Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Synthesis, Structure and Reactivity of Cuboidal-type Cluster Aqua Complexes with W3PdS44+ Core ; _publ_contact_author_name 'Rita Hernandez-Molina' _publ_contact_author_email RRHERNAN@ULL.ES loop_ _publ_author_name R.Hernandez-Molina M.Clausen J.G.Platas I.Kalinina R.Llusar M.Sokolov C.Vicent # Attachment 'STR593M.CIF' data_[W3S4Pd(P(OH)3)(H2O)8Cl]CUC[6]12.5H2O _database_code_depnum_ccdc_archive 'CCDC 621859' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H80 Cl4 N24 O35.50 P Pd S4 W3' _chemical_formula_weight 2376.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 12.403(10) _cell_length_b 12.503(10) _cell_length_c 24.41(2) _cell_angle_alpha 99.730(19) _cell_angle_beta 90.22(2) _cell_angle_gamma 95.631(17) _cell_volume 3712(5) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2326 _exptl_absorpt_coefficient_mu 5.253 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.874550 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30113 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.1731 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 30.00 _reflns_number_total 20944 _reflns_number_gt 11083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20944 _refine_ls_number_parameters 925 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 W1 W 0.63408(4) 0.73214(4) 0.808218(19) 0.01919(11) Uani 1 1 d . . . W2 W 0.77440(4) 0.57716(4) 0.81099(2) 0.02353(12) Uani 1 1 d . . . W3 W 0.80983(4) 0.72553(4) 0.74275(2) 0.02488(12) Uani 1 1 d . . . Pd1 Pd 0.63204(7) 0.56016(7) 0.71618(4) 0.0280(2) Uani 1 1 d . . . S1 S 0.6340(2) 0.7496(2) 0.71445(13) 0.0281(7) Uani 1 1 d . . . S2 S 0.8227(2) 0.5372(3) 0.71770(14) 0.0345(8) Uani 1 1 d . . . S3 S 0.5852(2) 0.5461(2) 0.80957(13) 0.0245(6) Uani 1 1 d . . . S4 S 0.8149(2) 0.7663(2) 0.84044(12) 0.0224(6) Uani 1 1 d . . . P1 P 0.5232(3) 0.4642(4) 0.64727(17) 0.0499(10) Uani 1 1 d . . . Cl1 Cl 0.7769(5) 0.3788(4) 0.8048(3) 0.0912(17) Uani 1 1 d . . . N20 N 0.9258(9) 0.7527(9) 0.3264(5) 0.036(3) Uani 1 1 d . . . N21 N 0.8266(10) 0.8915(9) 0.3245(5) 0.044(3) Uani 1 1 d . . . N22 N 0.7874(8) 1.0730(8) 0.3678(4) 0.030(2) Uani 1 1 d . . . N23 N 0.8152(9) 1.2319(9) 0.4253(5) 0.038(3) Uani 1 1 d . . . N24 N 0.9146(10) 1.3570(9) 0.4975(5) 0.041(3) Uani 1 1 d . . . N25 N 1.0482(9) 1.3896(9) 0.5622(5) 0.036(3) Uani 1 1 d . . . N26 N 0.8095(9) 0.6918(8) 0.3966(5) 0.036(3) Uani 1 1 d . . . N27 N 0.7084(9) 0.8292(9) 0.3967(5) 0.037(3) Uani 1 1 d . . . N28 N 0.6554(8) 1.0093(8) 0.4309(5) 0.033(2) Uani 1 1 d . . . N29 N 0.6896(9) 1.1654(8) 0.4887(4) 0.035(3) Uani 1 1 d . . . N30 N 0.7937(9) 1.2844(9) 0.5634(5) 0.035(3) Uani 1 1 d . . . N31 N 0.9264(9) 1.3125(9) 0.6270(5) 0.039(3) Uani 1 1 d . . . N40 N 0.2236(7) 0.7500(7) -0.0680(4) 0.024(2) Uani 1 1 d . . . N41 N 0.2546(7) 0.8676(8) -0.1253(4) 0.030(2) Uani 1 1 d . . . N42 N 0.1988(7) 1.0226(7) -0.1652(4) 0.022(2) Uani 1 1 d . . . N43 N 0.0773(7) 1.1427(7) -0.1629(4) 0.025(2) Uani 1 1 d . . . N44 N 0.0826(7) 0.7819(7) 0.1214(4) 0.021(2) Uani 1 1 d . . . N45 N 0.1262(8) 0.6496(8) -0.0044(4) 0.025(2) Uani 1 1 d . . . N46 N 0.2268(7) 0.7822(8) 0.0682(4) 0.024(2) Uani 1 1 d . . . N47 N 0.3459(8) 0.8595(8) 0.0022(4) 0.027(2) Uani 1 1 d . . . N48 N 0.3593(8) 0.9868(7) -0.0512(4) 0.025(2) Uani 1 1 d . . . N49 N 0.2932(8) 1.1406(8) -0.0840(4) 0.028(2) Uani 1 1 d . . . N50 N 0.1718(8) 1.2571(8) -0.0832(4) 0.027(2) Uani 1 1 d . . . N51 N 0.0164(7) 1.3490(8) -0.0503(4) 0.024(2) Uani 1 1 d . . . C20 C 0.9291(10) 0.8592(11) 0.3157(5) 0.032(3) Uani 1 1 d . . . C21 C 0.7989(12) 0.9976(11) 0.3164(6) 0.042(3) Uani 1 1 d . . . H21A H 0.7313 0.9883 0.2952 0.051 Uiso 1 1 calc R . . H21B H 0.8546 1.0294 0.2946 0.051 Uiso 1 1 calc R . . C22 C 0.8600(10) 1.1627(10) 0.3831(5) 0.030(3) Uani 1 1 d . . . C23 C 0.8610(11) 1.3415(11) 0.4450(6) 0.039(3) Uani 1 1 d . . . H23A H 0.9123 1.3630 0.4180 0.047 Uiso 1 1 calc R . . H23B H 0.8036 1.3893 0.4473 0.047 Uiso 1 1 calc R . . C24 C 1.0259(11) 1.3674(10) 0.5061(5) 0.034(3) Uani 1 1 d . . . C25 C 0.8189(11) 0.7106(11) 0.3413(6) 0.038(3) Uani 1 1 d . . . H25 H 0.7912 0.6458 0.3148 0.046 Uiso 1 1 calc R . . C26 C 0.7463(11) 0.8077(10) 0.3404(6) 0.036(3) Uani 1 1 d . . . H26 H 0.6864 0.7877 0.3132 0.044 Uiso 1 1 calc R . . C27 C 0.6828(11) 1.0879(11) 0.3970(6) 0.037(3) Uani 1 1 d . . . H27 H 0.6240 1.0897 0.3704 0.045 Uiso 1 1 calc R . . C28 C 0.7051(10) 1.1958(10) 0.4345(5) 0.029(3) Uani 1 1 d . . . H28 H 0.6554 1.2482 0.4271 0.035 Uiso 1 1 calc R . . C29 C 0.8592(10) 1.3776(10) 0.5483(6) 0.034(3) Uani 1 1 d . . . H29 H 0.8179 