 0.1272(3) 0.059(2) Uani 1 d . . C4 C 0.0961(9) 0.5360(7) 0.1501(6) 0.139(4) Uani 1 d U . H4A H 0.0515(31) 0.5111(52) 0.1097(14) 0.209 Uiso 1 calc R . H4B H 0.0526(32) 0.5855(13) 0.1672(44) 0.209 Uiso 1 calc R . H4C H 0.1051(9) 0.4933(44) 0.1876(34) 0.209 Uiso 1 calc R . C5 C 0.2819(12) 0.5897(8) 0.1930(6) 0.160(4) Uani 1 d U . H5A H 0.2490(69) 0.6442(37) 0.2083(29) 0.240 Uiso 1 calc R . H5B H 0.3680(17) 0.5958(68) 0.1873(16) 0.240 Uiso 1 calc R . H5C H 0.2680(86) 0.5458(36) 0.2283(16) 0.240 Uiso 1 calc R . C6 C 0.2682(11) 0.4897(6) 0.0899(6) 0.148(4) Uani 1 d U . H6A H 0.2120(44) 0.4755(38) 0.0508(32) 0.222 Uiso 1 calc R . H6B H 0.2751(85) 0.4413(18) 0.1223(15) 0.222 Uiso 1 calc R . H6C H 0.3468(39) 0.5024(22) 0.0718(44) 0.222 Uiso 1 calc R . C7 C 0.0068(4) 0.8085(3) -0.0759(2) 0.0347(10) Uani 1 d . . C8 C -0.0200(4) 0.8954(3) -0.0401(3) 0.0470(12) Uani 1 d . . H8A H -0.0838(23) 0.9250(11) -0.0672(11) 0.070 Uiso 1 calc R . H8B H 0.0523(10) 0.9306(10) -0.0382(17) 0.070 Uiso 1 calc R . H8C H -0.0454(31) 0.8850(3) 0.0076(7) 0.070 Uiso 1 calc R . C9 C 0.0549(5) 0.8241(4) -0.1500(3) 0.0542(14) Uani 1 d . . H9A H 0.0707(35) 0.7692(4) -0.1723(9) 0.081 Uiso 1 calc R . H9B H 0.1291(21) 0.8573(23) -0.1456(3) 0.081 Uiso 1 calc R . H9C H -0.0047(16) 0.8558(24) -0.1788(8) 0.081 Uiso 1 calc R . C10 C -0.1105(4) 0.7543(4) -0.0827(3) 0.0527(14) Uani 1 d . . H10A H -0.0942(9) 0.7002(11) -0.1062(18) 0.079 Uiso 1 calc R . H10B H -0.1718(12) 0.7860(11) -0.1102(18) 0.079 Uiso 1 calc R . H10C H -0.1390(20) 0.7427(21) -0.0358(3) 0.079 Uiso 1 calc R . C11 C 0.5756(4) 0.7973(3) 0.1430(2) 0.0336(9) Uani 1 d . . C12 C 0.3394(4) 0.8745(3) 0.1782(2) 0.0317(9) Uani 1 d . . C13 C 0.7069(4) 0.7627(3) 0.1561(2) 0.0385(11) Uani 1 d . . C14 C 0.7137(5) 0.6706(4) 0.1255(3) 0.060(2) Uani 1 d . . H14A H 0.6598(28) 0.6330(7) 0.1503(15) 0.089 Uiso 1 calc R . H14B H 0.7958(9) 0.6493(11) 0.1316(20) 0.089 Uiso 1 calc R . H14C H 0.6898(36) 0.6717(6) 0.0755(6) 0.089 Uiso 1 calc R . C15 C 0.7917(5) 0.8226(4) 0.1169(3) 0.063(2) Uani 1 d . . H15A H 0.7632(23) 0.8279(23) 0.0678(6) 0.094 Uiso 1 calc R . H15B H 0.8726(10) 0.7986(15) 0.1191(21) 0.094 Uiso 1 calc R . H15C H 0.7928(31) 0.8790(9) 0.1391(15) 0.094 Uiso 1 calc R . C16 C 0.7488(5) 0.7610(4) 0.2348(3) 0.058(2) Uani 1 d . . H16A H 0.6972(24) 0.7227(21) 0.2604(5) 0.087 Uiso 1 calc R . H16B H 0.7442(36) 0.8187(6) 0.2543(6) 0.087 Uiso 1 calc R . H16C H 0.8315(14) 0.7406(27) 0.2392(3) 0.087 Uiso 1 calc R . C17 C 0.2456(4) 0.9163(3) 0.2245(3) 0.0440(12) Uani 1 d . . C18 C 0.2691(5) 0.8992(5) 0.3044(3) 0.064(2) Uani 1 d . . H18A H 0.2060(22) 0.9260(24) 0.3307(3) 0.096 Uiso 1 calc R . H18B H 0.3468(19) 0.9233(25) 0.3197(6) 0.096 Uiso 1 calc R . H18C H 0.2694(39) 0.8375(5) 0.3130(4) 0.096 Uiso 1 calc R . C19 C 0.1192(5) 0.8818(5) 0.2008(4) 0.070(2) Uani 1 d . . H19A H 0.0584(6) 0.9092(23) 0.2285(17) 0.106 Uiso 1 calc R . H19B H 0.1167(14) 0.8199(7) 0.2080(23) 0.106 Uiso 1 calc R . H19C H 0.1032(18) 0.8946(27) 0.1510(7) 0.106 Uiso 1 calc R . C20 C 0.2514(6) 1.0144(4) 0.2106(3) 0.068(2) Uani 1 d . . H20A H 0.1873(26) 1.0431(5) 0.2348(20) 0.102 Uiso 1 calc R . H20B H 0.2416(41) 1.0252(4) 0.1601(4) 0.102 Uiso 1 calc R . H20C H 0.3290(17) 1.0366(6) 0.2281(22) 0.102 Uiso 1 calc R . C21 C 0.5186(7) 0.6702(5) -0.0615(4) 0.091(3) Uani 1 d . . H21A H 0.5361(47) 0.6520(20) -0.1091(4) 0.137 Uiso 1 calc R . H21B H 0.4698(22) 0.6268(11) -0.0395(28) 0.137 Uiso 1 calc R . H21C H 0.5937(25) 0.6777(11) -0.0337(27) 0.137 Uiso 1 calc R . C22 C 0.5202(6) 0.8185(5) -0.0993(3) 0.076(2) Uani 1 d . . H22A H 0.5395(6) 0.8009(5) -0.1474(3) 0.091 Uiso 1 calc R . H22B H 0.5960(6) 0.8309(5) -0.0725(3) 0.091 Uiso 1 calc R . C24 C 0.3377(5) 0.9925(4) -0.0305(4) 0.071(2) Uani 1 d . . H24A H 0.3136(34) 1.0017(17) 0.0176(6) 0.106 Uiso 1 calc R . H24B H 0.2665(21) 0.9841(13) -0.0615(19) 0.106 Uiso 1 calc R . H24C H 0.3819(15) 1.0425(6) -0.0461(23) 0.106 Uiso 1 calc R . C23 C 0.4431(6) 0.8965(5) -0.1024(3) 0.074(2) Uani 1 d . . H23A H 0.4864(6) 0.9446(5) -0.1234(3) 0.089 Uiso 1 calc R . H23B H 0.3693(6) 0.8855(5) -0.1316(3) 0.089 Uiso 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 Fe1 0.0247(3) 0.0386(4) 0.0305(3) 0.0004(3) -0.0068(2) 0.0022(3) As1 0.0459(3) 0.0414(3) 0.0674(4) 0.0111(3) -0.0119(3) -0.0130(2) As2 0.0338(3) 0.0543(3) 0.0294(3) -0.0003(2) -0.0057(2) 0.0097(2) O1 0.045(2) 0.038(2) 0.055(2) 0.011(2) -0.009(2) 0.005(2) O2 0.028(2) 0.038(2) 0.040(2) 0.0046(14) -0.0103(13) -0.0042(13) O3 0.0260(15) 0.055(2) 0.030(2) 0.0028(14) -0.0070(12) 0.0022(14) O4 0.037(2) 0.047(2) 0.037(2) -0.0032(14) -0.0081(13) 0.0149(15) O5 0.048(2) 0.087(3) 0.044(2) -0.018(2) -0.010(2) 0.023(2) O6 0.037(2) 0.065(2) 0.044(2) 0.016(2) -0.0089(15) -0.013(2) C1 0.057(3) 0.026(2) 0.047(3) -0.002(2) -0.005(2) 0.004(2) C2 0.031(2) 0.033(2) 0.034(2) -0.006(2) -0.002(2) -0.001(2) C3 0.086(4) 0.029(3) 0.060(4) 0.009(2) -0.013(3) -0.006(3) C4 0.131(7) 0.132(7) 0.157(7) 0.079(6) 0.026(6) 0.011(6) C5 0.206(8) 0.128(6) 0.140(6) 0.054(6) -0.048(6) -0.047(6) C6 0.204(8) 0.086(6) 0.157(7) 0.041(5) 0.055(7) 0.051(6) C7 0.023(2) 0.046(3) 0.034(2) -0.007(2) -0.006(2) 0.001(2) C8 0.039(3) 0.042(3) 0.059(3) -0.000(2) -0.005(2) 0.011(2) C9 0.040(3) 0.085(4) 0.037(3) 0.003(3) -0.011(2) 0.006(3) C10 0.034(3) 0.067(4) 0.056(3) -0.003(3) -0.019(2) -0.007(2) C11 0.026(2) 0.034(2) 0.040(2) 0.008(2) -0.006(2) 0.001(2) C12 0.033(2) 0.024(2) 0.037(3) -0.000(2) -0.004(2) 0.003(2) C13 0.027(2) 0.051(3) 0.036(2) 0.006(2) -0.009(2) 0.006(2) C14 0.054(3) 0.062(4) 0.061(4) -0.006(3) -0.018(3) 0.025(3) C15 0.029(3) 0.087(5) 0.072(4) 0.024(3) -0.001(2) 0.004(3) C16 0.042(3) 0.093(4) 0.039(3) 0.004(3) -0.015(2) 0.017(3) C17 0.036(2) 0.052(3) 0.044(3) -0.010(2) -0.003(2) 0.009(2) C18 0.055(3) 0.093(5) 0.045(3) -0.006(3) 0.006(3) 0.022(3) C19 0.033(3) 0.103(5) 0.075(4) -0.027(4) 0.002(3) 0.001(3) C20 0.079(4) 0.052(4) 0.074(4) -0.015(3) 0.001(3) 0.025(3) C21 0.087(5) 0.124(7) 0.060(4) -0.043(4) -0.031(4) 0.055(5) C22 0.056(4) 0.123(6) 0.049(4) -0.021(4) 0.016(3) -0.028(4) C24 0.048(3) 0.050(3) 0.112(5) 0.038(3) -0.024(3) -0.010(3) C23 0.053(4) 0.113(6) 0.056(4) 0.016(4) -0.002(3) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 2.006(3) . ? Fe1 O1 2.025(3) . ? Fe1 O4 2.036(3) . ? Fe1 O3 2.038(3) . ? Fe1 O5 2.183(4) . ? Fe1 O6 2.203(3) . ? As1 C2 1.906(5) . ? As1 C1 1.908(5) . ? As2 C11 1.893(5) . ? As2 C12 1.923(4) . ? O1 C1 1.260(6) . ? O2 C2 1.253(5) . ? O3 C11 1.268(5) . ? O4 C12 1.240(5) . ? O5 C21 1.394(7) . ? O5 C22 1.451(8) . ? O6 C23 1.388(7) . ? O6 C24 1.439(7) . ? C1 C3 1.540(7) . ? C2 C7 1.535(6) . ? C3 C5 1.408(11) . ? C3 C6 1.445(11) . ? C3 C4 1.554(11) . ? C7 C9 1.523(7) . ? C7 C8 1.526(7) . ? C7 C10 1.533(6) . ? C11 C13 1.544(6) . ? C12 C17 1.519(6) . ? C13 C16 1.520(6) . ? C13 C15 1.520(7) . ? C13 C14 1.528(7) . ? C17 C18 1.526(7) . ? C17 C20 1.530(8) . ? C17 C19 1.531(7) . ? C22 C23 1.465(10) . ? 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 O2 Fe1 O1 89.06(13) . . ? O2 Fe1 O4 96.19(13) . . ? O1 Fe1 O4 94.43(14) . . ? O2 Fe1 O3 174.42(12) . . ? O1 Fe1 O3 94.17(13) . . ? O4 Fe1 O3 88.10(12) . . ? O2 Fe1 O5 89.38(13) . . ? O1 Fe1 O5 98.1(2) . . ? O4 Fe1 O5 166.4(2) . . ? O3 Fe1 O5 85.67(13) . . ? O2 Fe1 O6 84.76(12) . . ? O1 Fe1 O6 171.05(14) . . ? O4 Fe1 O6 92.68(14) . . ? O3 Fe1 O6 91.50(12) . . ? O5 Fe1 O6 75.4(2) . . ? C2 As1 C1 100.2(2) . . ? C11 As2 C12 101.2(2) . . ? C1 O1 Fe1 136.7(3) . . ? C2 O2 Fe1 137.1(3) . . ? C11 O3 Fe1 133.0(3) . . ? C12 O4 Fe1 134.8(3) . . ? C21 O5 C22 113.7(5) . . ? C21 O5 Fe1 120.9(4) . . ? C22 O5 Fe1 109.7(3) . . ? C23 O6 C24 111.5(5) . . ? C23 O6 Fe1 112.3(4) . . ? C24 O6 Fe1 119.4(3) . . ? O1 C1 C3 115.0(5) . . ? O1 C1 As1 127.2(4) . . ? C3 C1 As1 117.8(4) . . ? O2 C2 C7 114.6(4) . . ? O2 C2 As1 127.9(3) . . ? C7 C2 As1 117.4(3) . . ? C5 C3 C6 119.3(9) . . ? C5 C3 C1 110.5(6) . . ? C6 C3 C1 108.7(6) . . ? C5 C3 C4 102.3(8) . . ? C6 C3 C4 103.2(7) . . ? C1 C3 C4 112.4(5) . . ? C9 C7 C8 110.1(4) . . ? C9 C7 C10 109.6(4) . . ? C8 C7 C10 109.4(4) . . ? C9 C7 C2 108.6(4) . . ? C8 C7 C2 105.6(3) . . ? C10 C7 C2 113.5(4) . . ? O3 C11 C13 114.4(4) . . ? O3 C11 As2 127.7(3) . . ? C13 C11 As2 118.0(3) . . ? O4 C12 C17 115.8(4) . . ? O4 C12 As2 125.7(3) . . ? C17 C12 As2 118.4(3) . . ? C16 C13 C15 108.1(4) . . ? C16 C13 C14 109.2(4) . . ? C15 C13 C14 109.7(5) . . ? C16 C13 C11 113.5(4) . . ? C15 C13 C11 107.6(4) . . ? C14 C13 C11 108.7(4) . . ? C12 C17 C18 113.4(4) . . ? C12 C17 C20 106.5(4) . . ? C18 C17 C20 109.3(5) . . ? C12 C17 C19 108.5(4) . . ? C18 C17 C19 109.5(5) . . ? C20 C17 C19 109.6(5) . . ? O5 C22 C23 108.9(5) . . ? O6 C23 C22 107.5(5) . . ? 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 O2 Fe1 O1 C1 -15.1(5) . . . . ? O4 Fe1 O1 C1 81.1(5) . . . . ? O3 Fe1 O1 C1 169.5(5) . . . . ? O5 Fe1 O1 C1 -104.3(5) . . . . ? O6 Fe1 O1 C1 -61.3(11) . . . . ? O1 Fe1 O2 C2 13.3(4) . . . . ? O4 Fe1 O2 C2 -81.1(4) . . . . ? O3 Fe1 O2 C2 138.7(13) . . . . ? O5 Fe1 O2 C2 111.3(4) . . . . ? O6 Fe1 O2 C2 -173.2(4) . . . . ? O2 Fe1 O3 C11 171.7(12) . . . . ? O1 Fe1 O3 C11 -63.1(4) . . . . ? O4 Fe1 O3 C11 31.2(4) . . . . ? O5 Fe1 O3 C11 -160.9(4) . . . . ? O6 Fe1 O3 C11 123.9(4) . . . . ? O2 Fe1 O4 C12 149.5(4) . . . . ? O1 Fe1 O4 C12 59.9(4) . . . . ? O3 Fe1 O4 C12 -34.1(4) . . . . ? O5 Fe1 O4 C12 -96.8(7) . . . . ? O6 Fe1 O4 C12 -125.5(4) . . . . ? O2 Fe1 O5 C21 -124.0(5) . . . . ? O1 Fe1 O5 C21 -35.0(5) . . . . ? O4 Fe1 O5 C21 121.5(7) . . . . ? O3 Fe1 O5 C21 58.6(5) . . . . ? O6 Fe1 O5 C21 151.3(5) . . . . ? O2 Fe1 O5 C22 100.6(4) . . . . ? O1 Fe1 O5 C22 -170.4(4) . . . . ? O4 Fe1 O5 C22 -13.8(7) . . . . ? O3 Fe1 O5 C22 -76.8(4) . . . . ? O6 Fe1 O5 C22 15.9(4) . . . . ? O2 Fe1 O6 C23 -75.7(3) . . . . ? O1 Fe1 O6 C23 -29.2(10) . . . . ? O4 Fe1 O6 C23 -171.7(3) . . . . ? O3 Fe1 O6 C23 100.1(3) . . . . ? O5 Fe1 O6 C23 15.0(3) . . . . ? O2 Fe1 O6 C24 57.6(4) . . . . ? O1 Fe1 O6 C24 104.1(9) . . . . ? O4 Fe1 O6 C24 -38.3(4) . . . . ? O3 Fe1 O6 C24 -126.5(4) . . . . ? O5 Fe1 O6 C24 148.4(4) . . . . ? Fe1 O1 C1 C3 -168.1(4) . . . . ? Fe1 O1 C1 As1 12.6(7) . . . . ? C2 As1 C1 O1 -2.2(5) . . . . ? C2 As1 C1 C3 178.5(4) . . . . ? Fe1 O2 C2 C7 168.6(3) . . . . ? Fe1 O2 C2 As1 -9.3(7) . . . . ? C1 As1 C2 O2 0.6(4) . . . . ? C1 As1 C2 C7 -177.2(3) . . . . ? O1 C1 C3 C5 46.6(9) . . . . ? As1 C1 C3 C5 -134.0(8) . . . . ? O1 C1 C3 C6 -86.2(7) . . . . ? As1 C1 C3 C6 93.2(7) . . . . ? O1 C1 C3 C4 160.1(7) . . . . ? As1 C1 C3 C4 -20.5(8) . . . . ? O2 C2 C7 C9 51.2(5) . . . . ? As1 C2 C7 C9 -130.7(4) . . . . ? O2 C2 C7 C8 -66.8(5) . . . . ? As1 C2 C7 C8 111.3(4) . . . . ? O2 C2 C7 C10 173.4(4) . . . . ? As1 C2 C7 C10 -8.5(5) . . . . ? Fe1 O3 C11 C13 159.9(3) . . . . ? Fe1 O3 C11 As2 -20.0(6) . . . . ? C12 As2 C11 O3 -2.2(5) . . . . ? C12 As2 C11 C13 177.9(3) . . . . ? Fe1 O4 C12 C17 -159.2(3) . . . . ? Fe1 O4 C12 As2 23.9(6) . . . . ? C11 As2 C12 O4 0.7(4) . . . . ? C11 As2 C12 C17 -176.1(3) . . . . ? O3 C11 C13 C16 -178.0(4) . . . . ? As2 C11 C13 C16 1.9(6) . . . . ? O3 C11 C13 C15 62.4(6) . . . . ? As2 C11 C13 C15 -117.7(4) . . . . ? O3 C11 C13 C14 -56.4(5) . . . . ? As2 C11 C13 C14 123.6(4) . . . . ? O4 C12 C17 C18 167.0(5) . . . . ? As2 C12 C17 C18 -15.9(6) . . . . ? O4 C12 C17 C20 -72.8(5) . . . . ? As2 C12 C17 C20 104.3(4) . . . . ? O4 C12 C17 C19 45.1(6) . . . . ? As2 C12 C17 C19 -137.8(4) . . . . ? C21 O5 C22 C23 177.5(5) . . . . ? Fe1 O5 C22 C23 -43.6(5) . . . . ? C24 O6 C23 C22 -179.6(5) . . . . ? Fe1 O6 C23 C22 -42.5(5) . . . . ? O5 C22 C23 O6 57.2(6) . . . . ? _refine_diff_density_max 1.313 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.097 data_compound 13 _database_code_CSD 165260 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H58 As Cl O3 P2 Ru' _chemical_formula_weight 980.34 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' 'As' 'As' 0.0499 2.0058 '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' 'Ru' 'Ru' -1.2594 0.8363 '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' 'P' 'P' 0.1023 0.0942 '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 10.660(3) _cell_length_b 10.809(3) _cell_length_c 20.260(3) _cell_angle_alpha 97.70(2) _cell_angle_beta 91.46(2) _cell_angle_gamma 92.32(3) _cell_volume 2310.