1.4410 0.5501 0.040 Uiso 1 1 calc R . . C30 C 0.9521(10) 1.3980(10) 0.5929(5) 0.032(3) Uani 1 1 d . . . H30 H 0.9523 1.4707 0.6155 0.039 Uiso 1 1 calc R . . C31 C 0.8438(10) 0.5944(10) 0.4155(6) 0.036(3) Uani 1 1 d . . . H31A H 0.7946 0.5741 0.4436 0.043 Uiso 1 1 calc R . . H31B H 0.8387 0.5344 0.3844 0.043 Uiso 1 1 calc R . . C32 C 0.7387(10) 0.7563(11) 0.4276(5) 0.033(3) Uani 1 1 d . . . C33 C 0.6199(10) 0.8946(10) 0.4107(6) 0.036(3) Uani 1 1 d . . . H33A H 0.5773 0.8656 0.4392 0.043 Uiso 1 1 calc R . . H33B H 0.5734 0.8890 0.3781 0.043 Uiso 1 1 calc R . . C34 C 0.6579(10) 1.0578(11) 0.4857(6) 0.034(3) Uani 1 1 d . . . C35 C 0.6871(11) 1.2436(12) 0.5387(6) 0.040(3) Uani 1 1 d . . . H35A H 0.6442 1.2105 0.5657 0.048 Uiso 1 1 calc R . . H35B H 0.6511 1.3048 0.5306 0.048 Uiso 1 1 calc R . . C36 C 0.8319(10) 1.2530(11) 0.6096(6) 0.036(3) Uani 1 1 d . . . C37 C 0.9829(11) 1.3054(12) 0.6800(6) 0.043(3) Uani 1 1 d . . . H37A H 1.0049 1.3787 0.6993 0.051 Uiso 1 1 calc R . . H37B H 0.9320 1.2709 0.7034 0.051 Uiso 1 1 calc R . . C40 C 0.3338(9) 0.8005(9) -0.0519(5) 0.028(3) Uani 1 1 d . . . H40 H 0.3872 0.7473 -0.0592 0.034 Uiso 1 1 calc R . . C41 C 0.1836(9) 0.7847(9) -0.1139(5) 0.023(2) Uani 1 1 d . . . C42 C 0.2436(10) 0.9193(9) -0.1759(4) 0.024(3) Uani 1 1 d . . . H42A H 0.3146 0.9297 -0.1919 0.029 Uiso 1 1 calc R . . H42B H 0.1978 0.8696 -0.2032 0.029 Uiso 1 1 calc R . . C43 C 0.2617(9) 1.1249(8) -0.1439(5) 0.024(3) Uani 1 1 d . . . H43 H 0.3232 1.1404 -0.1674 0.029 Uiso 1 1 calc R . . C44 C 0.1770(9) 1.2096(9) -0.1420(5) 0.027(3) Uani 1 1 d . . . H44 H 0.1981 1.2650 -0.1649 0.033 Uiso 1 1 calc R . . C45 C 0.0934(10) 1.0349(9) -0.1743(5) 0.026(3) Uani 1 1 d . . . C46 C -0.0220(9) 1.1888(10) -0.1719(5) 0.023(2) Uani 1 1 d . . . H46A H -0.0676 1.1367 -0.1982 0.028 Uiso 1 1 calc R . . H46B H -0.0051 1.2535 -0.1885 0.028 Uiso 1 1 calc R . . C47 C 0.0724(9) 0.6737(9) 0.0889(5) 0.021(2) Uani 1 1 d . . . H47 H 0.0722 0.6180 0.1127 0.025 Uiso 1 1 calc R . . C48 C 0.1745(9) 0.6738(9) 0.0519(5) 0.024(2) Uani 1 1 d . . . H48 H 0.2213 0.6184 0.0586 0.028 Uiso 1 1 calc R . . C49 C 0.1855(9) 0.6437(9) -0.0550(5) 0.024(2) Uani 1 1 d . . . H49A H 0.1394 0.6040 -0.0854 0.029 Uiso 1 1 calc R . . H49B H 0.2473 0.6029 -0.0520 0.029 Uiso 1 1 calc R . . C50 C 0.1781(9) 0.8422(9) 0.1111(5) 0.023(2) Uani 1 1 d . . . C51 C 0.3373(9) 0.8144(11) 0.0531(5) 0.027(3) Uani 1 1 d . . . H51A H 0.3709 0.8680 0.0832 0.033 Uiso 1 1 calc R . . H51B H 0.3779 0.7511 0.0492 0.033 Uiso 1 1 calc R . . C52 C 0.3618(9) 0.9702(9) 0.0031(5) 0.024(2) Uani 1 1 d . . . C53 C 0.3501(8) 0.8869(8) -0.0892(5) 0.023(3) Uani 1 1 d . . . H53 H 0.4161 0.8788 -0.1108 0.028 Uiso 1 1 calc R . . C54 C 0.3878(9) 1.0928(9) -0.0641(5) 0.026(3) Uani 1 1 d . . . H54A H 0.4425 1.0885 -0.0925 0.031 Uiso 1 1 calc R . . H54B H 0.4191 1.1404 -0.0311 0.031 Uiso 1 1 calc R . . C55 C 0.2443(9) 1.2184(9) -0.0502(5) 0.024(3) Uani 1 1 d . . . C56 C 0.1281(9) 1.3604(9) -0.0660(5) 0.024(2) Uani 1 1 d . . . H56A H 0.1710 1.4016 -0.0347 0.029 Uiso 1 1 calc R . . H56B H 0.1347 1.4019 -0.0962 0.029 Uiso 1 1 calc R . . C57 C -0.0132(9) 1.3618(9) 0.0046(5) 0.026(3) Uani 1 1 d . . . O1 O 0.4582(6) 0.7451(6) 0.8015(3) 0.0283(19) Uani 1 1 d . . . O2 O 0.5888(7) 0.7600(7) 0.8959(3) 0.0304(19) Uani 1 1 d . . . O3 O 0.6285(6) 0.9079(6) 0.8304(3) 0.0276(18) Uani 1 1 d . . . O4 O 0.7706(7) 0.5661(7) 0.8993(4) 0.034(2) Uani 1 1 d . . . O5 O 0.9420(7) 0.5709(7) 0.8357(4) 0.037(2) Uani 1 1 d . . . O6 O 0.8529(8) 0.7310(9) 0.6578(4) 0.055(3) Uani 1 1 d . . . O7 O 0.8457(8) 0.8968(7) 0.7463(4) 0.042(2) Uani 1 1 d . . . O8 O 0.9860(7) 0.7457(7) 0.7500(4) 0.040(2) Uani 1 1 d . . . O10 O 0.5050(11) 0.3385(9) 0.6415(6) 0.087(4) Uani 1 1 d . . . O11 O 0.4010(10) 0.4933(12) 0.6459(7) 0.108(6) Uani 1 1 d . . . O12 O 0.5637(12) 0.4741(12) 0.5872(5) 0.093(5) Uani 1 1 d . . . O20 O 1.0051(8) 0.9114(8) 0.3015(4) 0.047(3) Uani 1 1 d . . . O21 O 0.9475(8) 1.1764(8) 0.3627(4) 0.049(3) Uani 1 1 d . . . O22 O 1.0918(8) 1.3624(8) 0.4688(4) 0.044(2) Uani 1 1 d . . . O23 O 0.7092(8) 0.7513(8) 0.4746(4) 0.045(2) Uani 1 1 d . . . O24 O 0.6323(9) 1.0105(8) 0.5240(5) 0.058(3) Uani 1 1 d . . . O25 O 0.7871(7) 1.1803(8) 0.6334(4) 0.047(3) Uani 1 1 d . . . O40 O 0.1022(7) 0.7480(7) -0.1400(4) 0.034(2) Uani 1 1 d . . . O41 O 0.0247(7) 0.9610(6) -0.1926(4) 0.039(2) Uani 1 1 d . . . O42 O 0.2102(7) 0.9325(6) 0.1369(4) 0.035(2) Uani 1 1 d . . . O43 O 0.3762(7) 1.0384(7) 0.0453(4) 0.038(2) Uani 1 1 d . . . O44 O 0.2625(7) 1.2490(7) -0.0026(4) 0.035(2) Uani 1 1 d . . . O45 O 0.0412(7) 1.3826(8) 0.0463(4) 0.042(2) Uani 1 1 d . . . Cl20 Cl 0.4040(4) 0.4135(4) 0.9160(2) 0.0771(15) Uani 1 1 d . . . Cl21 Cl 0.6630(3) 0.2747(4) 0.30769(18) 0.0625(12) Uani 1 1 d . . . Cl22 Cl 0.8713(3) 0.5531(3) 0.20607(15) 0.0418(8) Uani 1 1 d . . . O100 O 0.5634(17) 0.8167(17) 0.5731(9) 0.157(8) Uiso 1 1 d . . . O101 O 0.7944(13) 0.9707(13) 0.6623(7) 0.105(5) Uiso 1 1 d . . . O102 O 0.6965(10) 0.6548(10) 0.5778(5) 0.073(4) Uiso 1 1 d . . . O103 O 0.4928(9) 0.9363(9) 0.2144(5) 0.063(3) Uiso 1 1 d . . . O104 O 0.4224(10) 0.4067(10) 0.0461(5) 0.075(4) Uiso 1 1 d . . . O105 O 0.1137(8) 0.6035(8) 0.7060(4) 0.043(2) Uiso 1 1 d . . . O106 O 0.6638(8) 0.4076(8) 0.1572(4) 0.048(3) Uiso 1 1 d . . . O107 O 0.3686(19) 0.5460(19) 0.5281(10) 0.176(9) Uiso 1 1 d . . . O108 O 0.1309(19) 0.103(2) 0.4483(10) 0.186(9) Uiso 1 1 d . . . O109 O 0.577(2) 0.989(2) 0.6499(13) 0.097(9) Uiso 0.50 1 d P . . O110 O 0.4178(19) 0.7183(19) 0.1512(10) 0.179(9) Uiso 1 1 d . . . O111 O 0.375(4) 0.312(4) 0.7764(19) 0.169(17) Uiso 0.50 1 d P . . O112 O 0.6276(16) 0.2484(16) 0.7064(9) 0.146(7) Uiso 1 1 d . . . O113 O -0.013(6) 0.066(6) 0.509(3) 0.13(3) Uiso 0.25 1 d P . . O114 O 1.011(9) 0.018(9) 0.026(4) 0.19(4) Uiso 0.25 1 d P . . 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 W1 0.0174(2) 0.0179(2) 0.0208(2) 0.00004(18) 0.00237(17) 0.00003(17) W2 0.0193(2) 0.0199(2) 0.0297(3) -0.0003(2) -0.00283(19) 0.00113(18) W3 0.0200(2) 0.0260(2) 0.0248(3) -0.0017(2) 0.00534(19) -0.00608(19) Pd1 0.0245(5) 0.0264(5) 0.0287(5) -0.0042(4) 0.0009(4) -0.0033(4) S1 0.0276(16) 0.0287(16) 0.0269(16) 0.0061(13) 0.0002(13) -0.0042(13) S2 0.0225(16) 0.0343(17) 0.0400(19) -0.0116(15) 0.0062(14) 0.0006(13) S3 0.0202(14) 0.0210(14) 0.0311(16) 0.0032(12) -0.0001(12) -0.0023(11) S4 0.0188(14) 0.0221(14) 0.0232(14) -0.0019(12) 0.0015(11) -0.0030(11) P1 0.044(2) 0.056(2) 0.040(2) -0.0153(19) -0.0043(18) -0.0053(19) Cl1 0.082(4) 0.077(3) 0.116(5) 0.026(3) -0.035(3) -0.003(3) N20 0.039(6) 0.035(6) 0.036(6) 0.009(5) 0.016(5) 0.003(5) N21 0.052(8) 0.033(6) 0.049(8) 0.010(6) 0.006(6) -0.001(6) N22 0.028(5) 0.032(6) 0.030(6) 0.007(5) 0.006(4) -0.006(4) N23 0.035(6) 0.035(6) 0.046(7) 0.022(6) 0.003(5) -0.009(5) N24 0.053(8) 0.033(6) 0.038(7) 0.013(5) 0.000(6) -0.001(5) N25 0.030(6) 0.036(6) 0.041(7) 0.006(5) 0.006(5) 0.003(5) N26 0.039(6) 0.026(5) 0.039(7) -0.003(5) 0.014(5) -0.001(5) N27 0.033(6) 0.037(6) 0.041(7) 0.011(5) 0.010(5) 0.004(5) N28 0.033(6) 0.024(5) 0.041(7) 0.006(5) 0.006(5) -0.003(4) N29 0.043(7) 0.030(6) 0.030(6) 0.007(5) 0.009(5) -0.004(5) N30 0.034(6) 0.034(6) 0.037(6) 0.017(5) 0.000(5) -0.006(5) N31 0.044(7) 0.040(6) 0.033(6) 0.005(5) -0.001(5) -0.006(5) N40 0.022(5) 0.015(4) 0.032(6) 0.002(4) -0.005(4) -0.002(4) N41 0.016(5) 0.033(6) 0.040(6) 0.009(5) -0.008(4) -0.001(4) N42 0.020(5) 0.018(5) 0.026(5) 0.003(4) -0.004(4) 0.000(4) N43 0.012(4) 0.021(5) 0.041(6) 0.005(4) -0.006(4) 0.000(4) N44 0.025(5) 0.018(5) 0.019(5) 0.000(4) 0.004(4) -0.002(4) N45 0.023(5) 0.028(5) 0.022(5) 0.002(4) -0.007(4) -0.004(4) N46 0.019(5) 0.026(5) 0.026(5) 0.002(4) -0.001(4) -0.006(4) N47 0.036(6) 0.025(5) 0.020(5) 0.006(4) 0.004(4) -0.006(4) N48 0.028(5) 0.018(5) 0.027(5) 0.002(4) 0.000(4) 0.004(4) N49 0.031(6) 0.021(5) 0.032(6) 0.001(4) -0.009(5) 0.005(4) N50 0.024(5) 0.024(5) 0.031(6) 0.001(4) -0.010(4) -0.004(4) N51 0.016(5) 0.026(5) 0.028(5) 0.001(4) -0.002(4) 0.004(4) C20 0.030(7) 0.053(8) 0.014(6) 0.003(6) 0.014(5) 0.005(6) C21 0.044(8) 0.038(8) 0.045(9) 0.010(7) 0.010(7) -0.002(6) C22 0.031(7) 0.026(6) 0.031(7) 0.006(5) 0.001(6) -0.006(5) C23 0.048(9) 0.036(7) 0.035(8) 0.018(6) 0.005(6) -0.005(6) C24 0.045(8) 0.032(7) 0.023(7) 0.003(6) 0.011(6) 0.002(6) C25 0.045(8) 0.035(7) 0.032(7) 0.000(6) 0.005(6) 0.001(6) C26 0.039(8) 0.025(6) 0.044(8) 0.008(6) -0.011(6) -0.006(6) C27 0.031(7) 0.039(8) 0.041(8) 0.011(7) 0.000(6) -0.002(6) C28 0.033(7) 0.026(6) 0.026(6) 0.003(5) 0.008(5) -0.004(5) C29 0.031(7) 0.026(6) 0.043(8) 0.002(6) 0.002(6) 0.007(5) C30 0.036(7) 0.025(6) 0.032(7) -0.006(5) 0.005(6) 0.002(5) C31 0.038(8) 0.022(6) 0.047(8) 0.004(6) -0.010(6) -0.001(5) C32 0.038(7) 0.036(7) 0.024(7) 0.000(6) 0.015(6) 0.003(6) C33 0.027(7) 0.035(7) 0.050(9) 0.019(7) 0.018(6) 0.002(6) C34 0.032(7) 0.037(7) 0.034(7) 0.018(6) 0.001(6) -0.003(6) C35 0.038(8) 0.044(8) 0.040(8) 0.008(7) 0.003(6) 0.006(6) C36 0.020(6) 0.035(7) 0.053(9) 0.010(7) -0.001(6) 0.001(5) C37 0.041(8) 0.046(8) 0.042(8) 0.009(7) 0.001(7) 0.007(7) C40 0.016(6) 0.024(6) 0.041(7) -0.005(5) -0.001(5) -0.003(5) C41 0.017(6) 0.031(6) 0.022(6) 0.000(5) 0.006(5) 0.009(5) C42 0.041(7) 0.016(5) 0.016(5) 