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cut needle _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.218 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8534 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.17 _reflns_number_total 8260 _reflns_number_gt 7022 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0792P)^2^+22.7714P] 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 8260 _refine_ls_number_parameters 531 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.002 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 Ru1 Ru 0.68596(4) 0.62901(4) 0.22855(2) 0.01743(14) Uani 1 1 d . . . As1 As 0.68420(5) 0.49244(5) 0.11268(3) 0.02100(16) Uani 1 1 d . . . Cl1 Cl 0.89810(14) 0.71786(15) 0.24150(8) 0.0301(3) Uani 1 1 d . . . P1 P 0.63807(14) 0.68251(14) 0.34043(7) 0.0215(3) Uani 1 1 d . . . P2 P 0.61532(14) 0.79268(13) 0.18232(7) 0.0195(3) Uani 1 1 d . . . O1 O 0.5177(4) 0.5191(4) 0.21167(19) 0.0207(8) Uani 1 1 d . . . O2 O 0.7426(4) 0.4409(4) 0.24394(19) 0.0225(8) Uani 1 1 d . . . O3 O 0.1656(6) 1.1360(7) 0.3118(4) 0.0717(19) Uani 1 1 d . . . C1 C 0.5262(5) 0.4539(5) 0.1570(3) 0.0197(11) Uani 1 1 d . . . C2 C 0.7836(6) 0.4376(5) 0.1870(3) 0.0239(12) Uani 1 1 d . . . C3 C 0.4275(6) 0.3573(6) 0.1287(3) 0.0265(13) Uani 1 1 d . . . C4 C 0.3783(6) 0.3949(6) 0.0628(3) 0.0326(14) Uani 1 1 d . . . H4A H 0.3326 0.4698 0.0716 0.049 Uiso 1 1 calc R . . H4B H 0.3236 0.3289 0.0403 0.049 Uiso 1 1 calc R . . H4C H 0.4477 0.4094 0.0351 0.049 Uiso 1 1 calc R . . C5 C 0.3214(6) 0.3499(6) 0.1766(4) 0.0345(15) Uani 1 1 d . . . H5A H 0.3527 0.3221 0.2167 0.052 Uiso 1 1 calc R . . H5B H 0.2565 0.2920 0.1564 0.052 Uiso 1 1 calc R . . H5C H 0.2877 0.4310 0.1872 0.052 Uiso 1 1 calc R . . C6 C 0.4900(6) 0.2297(6) 0.1155(3) 0.0305(14) Uani 1 1 d . . . H6A H 0.5566 0.2354 0.0848 0.046 Uiso 1 1 calc R . . H6B H 0.4286 0.1665 0.0967 0.046 Uiso 1 1 calc R . . H6C H 0.5237 0.2082 0.1567 0.046 Uiso 1 1 calc R . . C7 C 0.9121(6) 0.3849(6) 0.1698(3) 0.0302(14) Uani 1 1 d . . . C8 C 0.9767(6) 0.4536(8) 0.1187(4) 0.0429(18) Uani 1 1 d . . . H8A H 0.9905 0.5401 0.1365 0.064 Uiso 1 1 calc R . . H8B H 0.9246 0.4467 0.0789 0.064 Uiso 1 1 calc R . . H8C H 1.0558 0.4175 0.1084 0.064 Uiso 1 1 calc R . . C9 C 0.8861(7) 0.2478(7) 0.1400(4) 0.0431(18) Uani 1 1 d . . . H9A H 0.8349 0.2439 0.1000 0.065 Uiso 1 1 calc R . . H9B H 0.8429 0.2042 0.1716 0.065 Uiso 1 1 calc R . . H9C H 0.9642 0.2094 0.1297 0.065 Uiso 1 1 calc R . . C10 C 0.9923(6) 0.3940(8) 0.2342(4) 0.0426(18) Uani 1 1 d . . . H10A H 1.0634 0.3428 0.2267 0.064 Uiso 1 1 calc R . . H10B H 0.9429 0.3657 0.2687 0.064 Uiso 1 1 calc R . . H10C H 1.0208 0.4793 0.2475 0.064 Uiso 1 1 calc R . . C11 C 0.4681(6) 0.6829(7) 0.3498(3) 0.0345(16) Uani 1 1 d . . . C12 C 0.4075(8) 0.7979(9) 0.3586(4) 0.056(3) Uani 1 1 d . . . H12 H 0.4548 0.8729 0.3668 0.068 Uiso 1 1 calc R . . C13 C 0.2762(9) 0.7983(11) 0.3550(5) 0.067(2) Uani 1 1 d U . . H13 H 0.2365 0.8739 0.3599 0.080 Uiso 1 1 calc R . . C14 C 0.2070(10) 0.6904(12) 0.3446(5) 0.071(3) Uani 1 1 d U . . H14 H 0.1199 0.6924 0.3425 0.085 Uiso 1 1 calc R . . C15 C 0.2628(8) 0.5769(12) 0.3369(4) 0.070(3) Uani 1 1 d . . . H15 H 0.2138 0.5029 0.3304 0.084 Uiso 1 1 calc R . . C16 C 0.3946(7) 0.5739(9) 0.3389(3) 0.046(2) Uani 1 1 d . . . H16 H 0.4325 0.4974 0.3328 0.056 Uiso 1 1 calc R . . C17 C 0.6930(7) 0.8234(6) 0.3963(3) 0.0366(16) Uani 1 1 d . . . C18 C 0.6368(8) 0.8612(9) 0.4555(4) 0.057(2) Uani 1 1 d . . . H18 H 0.5672 0.8146 0.4668 0.068 Uiso 1 1 calc R . . C19 C 0.6778(11) 0.9633(10) 0.4985(5) 0.068(3) Uani 1 1 d . . . H19 H 0.6383 0.9839 0.5386 0.082 Uiso 1 1 calc R . . C20 C 0.7698(14) 1.0298(12) 0.4834(6) 0.087(3) Uani 1 1 d U . . H20 H 0.7951 1.1011 0.5124 0.104 Uiso 1 1 calc R . . C21 C 0.8335(17) 1.0019(17) 0.4267(9) 0.131(5) Uani 1 1 d U . . H21 H 0.9041 1.0494 0.4175 0.157 Uiso 1 1 calc R . . C22 C 0.7868(12) 0.8957(12) 0.3814(6) 0.088(3) Uani 1 1 d U . . H22 H 0.8241 0.8776 0.3405 0.106 Uiso 1 1 calc R . . C23 C 0.6964(6) 0.5647(5) 0.3907(3) 0.0236(12) Uani 1 1 d . . . C24 C 0.6271(7) 0.5029(7) 0.4342(3) 0.0359(15) Uani 1 1 d . . . H24 H 0.5419 0.5165 0.4384 0.043 Uiso 1 1 calc R . . C25 C 0.6841(9) 0.4210(8) 0.4714(4) 0.051(2) Uani 1 1 d . . . H25 H 0.6371 0.3786 0.5001 0.061 Uiso 1 1 calc R . . C26 C 0.8120(8) 0.4027(7) 0.4656(4) 0.047(2) Uani 1 1 d . . . H26 H 0.8505 0.3482 0.4908 0.057 Uiso 1 1 calc R . . C27 C 0.8809(8) 0.4633(9) 0.4238(4) 0.052(2) Uani 1 1 d . . . H27 H 0.9664 0.4507 0.4206 0.063 Uiso 1 1 calc R . . C28 C 0.8243(7) 0.5444(7) 0.3855(3) 0.0383(16) Uani 1 1 d . . . H28 H 0.8718 0.5851 0.3564 0.046 Uiso 1 1 calc R . . C29 C 0.5997(6) 0.9458(6) 0.2315(3) 0.0231(12) Uani 1 1 d . . . C30 C 0.4868(7) 0.9983(7) 0.2500(4) 0.0437(18) Uani 1 1 d . . . H30 H 0.4117 0.9547 0.2359 0.052 Uiso 1 1 calc R . . C31 C 0.4831(7) 1.1137(7) 0.2887(4) 0.0434(18) Uani 1 1 d . . . H31 H 0.4060 1.1462 0.3002 0.052 Uiso 1 1 calc R . . C32 C 0.5905(8) 1.1798(7) 0.3100(4) 0.0440(18) Uani 1 1 d . . . H32 H 0.5878 1.2560 0.3373 0.053 Uiso 1 1 calc R . . C33 C 0.7038(9) 1.1323(10) 0.2906(6) 0.084(4) Uani 1 1 d . . . H33 H 0.7784 1.1781 0.3031 0.101 Uiso 1 1 calc R . . C34 C 0.7064(8) 1.0170(9) 0.2529(5) 0.068(3) Uani 1 1 d . . . H34 H 0.7839 0.9856 0.2413 0.082 Uiso 1 1 calc R . . C35 C 0.4568(5) 0.7576(5) 0.1443(3) 0.0203(11) Uani 1 1 d . . . C36 C 0.3597(5) 0.7272(6) 0.1855(3) 0.0243(12) Uani 1 1 d . . . H36 H 0.3779 0.7233 0.2303 0.029 Uiso 1 1 calc R . . C37 C 0.2380(6) 0.7028(6) 0.1612(3) 0.0299(14) Uani 1 1 d . . . H37 H 0.1751 0.6846 0.1899 0.036 Uiso 1 1 calc R . . C38 C 0.2091(6) 0.7053(6) 0.0948(3) 0.0306(14) Uani 1 1 d . . . H38 H 0.1267 0.6911 0.0785 0.037 Uiso 1 1 calc R . . C39 C 0.3055(6) 0.7295(6) 0.0523(3) 0.0294(14) Uani 1 1 d . . . H39 H 0.2883 0.7264 0.0069 0.035 Uiso 1 1 calc R . . C40 C 0.4259(6) 0.7579(5) 0.0775(3) 0.0249(12) Uani 1 1 d . . . H40 H 0.4882 0.7779 0.0489 0.030 Uiso 1 1 calc R . . C41 C 0.7043(6) 0.8450(5) 0.1134(3) 0.0236(12) Uani 1 1 d . . . C42 C 0.6614(6) 0.9441(5) 0.0821(3) 0.0287(13) Uani 1 1 d . . . H42 H 0.5900 0.9841 0.0974 0.034 Uiso 1 1 calc R . . C43 C 0.7224(7) 0.9835(6) 0.0292(3) 0.0347(15) Uani 1 1 d . . . H43 H 0.6914 1.0484 0.0086 0.042 Uiso 1 1 calc R . . C44 C 0.8305(7) 0.9263(7) 0.0064(3) 0.0363(16) Uani 1 1 d . . . H44 H 0.8720 0.9524 -0.0295 0.044 Uiso 1 1 calc R . . C45 C 0.8759(6) 0.8304(7) 0.0374(3) 0.0333(15) Uani 1 1 d . . . H45 H 0.9490 0.7928 0.0228 0.040 Uiso 1 1 calc R . . C46 C 0.8137(6) 0.7901(6) 0.0898(3) 0.0272(13) Uani 1 1 d . . . H46 H 0.8452 0.7249 0.1099 0.033 Uiso 1 1 calc R . . C47 C 0.2261(15) 1.2717(15) 0.4093(8) 0.114(5) Uani 1 1 d U . . H47A H 0.3005 1.2267 0.4151 0.171 Uiso 1 1 calc R . . H47B H 0.1981 1.3072 0.4521 0.171 Uiso 1 1 calc R . . H47C H 0.2443 1.3372 0.3829 0.171 Uiso 1 1 calc R . . C48 C 0.1293(11) 1.1877(11) 0.3762(7) 0.083(3) Uani 1 1 d . . . H48A H 0.1118 1.1209 0.4026 0.099 Uiso 1 1 calc R . . H48B H 0.0529 1.2324 0.3723 0.099 Uiso 1 1 calc R . . C49 C 0.0704(10) 1.0555(10) 0.2778(6) 0.074(3) Uani 1 1 d . . . H49A H -0.0069 1.0992 0.2750 0.089 Uiso 1 1 calc R . . H49B H 0.0544 0.9840 0.3011 0.089 Uiso 1 1 calc R . . C50 C 0.1155(9) 1.0140(9) 0.2100(6) 0.069(3) Uani 1 1 d . . . H50A H 0.1325 1.0857 0.1877 0.104 Uiso 1 1 calc R . . H50B H 0.0522 0.9602 0.1850 0.104 Uiso 1 1 calc R . . H50C H 0.1909 0.9694 0.2133 0.104 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 Ru1 0.0177(2) 0.0184(2) 0.0165(2) 0.00408(17) 0.00171(16) -0.00050(17) As1 0.0213(3) 0.0242(3) 0.0177(3) 0.0032(2) 0.0042(2) 0.0014(2) Cl1 0.0232(7) 0.0325(8) 0.0353(8) 0.0108(6) -0.0035(6) -0.0072(6) P1 0.0244(8) 0.0232(8) 0.0170(7) 0.0024(6) 0.0018(6) 0.0017(6) P2 0.0209(7) 0.0199(7) 0.0183(7) 0.0046(5) 0.0027(5) 0.0001(6) O1 0.0176(19) 0.021(2) 0.024(2) 0.0040(16) 0.0034(16) -0.0002(15) O2 0.026(2) 0.021(2) 0.021(2) 0.0041(16) 0.0023(16) 0.0023(16) O3 0.042(3) 0.076(5) 0.096(5) 0.008(4) -0.005(3) -0.001(3) C1 0.019(3) 0.021(3) 0.021(3) 0.010(2) 0.005(2) 0.003(2) C2 0.027(3) 0.019(3) 0.025(3) 0.001(2) 0.003(2) 0.001(2) C3 0.023(3) 0.025(3) 0.031(3) 0.000(2) 0.002(2) 0.002(2) C4 0.034(4) 0.028(3) 0.034(4) 0.000(3) -0.011(3) 0.001(3) C5 0.027(3) 0.025(3) 0.048(4) -0.003(3) 0.005(3) -0.010(3) C6 0.033(3) 0.019(3) 0.039(4) 0.003(3) 0.000(3) 0.000(3) C7 0.023(3) 0.034(3) 0.035(4) 0.009(3) -0.001(3) 0.003(3) C8 0.024(3) 0.067(5) 0.041(4) 0.010(4) 0.016(3) 0.008(3) C9 0.041(4) 0.044(4) 0.043(4) -0.002(3) -0.002(3) 0.022(3) C10 0.023(3) 0.066(5) 0.041(4) 0.012(4) 0.001(3) 0.009(3) C11 0.032(4) 0.061(5) 0.011(3) 0.001(3) 0.001(2) 0.014(3) C12 0.045(4) 0.086(6) 0.033(4) -0.020(4) -0.012(3) 0.039(4) C13 0.059(4) 0.085(5) 0.053(4) -0.012(3) -0.004(3) 0.028(4) C14 0.059(4) 0.098(5) 0.056(4) 0.004(4) 0.007(3) 0.017(4) C15 0.043(5) 0.140(10) 0.026(4) 0.017(5) -0.001(3) -0.024(6) C16 0.035(4) 0.085(6) 0.020(3) 0.016(3) 0.008(3) -0.014(4) C17 0.060(5) 0.026(3) 0.024(3) 0.008(3) -0.003(3) -0.003(3) C18 0.047(5) 0.077(6) 0.038(4) -0.029(4) -0.009(4) 0.021(4) C19 0.085(7) 0.067(6) 0.046(5) -0.021(4) -0.014(5) 0.029(6) C20 0.111(5) 0.079(5) 0.067(5) 0.003(4) 0.006(4) -0.007(4) C21 0.140(7) 0.124(7) 0.125(7) 0.013(5) 0.022(5) -0.030(5) C22 0.103(5) 0.086(5) 0.069(5) -0.004(4) 0.020(4) -0.031(4) C23 0.029(3) 0.021(3) 0.021(3) 0.002(2) 0.001(2) 0.002(2) C24 0.042(4) 0.039(4) 0.029(3) 0.011(3) 0.004(3) 0.001(3) C25 0.080(6) 0.044(4) 0.031(4) 0.016(3) 0.003(4) -0.002(4) C26 0.071(6) 0.041(4) 0.034(4) 0.013(3) -0.002(4) 0.022(4) C27 0.050(5) 0.072(6) 0.041(4) 0.022(4) 0.000(4) 0.031(4) C28 0.036(4) 0.056(5) 0.027(3) 0.015(3) 0.002(3) 0.012(3) C29 0.025(3) 0.027(3) 0.019(3) 0.005(2) 0.005(2) 0.000(2) C30 0.030(4) 0.039(4) 0.059(5) -0.009(3) -0.003(3) 0.010(3) C31 0.036(4) 0.034(4) 0.058(5) -0.007(3) 0.004(3) 0.013(3) C32 0.053(5) 0.037(4) 0.038(4) -0.011(3) 0.007(3) 0.002(3) C33 0.038(5) 0.081(7) 0.112(9) -0.062(7) 0.013(5) -0.021(5) C34 0.028(4) 0.065(6) 0.094(7) -0.049(5) 0.016(4) -0.008(4) C35 0.024(3) 0.017(3) 0.020(3) 0.002(2) 0.001(2) 0.002(2) C36 0.023(3) 0.027(3) 0.022(3) 0.001(2) 0.002(2) 0.002(2) C37 0.025(3) 0.031(3) 0.034(3) 0.006(3) 0.003(3) 0.001(3) C38 0.022(3) 0.031(3) 0.040(4) 0.011(3) -0.007(3) 0.002(3) C39 0.041(4) 0.026(3) 0.022(3) 0.007(2) -0.007(3) 0.000(3) C40 0.031(3) 0.020(3) 0.025(3) 0.009(2) 0.003(2) 0.000(2) C41 0.026(3) 0.018(3) 0.026(3) 0.003(2) 0.003(2) -0.001(2) C42 0.040(4) 0.018(3) 0.029(3) 0.004(2) 0.008(3) 0.003(3) C43 0.049(4) 0.025(3) 0.032(3) 0.013(3) 0.001(3) -0.004(3) C44 0.038(4) 0.041(4) 0.031(3) 0.012(3) 0.005(3) -0.015(3) C45 0.024(3) 0.043(4) 0.034(4) 0.009(3) 0.004(3) -0.001(3) C46 0.028(3) 0.031(3) 0.025(3) 0.011(3) 0.003(2) 0.000(3) C47 0.118(6) 0.108(6) 0.112(6) 0.005(5) -0.008(5) 0.012(5) C48 0.065(7) 0.077(8) 0.112(10) 0.027(7) 0.008(6) 0.022(6) C49 0.053(6) 0.069(7) 0.098(8) 0.003(6) -0.013(5) -0.006(5) C50 0.051(5) 0.059(6) 0.094(8) -0.001(5) -0.011(5) 0.013(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 Ru1 O1 2.106(4) . ? Ru1 O2 2.203(4) . ? Ru1 P2 2.2561(16) . ? Ru1 P1 2.3376(16) . ? Ru1 Cl1 2.4148(17) . ? Ru1 As1 2.5992(9) . ? As1 C1 1.984(5) . ? As1 C2 1.988(6) . ? P1 C11 1.826(7) . ? P1 C17 1.838(7) . ? P1 C23 1.850(6) . ? P2 C29 1.830(6) . ? P2 C35 1.843(6) . ? P2 C41 1.846(6) . ? O1 C1 1.238(7) . ? O2 C2 1.240(7) . ? O3 C49 1.411(12) . ? O3 C48 1.419(14) . ? C1 C3 1.498(8) . ? C2 C7 1.535(8) . ? C3 C5 1.516(9) . ? C3 C4 1.534(9) . ? C3 C6 1.551(8) . ? C7 C8 1.516(9) . ? C7 C10 1.531(9) . ? C7 C9 1.535(10) . ? C11 C16 1.378(11) . ? C11 C12 1.416(11) . ? C12 C13 1.400(12) . ? C13 C14 1.343(15) . ? C14 C15 1.376(16) . ? C15 C16 1.406(12) . ? C17 C22 1.310(13) . ? C17 C18 1.375(11) . ? C18 C19 1.360(12) . ? C19 C20 1.261(16) . ? C20 C21 1.355(19) . ? C21 C22 1.433(19) . ? C23 C24 1.385(9) . ? C23 C28 1.394(9) . ? C24 C25 1.387(10) . ? C25 C26 1.392(12) . ? C26 C27 1.353(12) . ? C27 C28 1.391(10) . ? C29 C34 1.374(10) . ? C29 C30 1.390(9) . ? C30 C31 1.384(10) . ? C31 C32 1.353(11) . ? C32 C33 1.377(12) . ? C33 C34 1.374(12) . ? C35 C40 1.385(8) . ? C35 C36 1.402(8) . ? C36 C37 1.378(9) . ? C37 C38 1.377(9) . ? C38 C39 1.396(9) . ? C39 C40 1.376(9) . ? C41 C46 1.396(9) . ? C41 C42 1.403(8) . ? C42 C43 1.374(9) . ? C43 C44 1.391(10) . ? C44 C45 1.379(10) . ? C45 C46 1.375(9) . ? C47 C48 1.437(18) . ? C49 C50 1.485(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 O2 76.51(15) . . ? O1 Ru1 P2 95.51(11) . . ? O2 Ru1 P2 163.14(11) . . ? O1 Ru1 P1 90.50(11) . . ? O2 Ru1 P1 93.01(11) . . ? P2 Ru1 P1 101.98(6) . . ? O1 Ru1 Cl1 169.00(11) . . ? O2 Ru1 Cl1 93.58(11) . . ? P2 Ru1 Cl1 92.79(6) . . ? P1 Ru1 Cl1 94.84(6) . . ? O1 Ru1 As1 69.31(11) . . ? O2 Ru1 As1 72.20(10) . . ? P2 Ru1 As1 91.14(5) . . ? P1 Ru1 As1 157.02(5) . . ? Cl1 Ru1 As1 103.36(5) . . ? C1 As1 C2 90.2(2) . . ? C1 As1 Ru1 71.75(17) . . ? C2 As1 Ru1 61.79(17) . . ? C11 P1 C17 102.4(3) . . ? C11 P1 C23 106.4(3) . . ? C17 P1 C23 98.1(3) . . ? C11 P1 Ru1 110.4(2) . . ? C17 P1 Ru1 127.2(2) . . ? C23 P1 Ru1 110.26(19) . . ? C29 P2 C35 102.7(3) . . ? C29 P2 C41 98.0(3) . . ? C35 P2 C41 102.6(3) . . ? C29 P2 Ru1 121.69(19) . . ? C35 P2 Ru1 111.35(19) . . ? C41 P2 Ru1 117.8(2) . . ? C1 O1 Ru1 106.7(3) . . ? C2 O2 Ru1 84.0(3) . . ? C49 O3 C48 112.1(8) . . ? O1 C1 C3 123.0(5) . . ? O1 C1 As1 112.2(4) . . ? C3 C1 As1 124.8(4) . . ? O2 C2 C7 121.3(5) . . ? O2 C2 As1 122.1(4) . . ? C7 C2 As1 116.6(4) . . ? C1 C3 C5 110.8(5) . . ? C1 C3 C4 107.5(5) . . ? C5 C3 C4 110.5(5) . . ? C1 C3 C6 108.0(5) . . ? C5 C3 C6 110.2(5) . . ? C4 C3 C6 109.8(5) . . ? C8 C7 C10 111.0(6) . . ? C8 C7 C9 109.0(6) . . ? C10 C7 C9 110.7(6) . . ? C8 C7 C2 111.5(5) . . ? C10 C7 C2 108.3(5) . . ? C9 C7 C2 106.1(5) . . ? C16 C11 C12 118.2(7) . . ? C16 C11 P1 121.4(6) . . ? C12 C11 P1 119.7(7) . . ? C13 C12 C11 119.8(10) . . ? C14 C13 C12 120.6(10) . . ? C13 C14 C15 121.2(10) . . ? C14 C15 C16 119.4(11) . . ? C11 C16 C15 120.8(9) . . ? C22 C17 C18 115.8(8) . . ? C22 C17 P1 121.9(7) . . ? C18 C17 P1 122.3(6) . . ? C19 C18 C17 123.3(10) . . ? C20 C19 C18 119.5(11) . . ? C19 C20 C21 122.7(13) . . ? C20 C21 C22 116.8(14) . . ? C17 C22 C21 121.7(12) . . ? C24 C23 C28 119.1(6) . . ? C24 C23 P1 126.2(5) . . ? C28 C23 P1 114.6(5) . . ? C23 C24 C25 120.3(7) . . ? C24 C25 C26 119.5(7) . . ? C27 C26 C25 120.7(7) . . ? C26 C27 C28 120.3(8) . . ? C27 C28 C23 120.1(7) . . ? C34 C29 C30 115.7(6) . . ? C34 C29 P2 119.0(5) . . ? C30 C29 P2 125.3(5) . . ? C31 C30 C29 121.7(7) . . ? C32 C31 C30 120.8(7) . . ? C31 C32 C33 118.9(7) . . ? C34 C33 C32 119.8(8) . . ? C29 C34 C33 123.1(7) . . ? C40 C35 C36 117.0(5) . . ? C40 C35 P2 124.9(5) . . ? C36 C35 P2 118.1(4) . . ? C37 C36 C35 121.6(6) . . ? C38 C37 C36 120.3(6) . . ? C37 C38 C39 118.9(6) . . ? C40 C39 C38 120.2(6) . . ? C39 C40 C35 121.8(6) . . ? C46 C41 C42 117.2(5) . . ? C46 C41 P2 123.3(5) . . ? C42 C41 P2 119.5(5) . . ? C43 C42 C41 121.5(6) . . ? C42 C43 C44 120.0(6) . . ? C45 C44 C43 119.5(6) . . ? C46 C45 C44 120.4(6) . . ? C45 C46 C41 121.4(6) . . ? O3 C48 C47 111.2(11) . . ? O3 C49 C50 107.2(9) . . ? 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 O1 Ru1 As1 C1 -1.5(2) . . . . ? O2 Ru1 As1 C1 80.4(2) . . . . ? P2 Ru1 As1 C1 -97.00(17) . . . . ? P1 Ru1 As1 C1 28.4(2) . . . . ? Cl1 Ru1 As1 C1 169.86(17) . . . . ? O1 Ru1 As1 C2 -101.9(2) . . . . ? O2 Ru1 As1 C2 -20.0(2) . . . . ? P2 Ru1 As1 C2 162.6(2) . . . . ? P1 Ru1 As1 C2 -72.0(2) . . . . ? Cl1 Ru1 As1 C2 69.5(2) . . . . ? O1 Ru1 P1 C11 -29.8(3) . . . . ? O2 Ru1 P1 C11 -106.3(3) . . . . ? P2 Ru1 P1 C11 66.0(3) . . . . ? Cl1 Ru1 P1 C11 159.9(3) . . . . ? As1 Ru1 P1 C11 -57.6(3) . . . . ? O1 Ru1 P1 C17 -154.5(3) . . . . ? O2 Ru1 P1 C17 129.0(3) . . . . ? P2 Ru1 P1 C17 -58.7(3) . . . . ? Cl1 Ru1 P1 C17 35.1(3) . . . . ? As1 Ru1 P1 C17 177.7(3) . . . . ? O1 Ru1 P1 C23 87.6(2) . . . . ? O2 Ru1 P1 C23 11.1(2) . . . . ? P2 Ru1 P1 C23 -176.7(2) . . . . ? Cl1 Ru1 P1 C23 -82.8(2) . . . . ? As1 Ru1 P1 C23 59.8(2) . . . . ? O1 Ru1 P2 C29 115.9(3) . . . . ? O2 Ru1 P2 C29 176.5(4) . . . . ? P1 Ru1 P2 C29 24.2(2) . . . . ? Cl1 Ru1 P2 C29 -71.4(2) . . . . ? As1 Ru1 P2 C29 -174.8(2) . . . . ? O1 Ru1 P2 C35 -5.4(2) . . . . ? O2 Ru1 P2 C35 55.3(4) . . . . ? P1 Ru1 P2 C35 -97.1(2) . . . . ? Cl1 Ru1 P2 C35 167.4(2) . . . . ? As1 Ru1 P2 C35 63.9(2) . . . . ? O1 Ru1 P2 C41 -123.5(2) . . . . ? O2 Ru1 P2 C41 -62.8(4) . . . . ? P1 Ru1 P2 C41 144.9(2) . . . . ? Cl1 Ru1 P2 C41 49.3(2) . . . . ? As1 Ru1 P2 C41 -54.1(2) . . . . ? O2 Ru1 O1 C1 -73.3(3) . . . . ? P2 Ru1 O1 C1 91.6(3) . . . . ? P1 Ru1 O1 C1 -166.3(3) . . . . ? Cl1 Ru1 O1 C1 -47.2(8) . . . . ? As1 Ru1 O1 C1 2.5(3) . . . . ? O1 Ru1 O2 C2 101.4(4) . . . . ? P2 Ru1 O2 C2 38.2(6) . . . . ? P1 Ru1 O2 C2 -168.8(3) . . . . ? Cl1 Ru1 O2 C2 -73.8(3) . . . . ? As1 Ru1 O2 C2 29.1(3) . . . . ? Ru1 O1 C1 C3 176.6(4) . . . . ? Ru1 O1 C1 As1 -3.2(4) . . . . ? C2 As1 C1 O1 62.7(4) . . . . ? Ru1 As1 C1 O1 2.7(3) . . . . ? C2 As1 C1 C3 -117.1(5) . . . . ? Ru1 As1 C1 C3 -177.2(5) . . . . ? Ru1 O2 C2 C7 137.2(5) . . . . ? Ru1 O2 C2 As1 -45.7(4) . . . . ? C1 As1 C2 O2 -25.9(5) . . . . ? Ru1 As1 C2 O2 43.2(4) . . . . ? C1 As1 C2 C7 151.4(5) . . . . ? Ru1 As1 C2 C7 -139.5(5) . . . . ? O1 C1 C3 C5 -1.5(8) . . . . ? As1 C1 C3 C5 178.3(4) . . . . ? O1 C1 C3 C4 119.2(6) . . . . ? As1 C1 C3 C4 -60.9(6) . . . . ? O1 C1 C3 C6 -122.4(6) . . . . ? As1 C1 C3 C6 57.5(6) . . . . ? O2 C2 C7 C8 -146.0(6) . . . . ? As1 C2 C7 C8 36.7(7) . . . . ? O2 C2 C7 C10 -23.5(8) . . . . ? As1 C2 C7 C10 159.2(5) . . . . ? O2 C2 C7 C9 95.4(7) . . . . ? As1 C2 C7 C9 -81.9(6) . . . . ? C17 P1 C11 C16 -153.9(5) . . . . ? C23 P1 C11 C16 -51.5(6) . . . . ? Ru1 P1 C11 C16 68.2(6) . . . . ? C17 P1 C11 C12 35.7(6) . . . . ? C23 P1 C11 C12 138.1(5) . . . . ? Ru1 P1 C11 C12 -102.2(5) . . . . ? C16 C11 C12 C13 -1.0(11) . . . . ? P1 C11 C12 C13 169.7(6) . . . . ? C11 C12 C13 C14 1.3(14) . . . . ? C12 C13 C14 C15 -0.3(15) . . . . ? C13 C14 C15 C16 -1.0(14) . . . . ? C12 C11 C16 C15 -0.3(10) . . . . ? P1 C11 C16 C15 -170.8(5) . . . . ? C14 C15 C16 C11 1.3(11) . . . . ? C11 P1 C17 C22 -142.6(9) . . . . ? C23 P1 C17 C22 108.5(9) . . . . ? Ru1 P1 C17 C22 -14.7(10) . . . . ? C11 P1 C17 C18 35.9(7) . . . . ? C23 P1 C17 C18 -73.0(7) . . . . ? Ru1 P1 C17 C18 163.9(5) . . . . ? C22 C17 C18 C19 -3.1(14) . . . . ? P1 C17 C18 C19 178.3(7) . . . . ? C17 C18 C19 C20 1.9(16) . . . . ? C18 C19 C20 C21 -2(2) . . . . ? C19 C20 C21 C22 4(3) . . . . ? C18 C17 C22 C21 4.6(19) . . . . ? P1 C17 C22 C21 -176.8(12) . . . . ? C20 C21 C22 C17 -5(2) . . . . ? C11 P1 C23 C24 -8.4(6) . . . . ? C17 P1 C23 C24 97.1(6) . . . . ? Ru1 P1 C23 C24 -128.3(5) . . . . ? C11 P1 C23 C28 175.3(5) . . . . ? C17 P1 C23 C28 -79.2(5) . . . . ? Ru1 P1 C23 C28 55.5(5) . . . . ? C28 C23 C24 C25 -0.7(10) . . . . ? P1 C23 C24 C25 -176.7(6) . . . . ? C23 C24 C25 C26 1.0(11) . . . . ? C24 C25 C26 C27 -0.4(13) . . . . ? C25 C26 C27 C28 -0.5(13) . . . . ? C26 C27 C28 C23 0.7(13) . . . . ? C24 C23 C28 C27 -0.2(11) . . . . ? P1 C23 C28 C27 176.3(6) . . . . ? C35 P2 C29 C34 -162.9(7) . . . . ? C41 P2 C29 C34 -58.0(7) . . . . ? Ru1 P2 C29 C34 71.8(7) . . . . ? C35 P2 C29 C30 17.3(7) . . . . ? C41 P2 C29 C30 122.2(6) . . . . ? Ru1 P2 C29 C30 -108.0(6) . . . . ? C34 C29 C30 C31 -1.4(12) . . . . ? P2 C29 C30 C31 178.4(6) . . . . ? C29 C30 C31 C32 0.0(13) . . . . ? C30 C31 C32 C33 2.2(14) . . . . ? C31 C32 C33 C34 -3.0(18) . . . . ? C30 C29 C34 C33 0.5(16) . . . . ? P2 C29 C34 C33 -179.3(10) . . . . ? C32 C33 C34 C29 2(2) . . . . ? C29 P2 C35 C40 108.5(5) . . . . ? C41 P2 C35 C40 7.2(6) . . . . ? Ru1 P2 C35 C40 -119.7(5) . . . . ? C29 P2 C35 C36 -72.1(5) . . . . ? C41 P2 C35 C36 -173.4(4) . . . . ? Ru1 P2 C35 C36 59.7(5) . . . . ? C40 C35 C36 C37 -2.2(9) . . . . ? P2 C35 C36 C37 178.4(5) . . . . ? C35 C36 C37 C38 1.4(9) . . . . ? C36 C37 C38 C39 1.7(10) . . . . ? C37 C38 C39 C40 -4.0(9) . . . . ? C38 C39 C40 C35 3.2(9) . . . . ? C36 C35 C40 C39 -0.1(9) . . . . ? P2 C35 C40 C39 179.3(5) . . . . ? C29 P2 C41 C46 130.9(5) . . . . ? C35 P2 C41 C46 -124.1(5) . . . . ? Ru1 P2 C41 C46 -1.4(6) . . . . ? C29 P2 C41 C42 -49.5(5) . . . . ? C35 P2 C41 C42 55.5(5) . . . . ? Ru1 P2 C41 C42 178.2(4) . . . . ? C46 C41 C42 C43 1.7(9) . . . . ? P2 C41 C42 C43 -177.9(5) . . . . ? C41 C42 C43 C44 -1.2(10) . . . . ? C42 C43 C44 C45 -0.2(10) . . . . ? C43 C44 C45 C46 1.1(10) . . . . ? C44 C45 C46 C41 -0.6(10) . . . . ? C42 C41 C46 C45 -0.8(9) . . . . ? P2 C41 C46 C45 178.8(5) . . . . ? C49 O3 C48 C47 -178.6(10) . . . . ? C48 O3 C49 C50 176.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.894 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.143 data_compound 15 _database_code_CSD 165261 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H55 As Cl2 O2 P2 Ru' _chemical_formula_weight 984.76 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 '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' 'P' 'P' 0.1023 0.0942 '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 10.279(2) _cell_length_b 12.179(2) _cell_length_c 19.603(3) _cell_angle_alpha 91.63(2) _cell_angle_beta 90.43(2) _cell_angle_gamma 114.000(10) _cell_volume 2240.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.312 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8348 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.18 _reflns_number_total 7880 _reflns_number_gt 5255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1159P)^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 7880 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Ru1 Ru 0.21345(6) 0.15793(5) 0.22855(3) 0.01373(17) Uani 1 1 d . . . As1 As 0.11905(8) 0.18858(8) 0.41764(4) 0.0266(2) Uani 1 1 d . . . Cl1 Cl 0.3638(3) 0.0654(3) 0.18521(16) 0.0775(10) Uani 1 1 d . . . Cl2 Cl 0.1128(3) 0.1696(3) 0.1168(2) 0.0815(11) Uani 1 1 d . . . P1 P 0.03456(18) -0.04215(15) 0.23860(9) 0.0155(4) Uani 1 1 d . . . P2 P 0.39045(19) 0.35695(16) 0.20950(9) 0.0165(4) Uani 1 1 d . . . O1 O 0.0865(5) 0.2362(4) 0.2757(2) 0.0163(10) Uani 1 1 d . . . O2 O 0.3090(5) 0.1535(4) 0.3227(2) 0.0153(10) Uani 1 1 d . . . C1 C 0.0539(7) 0.2422(6) 0.3373(4) 0.0185(15) Uani 1 1 d . . . C2 C 0.2741(7) 0.1558(6) 0.3826(3) 0.0172(14) Uani 1 1 d . . . C3 C -0.0549(8) 0.2946(7) 0.3521(4) 0.0235(16) Uani 1 1 d . . . C4 C -0.0952(10) 0.3400(9) 0.2867(4) 0.045(2) Uani 1 1 d . . . H4A H -0.0139 0.4068 0.2710 0.067 Uiso 1 1 calc R . . H4B H -0.1708 0.3651 0.2958 0.067 Uiso 1 1 calc R . . H4C H -0.1263 0.2765 0.2522 0.067 Uiso 1 1 calc R . . C5 C -0.1888(8) 0.1980(8) 0.3826(4) 0.039(2) Uani 1 1 d . . . H5A H -0.2590 0.2301 0.3897 0.058 Uiso 1 1 calc R . . H5B H -0.1641 0.1743 0.4254 0.058 Uiso 1 1 calc R . . H5C H -0.2266 0.1293 0.3517 0.058 Uiso 1 1 calc R . . C6 C 0.0120(9) 0.4028(7) 0.4026(4) 0.037(2) Uani 1 1 d . . . H6A H 0.0285 0.3753 0.4460 0.056 Uiso 1 1 calc R . . H6B H -0.0517 0.4421 0.4082 0.056 Uiso 1 1 calc R . . H6C H 0.1007 0.4583 0.3853 0.056 Uiso 1 1 calc R . . C7 C 0.3733(8) 0.1381(7) 0.4360(3) 0.0214(16) Uani 1 1 d . . . C8 C 0.4330(8) 0.0488(7) 0.4065(4) 0.0254(17) Uani 1 1 d . . . H8A H 0.3574 -0.0300 0.4016 0.038 Uiso 1 1 calc R . . H8B H 0.5054 0.0465 0.4370 0.038 Uiso 1 1 calc R . . H8C H 0.4733 0.0747 0.3627 0.038 Uiso 1 1 calc R . . C9 C 0.4964(8) 0.2621(7) 0.4495(4) 0.0259(17) Uani 1 1 d . . . H9A H 0.5654 0.2543 0.4800 0.039 Uiso 1 1 calc R . . H9B H 0.4600 0.3163 0.4697 0.039 Uiso 1 1 calc R . . H9C H 0.5406 0.2931 0.4072 0.039 Uiso 1 1 calc R . . C10 C 0.2991(9) 0.0928(7) 0.5036(4) 0.0276(18) Uani 1 1 d . . . H10A H 0.3625 0.0758 0.5335 0.041 Uiso 1 1 calc R . . H10B H 0.2147 0.0208 0.4948 0.041 Uiso 1 1 calc R . . H10C H 0.2738 0.1533 0.5246 0.041 Uiso 1 1 calc R . . C11 C -0.0053(7) -0.1432(6) 0.1627(3) 0.0165(14) Uani 1 1 d . . . C12 C 0.0692(8) -0.1158(6) 0.1026(3) 0.0203(15) Uani 1 1 d . . . H12 H 0.1452 -0.0414 0.0991 0.024 Uiso 1 1 calc R . . C13 C 0.0324(8) -0.1973(6) 0.0473(4) 0.0242(16) Uani 1 1 d . . . H13 H 0.0830 -0.1768 0.0071 0.029 Uiso 1 1 calc R . . C14 C -0.0809(9) -0.3104(7) 0.0521(4) 0.0315(19) Uani 1 1 d . . . H14 H -0.1065 -0.3655 0.0153 0.038 Uiso 1 1 calc R . . C15 C -0.1539(9) -0.3387(7) 0.1127(4) 0.037(2) Uani 1 1 d . . . H15 H -0.2289 -0.4137 0.1164 0.044 Uiso 1 1 calc R . . C16 C -0.1179(8) -0.2584(7) 0.1672(4) 0.0296(18) Uani 1 1 d . . . H16 H -0.1679 -0.2797 0.2076 0.036 Uiso 1 1 calc R . . C17 C -0.1439(7) -0.0536(6) 0.2561(4) 0.0186(15) Uani 1 1 d . . . C18 C -0.1930(7) 0.0178(6) 0.2162(4) 0.0203(15) Uani 1 1 d . . . H18 H -0.1297 0.0728 0.1874 0.024 Uiso 1 1 calc R . . C19 C -0.3307(9) 0.0091(7) 0.2187(4) 0.0320(19) Uani 1 1 d . . . H19 H -0.3607 0.0555 0.1911 0.038 Uiso 1 1 calc R . . C20 C -0.4239(7) -0.0708(7) 0.2633(4) 0.0263(17) Uani 1 1 d . . . H20 H -0.5174 -0.0780 0.2657 0.032 Uiso 1 1 calc R . . C21 C -0.3785(8) -0.1394(8) 0.3040(4) 0.0310(19) Uani 1 1 d . . . H21 H -0.4409 -0.1907 0.3347 0.037 Uiso 1 1 calc R . . C22 C -0.2418(8) -0.1327(6) 0.2998(4) 0.0231(16) Uani 1 1 d . . . H22 H -0.2142 -0.1817 0.3266 0.028 Uiso 1 1 calc R . . C23 C 0.0779(7) -0.1319(6) 0.3013(3) 0.0184(15) Uani 1 1 d . . . C24 C 0.1504(8) -0.2004(6) 0.2805(4) 0.0230(16) Uani 1 1 d . . . H24 H 0.1755 -0.2006 0.2350 0.028 Uiso 1 1 calc R . . C25 C 0.1865(9) -0.2689(7) 0.3262(4) 0.0312(18) Uani 1 1 d . . . H25 H 0.2386 -0.3121 0.3120 0.037 Uiso 1 1 calc R . . C26 C 0.1445(9) -0.2721(7) 0.3926(4) 0.0311(19) Uani 1 1 d . . . H26 H 0.1644 -0.3208 0.4230 0.037 Uiso 1 1 calc R . . C27 C 0.0735(8) -0.2043(7) 0.4147(3) 0.0249(17) Uani 1 1 d . . . H27 H 0.0471 -0.2064 0.4601 0.030 Uiso 1 1 calc R . . C28 C 0.0408(7) -0.1329(6) 0.3702(3) 0.0203(15) Uani 1 1 d . . . H28 H -0.0056 -0.0857 0.3858 0.024 Uiso 1 1 calc R . . C29 C 0.5004(7) 0.4419(6) 0.2832(3) 0.0183(15) Uani 1 1 d . . . C30 C 0.4252(9) 0.4605(6) 0.3385(4) 0.0267(17) Uani 1 1 d . . . H30 H 0.3261 0.4261 0.3370 0.032 Uiso 1 1 calc R . . C31 C 0.4962(9) 0.5293(7) 0.3953(4) 0.0292(18) Uani 1 1 d . . . H31 H 0.4448 0.5420 0.4313 0.035 Uiso 1 1 calc R . . C32 C 0.6455(9) 0.5799(6) 0.3989(4) 0.0288(18) Uani 1 1 d . . . H32 H 0.6939 0.6250 0.4373 0.035 Uiso 1 1 calc R . . C33 C 0.7200(8) 0.5613(7) 0.3439(4) 0.0282(17) Uani 1 1 d . . . H33 H 0.8190 0.5949 0.3456 0.034 Uiso 1 1 calc R . . C34 C 0.6487(8) 0.4935(7) 0.2866(4) 