0.002(4) 0.005(5) 0.006(5) C43 0.017(5) 0.015(5) 0.039(7) 0.003(5) 0.000(5) -0.003(4) C44 0.024(6) 0.017(5) 0.042(7) 0.013(5) 0.000(5) -0.009(5) C45 0.034(7) 0.016(6) 0.027(6) 0.007(5) -0.004(5) -0.002(5) C46 0.019(6) 0.035(7) 0.017(6) 0.007(5) 0.002(4) 0.007(5) C47 0.022(6) 0.017(5) 0.024(6) 0.005(5) -0.006(5) 0.002(4) C48 0.019(6) 0.025(6) 0.029(6) 0.007(5) 0.005(5) 0.007(5) C49 0.026(6) 0.020(6) 0.026(6) 0.001(5) 0.008(5) 0.004(5) C50 0.023(6) 0.023(6) 0.022(6) 0.005(5) 0.004(5) -0.004(5) C51 0.019(6) 0.043(7) 0.021(6) 0.008(5) -0.012(5) 0.002(5) C52 0.019(6) 0.023(6) 0.028(6) 0.002(5) -0.002(5) -0.003(5) C53 0.013(5) 0.017(5) 0.038(7) -0.001(5) 0.008(5) 0.000(4) C54 0.017(6) 0.025(6) 0.029(6) -0.004(5) -0.001(5) -0.008(5) C55 0.025(6) 0.020(6) 0.022(6) 0.001(5) 0.003(5) -0.012(5) C56 0.024(6) 0.024(6) 0.021(6) -0.003(5) 0.003(5) -0.003(5) C57 0.025(6) 0.020(6) 0.034(7) 0.004(5) -0.001(5) 0.007(5) O1 0.027(4) 0.031(5) 0.025(4) 0.000(4) 0.001(4) 0.005(4) O2 0.033(5) 0.034(5) 0.022(4) 0.001(4) 0.005(4) 0.001(4) O3 0.027(4) 0.025(4) 0.028(4) -0.001(4) -0.001(4) -0.004(3) O4 0.031(5) 0.036(5) 0.034(5) 0.006(4) -0.011(4) -0.004(4) O5 0.027(5) 0.029(5) 0.048(6) -0.013(4) -0.009(4) 0.000(4) O6 0.048(6) 0.073(7) 0.037(6) 0.006(5) 0.003(5) -0.024(6) O7 0.052(6) 0.029(5) 0.040(6) 0.006(4) -0.010(5) -0.012(4) O8 0.029(5) 0.047(6) 0.034(5) -0.011(4) 0.013(4) -0.017(4) O10 0.091(10) 0.055(7) 0.091(10) -0.034(7) 0.011(8) -0.031(7) O11 0.048(8) 0.115(12) 0.140(14) -0.029(10) -0.052(9) -0.004(8) O12 0.118(12) 0.104(11) 0.044(7) -0.015(7) -0.001(8) -0.002(9) O20 0.049(6) 0.046(6) 0.048(6) 0.016(5) 0.013(5) -0.004(5) O21 0.038(6) 0.051(6) 0.059(7) 0.018(5) 0.008(5) -0.009(5) O22 0.048(6) 0.048(6) 0.033(5) 0.000(5) 0.010(5) 0.002(5) O23 0.046(6) 0.049(6) 0.042(6) 0.013(5) 0.011(5) 0.010(5) O24 0.071(8) 0.043(6) 0.058(7) 0.015(6) 0.005(6) -0.007(5) O25 0.034(5) 0.048(6) 0.063(7) 0.025(5) 0.002(5) -0.003(5) O40 0.031(5) 0.035(5) 0.035(5) 0.008(4) -0.001(4) -0.003(4) O41 0.032(5) 0.020(4) 0.062(6) 0.000(4) -0.014(5) -0.005(4) O42 0.037(5) 0.017(4) 0.046(6) -0.005(4) 0.007(4) -0.008(4) O43 0.040(5) 0.037(5) 0.034(5) -0.001(4) -0.004(4) -0.002(4) O44 0.042(5) 0.034(5) 0.028(5) 0.004(4) 0.001(4) 0.003(4) O45 0.026(5) 0.054(6) 0.042(6) 0.003(5) -0.009(4) -0.011(4) Cl20 0.064(3) 0.091(3) 0.071(3) 0.028(3) -0.004(2) -0.045(3) Cl21 0.045(2) 0.089(3) 0.062(3) 0.038(3) -0.009(2) 0.007(2) Cl22 0.0416(19) 0.0351(17) 0.048(2) 0.0019(16) 0.0024(16) 0.0082(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 2.181(8) . ? W1 O2 2.194(8) . ? W1 O1 2.210(8) . ? W1 S1 2.336(4) . ? W1 S4 2.349(3) . ? W1 S3 2.351(3) . ? W1 W3 2.7072(18) . ? W1 W2 2.7373(17) . ? W1 Pd1 2.833(2) . ? W2 O5 2.175(9) . ? W2 O4 2.183(9) . ? W2 S3 2.339(3) . ? W2 S2 2.341(4) . ? W2 S4 2.356(3) . ? W2 Cl1 2.462(6) . ? W2 W3 2.7017(17) . ? W2 Pd1 2.872(2) . ? W3 O7 2.131(9) . ? W3 O6 2.153(10) . ? W3 O8 2.178(9) . ? W3 S1 2.347(4) . ? W3 S4 2.352(3) . ? W3 S2 2.352(4) . ? W3 Pd1 2.8634(19) . ? Pd1 P1 2.253(4) . ? Pd1 S1 2.374(4) . ? Pd1 S3 2.386(4) . ? Pd1 S2 2.411(4) . ? P1 O10 1.548(12) . ? P1 O12 1.572(13) . ? P1 O11 1.593(14) . ? N20 C20 1.397(17) . ? N20 C37 1.399(17) 2_776 ? N20 C25 1.449(16) . ? N21 C20 1.378(17) . ? N21 C21 1.447(17) . ? N21 C26 1.474(16) . ? N22 C22 1.366(15) . ? N22 C21 1.454(17) . ? N22 C27 1.495(16) . ? N23 C22 1.383(17) . ? N23 C28 1.426(15) . ? N23 C23 1.433(16) . ? N24 C24 1.385(17) . ? N24 C29 1.416(17) . ? N24 C23 1.418(17) . ? N25 C24 1.371(16) . ? N25 C30 1.414(15) . ? N25 C31 1.427(16) 2_776 ? N26 C32 1.390(15) . ? N26 C25 1.412(16) . ? N26 C31 1.472(16) . ? N27 C32 1.357(16) . ? N27 C33 1.440(16) . ? N27 C26 1.445(17) . ? N28 C34 1.371(17) . ? N28 C27 1.406(16) . ? N28 C33 1.459(16) . ? N29 C34 1.353(16) . ? N29 C35 1.430(17) . ? N29 C28 1.446(15) . ? N30 C36 1.353(17) . ? N30 C29 1.455(15) . ? N30 C35 1.459(17) . ? N31 C36 1.352(16) . ? N31 C30 1.474(16) . ? N31 C37 1.489(17) . ? N40 C41 1.376(15) . ? N40 C49 1.452(13) . ? N40 C40 1.471(14) . ? N41 C41 1.358(14) . ? N41 C53 1.449(14) . ? N41 C42 1.500(14) . ? N42 C45 1.352(15) . ? N42 C42 1.441(14) . ? N42 C43 1.447(13) . ? N43 C45 1.364(14) . ? N43 C46 1.442(14) . ? N43 C44 1.461(13) . ? N44 C50 1.388(13) . ? N44 C47 1.443(13) . ? N44 C46 1.458(13) 2_575 ? N45 C57 1.395(14) 2_575 ? N45 C49 1.434(14) . ? N45 C48 1.469(15) . ? N46 C50 1.361(14) . ? N46 C48 1.435(14) . ? N46 C51 1.457(14) . ? N47 C52 1.375(14) . ? N47 C40 1.398(15) . ? N47 C51 1.449(14) . ? N48 C52 1.379(15) . ? N48 C53 1.418(14) . ? N48 C54 1.425(14) . ? N49 C55 1.358(15) . ? N49 C54 