0.0255(17) Uani 1 1 d . . . H34 H 0.7002 0.4825 0.2502 0.031 Uiso 1 1 calc R . . C35 C 0.5170(7) 0.3550(6) 0.1448(3) 0.0182(15) Uani 1 1 d . . . C36 C 0.6199(7) 0.3114(6) 0.1598(4) 0.0219(16) Uani 1 1 d . . . H36 H 0.6251 0.2852 0.2035 0.026 Uiso 1 1 calc R . . C37 C 0.7142(8) 0.3063(7) 0.1112(4) 0.0286(18) Uani 1 1 d . . . H37 H 0.7834 0.2785 0.1222 0.034 Uiso 1 1 calc R . . C38 C 0.7045(9) 0.3429(7) 0.0467(4) 0.0339(19) Uani 1 1 d . . . H38 H 0.7689 0.3415 0.0139 0.041 Uiso 1 1 calc R . . C39 C 0.5985(9) 0.3822(7) 0.0297(4) 0.0319(19) Uani 1 1 d . . . H39 H 0.5908 0.4046 -0.0147 0.038 Uiso 1 1 calc R . . C40 C 0.5058(9) 0.3880(6) 0.0782(4) 0.0273(17) Uani 1 1 d . . . H40 H 0.4353 0.4139 0.0666 0.033 Uiso 1 1 calc R . . C41 C 0.3294(8) 0.4705(6) 0.1798(3) 0.0219(16) Uani 1 1 d . . . C42 C 0.4286(9) 0.5893(6) 0.1745(4) 0.0263(17) Uani 1 1 d . . . H42 H 0.5239 0.6094 0.1855 0.032 Uiso 1 1 calc R . . C43 C 0.3870(10) 0.6762(7) 0.1535(4) 0.034(2) Uani 1 1 d . . . H43 H 0.4544 0.7547 0.1496 0.041 Uiso 1 1 calc R . . C44 C 0.2457(10) 0.6486(7) 0.1379(4) 0.035(2) Uani 1 1 d . . . H44 H 0.2178 0.7082 0.1238 0.041 Uiso 1 1 calc R . . C45 C 0.1461(9) 0.5320(8) 0.1433(4) 0.0319(19) Uani 1 1 d . . . H45 H 0.0507 0.5129 0.1331 0.038 Uiso 1 1 calc R . . C46 C 0.1887(8) 0.4426(7) 0.1641(4) 0.0297(18) Uani 1 1 d . . . H46 H 0.1215 0.3639 0.1674 0.036 Uiso 1 1 calc R . . C47 C 0.4720(10) 0.0456(8) -0.0060(5) 0.043(2) Uani 1 1 d . . . H47A H 0.4790 0.0916 0.0361 0.051 Uiso 1 1 calc R . . H47B H 0.5298 0.1005 -0.0396 0.051 Uiso 1 1 calc R . . C48 C 0.3325(7) -0.0046(6) -0.0287(4) 0.0194(15) Uani 1 1 d . . . H48A H 0.2754 -0.0610 0.0044 0.023 Uiso 1 1 calc R . . H48B H 0.3262 -0.0492 -0.0713 0.023 Uiso 1 1 calc R . . C49 C 0.2752(10) 0.0819(8) -0.0392(5) 0.044(2) Uani 1 1 d . . . H49A H 0.2864 0.1297 0.0019 0.066 Uiso 1 1 calc R . . H49B H 0.1759 0.0415 -0.0513 0.066 Uiso 1 1 calc R . . H49C H 0.3247 0.1328 -0.0754 0.066 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 Ru1 0.0119(3) 0.0138(3) 0.0134(3) 0.0008(2) -0.0001(2) 0.0031(2) As1 0.0286(5) 0.0411(5) 0.0178(4) 0.0053(3) 0.0058(3) 0.0218(4) Cl1 0.0672(19) 0.0593(18) 0.0703(19) 0.0219(15) -0.0235(15) -0.0117(15) Cl2 0.0571(18) 0.0440(16) 0.138(3) 0.0035(17) 0.0364(19) 0.0148(14) P1 0.0132(9) 0.0115(9) 0.0178(9) 0.0011(7) 0.0013(7) 0.0010(7) P2 0.0158(9) 0.0133(9) 0.0159(9) 0.0019(7) 0.0009(7) 0.0014(7) O1 0.018(2) 0.015(2) 0.015(2) 0.0011(18) 0.0056(19) 0.005(2) O2 0.018(2) 0.017(2) 0.012(2) -0.0009(18) -0.0012(18) 0.008(2) C1 0.020(4) 0.010(3) 0.026(4) -0.003(3) 0.001(3) 0.007(3) C2 0.014(3) 0.013(3) 0.022(4) 0.000(3) -0.002(3) 0.003(3) C3 0.023(4) 0.025(4) 0.027(4) -0.003(3) 0.004(3) 0.015(3) C4 0.043(5) 0.066(7) 0.035(5) 0.004(4) 0.006(4) 0.032(5) C5 0.023(4) 0.053(6) 0.039(5) 0.001(4) 0.004(4) 0.014(4) C6 0.044(5) 0.021(4) 0.049(5) -0.011(4) 0.002(4) 0.016(4) C7 0.022(4) 0.029(4) 0.016(3) -0.005(3) -0.004(3) 0.014(3) C8 0.023(4) 0.035(5) 0.019(4) 0.001(3) -0.001(3) 0.013(4) C9 0.024(4) 0.027(4) 0.027(4) -0.007(3) -0.010(3) 0.010(3) C10 0.040(5) 0.033(5) 0.018(4) 0.009(3) 0.000(3) 0.023(4) C11 0.016(3) 0.014(3) 0.021(3) -0.005(3) -0.006(3) 0.008(3) C12 0.021(4) 0.014(4) 0.020(4) 0.005(3) 0.003(3) 0.001(3) C13 0.029(4) 0.020(4) 0.018(4) 0.005(3) -0.001(3) 0.005(3) C14 0.034(5) 0.029(4) 0.026(4) -0.014(3) -0.006(3) 0.009(4) C15 0.029(5) 0.023(4) 0.043(5) -0.001(4) 0.001(4) -0.005(4) C16 0.028(4) 0.024(4) 0.021(4) -0.005(3) 0.009(3) -0.005(3) C17 0.016(4) 0.010(3) 0.027(4) -0.003(3) 0.000(3) 0.004(3) C18 0.015(4) 0.018(4) 0.027(4) -0.001(3) 0.003(3) 0.006(3) C19 0.032(5) 0.031(5) 0.034(4) 0.002(4) -0.008(4) 0.014(4) C20 0.010(3) 0.035(5) 0.032(4) -0.008(3) -0.003(3) 0.008(3) C21 0.022(4) 0.039(5) 0.026(4) -0.008(3) 0.002(3) 0.007(4) C22 0.023(4) 0.021(4) 0.025(4) 0.000(3) 0.000(3) 0.009(3) C23 0.015(3) 0.015(4) 0.020(4) 0.002(3) 0.001(3) 0.000(3) C24 0.025(4) 0.020(4) 0.022(4) 0.001(3) -0.002(3) 0.007(3) C25 0.034(5) 0.028(4) 0.036(5) 0.004(3) -0.002(4) 0.016(4) C26 0.034(5) 0.026(4) 0.029(4) 0.007(3) -0.009(3) 0.008(4) C27 0.027(4) 0.026(4) 0.013(3) 0.000(3) -0.003(3) 0.001(3) C28 0.020(4) 0.019(4) 0.018(3) -0.002(3) -0.002(3) 0.004(3) C29 0.016(4) 0.016(4) 0.021(4) 0.004(3) -0.004(3) 0.005(3) C30 0.032(4) 0.018(4) 0.025(4) 0.000(3) 0.006(3) 0.006(3) C31 0.035(5) 0.020(4) 0.029(4) -0.002(3) 0.006(3) 0.008(4) C32 0.042(5) 0.014(4) 0.026(4) -0.009(3) -0.011(4) 0.007(4) C33 0.023(4) 0.024(4) 0.034(4) -0.001(3) -0.006(3) 0.007(3) C34 0.026(4) 0.022(4) 0.027(4) 0.001(3) 0.000(3) 0.009(3) C35 0.022(4) 0.016(4) 0.011(3) 0.000(3) 0.007(3) 0.001(3) C36 0.016(4) 0.020(4) 0.022(4) -0.001(3) 0.000(3) 0.000(3) C37 0.028(4) 0.026(4) 0.032(4) -0.002(3) 0.006(3) 0.012(4) C38 0.032(5) 0.033(5) 0.030(4) 0.001(4) 0.012(4) 0.006(4) C39 0.047(5) 0.029(4) 0.015(4) -0.004(3) 0.004(3) 0.010(4) C40 0.034(4) 0.018(4) 0.024(4) -0.005(3) 0.002(3) 0.005(3) C41 0.030(4) 0.022(4) 0.018(3) -0.001(3) 0.006(3) 0.014(3) C42 0.032(4) 0.016(4) 0.025(4) -0.001(3) -0.001(3) 0.004(3) C43 0.055(6) 0.020(4) 0.022(4) 0.002(3) 0.004(4) 0.009(4) C44 0.071(7) 0.032(5) 0.017(4) 0.008(3) 0.004(4) 0.038(5) C45 0.036(5) 0.044(5) 0.025(4) 0.007(4) 0.004(3) 0.025(4) C46 0.028(4) 0.028(4) 0.029(4) 0.005(3) -0.003(3) 0.007(4) C47 0.040(5) 0.037(5) 0.044(5) 0.003(4) -0.003(4) 0.010(4) C48 0.015(4) 0.015(4) 0.024(4) 0.002(3) -0.002(3) 0.001(3) C49 0.042(5) 0.047(6) 0.040(5) -0.008(4) 0.004(4) 0.015(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 Ru1 O2 2.097(4) . ? Ru1 O1 2.109(4) . ? Ru1 P1 2.3970(18) . ? Ru1 Cl1 2.400(4) . ? Ru1 P2 2.4080(19) . ? Ru1 Cl2 2.448(4) . ? As1 C2 1.921(7) . ? As1 C1 1.937(7) . ? P1 C17 1.819(7) . ? P1 C23 1.836(7) . ? P1 C11 1.837(7) . ? P2 C35 1.831(7) . ? P2 C29 1.836(7) . ? P2 C41 1.841(7) . ? O1 C1 1.263(8) . ? O2 C2 1.234(8) . ? C1 C3 1.523(9) . ? C2 C7 1.535(9) . ? C3 C4 1.530(11) . ? C3 C6 1.539(10) . ? C3 C5 1.539(11) . ? C7 C10 1.534(10) . ? C7 C9 1.540(10) . ? C7 C8 1.552(10) . ? C11 C12 1.383(10) . ? C11 C16 1.415(10) . ? C12 C13 1.389(10) . ? C13 C14 1.403(11) . ? C14 C15 1.385(11) . ? C15 C16 1.370(10) . ? C17 C22 1.395(10) . ? C17 C18 1.418(10) . ? C18 C19 1.377(10) . ? C19 C20 1.390(11) . ? C20 C21 1.380(11) . ? C21 C22 1.377(10) . ? C23 C24 1.381(10) . ? C23 C28 1.406(9) . ? C24 C25 1.389(10) . ? C25 C26 1.371(11) . ? C26 C27 1.369(11) . ? C27 C28 1.381(10) . ? C29 C34 1.393(10) . ? C29 C30 1.402(10) . ? C30 C31 1.383(10) . ? C31 C32 1.403(11) . ? C32 C33 1.392(11) . ? C33 C34 1.387(10) . ? C35 C40 1.394(10) . ? C35 C36 1.396(10) . ? C36 C37 1.382(10) . ? C37 C38 1.369(11) . ? C38 C39 1.399(12) . ? C39 C40 1.371(11) . ? C41 C46 1.375(11) . ? C41 C42 1.398(10) . ? C42 C43 1.365(11) . ? C43 C44 1.381(12) . ? C44 C45 1.380(12) . ? C45 C46 1.398(11) . ? C47 C48 1.375(11) . ? C47 C47 1.466(17) 2_655 ? C48 C49 1.419(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ru1 O1 90.94(17) . . ? O2 Ru1 P1 92.57(13) . . ? O1 Ru1 P1 92.80(13) . . ? O2 Ru1 Cl1 83.87(14) . . ? O1 Ru1 Cl1 174.71(14) . . ? P1 Ru1 Cl1 86.42(8) . . ? O2 Ru1 P2 91.26(13) . . ? O1 Ru1 P2 88.86(13) . . ? P1 Ru1 P2 175.79(6) . . ? Cl1 Ru1 P2 92.28(8) . . ? O2 Ru1 Cl2 177.32(14) . . ? O1 Ru1 Cl2 90.26(14) . . ? P1 Ru1 Cl2 89.76(8) . . ? Cl1 Ru1 Cl2 94.97(10) . . ? P2 Ru1 Cl2 86.37(8) . . ? C2 As1 C1 101.9(3) . . ? C17 P1 C23 107.5(3) . . ? C17 P1 C11 99.3(3) . . ? C23 P1 C11 100.6(3) . . ? C17 P1 Ru1 115.7(2) . . ? C23 P1 Ru1 114.4(2) . . ? C11 P1 Ru1 117.3(2) . . ? C35 P2 C29 105.3(3) . . ? C35 P2 C41 103.7(3) . . ? C29 P2 C41 98.8(3) . . ? C35 P2 Ru1 111.7(2) . . ? C29 P2 Ru1 117.5(2) . . ? C41 P2 Ru1 118.0(2) . . ? C1 O1 Ru1 131.7(4) . . ? C2 O2 Ru1 133.9(4) . . ? O1 C1 C3 117.2(6) . . ? O1 C1 As1 128.9(5) . . ? C3 C1 As1 113.8(5) . . ? O2 C2 C7 115.5(6) . . ? O2 C2 As1 128.2(5) . . ? C7 C2 As1 116.1(5) . . ? C1 C3 C4 110.4(6) . . ? C1 C3 C6 108.9(6) . . ? C4 C3 C6 107.7(7) . . ? C1 C3 C5 109.7(6) . . ? C4 C3 C5 109.9(7) . . ? C6 C3 C5 110.2(6) . . ? C10 C7 C2 112.7(6) . . ? C10 C7 C9 108.8(6) . . ? C2 C7 C9 106.5(6) . . ? C10 C7 C8 109.9(6) . . ? C2 C7 C8 109.3(5) . . ? C9 C7 C8 109.5(6) . . ? C12 C11 C16 118.2(6) . . ? C12 C11 P1 124.7(5) . . ? C16 C11 P1 117.1(5) . . ? C11 C12 C13 121.3(7) . . ? C12 C13 C14 120.0(7) . . ? C15 C14 C13 118.8(7) . . ? C16 C15 C14 121.3(7) . . ? C15 C16 C11 120.5(7) . . ? C22 C17 C18 116.7(6) . . ? C22 C17 P1 126.9(5) . . ? C18 C17 P1 116.2(5) . . ? C19 C18 C17 122.6(7) . . ? C18 C19 C20 118.5(7) . . ? C21 C20 C19 120.3(7) . . ? C22 C21 C20 120.8(8) . . ? C21 C22 C17 121.1(7) . . ? C24 C23 C28 118.6(6) . . ? C24 C23 P1 119.1(5) . . ? C28 C23 P1 122.3(5) . . ? C23 C24 C25 121.2(7) . . ? C26 C25 C24 119.2(8) . . ? C27 C26 C25 120.7(7) . . ? C26 C27 C28 120.7(7) . . ? C27 C28 C23 119.6(7) . . ? C34 C29 C30 118.7(7) . . ? C34 C29 P2 125.8(6) . . ? C30 C29 P2 115.4(5) . . ? C31 C30 C29 121.0(7) . . ? C30 C31 C32 120.1(7) . . ? C33 C32 C31 118.9(7) . . ? C34 C33 C32 121.0(7) . . ? C33 C34 C29 120.4(7) . . ? C40 C35 C36 118.5(6) . . ? C40 C35 P2 120.9(6) . . ? C36 C35 P2 120.4(5) . . ? C37 C36 C35 121.3(7) . . ? C38 C37 C36 119.2(8) . . ? C37 C38 C39 120.5(7) . . ? C40 C39 C38 120.2(7) . . ? C39 C40 C35 120.2(8) . . ? C46 C41 C42 118.9(7) . . ? C46 C41 P2 122.0(6) . . ? C42 C41 P2 119.0(6) . . ? C43 C42 C41 120.7(8) . . ? C42 C43 C44 120.6(8) . . ? C45 C44 C43 119.6(7) . . ? C44 C45 C46 120.0(8) . . ? C41 C46 C45 120.3(8) . . ? C48 C47 C47 112.2(10) . 2_655 ? C47 C48 C49 113.1(7) . . ? 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 O2 Ru1 P1 C17 107.7(3) . . . . ? O1 Ru1 P1 C17 16.6(3) . . . . ? Cl1 Ru1 P1 C17 -168.6(3) . . . . ? P2 Ru1 P1 C17 -96.6(9) . . . . ? Cl2 Ru1 P1 C17 -73.6(3) . . . . ? O2 Ru1 P1 C23 -18.1(3) . . . . ? O1 Ru1 P1 C23 -109.2(3) . . . . ? Cl1 Ru1 P1 C23 65.6(3) . . . . ? P2 Ru1 P1 C23 137.6(9) . . . . ? Cl2 Ru1 P1 C23 160.6(3) . . . . ? O2 Ru1 P1 C11 -135.6(3) . . . . ? O1 Ru1 P1 C11 133.4(3) . . . . ? Cl1 Ru1 P1 C11 -51.9(2) . . . . ? P2 Ru1 P1 C11 20.2(10) . . . . ? Cl2 Ru1 P1 C11 43.1(2) . . . . ? O2 Ru1 P2 C35 106.3(3) . . . . ? O1 Ru1 P2 C35 -162.8(3) . . . . ? P1 Ru1 P2 C35 -49.4(10) . . . . ? Cl1 Ru1 P2 C35 22.4(3) . . . . ? Cl2 Ru1 P2 C35 -72.4(3) . . . . ? O2 Ru1 P2 C29 -15.4(3) . . . . ? O1 Ru1 P2 C29 75.5(3) . . . . ? P1 Ru1 P2 C29 -171.2(9) . . . . ? Cl1 Ru1 P2 C29 -99.4(3) . . . . ? Cl2 Ru1 P2 C29 165.8(3) . . . . ? O2 Ru1 P2 C41 -133.7(3) . . . . ? O1 Ru1 P2 C41 -42.8(3) . . . . ? P1 Ru1 P2 C41 70.6(9) . . . . ? Cl1 Ru1 P2 C41 142.4(3) . . . . ? Cl2 Ru1 P2 C41 47.6(3) . . . . ? O2 Ru1 O1 C1 -18.0(6) . . . . ? P1 Ru1 O1 C1 74.7(6) . . . . ? Cl1 Ru1 O1 C1 -6.8(19) . . . . ? P2 Ru1 O1 C1 -109.2(6) . . . . ? Cl2 Ru1 O1 C1 164.4(6) . . . . ? O1 Ru1 O2 C2 21.5(6) . . . . ? P1 Ru1 O2 C2 -71.4(6) . . . . ? Cl1 Ru1 O2 C2 -157.5(6) . . . . ? P2 Ru1 O2 C2 110.3(6) . . . . ? Cl2 Ru1 O2 C2 138(3) . . . . ? Ru1 O1 C1 C3 -173.4(4) . . . . ? Ru1 O1 C1 As1 4.4(9) . . . . ? C2 As1 C1 O1 11.6(7) . . . . ? C2 As1 C1 C3 -170.5(5) . . . . ? Ru1 O2 C2 C7 174.3(4) . . . . ? Ru1 O2 C2 As1 -10.1(10) . . . . ? C1 As1 C2 O2 -9.0(7) . . . . ? C1 As1 C2 C7 166.6(5) . . . . ? O1 C1 C3 C4 -4.5(9) . . . . ? As1 C1 C3 C4 177.3(6) . . . . ? O1 C1 C3 C6 -122.7(7) . . . . ? As1 C1 C3 C6 59.2(7) . . . . ? O1 C1 C3 C5 116.7(7) . . . . ? As1 C1 C3 C5 -61.5(7) . . . . ? O2 C2 C7 C10 -157.4(6) . . . . ? As1 C2 C7 C10 26.4(8) . . . . ? O2 C2 C7 C9 83.4(7) . . . . ? As1 C2 C7 C9 -92.8(6) . . . . ? O2 C2 C7 C8 -34.9(8) . . . . ? As1 C2 C7 C8 149.0(5) . . . . ? C17 P1 C11 C12 131.6(6) . . . . ? C23 P1 C11 C12 -118.5(6) . . . . ? Ru1 P1 C11 C12 6.3(7) . . . . ? C17 P1 C11 C16 -50.2(6) . . . . ? C23 P1 C11 C16 59.7(6) . . . . ? Ru1 P1 C11 C16 -175.6(5) . . . . ? C16 C11 C12 C13 1.8(11) . . . . ? P1 C11 C12 C13 180.0(5) . . . . ? C11 C12 C13 C14 -0.9(11) . . . . ? C12 C13 C14 C15 -0.3(12) . . . . ? C13 C14 C15 C16 0.3(13) . . . . ? C14 C15 C16 C11 0.7(13) . . . . ? C12 C11 C16 C15 -1.7(11) . . . . ? P1 C11 C16 C15 180.0(7) . . . . ? C23 P1 C17 C22 -11.1(7) . . . . ? C11 P1 C17 C22 93.2(7) . . . . ? Ru1 P1 C17 C22 -140.4(6) . . . . ? C23 P1 C17 C18 175.1(5) . . . . ? C11 P1 C17 C18 -80.6(6) . . . . ? Ru1 P1 C17 C18 45.9(6) . . . . ? C22 C17 C18 C19 -1.4(10) . . . . ? P1 C17 C18 C19 173.0(6) . . . . ? C17 C18 C19 C20 1.7(11) . . . . ? C18 C19 C20 C21 0.0(11) . . . . ? C19 C20 C21 C22 -2.0(12) . . . . ? C20 C21 C22 C17 2.2(11) . . . . ? C18 C17 C22 C21 -0.6(10) . . . . ? P1 C17 C22 C21 -174.3(6) . . . . ? C17 P1 C23 C24 140.1(6) . . . . ? C11 P1 C23 C24 36.7(6) . . . . ? Ru1 P1 C23 C24 -90.0(6) . . . . ? C17 P1 C23 C28 -40.4(6) . . . . ? C11 P1 C23 C28 -143.9(6) . . . . ? Ru1 P1 C23 C28 89.5(6) . . . . ? C28 C23 C24 C25 -0.1(11) . . . . ? P1 C23 C24 C25 179.4(6) . . . . ? C23 C24 C25 C26 2.5(12) . . . . ? C24 C25 C26 C27 -3.1(12) . . . . ? C25 C26 C27 C28 1.1(12) . . . . ? C26 C27 C28 C23 1.4(11) . . . . ? C24 C23 C28 C27 -1.9(10) . . . . ? P1 C23 C28 C27 178.6(5) . . . . ? C35 P2 C29 C34 0.6(7) . . . . ? C41 P2 C29 C34 -106.3(7) . . . . ? Ru1 P2 C29 C34 125.6(6) . . . . ? C35 P2 C29 C30 176.8(5) . . . . ? C41 P2 C29 C30 69.9(6) . . . . ? Ru1 P2 C29 C30 -58.2(6) . . . . ? C34 C29 C30 C31 0.4(11) . . . . ? P2 C29 C30 C31 -176.1(6) . . . . ? C29 C30 C31 C32 -1.1(12) . . . . ? C30 C31 C32 C33 1.1(11) . . . . ? C31 C32 C33 C34 -0.4(12) . . . . ? C32 C33 C34 C29 -0.4(12) . . . . ? C30 C29 C34 C33 0.4(11) . . . . ? P2 C29 C34 C33 176.5(6) . . . . ? C29 P2 C35 C40 -129.7(6) . . . . ? C41 P2 C35 C40 -26.4(6) . . . . ? Ru1 P2 C35 C40 101.7(6) . . . . ? C29 P2 C35 C36 55.3(6) . . . . ? C41 P2 C35 C36 158.7(6) . . . . ? Ru1 P2 C35 C36 -73.2(6) . . . . ? C40 C35 C36 C37 3.3(10) . . . . ? P2 C35 C36 C37 178.4(6) . . . . ? C35 C36 C37 C38 -1.2(11) . . . . ? C36 C37 C38 C39 -1.5(12) . . . . ? C37 C38 C39 C40 2.0(12) . . . . ? C38 C39 C40 C35 0.2(11) . . . . ? C36 C35 C40 C39 -2.8(10) . . . . ? P2 C35 C40 C39 -177.8(6) . . . . ? C35 P2 C41 C46 119.7(6) . . . . ? C29 P2 C41 C46 -132.1(6) . . . . ? Ru1 P2 C41 C46 -4.4(7) . . . . ? C35 P2 C41 C42 -61.9(6) . . . . ? C29 P2 C41 C42 46.3(6) . . . . ? Ru1 P2 C41 C42 174.0(5) . . . . ? C46 C41 C42 C43 -0.8(11) . . . . ? P2 C41 C42 C43 -179.2(6) . . . . ? C41 C42 C43 C44 0.9(12) . . . . ? C42 C43 C44 C45 -0.4(12) . . . . ? C43 C44 C45 C46 -0.4(11) . . . . ? C42 C41 C46 C45 0.0(11) . . . . ? P2 C41 C46 C45 178.4(6) . . . . ? C44 C45 C46 C41 0.5(12) . . . . ? C47 C47 C48 C49 178.7(10) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.546 _refine_diff_density_min -1.876 _refine_diff_density_rms 0.197 data_compound 16 _database_code_CSD 165262 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H46 As2 Co O6' _chemical_formula_weight 639.38 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.994(5) _cell_length_b 15.383(5) _cell_length_c 18.616(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.61(2) _cell_angle_gamma 90.00 _cell_volume 3145(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 2.664 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5834 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.19 _reflns_number_total 5647 _reflns_number_gt 3279 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1158P)^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 5647 _refine_ls_number_parameters 312 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1686 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2981 _refine_ls_wR_factor_gt 0.2372 _refine_ls_goodness_of_fit_ref 1.703 _refine_ls_restrained_S_all 1.743 _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 0.48409(10) 0.82900(8) 0.22222(5) 0.0460(4) Uani 1 1 d . . . As2 As 0.07455(12) 0.66629(9) 0.02762(7) 0.0634(5) Uani 1 1 d . . . Co1 Co 0.36950(12) 0.80056(10) 0.02767(7) 0.0387(4) Uani 1 1 d . . . O1 O 0.5385(6) 0.7950(5) 0.0755(3) 0.0461(18) Uani 1 1 d . . . O2 O 0.3088(6) 0.8727(5) 0.1101(3) 0.0454(17) Uani 1 1 d . . . O3 O 0.2117(6) 0.8074(5) -0.0274(4) 0.0437(17) Uani 1 1 d . . . O4 O 0.3274(7) 0.6848(5) 0.0707(4) 0.0544(19) Uani 1 1 d . . . O5 O 0.4169(7) 0.9165(6) -0.0322(4) 0.059(2) Uani 1 1 d . . . O6 O 0.4523(8) 0.7497(7) -0.0654(4) 0.072(3) Uani 1 1 d . . . C1 C 0.5728(8) 0.7946(7) 0.1413(5) 0.043(2) Uani 1 1 d . . . C2 C 0.3393(10) 0.8697(6) 0.1764(5) 0.040(2) Uani 1 1 d . . . C3 C 0.7046(9) 0.7607(8) 0.1571(5) 0.046(3) Uani 1 1 d . . . C4 C 0.7169(12) 0.6704(11) 0.1265(7) 0.080(5) Uani 1 1 d . . . H4A H 0.7011 0.6722 0.0753 0.119 Uiso 1 1 calc R . . H4B H 0.6595 0.6323 0.1477 0.119 Uiso 1 1 calc R . . H4C H 0.7980 0.6493 0.1368 0.119 Uiso 1 1 calc R . . C5 C 0.7883(11) 0.8254(11) 0.1193(8) 0.080(5) Uani 1 1 d . . . H5A H 0.7600 0.8324 0.0701 0.120 Uiso 1 1 calc R . . H5B H 0.8701 0.8033 0.1210 0.120 Uiso 1 1 calc R . . H5C H 0.7869 0.8806 0.1433 0.120 Uiso 1 1 calc R . . C6 C 0.7445(12) 0.7582(11) 0.2358(6) 0.071(4) Uani 1 1 d . . . H6A H 0.6918 0.7202 0.2610 0.107 Uiso 1 1 calc R . . H6B H 0.7404 0.8157 0.2557 0.107 Uiso 1 1 calc R . . H6C H 0.8266 0.7372 0.2409 0.107 Uiso 1 1 calc R . . C7 C 0.2432(10) 0.9134(7) 0.2235(5) 0.051(3) Uani 1 1 d . . . C8 C 0.2670(11) 0.8967(11) 0.3036(6) 0.076(4) Uani 1 1 d . . . H8A H 0.2035 0.9228 0.3300 0.114 Uiso 1 1 calc R . . H8B H 0.3440 0.9215 0.3189 0.114 Uiso 1 1 calc R . . H8C H 0.2685 0.8352 0.3123 0.114 Uiso 1 1 calc R . . C9 C 0.1163(10) 0.8827(11) 0.1989(7) 0.076(4) Uani 1 1 d . . . H9A H 0.0564 0.9194 0.2195 0.114 Uiso 1 1 calc R . . H9B H 0.1048 0.8238 0.2143 0.114 Uiso 1 1 calc R . . H9C H 0.1076 0.8856 0.1474 0.114 Uiso 1 1 calc R . . C10 C 0.2542(13) 1.0126(9) 0.2089(7) 0.071(4) Uani 1 1 d . . . H10A H 0.3357 1.0314 0.2211 0.107 Uiso 1 1 calc R . . H10B H 0.1982 1.0436 0.2375 0.107 Uiso 1 1 calc R . . H10C H 0.2354 1.0240 0.1589 0.107 Uiso 1 1 calc R . . C11 C 0.1130(9) 0.7672(7) -0.0274(5) 0.043(2) Uani 1 1 d . . . C12 C 0.2270(13) 0.6438(7) 0.0753(6) 0.055(3) Uani 1 1 d . . . C13 C 0.0078(10) 0.8083(7) -0.0741(5) 0.044(2) Uani 1 1 d . . . C14 C -0.0206(11) 0.8949(7) -0.0382(6) 0.056(3) Uani 1 1 d . . . H14A H -0.0457 0.8844 0.0098 0.083 Uiso 1 1 calc R . . H14B H -0.0848 0.9238 -0.0654 0.083 Uiso 1 1 calc R . . H14C H 0.0509 0.9308 -0.0364 0.083 Uiso 1 1 calc R . . C15 C -0.1095(10) 0.7520(10) -0.0807(7) 0.066(4) Uani 1 1 d . . . H15A H -0.1385 0.7411 -0.0337 0.098 Uiso 1 1 calc R . . H15B H -0.0917 0.6977 -0.1034 0.098 Uiso 1 1 calc R . . H15C H -0.1710 0.7824 -0.1091 0.098 Uiso 1 1 calc R . . C16 C 0.0532(11) 0.8229(10) -0.1489(6) 0.064(4) Uani 1 1 d . . . H16A H -0.0027 0.8599 -0.1756 0.095 Uiso 1 1 calc R . . H16B H 0.0592 0.7681 -0.1732 0.095 Uiso 1 1 calc R . . H16C H 0.1320 0.8500 -0.1453 0.095 Uiso 1 1 calc R . . C17 C 0.2383(14) 0.5637(9) 0.1264(7) 0.073(4) Uani 1 1 d . . . C18 C 0.262(3) 0.4868(19) 0.0858(12) 0.164(9) Uani 1 1 d U . . H18A H 0.1881 0.4674 0.0615 0.247 Uiso 1 1 calc R . . H18B H 0.2928 0.4420 0.1177 0.247 Uiso 1 1 calc R . . H18C H 0.3214 0.4995 0.0510 0.247 Uiso 1 1 calc R . . C19 C 0.114(3) 0.538(2) 0.1560(19) 0.223(14) Uani 1 1 d U . . H19A H 0.0846 0.5850 0.1849 0.335 Uiso 1 1 calc R . . H19B H 0.1230 0.4869 0.1849 0.335 Uiso 1 1 calc R . . H19C H 0.0563 0.5275 0.1166 0.335 Uiso 1 1 calc R . . C20 C 0.305(3) 0.584(3) 0.1899(17) 0.239(16) Uani 1 1 d U . . H20A H 0.3192 0.6458 0.1917 0.359 Uiso 1 1 calc R . . H20B H 0.3809 0.5539 0.1913 0.359 Uiso 1 1 calc R . . H20C H 0.2591 0.5673 0.2304 0.359 Uiso 1 1 calc R . . C21 C 0.3320(12) 0.9920(8) -0.0288(8) 0.075(4) Uani 1 1 d . . . H21A H 0.3777 1.0452 -0.0289 0.112 Uiso 1 1 calc R . . H21B H 0.2879 0.9886 0.0145 0.112 Uiso 1 1 calc R . . H21C H 0.2756 0.9909 -0.0697 0.112 Uiso 1 1 calc R . . C22 C 0.4417(14) 0.8976(13) -0.1028(8) 0.096(6) Uani 1 1 d . . . H22A H 0.4842 0.9456 -0.1244 0.115 Uiso 1 1 calc R . . H22B H 0.3670 0.8865 -0.1311 0.115 Uiso 1 1 calc R . . C23 C 0.5203(14) 0.8180(12) -0.0992(7) 0.088(5) Uani 1 1 d . . . H23A H 0.5409 0.8004 -0.1472 0.105 Uiso 1 1 calc R . . H23B H 0.5952 0.8297 -0.0714 0.105 Uiso 1 1 calc R . . C24 C 0.5189(15) 0.6726(10) -0.0622(8) 0.085(4) Uani 1 1 d U . . H24A H 0.4681 0.6262 -0.0464 0.127 Uiso 1 1 calc R . . H24B H 0.5876 0.6792 -0.0290 0.127 Uiso 1 1 calc R . . H24C H 0.5468 0.6592 -0.1091 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 0.0391(6) 0.0655(8) 0.0340(5) -0.0010(5) 0.0067(4) 0.0082(5) As2 0.0570(8) 0.0557(8) 0.0771(9) 0.0145(6) 0.0001(6) -0.0167(6) Co1 0.0312(7) 0.0507(9) 0.0346(7) -0.0011(6) 0.0055(5) 0.0028(6) O1 0.038(4) 0.063(5) 0.038(4) 0.000(3) 0.013(3) 0.004(4) O2 0.041(4) 0.055(5) 0.040(4) -0.001(3) 0.006(3) 0.005(3) O3 0.039(4) 0.043(4) 0.049(4) 0.004(3) 0.008(3) -0.006(3) O4 0.051(5) 0.041(4) 0.070(5) 0.006(4) -0.002(4) 0.008(4) O5 0.043(4) 0.087(6) 0.046(4) 0.013(4) 0.002(3) -0.022(4) O6 0.059(5) 0.106(8) 0.051(5) -0.031(5) -0.006(4) 0.029(5) C1 0.026(5) 0.054(7) 0.050(6) 0.015(5) 0.010(4) 0.012(5) C2 0.059(7) 0.026(5) 0.035(5) -0.009(4) 0.015(5) -0.009(5) C3 0.034(5) 0.067(8) 0.036(5) 0.002(5) -0.003(4) 0.015(5) C4 0.052(8) 0.117(14) 0.070(8) -0.002(8) 0.001(6) 0.040(8) C5 0.036(7) 0.119(13) 0.086(9) 0.029(9) 0.015(6) 0.000(7) C6 0.046(7) 0.119(12) 0.048(7) 0.004(7) -0.004(5) 0.008(8) C7 0.054(7) 0.054(7) 0.046(6) -0.017(5) 0.015(5) 0.009(6) C8 0.056(8) 0.125(13) 0.049(7) -0.013(8) 0.024(6) 0.016(8) C9 0.036(6) 0.121(13) 0.072(8) -0.039(8) 0.010(6) -0.009(7) C10 0.077(9) 0.056(8) 0.082(9) -0.018(7) 0.010(7) 0.016(7) C11 0.041(6) 0.039(6) 0.049(6) 0.000(5) 0.009(5) 0.012(5) C12 0.083(9) 0.030(6) 0.052(6) -0.012(5) -0.005(6) 0.007(6) C13 0.040(6) 0.047(6) 0.046(6) -0.006(5) 0.012(4) -0.007(5) C14 0.052(7) 0.046(7) 0.069(7) -0.006(6) 0.006(6) 0.012(6) C15 0.035(6) 0.093(10) 0.069(8) 0.006(7) 0.002(5) -0.008(6) C16 0.039(6) 0.110(11) 0.042(6) 0.006(6) 0.001(5) 0.000(7) C17 0.091(10) 0.053(8) 0.076(9) 0.002(7) -0.005(8) -0.030(7) C18 0.187(10) 0.148(10) 0.160(10) 0.017(5) 0.021(5) 0.016(5) C19 0.221(15) 0.223(15) 0.227(15) 0.030(5) 0.020(5) 0.015(5) C20 0.255(16) 0.231(16) 0.229(16) 0.026(5) -0.022(5) -0.015(5) C21 0.071(9) 0.040(7) 0.112(11) 0.025(7) -0.007(8) 0.002(7) C22 0.060(9) 0.149(17) 0.083(10) 0.020(11) 0.029(8) -0.022(10) C23 0.063(9) 0.156(16) 0.048(7) -0.009(8) 0.040(7) -0.017(10) C24 0.084(6) 0.098(6) 0.071(5) -0.028(4) -0.012(4) 0.030(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 As1 C2 1.879(11) . ? As1 C1 1.906(10) . ? As2 C12 1.893(13) . ? As2 C11 1.918(11) . ? Co1 O3 1.977(7) . ? Co1 O4 2.015(8) . ? Co1 O1 2.025(7) . ? Co1 O2 2.031(7) . ? Co1 O6 2.141(8) . ? Co1 O5 2.179(8) . ? O1 C1 1.266(12) . ? O2 C2 1.265(11) . ? O3 C11 1.249(12) . ? O4 C12 1.277(15) . ? O5 C22 1.386(16) . ? O5 C21 1.494(15) . ? O6 C24 1.394(16) . ? O6 C23 1.450(17) . ? C1 C3 1.555(13) . ? C2 C7 1.556(13) . ? C3 C6 1.511(14) . ? C3 C4 1.511(19) . ? C3 C5 1.547(17) . ? C7 C9 1.523(16) . ? C7 C8 1.525(15) . ? C7 C10 1.555(18) . ? C11 C13 1.549(15) . ? C12 C17 1.559(18) . ? C13 C16 1.518(14) . ? C13 C14 1.529(15) . ? C13 C15 1.553(16) . ? C17 C20 1.40(3) . ? C17 C18 1.43(3) . ? C17 C19 1.55(3) . ? C22 C23 1.50(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 C2 As1 C1 100.8(4) . . ? C12 As2 C11 100.7(5) . . ? O3 Co1 O4 92.4(3) . . ? O3 Co1 O1 174.8(3) . . ? O4 Co1 O1 90.6(3) . . ? O3 Co1 O2 93.0(3) . . ? O4 Co1 O2 95.3(3) . . ? O1 Co1 O2 91.0(3) . . ? O3 Co1 O6 89.7(3) . . ? O4 Co1 O6 96.5(4) . . ? O1 Co1 O6 85.7(3) . . ? O2 Co1 O6 167.8(4) . . ? O3 Co1 O5 85.2(3) . . ? O4 Co1 O5 172.4(3) . . ? O1 Co1 O5 91.3(3) . . ? O2 Co1 O5 91.9(3) . . ? O6 Co1 O5 76.4(4) . . ? C1 O1 Co1 130.7(6) . . ? C2 O2 Co1 129.4(7) . . ? C11 O3 Co1 135.7(7) . . ? C12 O4 Co1 132.7(7) . . ? C22 O5 C21 110.8(11) . . ? C22 O5 Co1 112.1(9) . . ? C21 O5 Co1 116.8(7) . . ? C24 O6 C23 110.8(12) . . ? C24 O6 Co1 121.2(8) . . ? C23 O6 Co1 109.5(8) . . ? O1 C1 C3 114.8(8) . . ? O1 C1 As1 128.6(7) . . ? C3 C1 As1 116.7(7) . . ? O2 C2 C7 112.1(9) . . ? O2 C2 As1 129.6(7) . . ? C7 C2 As1 118.1(7) . . ? C6 C3 C4 108.4(11) . . ? C6 C3 C5 107.8(11) . . ? C4 C3 C5 110.7(10) . . ? C6 C3 C1 114.8(9) . . ? C4 C3 C1 109.6(9) . . ? C5 C3 C1 105.5(9) . . ? C9 C7 C8 110.9(10) . . ? C9 C7 C10 109.2(11) . . ? C8 C7 C10 109.0(10) . . ? C9 C7 C2 109.5(9) . . ? C8 C7 C2 112.8(10) . . ? C10 C7 C2 105.4(9) . . ? O3 C11 C13 115.2(9) . . ? O3 C11 As2 127.8(8) . . ? C13 C11 As2 116.9(7) . . ? O4 C12 C17 112.7(11) . . ? O4 C12 As2 128.9(9) . . ? C17 C12 As2 118.3(10) . . ? C16 C13 C14 110.7(10) . . ? C16 C13 C11 107.9(8) . . ? C14 C13 C11 105.8(9) . . ? C16 C13 C15 108.5(9) . . ? C14 C13 C15 109.6(9) . . ? C11 C13 C15 114.4(10) . . ? C20 C17 C18 122(2) . . ? C20 C17 C19 101(2) . . ? C18 C17 C19 100(2) . . ? C20 C17 C12 111.2(18) . . ? C18 C17 C12 110.0(14) . . ? C19 C17 C12 111.7(17) . . ? O5 C22 C23 105.5(12) . . ? O6 C23 C22 107.7(10) . . ? 