1.485(15) . ? N49 C43 1.487(15) . ? N50 C55 1.380(15) . ? N50 C56 1.448(14) . ? N50 C44 1.461(16) . ? N51 C57 1.378(15) . ? N51 C47 1.421(14) 2_575 ? N51 C56 1.439(13) . ? C20 O20 1.180(14) . ? C22 O21 1.205(14) . ? C24 O22 1.224(14) . ? C25 C26 1.584(19) . ? C27 C28 1.498(17) . ? C29 C30 1.556(18) . ? C31 N25 1.427(16) 2_776 ? C32 O23 1.215(14) . ? C34 O24 1.216(15) . ? C36 O25 1.247(15) . ? C37 N20 1.399(17) 2_776 ? C40 C53 1.526(16) . ? C41 O40 1.202(13) . ? C43 C44 1.559(16) . ? C45 O41 1.218(13) . ? C46 N44 1.458(13) 2_575 ? C47 N51 1.421(14) 2_575 ? C47 C48 1.559(15) . ? C50 O42 1.225(13) . ? C52 O43 1.221(14) . ? C55 O44 1.174(13) . ? C57 O45 1.196(14) . ? C57 N45 1.395(14) 2_575 ? O113 O113 1.71(14) 2_556 ? O114 O114 1.30(18) 2_755 ? 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 O3 W1 O2 74.7(3) . . ? O3 W1 O1 78.8(3) . . ? O2 W1 O1 78.3(3) . . ? O3 W1 S1 89.2(2) . . ? O2 W1 S1 158.3(2) . . ? O1 W1 S1 84.4(2) . . ? O3 W1 S4 85.6(2) . . ? O2 W1 S4 86.6(2) . . ? O1 W1 S4 160.6(2) . . ? S1 W1 S4 106.96(11) . . ? O3 W1 S3 157.5(2) . . ? O2 W1 S3 86.2(2) . . ? O1 W1 S3 85.7(2) . . ? S1 W1 S3 105.61(11) . . ? S4 W1 S3 105.55(10) . . ? O3 W1 W3 100.4(2) . . ? O2 W1 W3 141.5(2) . . ? O1 W1 W3 139.2(2) . . ? S1 W1 W3 54.88(8) . . ? S4 W1 W3 54.89(9) . . ? S3 W1 W3 101.98(8) . . ? O3 W1 W2 140.1(2) . . ? O2 W1 W2 99.5(2) . . ? O1 W1 W2 139.7(2) . . ? S1 W1 W2 102.23(8) . . ? S4 W1 W2 54.54(8) . . ? S3 W1 W2 54.10(8) . . ? W3 W1 W2 59.50(4) . . ? O3 W1 Pd1 142.7(2) . . ? O2 W1 Pd1 139.9(2) . . ? O1 W1 Pd1 93.7(2) . . ? S1 W1 Pd1 53.64(9) . . ? S4 W1 Pd1 105.70(8) . . ? S3 W1 Pd1 53.82(9) . . ? W3 W1 Pd1 62.19(4) . . ? W2 W1 Pd1 62.04(5) . . ? O5 W2 O4 74.5(3) . . ? O5 W2 S3 159.4(3) . . ? O4 W2 S3 87.6(2) . . ? O5 W2 S2 89.4(3) . . ? O4 W2 S2 158.0(2) . . ? S3 W2 S2 104.78(11) . . ? O5 W2 S4 83.5(2) . . ? O4 W2 S4 85.9(2) . . ? S3 W2 S4 105.71(10) . . ? S2 W2 S4 107.51(11) . . ? O5 W2 Cl1 80.1(3) . . ? O4 W2 Cl1 80.3(3) . . ? S3 W2 Cl1 87.02(15) . . ? S2 W2 Cl1 82.17(18) . . ? S4 W2 Cl1 160.87(15) . . ? O5 W2 W3 97.9(2) . . ? O4 W2 W3 140.8(2) . . ? S3 W2 W3 102.45(8) . . ? S2 W2 W3 55.06(9) . . ? S4 W2 W3 54.91(9) . . ? Cl1 W2 W3 137.23(16) . . ? O5 W2 W1 137.8(2) . . ? O4 W2 W1 100.0(2) . . ? S3 W2 W1 54.50(8) . . ? S2 W2 W1 101.99(9) . . ? S4 W2 W1 54.31(8) . . ? Cl1 W2 W1 141.28(13) . . ? W3 W2 W1 59.70(4) . . ? O5 W2 Pd1 143.3(2) . . ? O4 W2 Pd1 140.9(2) . . ? S3 W2 Pd1 53.30(8) . . ? S2 W2 Pd1 53.93(10) . . ? S4 W2 Pd1 104.33(8) . . ? Cl1 W2 Pd1 94.72(13) . . ? W3 W2 Pd1 61.74(4) . . ? W1 W2 Pd1 60.62(4) . . ? O7 W3 O6 79.4(4) . . ? O7 W3 O8 77.7(4) . . ? O6 W3 O8 79.0(4) . . ? O7 W3 S1 86.5(3) . . ? O6 W3 S1 85.6(3) . . ? O8 W3 S1 159.6(3) . . ? O7 W3 S4 85.3(3) . . ? O6 W3 S4 159.9(3) . . ? O8 W3 S4 85.1(2) . . ? S1 W3 S4 106.49(11) . . ? O7 W3 S2 159.6(3) . . ? O6 W3 S2 84.4(3) . . ? O8 W3 S2 87.2(3) . . ? S1 W3 S2 104.60(11) . . ? S4 W3 S2 107.25(11) . . ? O7 W3 W2 140.3(2) . . ? O6 W3 W2 139.0(3) . . ? O8 W3 W2 97.4(3) . . ? S1 W3 W2 102.98(8) . . ? S4 W3 W2 55.05(8) . . ? S2 W3 W2 54.65(10) . . ? O7 W3 W1 97.8(3) . . ? O6 W3 W1 140.1(3) . . ? O8 W3 W1 139.8(2) . . ? S1 W3 W1 54.49(9) . . ? S4 W3 W1 54.79(8) . . ? S2 W3 W1 102.57(8) . . ? W2 W3 W1 60.81(3) . . ? O7 W3 Pd1 139.6(3) . . ? O6 W3 Pd1 95.4(3) . . ? O8 W3 Pd1 141.2(2) . . ? S1 W3 Pd1 53.09(9) . . ? S4 W3 Pd1 104.69(7) . . ? S2 W3 Pd1 53.98(9) . . ? W2 W3 Pd1 62.06(5) . . ? W1 W3 Pd1 61.07(5) . . ? P1 Pd1 S1 109.93(15) . . ? P1 Pd1 S3 117.86(14) . . ? S1 Pd1 S3 103.33(11) . . ? P1 Pd1 S2 120.16(14) . . ? S1 Pd1 S2 102.00(12) . . ? S3 Pd1 S2 101.25(12) . . ? P1 Pd1 W1 141.96(12) . . ? S1 Pd1 W1 52.40(9) . . ? S3 Pd1 W1 52.71(8) . . ? S2 Pd1 W1 97.55(8) . . ? P1 Pd1 W3 144.92(12) . . ? S1 Pd1 W3 52.24(8) . . ? S3 Pd1 W3 96.76(8) . . ? S2 Pd1 W3 52.12(9) . . ? W1 Pd1 W3 56.74(4) . . ? P1 Pd1 W2 152.59(13) . . ? S1 Pd1 W2 97.47(8) . . ? S3 Pd1 W2 51.84(9) . . ? S2 Pd1 W2 51.71(9) . . ? W1 Pd1 W2 57.34(4) . . ? W3 Pd1 W2 56.21(4) . . ? W1 S1 W3 70.63(9) . . ? W1 S1 Pd1 73.96(9) . . ? W3 S1 Pd1 74.67(10) . . ? W2 S2 W3 70.29(9) . . ? W2 S2 Pd1 74.36(10) . . ? W3 S2 Pd1 73.89(10) . . ? W2 S3 W1 71.40(8) . . ? W2 S3 Pd1 74.86(9) . . ? W1 S3 Pd1 73.47(9) . . ? W1 S4 W3 70.32(9) . . ? W1 S4 W2 71.15(8) . . ? W3 S4 W2 70.04(8) . . ? O10 P1 O12 99.6(8) . . ? O10 P1 O11 100.6(8) . . ? O12 P1 O11 103.5(9) . . ? O10 P1 Pd1 119.5(6) . . ? O12 P1 Pd1 114.2(6) . . ? O11 P1 Pd1 116.9(6) . . ? C20 N20 C37 121.5(11) . 