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 Co1 O1 C1 171(3) . . . . ? O4 Co1 O1 C1 -64.0(10) . . . . ? O2 Co1 O1 C1 31.4(10) . . . . ? O6 Co1 O1 C1 -160.4(10) . . . . ? O5 Co1 O1 C1 123.3(10) . . . . ? O3 Co1 O2 C2 149.2(9) . . . . ? O4 Co1 O2 C2 56.5(9) . . . . ? O1 Co1 O2 C2 -34.2(9) . . . . ? O6 Co1 O2 C2 -108.3(15) . . . . ? O5 Co1 O2 C2 -125.6(9) . . . . ? O4 Co1 O3 C11 12.2(10) . . . . ? O1 Co1 O3 C11 137(3) . . . . ? O2 Co1 O3 C11 -83.3(10) . . . . ? O6 Co1 O3 C11 108.6(10) . . . . ? O5 Co1 O3 C11 -175.0(10) . . . . ? O3 Co1 O4 C12 -15.7(10) . . . . ? O1 Co1 O4 C12 168.6(10) . . . . ? O2 Co1 O4 C12 77.5(10) . . . . ? O6 Co1 O4 C12 -105.7(10) . . . . ? O5 Co1 O4 C12 -86(2) . . . . ? O3 Co1 O5 C22 -74.8(9) . . . . ? O4 Co1 O5 C22 -4(3) . . . . ? O1 Co1 O5 C22 101.4(9) . . . . ? O2 Co1 O5 C22 -167.6(8) . . . . ? O6 Co1 O5 C22 16.1(8) . . . . ? O3 Co1 O5 C21 54.5(8) . . . . ? O4 Co1 O5 C21 126(2) . . . . ? O1 Co1 O5 C21 -129.4(8) . . . . ? O2 Co1 O5 C21 -38.3(8) . . . . ? O6 Co1 O5 C21 145.4(8) . . . . ? O3 Co1 O6 C24 -127.2(10) . . . . ? O4 Co1 O6 C24 -34.8(11) . . . . ? O1 Co1 O6 C24 55.3(10) . . . . ? O2 Co1 O6 C24 130.0(15) . . . . ? O5 Co1 O6 C24 147.7(11) . . . . ? O3 Co1 O6 C23 102.0(8) . . . . ? O4 Co1 O6 C23 -165.7(8) . . . . ? O1 Co1 O6 C23 -75.5(8) . . . . ? O2 Co1 O6 C23 -0.9(18) . . . . ? O5 Co1 O6 C23 16.9(8) . . . . ? Co1 O1 C1 C3 161.4(7) . . . . ? Co1 O1 C1 As1 -18.0(16) . . . . ? C2 As1 C1 O1 -3.7(11) . . . . ? C2 As1 C1 C3 176.9(8) . . . . ? Co1 O2 C2 C7 -161.2(7) . . . . ? Co1 O2 C2 As1 23.9(14) . . . . ? C1 As1 C2 O2 0.5(11) . . . . ? C1 As1 C2 C7 -174.1(8) . . . . ? O1 C1 C3 C6 -178.6(11) . . . . ? As1 C1 C3 C6 1.0(14) . . . . ? O1 C1 C3 C4 -56.3(13) . . . . ? As1 C1 C3 C4 123.2(9) . . . . ? O1 C1 C3 C5 62.9(13) . . . . ? As1 C1 C3 C5 -117.6(9) . . . . ? O2 C2 C7 C9 46.1(13) . . . . ? As1 C2 C7 C9 -138.4(10) . . . . ? O2 C2 C7 C8 170.0(10) . . . . ? As1 C2 C7 C8 -14.5(13) . . . . ? O2 C2 C7 C10 -71.2(12) . . . . ? As1 C2 C7 C10 104.3(9) . . . . ? Co1 O3 C11 C13 170.4(6) . . . . ? Co1 O3 C11 As2 -5.3(15) . . . . ? C12 As2 C11 O3 -3.0(10) . . . . ? C12 As2 C11 C13 -178.6(7) . . . . ? Co1 O4 C12 C17 -169.3(8) . . . . ? Co1 O4 C12 As2 12.4(16) . . . . ? C11 As2 C12 O4 -0.7(11) . . . . ? C11 As2 C12 C17 -178.9(9) . . . . ? O3 C11 C13 C16 52.4(12) . . . . ? As2 C11 C13 C16 -131.4(8) . . . . ? O3 C11 C13 C14 -66.1(11) . . . . ? As2 C11 C13 C14 110.1(9) . . . . ? O3 C11 C13 C15 173.2(9) . . . . ? As2 C11 C13 C15 -10.6(12) . . . . ? O4 C12 C17 C20 44(2) . . . . ? As2 C12 C17 C20 -137.1(19) . . . . ? O4 C12 C17 C18 -94.0(17) . . . . ? As2 C12 C17 C18 84.4(17) . . . . ? O4 C12 C17 C19 156.4(18) . . . . ? As2 C12 C17 C19 -25(2) . . . . ? C21 O5 C22 C23 -176.4(11) . . . . ? Co1 O5 C22 C23 -44.1(12) . . . . ? C24 O6 C23 C22 178.2(11) . . . . ? Co1 O6 C23 C22 -45.5(13) . . . . ? O5 C22 C23 O6 59.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.581 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.250 data_compound 19 _database_code_CSD 165263 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H48 As Cl O2 P2 Pt' _chemical_formula_weight 844.11 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4700(10) _cell_length_b 10.104(2) _cell_length_c 21.9751(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.350(10) _cell_angle_gamma 90.00 _cell_volume 3431.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cut needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 5.244 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.10 _exptl_absorpt_correction_T_max 0.23 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type cad4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7571 _diffrn_reflns_av_R_equivalents 0.1142 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.30 _reflns_number_total 6936 _reflns_number_gt 5636 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0298P)^2^+14.1182P] 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 6936 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.10301(9) 0.42445(13) 0.32110(6) 0.0278(3) Uani 1 1 d . . . As1 As 0.31894(3) 0.71282(5) 0.41117(2) 0.01664(11) Uani 1 1 d . . . Pt1 Pt 0.207526(12) 0.576154(17) 0.364713(8) 0.01509(6) Uani 1 1 d . . . P1 P 0.27609(9) 0.38684(12) 0.40213(6) 0.0182(3) Uani 1 1 d . . . P2 P 0.13297(8) 0.74809(12) 0.31594(6) 0.0174(3) Uani 1 1 d . . . O1 O 0.2973(2) 0.9683(3) 0.46015(17) 0.0248(8) Uani 1 1 d . . . O2 O 0.3386(3) 0.7913(5) 0.29016(18) 0.0378(10) Uani 1 1 d . . . C1 C 0.2659(3) 0.8575(5) 0.4599(2) 0.0199(11) Uani 1 1 d . . . C2 C 0.1920(3) 0.8248(5) 0.4989(2) 0.0188(10) Uani 1 1 d . . . C3 C 0.1712(4) 0.6954(5) 0.5141(3) 0.0265(12) Uani 1 1 d . . . H3 H 0.2035 0.6255 0.4996 0.032 Uiso 1 1 calc R . . C4 C 0.1028(4) 0.6707(6) 0.5506(3) 0.0343(14) Uani 1 1 d . . . H4 H 0.0909 0.5840 0.5619 0.041 Uiso 1 1 calc R . . C5 C 0.0516(4) 0.7718(7) 0.5709(3) 0.0334(14) Uani 1 1 d . . . H5 H 0.0052 0.7543 0.5953 0.040 Uiso 1 1 calc R . . C6 C 0.0708(4) 0.8992(6) 0.5541(3) 0.0350(14) Uani 1 1 d . . . H6 H 0.0359 0.9683 0.5664 0.042 Uiso 1 1 calc R . . C7 C 0.1405(4) 0.9267(6) 0.5194(3) 0.0311(13) Uani 1 1 d . . . H7 H 0.1532 1.0139 0.5095 0.037 Uiso 1 1 calc R . . C8 C 0.3627(3) 0.8198(5) 0.3416(2) 0.0207(11) Uani 1 1 d . . . C9 C 0.4333(3) 0.9187(5) 0.3522(2) 0.0220(10) Uani 1 1 d . . . C10 C 0.4602(4) 0.9966(6) 0.3040(3) 0.0333(14) Uani 1 1 d . . . H10 H 0.4303 0.9917 0.2665 0.040 Uiso 1 1 calc R . . C11 C 0.5301(4) 1.0804(6) 0.3110(3) 0.0394(15) Uani 1 1 d . . . H11 H 0.5471 1.1317 0.2784 0.047 Uiso 1 1 calc R . . C12 C 0.5744(4) 1.0880(6) 0.3663(3) 0.0403(16) Uani 1 1 d . . . H12 H 0.6223 1.1434 0.3708 0.048 Uiso 1 1 calc R . . C13 C 0.5487(4) 1.0143(6) 0.4152(3) 0.0345(14) Uani 1 1 d . . . H13 H 0.5787 1.0199 0.4527 0.041 Uiso 1 1 calc R . . C14 C 0.4780(3) 0.9321(5) 0.4077(3) 0.0247(11) Uani 1 1 d . . . H14 H 0.4597 0.8842 0.4409 0.030 Uiso 1 1 calc R . . C15 C 0.3684(4) 0.4055(5) 0.4559(3) 0.0266(12) Uani 1 1 d . . . H15A H 0.4102 0.4636 0.4379 0.032 Uiso 1 1 calc R . . H15B H 0.3487 0.4489 0.4922 0.032 Uiso 1 1 calc R . . C16 C 0.4141(5) 0.2777(6) 0.4749(3) 0.0428(17) Uani 1 1 d . . . H16A H 0.4641 0.2981 0.5005 0.064 Uiso 1 1 calc R . . H16B H 0.4316 0.2314 0.4393 0.064 Uiso 1 1 calc R . . H16C H 0.3753 0.2231 0.4969 0.064 Uiso 1 1 calc R . . C17 C 0.2057(4) 0.2700(5) 0.4388(2) 0.0241(11) Uani 1 1 d . . . H17A H 0.1624 0.2385 0.4090 0.029 Uiso 1 1 calc R . . H17B H 0.2397 0.1943 0.4526 0.029 Uiso 1 1 calc R . . C18 C 0.1599(4) 0.3277(6) 0.4928(3) 0.0380(15) Uani 1 1 d . . . H18A H 0.1221 0.2623 0.5090 0.057 Uiso 1 1 calc R . . H18B H 0.1267 0.4036 0.4798 0.057 Uiso 1 1 calc R . . H18C H 0.2021 0.3536 0.5238 0.057 Uiso 1 1 calc R . . C19 C 0.3172(4) 0.2908(5) 0.3395(3) 0.0251(12) Uani 1 1 d . . . H19A H 0.3437 0.2106 0.3558 0.030 Uiso 1 1 calc R . . H19B H 0.2690 0.2650 0.3125 0.030 Uiso 1 1 calc R . . C20 C 0.3829(4) 0.3644(7) 0.3030(3) 0.0379(15) Uani 1 1 d . . . H20A H 0.4011 0.3090 0.2704 0.057 Uiso 1 1 calc R . . H20B H 0.4320 0.3871 0.3290 0.057 Uiso 1 1 calc R . . H20C H 0.3571 0.4436 0.2864 0.057 Uiso 1 1 calc R . . C21 C 0.0168(3) 0.7228(6) 0.3214(3) 0.0256(12) Uani 1 1 d . . . H21A H -0.0137 0.7977 0.3031 0.031 Uiso 1 1 calc R . . H21B H -0.0002 0.6442 0.2986 0.031 Uiso 1 1 calc R . . C22 C -0.0098(4) 0.7072(6) 0.3874(3) 0.0336(14) Uani 1 1 d . . . H22A H -0.0710 0.6923 0.3880 0.050 Uiso 1 1 calc R . . H22B H 0.0047 0.7863 0.4098 0.050 Uiso 1 1 calc R . . H22C H 0.0203 0.6333 0.4057 0.050 Uiso 1 1 calc R . . C23 C 0.1510(4) 0.7586(5) 0.2340(2) 0.0255(12) Uani 1 1 d . . . H23A H 0.0972 0.7840 0.2130 0.031 Uiso 1 1 calc R . . H23B H 0.1928 0.8281 0.2274 0.031 Uiso 1 1 calc R . . C24 C 0.1832(4) 0.6313(6) 0.2057(3) 0.0335(13) Uani 1 1 d . . . H24A H 0.1926 0.6457 0.1633 0.050 Uiso 1 1 calc R . . H24B H 0.1409 0.5628 0.2098 0.050 Uiso 1 1 calc R . . H24C H 0.2366 0.6049 0.2260 0.050 Uiso 1 1 calc R . . C25 C 0.1465(3) 0.9207(5) 0.3412(2) 0.0229(11) Uani 1 1 d . . . H25A H 0.1303 0.9269 0.3833 0.027 Uiso 1 1 calc R . . H25B H 0.2073 0.9438 0.3399 0.027 Uiso 1 1 calc R . . C26 C 0.0940(4) 1.0220(6) 0.3037(3) 0.0337(14) Uani 1 1 d . . . H26A H 0.1053 1.1091 0.3196 0.051 Uiso 1 1 calc R . . H26B H 0.0335 1.0025 0.3060 0.051 Uiso 1 1 calc R . . H26C H 0.1102 1.0181 0.2621 0.051 Uiso 1 1 calc R . . C01 C 0.2326(4) 0.2979(7) 0.1721(3) 0.0433(16) Uani 1 1 d . . . H01A H 0.2688 0.3679 0.1883 0.065 Uiso 1 1 calc R . . H01B H 0.1923 0.2720 0.2019 0.065 Uiso 1 1 calc R . . H01C H 0.2016 0.3283 0.1360 0.065 Uiso 1 1 calc R . . C02 C 0.2885(4) 0.1799(6) 0.1565(3) 0.0264(12) Uani 1 1 d . . . C03 C 0.2541(4) 0.0538(6) 0.1510(3) 0.0339(14) Uani 1 1 d . . . H03 H 0.1960 0.0402 0.1586 0.041 Uiso 1 1 calc R . . C04 C 0.3046(4) -0.0528(6) 0.1343(3) 0.0391(15) Uani 1 1 d . . . H04 H 0.2803 -0.1367 0.1306 0.047 Uiso 1 1 calc R . . C05 C 0.3907(4) -0.0341(6) 0.1234(3) 0.0370(14) Uani 1 1 d . . . H05 H 0.4248 -0.1045 0.1115 0.044 Uiso 1 1 calc R . . C06 C 0.4256(4) 0.0908(6) 0.1305(3) 0.0396(15) Uani 1 1 d . . . H06 H 0.4841 0.1040 0.1242 0.048 Uiso 1 1 calc R . . C07 C 0.3755(4) 0.1954(6) 0.1465(3) 0.0334(14) Uani 1 1 d . . . H07 H 0.4005 0.2788 0.1509 0.040 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 Cl1 0.0273(6) 0.0170(6) 0.0382(7) -0.0008(6) -0.0078(5) -0.0051(6) As1 0.0158(2) 0.0113(2) 0.0226(2) 0.0004(2) -0.00186(19) 0.00067(19) Pt1 0.01571(9) 0.00979(9) 0.01962(9) 0.00014(8) -0.00120(6) 0.00042(8) P1 0.0217(6) 0.0094(5) 0.0234(6) 0.0007(5) 0.0003(5) 0.0024(5) P2 0.0176(6) 0.0138(6) 0.0204(6) 0.0011(5) -0.0024(5) 0.0020(5) O1 0.024(2) 0.0141(17) 0.036(2) -0.0027(16) 0.0010(16) -0.0033(15) O2 0.036(2) 0.054(3) 0.022(2) 0.000(2) -0.0028(17) -0.013(2) C1 0.023(3) 0.012(2) 0.025(3) -0.003(2) -0.006(2) 0.002(2) C2 0.017(2) 0.019(2) 0.019(2) -0.002(2) -0.0048(19) 0.001(2) C3 0.033(3) 0.016(3) 0.031(3) -0.005(2) 0.007(2) 0.002(2) C4 0.040(4) 0.029(3) 0.034(3) 0.002(3) 0.007(3) -0.006(3) C5 0.024(3) 0.050(4) 0.027(3) 0.002(3) 0.008(2) 0.000(3) C6 0.034(3) 0.036(3) 0.035(3) -0.001(3) 0.009(3) 0.014(3) C7 0.044(3) 0.019(3) 0.031(3) 0.001(2) 0.008(3) 0.006(3) C8 0.016(2) 0.024(3) 0.021(3) 0.001(2) 0.001(2) 0.002(2) C9 0.019(2) 0.018(2) 0.030(3) 0.001(2) 0.008(2) 0.002(2) C10 0.036(3) 0.024(3) 0.042(3) 0.010(3) 0.012(3) 0.003(3) C11 0.040(3) 0.025(3) 0.055(4) 0.009(3) 0.023(3) 0.000(3) C12 0.027(3) 0.021(3) 0.074(5) -0.009(3) 0.014(3) -0.007(3) C13 0.024(3) 0.028(3) 0.052(4) -0.013(3) 0.004(3) -0.003(3) C14 0.018(2) 0.022(3) 0.035(3) -0.003(2) 0.005(2) 0.003(2) C15 0.029(3) 0.019(3) 0.032(3) 0.000(2) -0.004(2) 0.006(2) C16 0.050(4) 0.024(3) 0.052(4) 0.007(3) -0.023(3) 0.009(3) C17 0.031(3) 0.014(2) 0.028(3) 0.007(2) 0.007(2) 0.005(2) C18 0.048(4) 0.030(3) 0.037(3) 0.003(3) 0.016(3) -0.013(3) C19 0.030(3) 0.014(2) 0.031(3) -0.001(2) 0.003(2) 0.003(2) C20 0.040(4) 0.040(4) 0.035(3) -0.002(3) 0.010(3) 0.006(3) C21 0.019(3) 0.024(3) 0.034(3) 0.000(2) -0.009(2) 0.002(2) C22 0.024(3) 0.040(3) 0.037(3) 0.001(3) 0.003(2) -0.001(3) C23 0.030(3) 0.024(3) 0.023(3) 0.002(2) -0.001(2) 0.006(2) C24 0.043(4) 0.033(3) 0.024(3) -0.004(3) 0.000(3) 0.005(3) C25 0.026(3) 0.014(2) 0.028(3) 0.000(2) -0.002(2) 0.002(2) C26 0.041(4) 0.024(3) 0.036(3) 0.004(3) -0.011(3) 0.011(3) C01 0.035(4) 0.035(4) 0.059(4) -0.014(3) -0.007(3) 0.005(3) C02 0.027(3) 0.025(3) 0.027(3) 0.003(2) -0.003(2) 0.000(2) C03 0.024(3) 0.034(3) 0.044(3) 0.006(3) -0.001(3) -0.007(3) C04 0.039(4) 0.025(3) 0.052(4) 0.010(3) -0.005(3) 0.000(3) C05 0.041(4) 0.028(3) 0.041(4) -0.002(3) -0.002(3) 0.003(3) C06 0.028(3) 0.038(4) 0.054(4) 0.002(3) 0.014(3) -0.003(3) C07 0.031(3) 0.031(3) 0.039(3) 0.000(3) 0.006(3) -0.011(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 Cl1 Pt1 2.3989(13) . ? As1 C1 2.006(5) . ? As1 C8 2.012(5) . ? As1 Pt1 2.4032(6) . ? Pt1 P1 2.3212(13) . ? Pt1 P2 2.3228(13) . ? P1 C17 1.818(5) . ? P1 C19 1.819(5) . ? P1 C15 1.826(6) . ? P2 C21 1.824(5) . ? P2 C23 1.836(5) . ? P2 C25 1.840(5) . ? O1 C1 1.220(6) . ? O2 C8 1.210(6) . ? C1 C2 1.494(7) . ? C2 C3 1.390(7) . ? C2 C7 1.389(7) . ? C3 C4 1.377(8) . ? C4 C5 1.377(9) . ? C5 C6 1.375(9) . ? C6 C7 1.374(8) . ? C8 C9 1.492(7) . ? C9 C14 1.384(8) . ? C9 C10 1.396(8) . ? C10 C11 1.377(9) . ? C11 C12 1.373(10) . ? C12 C13 1.379(9) . ? C13 C14 1.378(8) . ? C15 C16 1.522(7) . ? C17 C18 1.523(8) . ? C19 C20 1.515(8) . ? C21 C22 1.531(8) . ? C23 C24 1.522(8) . ? C25 C26 1.527(7) . ? C01 C02 1.520(8) . ? C02 C07 1.381(8) . ? C02 C03 1.385(8) . ? C03 C04 1.388(9) . ? C04 C05 1.376(9) . ? C05 C06 1.379(9) . ? C06 C07 1.366(9) . ? 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 C8 99.9(2) . . ? C1 As1 Pt1 110.08(15) . . ? C8 As1 Pt1 104.09(15) . . ? P1 Pt1 P2 172.20(5) . . ? P1 Pt1 Cl1 84.59(5) . . ? P2 Pt1 Cl1 88.84(5) . . ? P1 Pt1 As1 90.78(4) . . ? P2 Pt1 As1 95.75(4) . . ? Cl1 Pt1 As1 175.36(3) . . ? C17 P1 C19 102.9(2) . . ? C17 P1 C15 104.3(3) . . ? C19 P1 C15 104.8(3) . . ? C17 P1 Pt1 114.76(18) . . ? C19 P1 Pt1 109.91(18) . . ? C15 P1 Pt1 118.56(18) . . ? C21 P2 C23 105.2(3) . . ? C21 P2 C25 102.3(3) . . ? C23 P2 C25 102.8(3) . . ? C21 P2 Pt1 109.68(18) . . ? C23 P2 Pt1 113.77(18) . . ? C25 P2 Pt1 121.42(17) . . ? O1 C1 C2 120.9(5) . . ? O1 C1 As1 120.0(4) . . ? C2 C1 As1 119.0(3) . . ? C3 C2 C7 118.5(5) . . ? C3 C2 C1 122.5(5) . . ? C7 C2 C1 119.0(5) . . ? C4 C3 C2 120.2(5) . . ? C3 C4 C5 121.3(6) . . ? C6 C5 C4 118.3(5) . . ? C5 C6 C7 121.4(5) . . ? C6 C7 C2 120.2(5) . . ? O2 C8 C9 120.0(5) . . ? O2 C8 As1 118.8(4) . . ? C9 C8 As1 120.6(4) . . ? C14 C9 C10 117.3(5) . . ? C14 C9 C8 122.6(5) . . ? C10 C9 C8 119.9(5) . . ? C11 C10 C9 121.3(6) . . ? C12 C11 C10 119.6(6) . . ? C11 C12 C13 120.6(6) . . ? C14 C13 C12 119.0(6) . . ? C13 C14 C9 122.1(6) . . ? C16 C15 P1 115.6(4) . . ? C18 C17 P1 113.8(4) . . ? C20 C19 P1 113.7(4) . . ? C22 C21 P2 112.4(4) . . ? C24 C23 P2 114.7(4) . . ? C26 C25 P2 114.9(4) . . ? C07 C02 C03 117.7(5) . . ? C07 C02 C01 120.9(5) . . ? C03 C02 C01 121.4(5) . . ? C02 C03 C04 121.2(5) . . ? C05 C04 C03 120.0(6) . . ? C04 C05 C06 118.9(6) . . ? C07 C06 C05 120.9(6) . . ? C06 C07 C02 121.3(6) . . ? 