2_776 ? C20 N20 C25 112.7(11) . . ? C37 N20 C25 125.7(11) 2_776 . ? C20 N21 C21 122.6(11) . . ? C20 N21 C26 114.7(11) . . ? C21 N21 C26 122.7(12) . . ? C22 N22 C21 121.2(10) . . ? C22 N22 C27 110.5(10) . . ? C21 N22 C27 124.5(10) . . ? C22 N23 C28 112.2(10) . . ? C22 N23 C23 123.0(10) . . ? C28 N23 C23 122.2(12) . . ? C24 N24 C29 111.7(11) . . ? C24 N24 C23 125.3(12) . . ? C29 N24 C23 122.6(12) . . ? C24 N25 C30 111.2(11) . . ? C24 N25 C31 122.5(11) . 2_776 ? C30 N25 C31 126.2(12) . 2_776 ? C32 N26 C25 113.3(11) . . ? C32 N26 C31 121.0(11) . . ? C25 N26 C31 123.5(11) . . ? C32 N27 C33 123.4(10) . . ? C32 N27 C26 112.2(10) . . ? C33 N27 C26 121.1(11) . . ? C34 N28 C27 110.1(10) . . ? C34 N28 C33 124.5(11) . . ? C27 N28 C33 125.2(11) . . ? C34 N29 C35 123.5(11) . . ? C34 N29 C28 112.4(11) . . ? C35 N29 C28 123.0(10) . . ? C36 N30 C29 112.7(11) . . ? C36 N30 C35 122.8(10) . . ? C29 N30 C35 123.4(11) . . ? C36 N31 C30 110.6(11) . . ? C36 N31 C37 123.2(11) . . ? C30 N31 C37 125.2(11) . . ? C41 N40 C49 120.6(10) . . ? C41 N40 C40 112.5(9) . . ? C49 N40 C40 121.0(9) . . ? C41 N41 C53 112.8(10) . . ? C41 N41 C42 122.7(10) . . ? C53 N41 C42 123.7(9) . . ? C45 N42 C42 123.8(9) . . ? C45 N42 C43 112.5(9) . . ? C42 N42 C43 123.7(9) . . ? C45 N43 C46 126.2(10) . . ? C45 N43 C44 111.1(9) . . ? C46 N43 C44 122.7(9) . . ? C50 N44 C47 112.2(9) . . ? C50 N44 C46 121.6(9) . 2_575 ? C47 N44 C46 123.0(9) . 2_575 ? C57 N45 C49 121.8(10) 2_575 . ? C57 N45 C48 112.9(9) 2_575 . ? C49 N45 C48 125.3(9) . . ? C50 N46 C48 113.7(9) . . ? C50 N46 C51 121.0(9) . . ? C48 N46 C51 122.9(10) . . ? C52 N47 C40 112.5(10) . . ? C52 N47 C51 121.3(10) . . ? C40 N47 C51 126.1(10) . . ? C52 N48 C53 111.7(9) . . ? C52 N48 C54 120.2(10) . . ? C53 N48 C54 126.6(10) . . ? C55 N49 C54 121.0(10) . . ? C55 N49 C43 115.6(10) . . ? C54 N49 C43 122.2(9) . . ? C55 N50 C56 121.8(10) . . ? C55 N50 C44 113.0(10) . . ? C56 N50 C44 121.1(10) . . ? C57 N51 C47 114.2(9) . 2_575 ? C57 N51 C56 121.8(10) . . ? C47 N51 C56 124.1(10) 2_575 . ? O20 C20 N21 126.5(13) . . ? O20 C20 N20 126.4(12) . . ? N21 C20 N20 107.0(10) . . ? N21 C21 N22 113.9(11) . . ? O21 C22 N22 124.4(12) . . ? O21 C22 N23 127.5(12) . . ? N22 C22 N23 108.1(10) . . ? N24 C23 N23 114.6(11) . . ? O22 C24 N25 126.8(13) . . ? O22 C24 N24 124.2(13) . . ? N25 C24 N24 108.9(11) . . ? N26 C25 N20 115.3(12) . . ? N26 C25 C26 102.7(11) . . ? N20 C25 C26 104.7(10) . . ? N27 C26 N21 115.8(11) . . ? N27 C26 C25 103.2(10) . . ? N21 C26 C25 100.9(11) . . ? N28 C27 N22 113.1(11) . . ? N28 C27 C28 107.3(11) . . ? N22 C27 C28 103.5(10) . . ? N23 C28 N29 112.7(11) . . ? N23 C28 C27 105.3(10) . . ? N29 C28 C27 101.7(10) . . ? N24 C29 N30 115.6(11) . . ? N24 C29 C30 103.3(10) . . ? N30 C29 C30 102.2(10) . . ? N25 C30 N31 115.5(11) . . ? N25 C30 C29 104.8(10) . . ? N31 C30 C29 104.0(10) . . ? N25 C31 N26 113.0(10) 2_776 . ? O23 C32 N27 124.7(12) . . ? O23 C32 N26 127.1(13) . . ? N27 C32 N26 108.1(10) . . ? N27 C33 N28 113.2(10) . . ? O24 C34 N29 127.1(13) . . ? O24 C34 N28 124.5(12) . . ? N29 C34 N28 108.4(10) . . ? N29 C35 N30 114.3(11) . . ? O25 C36 N31 124.0(13) . . ? O25 C36 N30 125.7(12) . . ? N31 C36 N30 110.3(11) . . ? N20 C37 N31 114.6(12) 2_776 . ? N47 C40 N40 115.5(10) . . ? N47 C40 C53 104.4(9) . . ? N40 C40 C53 102.2(9) . . ? O40 C41 N41 125.7(11) . . ? O40 C41 N40 126.9(11) . . ? N41 C41 N40 107.4(10) . . ? N42 C42 N41 114.0(9) . . ? N42 C43 N49 115.1(9) . . ? N42 C43 C44 103.0(8) . . ? N49 C43 C44 100.2(9) . . ? N43 C44 N50 112.7(9) . . ? N43 C44 C43 103.4(8) . . ? N50 C44 C43 104.6(10) . . ? O41 C45 N42 124.8(11) . . ? O41 C45 N43 125.2(11) . . ? N42 C45 N43 109.9(9) . . ? N43 C46 N44 113.9(9) . 2_575 ? N51 C47 N44 115.0(9) 2_575 . ? N51 C47 C48 104.4(9) 2_575 . ? N44 C47 C48 103.4(8) . . ? N46 C48 N45 115.5(9) . . ? N46 C48 C47 102.9(9) . . ? N45 C48 C47 102.1(9) . . ? N45 C49 N40 113.3(9) . . ? O42 C50 N46 127.9(10) . . ? O42 C50 N44 124.7(11) . . ? N46 C50 N44 107.3(9) . . ? N47 C51 N46 114.6(9) . . ? O43 C52 N47 124.6(11) . . ? O43 C52 N48 128.2(11) . . ? N47 C52 N48 107.2(10) . . ? N48 C53 N41 115.3(9) . . ? N48 C53 C40 103.8(9) . . ? N41 C53 C40 104.4(8) . . ? N48 C54 N49 112.2(9) . . ? O44 C55 N49 126.8(12) . . ? O44 C55 N50 126.8(12) . . ? N49 C55 N50 106.4(10) . . ? N51 C56 N50 113.3(9) . . ? O45 C57 N51 130.4(11) . . ? O45 C57 N45 123.1(12) . 2_575 ? N51 C57 N45 106.4(10) . 