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 Pt1 P1 -129.51(16) . . . . ? C8 As1 Pt1 P1 124.23(15) . . . . ? C1 As1 Pt1 P2 54.76(16) . . . . ? C8 As1 Pt1 P2 -51.50(15) . . . . ? C1 As1 Pt1 Cl1 -133.9(5) . . . . ? C8 As1 Pt1 Cl1 119.8(5) . . . . ? P2 Pt1 P1 C17 -80.8(4) . . . . ? Cl1 Pt1 P1 C17 -48.0(2) . . . . ? As1 Pt1 P1 C17 132.4(2) . . . . ? P2 Pt1 P1 C19 34.6(4) . . . . ? Cl1 Pt1 P1 C19 67.4(2) . . . . ? As1 Pt1 P1 C19 -112.3(2) . . . . ? P2 Pt1 P1 C15 155.1(4) . . . . ? Cl1 Pt1 P1 C15 -172.1(2) . . . . ? As1 Pt1 P1 C15 8.2(2) . . . . ? P1 Pt1 P2 C21 74.0(4) . . . . ? Cl1 Pt1 P2 C21 41.4(2) . . . . ? As1 Pt1 P2 C21 -139.27(19) . . . . ? P1 Pt1 P2 C23 -43.5(4) . . . . ? Cl1 Pt1 P2 C23 -76.1(2) . . . . ? As1 Pt1 P2 C23 103.2(2) . . . . ? P1 Pt1 P2 C25 -167.0(4) . . . . ? Cl1 Pt1 P2 C25 160.4(2) . . . . ? As1 Pt1 P2 C25 -20.3(2) . . . . ? C8 As1 C1 O1 -32.3(5) . . . . ? Pt1 As1 C1 O1 -141.4(4) . . . . ? C8 As1 C1 C2 152.0(4) . . . . ? Pt1 As1 C1 C2 42.9(4) . . . . ? O1 C1 C2 C3 -160.4(5) . . . . ? As1 C1 C2 C3 15.3(7) . . . . ? O1 C1 C2 C7 21.6(7) . . . . ? As1 C1 C2 C7 -162.8(4) . . . . ? C7 C2 C3 C4 -2.4(8) . . . . ? C1 C2 C3 C4 179.5(5) . . . . ? C2 C3 C4 C5 2.6(9) . . . . ? C3 C4 C5 C6 -0.5(9) . . . . ? C4 C5 C6 C7 -1.7(10) . . . . ? C5 C6 C7 C2 1.9(10) . . . . ? C3 C2 C7 C6 0.2(8) . . . . ? C1 C2 C7 C6 178.4(5) . . . . ? C1 As1 C8 O2 -123.1(5) . . . . ? Pt1 As1 C8 O2 -9.3(5) . . . . ? C1 As1 C8 C9 66.0(4) . . . . ? Pt1 As1 C8 C9 179.7(4) . . . . ? O2 C8 C9 C14 -163.8(5) . . . . ? As1 C8 C9 C14 7.0(7) . . . . ? O2 C8 C9 C10 12.2(8) . . . . ? As1 C8 C9 C10 -177.0(4) . . . . ? C14 C9 C10 C11 1.9(8) . . . . ? C8 C9 C10 C11 -174.3(5) . . . . ? C9 C10 C11 C12 0.0(9) . . . . ? C10 C11 C12 C13 -1.2(9) . . . . ? C11 C12 C13 C14 0.3(9) . . . . ? C12 C13 C14 C9 1.7(8) . . . . ? C10 C9 C14 C13 -2.8(8) . . . . ? C8 C9 C14 C13 173.3(5) . . . . ? C17 P1 C15 C16 55.1(5) . . . . ? C19 P1 C15 C16 -52.7(5) . . . . ? Pt1 P1 C15 C16 -175.8(4) . . . . ? C19 P1 C17 C18 -178.3(4) . . . . ? C15 P1 C17 C18 72.4(5) . . . . ? Pt1 P1 C17 C18 -59.0(5) . . . . ? C17 P1 C19 C20 -176.7(4) . . . . ? C15 P1 C19 C20 -67.8(5) . . . . ? Pt1 P1 C19 C20 60.6(5) . . . . ? C23 P2 C21 C22 178.2(4) . . . . ? C25 P2 C21 C22 -74.7(4) . . . . ? Pt1 P2 C21 C22 55.4(4) . . . . ? C21 P2 C23 C24 -99.1(5) . . . . ? C25 P2 C23 C24 154.1(4) . . . . ? Pt1 P2 C23 C24 21.0(5) . . . . ? C21 P2 C25 C26 -58.4(5) . . . . ? C23 P2 C25 C26 50.6(5) . . . . ? Pt1 P2 C25 C26 179.1(3) . . . . ? C07 C02 C03 C04 -1.8(9) . . . . ? C01 C02 C03 C04 177.5(6) . . . . ? C02 C03 C04 C05 0.5(10) . . . . ? C03 C04 C05 C06 1.3(10) . . . . ? C04 C05 C06 C07 -1.6(10) . . . . ? C05 C06 C07 C02 0.2(10) . . . . ? C03 C02 C07 C06 1.5(9) . . . . ? C01 C02 C07 C06 -177.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.085 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.143 data_compound 22 _database_code_CSD 165264 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 As2 Cl2 Li2 O8 Zn' _chemical_formula_weight 820.72 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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 10.166(4) _cell_length_b 11.290(5) _cell_length_c 20.312(5) _cell_angle_alpha 75.56(3) _cell_angle_beta 81.93(3) _cell_angle_gamma 62.24(4) _cell_volume 1997.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 2.431 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type cad4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7621 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.17 _reflns_number_total 7185 _reflns_number_gt 6114 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1051P)^2^+1.4139P] 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 7185 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.24435(5) -0.12944(4) 0.25418(2) 0.02080(14) Uani 1 1 d . . . As1 As 0.09635(4) -0.25218(4) 0.250461(18) 0.02088(13) Uani 1 1 d . . . As2 As 0.09126(4) 0.11340(4) 0.269459(19) 0.02207(13) Uani 1 1 d . . . Cl1 Cl 0.41204(11) -0.25299(9) 0.33947(5) 0.0314(2) Uani 1 1 d . . . Cl2 Cl 0.38473(11) -0.12498(10) 0.15550(5) 0.0283(2) Uani 1 1 d . . . O1 O 0.3829(3) -0.4822(3) 0.25325(14) 0.0290(6) Uani 1 1 d . . . O2 O 0.2266(3) -0.4312(3) 0.37561(14) 0.0316(6) Uani 1 1 d . . . O3 O 0.3672(3) 0.1250(3) 0.23468(14) 0.0315(6) Uani 1 1 d . . . O4 O 0.1642(3) 0.2112(3) 0.13250(14) 0.0312(6) Uani 1 1 d . . . O5 O 0.4782(4) 0.6152(3) 0.57000(17) 0.0489(9) Uani 1 1 d . . . O6 O 0.3360(3) 0.5670(3) 0.68396(17) 0.0415(7) Uani 1 1 d . . . O7 O 0.6087(3) 0.0244(3) 0.13792(16) 0.0389(7) Uani 1 1 d . . . O8 O 0.4185(4) 0.1756(3) 0.03933(15) 0.0412(7) Uani 1 1 d . . . Li1 Li 0.4356(8) -0.4821(7) 0.3420(3) 0.0326(15) Uani 1 1 d . . . Li2 Li 0.3818(8) 0.1026(7) 0.1402(3) 0.0306(15) Uani 1 1 d . . . C1 C 0.2741(4) -0.4041(4) 0.21892(19) 0.0233(8) Uani 1 1 d . . . C2 C 0.2662(5) -0.4267(4) 0.1486(2) 0.0330(9) Uani 1 1 d . . . C3 C 0.1806(9) -0.5096(6) 0.1578(3) 0.072(2) Uani 1 1 d . . . H3A H 0.0943 -0.4727 0.1865 0.108 Uiso 1 1 calc R . . H3B H 0.2429 -0.6031 0.1783 0.108 Uiso 1 1 calc R . . H3C H 0.1502 -0.5056 0.1142 0.108 Uiso 1 1 calc R . . C4 C 0.4233(7) -0.5009(8) 0.1197(3) 0.090(3) Uani 1 1 d . . . H4A H 0.4707 -0.5928 0.1458 0.136 Uiso 1 1 calc R . . H4B H 0.4797 -0.4535 0.1221 0.136 Uiso 1 1 calc R . . H4C H 0.4185 -0.5028 0.0732 0.136 Uiso 1 1 calc R . . C5 C 0.1842(6) -0.2928(5) 0.0982(2) 0.0424(11) Uani 1 1 d . . . H5A H 0.1865 -0.3117 0.0544 0.064 Uiso 1 1 calc R . . H5B H 0.2315 -0.2351 0.0948 0.064 Uiso 1 1 calc R . . H5C H 0.0828 -0.2473 0.1137 0.064 Uiso 1 1 calc R . . C6 C 0.1154(4) -0.3327(4) 0.34933(19) 0.0246(8) Uani 1 1 d . . . C7 C -0.0237(5) -0.2714(4) 0.3939(2) 0.0319(9) Uani 1 1 d . . . C8 C -0.0998(6) -0.1158(5) 0.3733(3) 0.0486(13) Uani 1 1 d . . . H8A H -0.1258 -0.0884 0.3264 0.073 Uiso 1 1 calc R . . H8B H -0.0334 -0.0810 0.3796 0.073 Uiso 1 1 calc R . . H8C H -0.1882 -0.0799 0.4011 0.073 Uiso 1 1 calc R . . C9 C -0.1300(6) -0.3241(6) 0.3814(3) 0.0539(14) Uani 1 1 d . . . H9A H -0.0784 -0.4218 0.3869 0.081 Uiso 1 1 calc R . . H9B H -0.1660 -0.2835 0.3360 0.081 Uiso 1 1 calc R . . H9C H -0.2124 -0.2999 0.4134 0.081 Uiso 1 1 calc R . . C10 C 0.0154(6) -0.3183(6) 0.4683(2) 0.0554(14) Uani 1 1 d . . . H10A H -0.0734 -0.2822 0.4958 0.083 Uiso 1 1 calc R . . H10B H 0.0829 -0.2859 0.4760 0.083 Uiso 1 1 calc R . . H10C H 0.0615 -0.4165 0.4804 0.083 Uiso 1 1 calc R . . C11 C 0.2785(4) 0.1197(4) 0.28056(19) 0.0242(8) Uani 1 1 d . . . C12 C 0.3052(5) 0.1276(4) 0.3518(2) 0.0307(9) Uani 1 1 d . . . C13 C 0.2355(6) 0.2820(5) 0.3514(2) 0.0419(11) Uani 1 1 d . . . H13A H 0.2851 0.3240 0.3172 0.063 Uiso 1 1 calc R . . H13B H 0.2463 0.2942 0.3951 0.063 Uiso 1 1 calc R . . H13C H 0.1318 0.3239 0.3416 0.063 Uiso 1 1 calc R . . C14 C 0.4715(6) 0.0583(6) 0.3637(3) 0.0551(14) Uani 1 1 d . . . H14A H 0.4878 0.0544 0.4098 0.083 Uiso 1 1 calc R . . H14B H 0.5167 0.1096 0.3331 0.083 Uiso 1 1 calc R . . H14C H 0.5149 -0.0329 0.3556 0.083 Uiso 1 1 calc R . . C15 C 0.2310(6) 0.0590(5) 0.4094(2) 0.0410(11) Uani 1 1 d . . . H15A H 0.2554 0.0626 0.4526 0.062 Uiso 1 1 calc R . . H15B H 0.2663 -0.0347 0.4067 0.062 Uiso 1 1 calc R . . H15C H 0.1251 0.1065 0.4047 0.062 Uiso 1 1 calc R . . C16 C 0.0730(4) 0.1830(4) 0.1704(2) 0.0257(8) Uani 1 1 d . . . C17 C -0.0669(5) 0.2064(4) 0.1373(2) 0.0321(9) Uani 1 1 d . . . C18 C -0.1791(5) 0.1793(5) 0.1883(3) 0.0431(11) Uani 1 1 d . . . H18A H -0.1351 0.0850 0.2116 0.065 Uiso 1 1 calc R . . H18B H -0.2650 0.1988 0.1649 0.065 Uiso 1 1 calc R . . H18C H -0.2082 0.2369 0.2207 0.065 Uiso 1 1 calc R . . C19 C -0.1397(5) 0.3536(4) 0.0967(2) 0.0392(10) Uani 1 1 d . . . H19A H -0.0696 0.3694 0.0633 0.059 Uiso 1 1 calc R . . H19B H -0.1705 0.4157 0.1268 0.059 Uiso 1 1 calc R . . H19C H -0.2248 0.3682 0.0743 0.059 Uiso 1 1 calc R . . C20 C -0.0110(6) 0.1079(5) 0.0882(3) 0.0468(12) Uani 1 1 d . . . H20A H 0.0346 0.0152 0.1135 0.070 Uiso 1 1 calc R . . H20B H 0.0605 0.1252 0.0564 0.070 Uiso 1 1 calc R . . H20C H -0.0934 0.1218 0.0640 0.070 Uiso 1 1 calc R . . C21 C 0.5511(7) 0.6661(6) 0.5141(2) 0.0534(14) Uani 1 1 d . . . H21A H 0.6566 0.6103 0.5172 0.080 Uiso 1 1 calc R . . H21B H 0.5276 0.7587 0.5146 0.080 Uiso 1 1 calc R . . H21C H 0.5185 0.6638 0.4725 0.080 Uiso 1 1 calc R . . C22 C 0.3236(6) 0.7017(6) 0.5741(3) 0.0593(15) Uani 1 1 d . . . H22A H 0.2804 0.7315 0.5297 0.071 Uiso 1 1 calc R . . H22B H 0.3054 0.7819 0.5904 0.071 Uiso 1 1 calc R . . C23 C 0.2571(6) 0.6189(6) 0.6229(3) 0.0520(13) Uani 1 1 d . . . H23A H 0.1526 0.6758 0.6315 0.062 Uiso 1 1 calc R . . H23B H 0.2661 0.5442 0.6042 0.062 Uiso 1 1 calc R . . C24 C 0.2818(6) 0.4905(6) 0.7343(3) 0.0544(13) Uani 1 1 d . . . H24A H 0.3412 0.4548 0.7739 0.082 Uiso 1 1 calc R . . H24B H 0.2862 0.4160 0.7178 0.082 Uiso 1 1 calc R . . H24C H 0.1806 0.5478 0.7459 0.082 Uiso 1 1 calc R . . C25 C 0.6915(6) -0.0939(6) 0.1878(3) 0.0573(15) Uani 1 1 d . . . H25A H 0.6494 -0.0798 0.2323 0.086 Uiso 1 1 calc R . . H25B H 0.7930 -0.1093 0.1856 0.086 Uiso 1 1 calc R . . H25C H 0.6877 -0.1720 0.1793 0.086 Uiso 1 1 calc R . . C26 C 0.6595(6) 0.0101(6) 0.0702(3) 0.0467(12) Uani 1 1 d . . . H26A H 0.6453 -0.0621 0.0593 0.056 Uiso 1 1 calc R . . H26B H 0.7644 -0.0130 0.0649 0.056 Uiso 1 1 calc R . . C27 C 0.5717(6) 0.1424(6) 0.0249(2) 0.0488(13) Uani 1 1 d . . . H27A H 0.5926 0.2130 0.0332 0.059 Uiso 1 1 calc R . . H27B H 0.5966 0.1355 -0.0223 0.059 Uiso 1 1 calc R . . C28 C 0.3245(7) 0.2968(5) -0.0048(2) 0.0503(13) Uani 1 1 d . . . H28A H 0.2235 0.3105 0.0033 0.076 Uiso 1 1 calc R . . H28B H 0.3539 0.2888 -0.0511 0.076 Uiso 1 1 calc R . . H28C H 0.3322 0.3733 0.0036 0.076 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 Zn1 0.0250(2) 0.0155(2) 0.0202(2) -0.00069(17) -0.00541(17) -0.00788(18) As1 0.0228(2) 0.0182(2) 0.0200(2) -0.00072(15) -0.00525(14) -0.00818(16) As2 0.0245(2) 0.0158(2) 0.0230(2) -0.00239(15) -0.00443(15) -0.00655(16) Cl1 0.0375(5) 0.0201(5) 0.0334(5) -0.0030(4) -0.0192(4) -0.0067(4) Cl2 0.0334(5) 0.0278(5) 0.0259(5) -0.0077(4) 0.0039(4) -0.0159(4) O1 0.0291(14) 0.0243(14) 0.0296(15) -0.0053(12) -0.0062(12) -0.0072(12) O2 0.0328(15) 0.0286(15) 0.0249(14) 0.0025(12) -0.0035(12) -0.0099(13) O3 0.0327(15) 0.0328(16) 0.0282(15) -0.0058(12) -0.0055(12) -0.0132(13) O4 0.0377(16) 0.0276(15) 0.0269(15) 0.0059(12) -0.0082(12) -0.0173(13) O5 0.0428(19) 0.0435(19) 0.045(2) 0.0110(16) -0.0185(15) -0.0124(16) O6 0.0337(16) 0.0356(17) 0.0491(19) -0.0117(15) -0.0115(14) -0.0065(14) O7 0.0327(16) 0.0487(19) 0.0384(17) -0.0113(15) 0.0007(13) -0.0202(15) O8 0.056(2) 0.0410(18) 0.0303(16) -0.0012(14) -0.0006(14) -0.0283(16) Li1 0.033(4) 0.028(4) 0.029(4) 0.002(3) -0.012(3) -0.008(3) Li2 0.033(4) 0.033(4) 0.020(3) -0.001(3) -0.004(3) -0.012(3) C1 0.030(2) 0.0178(18) 0.0232(19) -0.0059(15) -0.0030(15) -0.0104(16) C2 0.044(2) 0.031(2) 0.024(2) -0.0112(17) -0.0087(17) -0.0124(19) C3 0.152(7) 0.057(4) 0.044(3) -0.001(3) -0.028(4) -0.075(4) C4 0.065(4) 0.113(6) 0.055(4) -0.059(4) -0.012(3) 0.015(4) C5 0.067(3) 0.044(3) 0.024(2) -0.0042(19) -0.006(2) -0.031(3) C6 0.030(2) 0.0238(19) 0.0223(19) 0.0001(15) -0.0060(15) -0.0148(17) C7 0.032(2) 0.031(2) 0.029(2) -0.0037(17) 0.0032(17) -0.0138(18) C8 0.052(3) 0.031(2) 0.049(3) -0.011(2) 0.021(2) -0.013(2) C9 0.043(3) 0.067(4) 0.058(3) -0.009(3) 0.008(2) -0.034(3) C10 0.050(3) 0.071(4) 0.030(3) -0.007(2) 0.006(2) -0.019(3) C11 0.030(2) 0.0173(18) 0.026(2) -0.0052(15) -0.0068(16) -0.0099(16) C12 0.041(2) 0.024(2) 0.027(2) -0.0101(16) -0.0082(17) -0.0097(18) C13 0.066(3) 0.032(2) 0.039(3) -0.014(2) -0.009(2) -0.025(2) C14 0.049(3) 0.075(4) 0.044(3) -0.024(3) -0.016(2) -0.020(3) C15 0.067(3) 0.029(2) 0.023(2) -0.0058(18) -0.007(2) -0.016(2) C16 0.032(2) 0.0136(17) 0.0264(19) 0.0008(15) -0.0102(16) -0.0056(16) C17 0.033(2) 0.0202(19) 0.042(2) 0.0016(17) -0.0180(18) -0.0101(17) C18 0.037(2) 0.042(3) 0.050(3) 0.005(2) -0.017(2) -0.020(2) C19 0.039(2) 0.024(2) 0.041(3) 0.0048(19) -0.016(2) -0.0049(19) C20 0.044(3) 0.035(3) 0.061(3) -0.014(2) -0.026(2) -0.009(2) C21 0.069(4) 0.054(3) 0.033(3) 0.016(2) -0.020(2) -0.031(3) C22 0.046(3) 0.044(3) 0.071(4) 0.007(3) -0.032(3) -0.008(2) C23 0.036(3) 0.051(3) 0.061(3) -0.007(3) -0.018(2) -0.011(2) C24 0.044(3) 0.056(3) 0.061(3) -0.024(3) 0.007(2) -0.017(3) C25 0.034(3) 0.064(4) 0.063(3) 0.004(3) -0.022(2) -0.015(3) C26 0.045(3) 0.061(3) 0.050(3) -0.031(3) 0.013(2) -0.032(3) C27 0.069(3) 0.068(3) 0.033(2) -0.021(2) 0.018(2) -0.051(3) C28 0.086(4) 0.037(3) 0.026(2) 0.004(2) -0.008(2) -0.030(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 Zn1 Cl1 2.2939(15) . ? Zn1 Cl2 2.2957(13) . ? Zn1 As1 2.4933(10) . ? Zn1 As2 2.5198(15) . ? As1 C6 1.983(4) . ? As1 C1 1.988(4) . ? As2 C16 1.970(4) . ? As2 C11 1.984(4) . ? Cl1 Li1 2.471(7) . ? Cl2 Li2 2.497(7) . ? O1 C1 1.220(5) . ? O1 Li1 1.952(7) . ? O2 C6 1.225(5) . ? O2 Li1 1.990(8) . ? O3 C11 1.213(5) . ? O3 Li2 1.975(7) . ? O4 C16 1.227(5) . ? O4 Li2 1.975(8) . ? O5 C22 1.416(6) . ? O5 C21 1.416(6) . ? O5 Li1 2.023(7) 2_656 ? O6 C24 1.393(6) . ? O6 C23 1.415(6) . ? O6 Li1 2.103(8) 2_656 ? O7 C26 1.420(6) . ? O7 C25 1.427(6) . ? O7 Li2 2.048(8) . ? O8 C28 1.414(6) . ? O8 C27 1.426(6) . ? O8 Li2 2.060(7) . ? Li1 O5 2.023(7) 2_656 ? Li1 O6 2.103(8) 2_656 ? C1 C2 1.532(5) . ? C2 C3 1.515(7) . ? C2 C5 1.523(6) . ? C2 C4 1.527(7) . ? C6 C7 1.530(6) . ? C7 C10 1.516(6) . ? C7 C8 1.523(6) . ? C7 C9 1.528(7) . ? C11 C12 1.541(5) . ? C12 C14 1.522(6) . ? C12 C15 1.543(6) . ? C12 C13 1.544(6) . ? C16 C17 1.540(5) . ? C17 C18 1.518(6) . ? C17 C19 1.527(5) . ? C17 C20 1.537(6) . ? C22 C23 1.501(8) . ? C26 C27 1.476(8) . ? 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 Cl1 Zn1 Cl2 105.54(5) . . ? Cl1 Zn1 As1 108.78(4) . . ? Cl2 Zn1 As1 109.62(4) . . ? Cl1 Zn1 As2 110.03(5) . . ? Cl2 Zn1 As2 107.98(5) . . ? As1 Zn1 As2 114.51(4) . . ? C6 As1 C1 97.57(16) . . ? C6 As1 Zn1 92.61(11) . . ? C1 As1 Zn1 91.27(11) . . ? C16 As2 C11 98.76(16) . . ? C16 As2 Zn1 91.50(12) . . ? C11 As2 Zn1 88.56(11) . . ? Zn1 Cl1 Li1 98.45(16) . . ? Zn1 Cl2 Li2 100.83(16) . . ? C1 O1 Li1 131.1(3) . . ? C6 O2 Li1 126.1(3) . . ? C11 O3 Li2 131.1(3) . . ? C16 O4 Li2 124.4(3) . . ? C22 O5 C21 113.1(4) . . ? C22 O5 Li1 114.3(4) . 2_656 ? C21 O5 Li1 128.9(4) . 2_656 ? C24 O6 C23 112.8(4) . . ? C24 O6 Li1 119.4(3) . 2_656 ? C23 O6 Li1 107.6(4) . 2_656 ? C26 O7 C25 113.3(4) . . ? C26 O7 Li2 107.3(3) . . ? C25 O7 Li2 118.8(3) . . ? C28 O8 C27 111.9(4) . . ? C28 O8 Li2 128.7(4) . . ? C27 O8 Li2 111.4(3) . . ? O1 Li1 O2 90.1(3) . . ? O1 Li1 O5 139.3(4) . 2_656 ? O2 Li1 O5 93.3(3) . 2_656 ? O1 Li1 O6 92.4(3) . 2_656 ? O2 Li1 O6 170.9(4) . 2_656 ? O5 Li1 O6 79.1(3) 2_656 2_656 ? O1 Li1 Cl1 108.4(3) . . ? O2 Li1 Cl1 92.8(3) . . ? O5 Li1 Cl1 111.9(3) 2_656 . ? O6 Li1 Cl1 94.8(3) 2_656 . ? O4 Li2 O3 90.3(3) . . ? O4 Li2 O7 168.9(4) . . ? O3 Li2 O7 91.8(3) . . ? O4 Li2 O8 92.3(3) . . ? O3 Li2 O8 146.3(4) . . ? O7 Li2 O8 80.0(3) . . ? O4 Li2 Cl2 95.8(3) . . ? O3 Li2 Cl2 102.7(3) . . ? O7 Li2 Cl2 94.4(3) . . ? O8 Li2 Cl2 110.4(3) . . ? O1 C1 C2 119.4(3) . . ? O1 C1 As1 124.1(3) . . ? C2 C1 As1 116.4(3) . . ? C3 C2 C5 108.1(4) . . ? C3 C2 C4 111.9(5) . . ? C5 C2 C4 108.0(5) . . ? C3 C2 C1 106.9(4) . . ? C5 C2 C1 112.4(3) . . ? C4 C2 C1 109.6(4) . . ? O2 C6 C7 119.0(3) . . ? O2 C6 As1 124.6(3) . . ? C7 C6 As1 116.3(3) . . ? C10 C7 C8 110.9(4) . . ? C10 C7 C9 109.6(4) . . ? C8 C7 C9 108.3(4) . . ? C10 C7 C6 110.4(4) . . ? C8 C7 C6 111.0(3) . . ? C9 C7 C6 106.6(4) . . ? O3 C11 C12 119.0(3) . . ? O3 C11 As2 124.4(3) . . ? C12 C11 As2 116.5(3) . . ? C14 C12 C11 109.5(4) . . ? C14 C12 C15 108.5(4) . . ? C11 C12 C15 113.0(3) . . ? C14 C12 C13 111.3(4) . . ? C11 C12 C13 105.3(3) . . ? C15 C12 C13 109.3(4) . . ? O4 C16 C17 116.8(3) . . ? O4 C16 As2 125.0(3) . . ? C17 C16 As2 118.2(3) . . ? C18 C17 C19 109.7(4) . . ? C18 C17 C20 110.0(4) . . ? C19 C17 C20 109.1(4) . . ? C18 C17 C16 113.4(4) . . ? C19 C17 C16 108.8(3) . . ? C20 C17 C16 105.7(3) . . ? O5 C22 C23 106.5(4) . . ? O6 C23 C22 107.3(4) . . ? O7 C26 C27 107.2(4) . . ? O8 C27 C26 107.4(4) . . ? 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 Cl1 Zn1 As1 C6 29.79(12) . . . . ? Cl2 Zn1 As1 C6 144.73(12) . . . . ? As2 Zn1 As1 C6 -93.76(12) . . . . ? Cl1 Zn1 As1 C1 -67.84(12) . . . . ? Cl2 Zn1 As1 C1 47.10(12) . . . . ? As2 Zn1 As1 C1 168.61(11) . . . . ? Cl1 Zn1 As2 C16 148.04(12) . . . . ? Cl2 Zn1 As2 C16 33.33(12) . . . . ? As1 Zn1 As2 C16 -89.08(12) . . . . ? Cl1 Zn1 As2 C11 49.31(12) . . . . ? Cl2 Zn1 As2 C11 -65.41(12) . . . . ? As1 Zn1 As2 C11 172.19(11) . . . . ? Cl2 Zn1 Cl1 Li1 -91.56(18) . . . . ? As1 Zn1 Cl1 Li1 26.01(18) . . . . ? As2 Zn1 Cl1 Li1 152.19(17) . . . . ? Cl1 Zn1 Cl2 Li2 -97.32(17) . . . . ? As1 Zn1 Cl2 Li2 145.69(16) . . . . ? As2 Zn1 Cl2 Li2 20.33(16) . . . . ? C1 O1 Li1 O2 41.7(5) . . . . ? C1 O1 Li1 O5 136.9(6) . . . 2_656 ? C1 O1 Li1 O6 -147.1(4) . . . 2_656 ? C1 O1 Li1 Cl1 -51.3(5) . . . . ? C6 O2 Li1 O1 -54.7(5) . . . . ? C6 O2 Li1 O5 165.9(4) . . . 2_656 ? C6 O2 Li1 O6 -160(2) . . . 2_656 ? C6 O2 Li1 Cl1 53.8(4) . . . . ? Zn1 Cl1 Li1 O1 24.3(3) . . . . ? Zn1 Cl1 Li1 O2 -66.7(2) . . . . ? Zn1 Cl1 Li1 O5 -161.5(3) . . . 2_656 ? Zn1 Cl1 Li1 O6 118.4(2) . . . 2_656 ? C16 O4 Li2 O3 -57.1(5) . . . . ? C16 O4 Li2 O7 -158(2) . . . . ? C16 O4 Li2 O8 156.5(3) . . . . ? C16 O4 Li2 Cl2 45.7(4) . . . . ? C11 O3 Li2 O4 41.7(5) . . . . ? C11 O3 Li2 O7 -149.3(4) . . . . ? C11 O3 Li2 O8 136.2(6) . . . . ? C11 O3 Li2 Cl2 -54.4(5) . . . . ? C26 O7 Li2 O4 -72(2) . . . . ? C25 O7 Li2 O4 158(2) . . . . ? C26 O7 Li2 O3 -173.1(3) . . . . ? C25 O7 Li2 O3 56.9(5) . . . . ? C26 O7 Li2 O8 -25.9(4) . . . . ? C25 O7 Li2 O8 -156.0(4) . . . . ? C26 O7 Li2 Cl2 84.1(3) . . . . ? C25 O7 Li2 Cl2 -46.0(4) . . . . ? C28 O8 Li2 O4 22.0(5) . . . . ? C27 O8 Li2 O4 167.8(3) . . . . ? C28 O8 Li2 O3 -72.0(9) . . . . ? C27 O8 Li2 O3 73.9(8) . . . . ? C28 O8 Li2 O7 -149.9(4) . . . . ? C27 O8 Li2 O7 -4.1(4) . . . . ? C28 O8 Li2 Cl2 119.1(4) . . . . ? C27 O8 Li2 Cl2 -95.1(4) . . . . ? Zn1 Cl2 Li2 O4 -61.2(2) . . . . ? Zn1 Cl2 Li2 O3 30.4(3) . . . . ? Zn1 Cl2 Li2 O7 123.2(2) . . . . ? Zn1 Cl2 Li2 O8 -155.9(3) . . . . ? Li1 O1 C1 C2 177.2(4) . . . . ? Li1 O1 C1 As1 -6.7(6) . . . . ? C6 As1 C1 O1 -26.5(4) . . . . ? Zn1 As1 C1 O1 66.3(3) . . . . ? C6 As1 C1 C2 149.7(3) . . . . ? Zn1 As1 C1 C2 -117.5(3) . . . . ? O1 C1 C2 C3 94.7(5) . . . . ? As1 C1 C2 C3 -81.6(4) . . . . ? O1 C1 C2 C5 -146.8(4) . . . . ? As1 C1 C2 C5 36.8(5) . . . . ? O1 C1 C2 C4 -26.7(6) . . . . ? As1 C1 C2 C4 156.9(4) . . . . ? Li1 O2 C6 C7 -153.7(4) . . . . ? Li1 O2 C6 As1 30.7(5) . . . . ? C1 As1 C6 O2 13.5(4) . . . . ? Zn1 As1 C6 O2 -78.1(3) . . . . ? C1 As1 C6 C7 -162.2(3) . . . . ? Zn1 As1 C6 C7 106.2(3) . . . . ? O2 C6 C7 C10 17.2(6) . . . . ? As1 C6 C7 C10 -166.9(3) . . . . ? O2 C6 C7 C8 140.6(4) . . . . ? As1 C6 C7 C8 -43.5(5) . . . . ? O2 C6 C7 C9 -101.8(4) . . . . ? As1 C6 C7 C9 74.2(4) . . . . ? Li2 O3 C11 C12 174.0(4) . . . . ? Li2 O3 C11 As2 -10.2(6) . . . . ? C16 As2 C11 O3 -19.0(4) . . . . ? Zn1 As2 C11 O3 72.3(3) . . . . ? C16 As2 C11 C12 156.9(3) . . . . ? Zn1 As2 C11 C12 -111.8(3) . . . . ? O3 C11 C12 C14 -33.8(5) . . . . ? As2 C11 C12 C14 150.1(3) . . . . ? O3 C11 C12 C15 -154.9(4) . . . . ? As2 C11 C12 C15 29.0(4) . . . . ? O3 C11 C12 C13 85.9(5) . . . . ? As2 C11 C12 C13 -90.2(4) . . . . ? Li2 O4 C16 C17 -141.0(4) . . . . ? Li2 O4 C16 As2 39.9(5) . . . . ? C11 As2 C16 O4 3.2(4) . . . . ? Zn1 As2 C16 O4 -85.6(3) . . . . ? C11 As2 C16 C17 -175.9(3) . . . . ? Zn1 As2 C16 C17 95.4(3) . . . . ? O4 C16 C17 C18 -175.6(4) . . . . ? As2 C16 C17 C18 3.5(5) . . . . ? O4 C16 C17 C19 -53.3(5) . . . . ? As2 C16 C17 C19 125.8(3) . . . . ? O4 C16 C17 C20 63.7(5) . . . . ? As2 C16 C17 C20 -117.2(3) . . . . ? C21 O5 C22 C23 165.4(4) . . . . ? Li1 O5 C22 C23 -34.2(6) 2_656 . . . ? C24 O6 C23 C22 178.5(4) . . . . ? Li1 O6 C23 C22 -47.8(5) 2_656 . . . ? O5 C22 C23 O6 54.0(6) . . . . ? C25 O7 C26 C27 -175.9(4) . . . . ? Li2 O7 C26 C27 51.0(5) . . . . ? C28 O8 C27 C26 -176.0(4) . . . . ? Li2 O8 C27 C26 32.2(5) . . . . ? O7 C26 C27 O8 -55.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.930 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.133 data_compound 24 _database_code_CSD 165265 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 As2 O4' _chemical_formula_weight 570.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8988(10) _cell_length_b 10.9188(10) _cell_length_c 11.4628(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.876(2) _cell_angle_gamma 90.00 _cell_volume 1256.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cut plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.4125 _exptl_absorpt_correction_T_max 0.6884 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type cad4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5613 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1811 _reflns_number_gt 1534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0533P)^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 SHELXL _refine_ls_extinction_coef 0.0032(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1811 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.003 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 0.51385(3) 0.43978(3) 0.59319(3) 0.05634(18) Uani 1 1 d . . . O1 O 0.5177(3) 0.2601(2) 0.4157(3) 0.0918(8) Uani 1 1 d . . . O2 O 0.7643(2) 0.5042(2) 0.5960(2) 0.0729(6) Uani 1 1 d . . . C1 C 0.4676(3) 0.2807(3) 0.4900(3) 0.0604(7) Uani 1 1 d . . . C2 C 0.3724(3) 0.1953(3) 0.5105(3) 0.0597(7) Uani 1 1 d . . . C3 C 0.3119(4) 0.2214(4) 0.5929(4) 0.0819(10) Uani 1 1 d . . . C4 C 0.2210(5) 0.1368(6) 0.6067(5) 0.1052(16) Uani 1 1 d . . . C5 C 0.1937(5) 0.0320(5) 0.5405(6) 0.1026(16) Uani 1 1 d . . . C6 C 0.2541(5) 0.0044(4) 0.4608(5) 0.1030(14) Uani 1 1 d . . . C7 C 0.3434(4) 0.0854(3) 0.4447(4) 0.0831(11) Uani 1 1 d . . . C8 C 0.7106(3) 0.4250(3) 0.6335(3) 0.0530(7) Uani 1 1 d . . . C9 C 0.7868(3) 0.3229(3) 0.7149(3) 0.0533(7) Uani 1 1 d . . . C10 C 0.7302(4) 0.2451(3) 0.7730(3) 0.0708(9) Uani 1 1 d . . . C11 C 0.8054(5) 0.1532(5) 0.8515(4) 0.0968(14) Uani 1 1 d . . . C12 C 0.9362(5) 0.1392(5) 0.8688(4) 0.1004(14) Uani 1 1 d . . . C13 C 0.9936(4) 0.2165(4) 0.8113(4) 0.0884(11) Uani 1 1 d . . . C14 C 0.9196(3) 0.3080(4) 0.7335(3) 0.0692(9) Uani 1 1 d . . . H3 H 0.321(3) 0.297(3) 0.638(3) 0.085(11) Uiso 1 1 d . . . H4 H 0.190(5) 0.162(5) 0.656(4) 0.116(19) Uiso 1 1 d . . . H5 H 0.133(5) -0.020(5) 0.551(5) 0.131(17) Uiso 1 1 d . . . H6 H 0.247(6) -0.085(5) 0.416(6) 0.18(2) Uiso 1 1 d . . . H7 H 0.394(4) 0.070(3) 0.396(4) 0.093(14) Uiso 1 1 d . . . H10 H 0.639(3) 0.249(3) 0.760(3) 0.071(9) Uiso 1 1 d . . . H11 H 0.764(5) 0.101(4) 0.882(5) 0.125(17) Uiso 1 1 d . . . H12 H 0.983(5) 0.083(4) 0.932(5) 0.130(18) Uiso 1 1 d . . . H13 H 1.088(4) 0.212(4) 0.825(4) 0.112(13) Uiso 1 1 d . . . H14 H 0.962(3) 0.363(3) 0.697(3) 0.083(11) 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 As1 0.0443(2) 0.0575(2) 0.0654(3) -0.00112(14) 0.01927(17) 0.00655(12) O1 0.1013(19) 0.0882(18) 0.112(2) -0.0300(14) 0.0705(18) -0.0234(14) O2 0.0549(13) 0.0654(13) 0.0892(16) 0.0102(13) 0.0181(12) -0.0077(11) C1 0.0490(16) 0.0618(18) 0.0666(18) -0.0007(15) 0.0183(15) 0.0024(14) C2 0.0458(15) 0.0637(18) 0.0631(18) 0.0100(15) 0.0140(15) 0.0001(14) C3 0.078(2) 0.090(3) 0.081(2) 0.008(2) 0.035(2) -0.011(2) C4 0.104(3) 0.130(4) 0.098(3) 0.024(3) 0.056(3) -0.012(3) C5 0.078(3) 0.098(3) 0.114(4) 0.034(3) 0.018(3) -0.024(3) C6 0.095(3) 0.079(3) 0.125(4) 0.007(3) 0.031(3) -0.019(3) C7 0.076(3) 0.071(2) 0.097(3) -0.002(2) 0.029(2) -0.0098(19) C8 0.0441(16) 0.0540(17) 0.0576(17) -0.0049(13) 0.0160(14) -0.0026(13) C9 0.0461(15) 0.0596(17) 0.0499(15) -0.0009(14) 0.0139(13) 0.0065(13) C10 0.063(2) 0.083(2) 0.072(2) 0.0129(18) 0.0329(19) 0.0134(18) C11 0.107(3) 0.104(3) 0.090(3) 0.041(2) 0.050(3) 0.028(3) C12 0.102(3) 0.118(4) 0.079(3) 0.039(3) 0.033(2) 0.049(3) C13 0.060(2) 0.114(3) 0.084(2) 0.016(2) 0.021(2) 0.032(2) C14 0.0483(17) 0.086(2) 0.067(2) 0.0093(18) 0.0163(16) 0.0105(17) _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 C8 2.017(3) . ? As1 C1 2.051(3) . ? As1 As1 2.4254(6) 3_666 ? O1 C1 1.198(4) . ? O2 C8 1.212(3) . ? C1 C2 1.479(4) . ? C2 C3 1.376(5) . ? C2 C7 1.388(5) . ? C3 C4 1.408(6) . ? C4 C5 1.341(8) . ? C5 C6 1.351(7) . ? C6 C7 1.380(6) . ? C8 C9 1.483(4) . ? C9 C10 1.366(4) . ? C9 C14 1.388(4) . ? C10 C11 1.384(5) . ? C11 C12 1.369(6) . ? C12 C13 1.363(6) . ? C13 C14 1.373(5) . ? 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 C8 As1 C1 93.75(12) . . ? C8 As1 As1 90.13(9) . 3_666 ? C1 As1 As1 91.88(9) . 3_666 ? O1 C1 C2 122.4(3) . . ? O1 C1 As1 119.4(2) . . ? C2 C1 As1 118.2(2) . . ? C3 C2 C7 118.9(3) . . ? C3 C2 C1 122.1(3) . . ? C7 C2 C1 118.9(3) . . ? C2 C3 C4 119.2(5) . . ? C5 C4 C3 120.4(5) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C7 120.2(5) . . ? C2 C7 C6 120.3(5) . . ? O2 C8 C9 122.0(3) . . ? O2 C8 As1 118.6(2) . . ? C9 C8 As1 119.3(2) . . ? C10 C9 C14 119.6(3) . . ? C10 C9 C8 121.7(3) . . ? C14 C9 C8 118.7(3) . . ? C9 C10 C11 120.1(4) . . ? C12 C11 C10 119.7(4) . . ? C13 C12 C11 120.5(4) . . ? C12 C13 C14 120.0(4) . . ? C13 C14 C9 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.261 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.079