2_575 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.858 _refine_diff_density_min -1.876 _refine_diff_density_rms 0.282 # Attachment 'STR619M.CIF' data_[W3S4Pd(P(OH)2Ph)(H2O)7Cl2]Cl2CUC[6]9.5H2O _database_code_depnum_ccdc_archive 'CCDC 621860' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H58 Cl4 N12 O24.50 P Pd S4 W3' _chemical_formula_weight 1865.78 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' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.414(19) _cell_length_b 22.16(2) _cell_length_c 24.51(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11085(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7176 _exptl_absorpt_coefficient_mu 6.982 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.807685 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59969 _diffrn_reflns_av_R_equivalents 0.1607 _diffrn_reflns_av_sigmaI/netI 0.1054 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9747 _reflns_number_gt 5859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0749P)^2^+109.6154P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9747 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 W1 W 0.75477(3) 0.13083(3) 0.36219(3) 0.0351(2) Uani 1 1 d . . . W2 W 0.79497(3) 0.01670(3) 0.38124(3) 0.0365(2) Uani 1 1 d . . . W3 W 0.80845(3) 0.10175(3) 0.46074(3) 0.0334(2) Uani 1 1 d . . . Pd1 Pd 0.89364(6) 0.10795(6) 0.36756(5) 0.0334(3) Uani 1 1 d . . . S1 S 0.83241(19) 0.18781(19) 0.40893(18) 0.0334(10) Uani 1 1 d . . . S2 S 0.7080(2) 0.0655(2) 0.4263(2) 0.0437(12) Uani 1 1 d . . . S3 S 0.8160(2) 0.0719(2) 0.30131(18) 0.0384(11) Uani 1 1 d . . . S4 S 0.8881(2) 0.0315(2) 0.43512(19) 0.0405(11) Uani 1 1 d . . . Cl1 Cl 0.8567(3) -0.0648(3) 0.3356(3) 0.0856(19) Uani 1 1 d . . . Cl2 Cl 0.8916(2) 0.1404(2) 0.5277(2) 0.0525(13) Uani 1 1 d . . . O1 O 0.6683(6) 0.1098(6) 0.3120(6) 0.058(4) Uani 1 1 d . . . O2 O 0.6803(6) 0.1924(6) 0.3928(5) 0.051(3) Uani 1 1 d . . . O3 O 0.7619(6) 0.2020(6) 0.2971(5) 0.052(3) Uani 1 1 d . . . O4 O 0.7171(6) -0.0302(5) 0.3363(5) 0.047(3) Uani 1 1 d . . . O5 O 0.7697(6) -0.0572(5) 0.4362(5) 0.040(3) Uani 1 1 d . . . O6 O 0.7860(6) 0.0399(6) 0.5276(6) 0.057(4) Uani 1 1 d . . . O7 O 0.7465(6) 0.1579(5) 0.5126(5) 0.045(3) Uani 1 1 d . . . P1 P 0.9961(2) 0.1335(2) 0.34191(19) 0.0343(10) Uani 1 1 d . . . O10 O 1.0402(6) 0.0800(5) 0.3182(5) 0.050(3) Uani 1 1 d . . . O11 O 1.0403(6) 0.1657(6) 0.3868(6) 0.061(4) Uani 1 1 d . . . C50 C 1.0026(10) 0.1886(8) 0.2905(9) 0.051(5) Uani 1 1 d . . . C51 C 1.0642(10) 0.2095(10) 0.2667(9) 0.066(6) Uani 1 1 d . . . H51 H 1.1036 0.1944 0.2800 0.079 Uiso 1 1 calc R . . C52 C 1.0652(19) 0.2513(13) 0.2247(12) 0.110(11) Uani 1 1 d . . . H52 H 1.1052 0.2634 0.2103 0.131 Uiso 1 1 calc R . . C53 C 1.007(2) 0.2760(12) 0.2033(10) 0.091(10) Uani 1 1 d . . . H53 H 1.0080 0.3053 0.1761 0.109 Uiso 1 1 calc R . . C54 C 0.9514(15) 0.2560(10) 0.2231(11) 0.078(8) Uani 1 1 d . . . H54 H 0.9135 0.2712 0.2072 0.094 Uiso 1 1 calc R . . C55 C 0.9427(14) 0.2149(9) 0.2650(8) 0.073(8) Uani 1 1 d . . . H55 H 0.9011 0.2041 0.2768 0.088 Uiso 1 1 calc R . . C20 C -0.1516(8) 0.3116(9) 0.5023(8) 0.046(5) Uani 1 1 d . . . H20A H -0.1567 0.2688 0.5096 0.056 Uiso 1 1 calc R . . H20B H -0.1926 0.3260 0.4872 0.056 Uiso 1 1 calc R . . C21 C -0.1103(10) 0.3539(8) 0.4183(8) 0.045(5) Uani 1 1 d . . . C22 C -0.0517(9) 0.3718(8) 0.3289(7) 0.044(5) Uani 1 1 d . . . H22A H -0.0379 0.3404 0.3039 0.053 Uiso 1 1 calc R . . H22B H -0.0946 0.3855 0.3173 0.053 Uiso 1 1 calc R . . C23 C -0.0276(8) 0.4794(8) 0.3214(6) 0.033(4) Uani 1 1 d . . . C24 C 0.0229(9) 0.5769(9) 0.3012(7) 0.044(5) Uani 1 1 d . . . H24A H 0.0494 0.5865 0.2695 0.053 Uiso 1 1 calc R . . H24B H -0.0223 0.5860 0.2921 0.053 Uiso 1 1 calc R . . C25 C -0.0010(8) 0.6451(7) 0.3769(7) 0.032(4) Uani 1 1 d . . . C26 C -0.0451(8) 0.2790(7) 0.4576(8) 0.042(5) Uani 1 1 d . . . H26 H -0.0577 0.2364 0.4572 0.050 Uiso 1 1 calc R . . C27 C -0.0130(8) 0.2984(7) 0.4030(7) 0.034(4) Uani 1 1 d . . . H27 H -0.0110 0.2646 0.3773 0.041 Uiso 1 1 calc R . . C28 C 0.0615(8) 0.4144(8) 0.3146(7) 0.036(4) Uani 1 1 d . . . H28 H 0.0695 0.3899 0.2820 0.044 Uiso 1 1 calc R . . C29 C 0.0856(8) 0.4779(8) 0.3064(7) 0.040(4) Uani 1 1 d . . . H29 H 0.1054 0.4832 0.2703 0.047 Uiso 1 1 calc R . . C30 C 0.1097(8) 0.6342(7) 0.3576(7) 0.037(4) Uani 1 1 d . . . H30 H 0.1311 0.6519 0.3256 0.044 Uiso 1 1 calc R . . C31 C 0.1011(8) 0.6802(8) 0.4035(7) 0.040(4) Uani 1 1 d . . . H31 H 0.1175 0.7198 0.3919 0.048 Uiso 1 1 calc R . . C32 C 0.0002(8) 0.2730(8) 0.5546(7) 0.039(4) Uani 1 1 d . . . H32A H 0.0437 0.2649 0.5687 0.047 Uiso 1 1 calc R . . H32B H -0.0245 0.2356 0.5564 0.047 Uiso 1 1 calc R . . C33 C 0.0638(8) 0.3109(7) 0.4749(7) 0.036(4) Uani 1 1 d . . . C34 C 0.1018(8) 0.3323(8) 0.3796(7) 0.038(4) Uani 1 1 d . . . H34A H 0.1442 0.3248 0.3961 0.045 Uiso 1 1 calc R . . H34B H 0.0975 0.3055 0.3485 0.045 Uiso 1 1 calc R . . C35 C 0.1414(9) 0.4358(8) 0.3799(8) 0.039(4) Uani 1 1 d . . . C36 C 0.1777(8) 0.5376(8) 0.3553(8) 0.042(5) Uani 1 1 d . . . H36A H 0.2164 0.5242 0.3748 0.050 Uiso 1 1 calc R . . H36B H 0.1915 0.5506 0.3193 0.050 Uiso 1 1 calc R . . C37 C 0.1690(8) 0.6045(8) 0.4335(7) 0.036(4) Uani 1 1 d . . . N20 N -0.1023(6) 0.3187(6) 0.4623(6) 0.037(3) Uani 1 1 d . . . N21 N -0.0576(7) 0.3455(6) 0.3838(6) 0.038(4) Uani 1 1 d . . . N22 N -0.0076(7) 0.4204(6) 0.3246(6) 0.039(4) Uani 1 1 d . . . N23 N 0.0284(6) 0.5127(6) 0.3123(6) 0.037(3) Uani 1 1 d . . . N24 N 0.0428(6) 0.6153(6) 0.3459(6) 0.034(3) Uani 1 1 d . . . N25 N 0.0313(6) 0.6825(6) 0.4106(6) 0.039(4) Uani 1 1 d . . . N26 N 0.0058(6) 0.2908(6) 0.4980(6) 0.034(3) Uani 1 1 d . . . N27 N 0.0512(6) 0.3175(6) 0.4189(6) 0.037(4) Uani 1 1 d . . . N28 N 0.1001(6) 0.3924(6) 0.3607(5) 0.033(3) Uani 1 1 d . . . N29 N 0.1329(6) 0.4867(6) 0.3494(5) 0.028(3) Uani 1 1 d . . . N30 N 0.1502(7) 0.5875(6) 0.3832(5) 0.034(3) Uani 1 1 d . . . N31 N 0.1402(6) 0.6575(6) 0.4458(6) 0.039(4) Uani 1 1 d . . . O20 O -0.1556(6) 0.3884(6) 0.4093(5) 0.054(4) Uani 1 1 d . . . O21 O -0.0836(5) 0.4979(5) 0.3267(5) 0.045(3) Uani 1 1 d . . . O22 O -0.0622(6) 0.6397(6) 0.3750(5) 0.045(3) Uani 1 1 d . . . O23 O 0.1142(5) 0.3224(5) 0.4974(5) 0.040(3) Uani 1 1 d . . . O24 O 0.1794(6) 0.4282(5) 0.4185(5) 0.051(4) Uani 1 1 d . . . O25 O 0.2067(6) 0.5750(6) 0.4637(5) 0.048(3) Uani 1 1 d . . . Cl10 Cl 0.7470(6) 0.3092(7) 0.6803(6) 0.195(5) Uani 1 1 d . . . Cl11 Cl 0.9988(7) 0.5391(6) 0.8203(6) 0.212(6) Uani 1 1 d . . . O100 O 0.7717(7) 0.4275(7) 0.2215(6) 0.075(4) Uiso 1 1 d . . . O101 O 0.6743(9) 0.0684(8) 0.2102(7) 0.093(5) Uiso 1 1 d . . . O102 O 0.7760(11) 0.3002(10) 0.1211(9) 0.128(7) Uiso 1 1 d . . . O103 O 0.1627(14) 0.3161(12) 0.0578(12) 0.177(11) Uiso 1 1 d . . . O104 O 0.0390(13) 0.3883(11) -0.0189(11) 0.161(10) Uiso 1 1 d . . . O105 O 0.8827(16) -0.0137(14) 0.5783(14) 0.213(13) Uiso 1 1 d . . . O106 O 0.775(2) 0.317(2) 0.3165(19) 0.30(2) Uiso 1 1 d . . . O107 O 0.1090(16) 0.6074(14) 0.8397(13) 0.202(13) Uiso 1 1 d . . . O108 O 0.0000 0.5000 0.5000 0.37(4) Uiso 1 2 d S . . O109 O 0.175(2) 0.181(2) 0.422(2) 0.34(2) 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 W1 0.0237(4) 0.0363(4) 0.0454(4) -0.0026(3) 0.0044(3) -0.0034(3) W2 0.0322(4) 0.0309(4) 0.0464(5) -0.0042(3) 0.0141(3) -0.0084(3) W3 0.0305(4) 0.0319(4) 0.0377(4) -0.0008(3) 0.0116(3) -0.0042(3) Pd1 0.0256(7) 0.0362(8) 0.0385(8) -0.0005(6) 0.0074(6) -0.0042(5) S1 0.027(2) 0.033(2) 0.040(3) -0.004(2) 0.0034(19) -0.0067(18) S2 0.028(2) 0.043(3) 0.061(3) -0.009(2) 0.015(2) -0.009(2) S3 0.033(2) 0.041(3) 0.041(3) -0.005(2) 0.004(2) -0.0059(19) S4 0.040(3) 0.037(3) 0.044(3) 0.006(2) 0.010(2) 0.002(2) Cl1 0.078(4) 0.073(4) 0.106(5) -0.003(4) 0.015(4) -0.005(3) Cl2 0.058(3) 0.056(3) 0.043(3) 0.001(2) 0.001(2) -0.007(2) O1 0.034(7) 0.077(10) 0.065(9) -0.011(8) -0.006(7) 0.001(7) O2 0.031(7) 0.054(8) 0.069(9) -0.009(7) 0.005(6) 0.001(6) O3 0.055(8) 0.048(8) 0.054(8) 0.006(6) -0.019(7) 0.001(6) O4 0.038(7) 0.043(8) 0.060(9) -0.006(6) 0.008(6) -0.017(6) O5 0.044(7) 0.033(7) 0.043(7) 0.012(6) -0.003(6) -0.002(5) O6 0.057(9) 0.042(8) 0.072(10) 0.023(7) 0.022(7) 0.015(6) O7 0.041(7) 0.049(7) 0.046(8) -0.002(6) 0.015(6) 0.005(6) P1 0.025(2) 0.039(3) 0.038(3) -0.008(2) 0.0045(19) -0.0039(19) O10 0.042(8) 0.042(8) 0.067(9) -0.013(7) 0.016(7) 0.009(6) O11 0.045(8) 0.056(9) 0.083(11) -0.024(8) -0.015(7) -0.011(7) C50 0.049(12) 0.039(11) 0.065(14) -0.009(10) 0.012(11) -0.002(9) C51 0.049(13) 0.080(17) 0.068(16) 0.007(13) 0.015(11) -0.020(11) C52 0.16(3) 0.09(2) 0.08(2) -0.001(18) 0.08(2) -0.03(2) C53 0.19(4) 0.051(17) 0.035(15) -0.018(12) 0.012(19) -0.02(2) C54 0.12(2) 0.036(13) 0.083(19) -0.019(13) -0.021(17) -0.010(14) C55 0.14(2) 0.042(13) 0.040(13) -0.004(10) 0.013(14) -0.042(14) C20 0.027(10) 0.059(13) 0.053(13) -0.007(10) -0.003(9) -0.001(9) C21 0.066(14) 0.031(11) 0.038(12) -0.023(9) 0.007(10) -0.001(9) C22 0.051(12) 0.058(12) 0.022(10) 0.005(9) -0.012(8) 0.003(10) C23 0.020(9) 0.061(12) 0.020(9) -0.005(8) -0.007(7) 0.011(8) C24 0.038(11) 0.064(13) 0.031(11) 0.003(9) 0.007(8) 0.002(9) C25 0.039(11) 0.026(9) 0.031(10) -0.003(7) -0.012(8) -0.003(7) C26 0.029(10) 0.026(9) 0.071(14) -0.011(9) -0.008(9) 0.001(7) C27 0.032(10) 0.028(9) 0.042(11) -0.010(8) -0.016(8) 0.006(7) C28 0.031(10) 0.052(12) 0.027(10) -0.005(8) -0.016(8) 0.015(8) C29 0.033(10) 0.050(12) 0.036(11) 0.005(9) 0.015(8) 0.008(8) C30 0.027(9) 0.041(10) 0.043(11) 0.016(9) -0.006(8) -0.001(8) C31 0.032(10) 0.043(11) 0.044(11) 0.003(9) -0.003(9) -0.002(8) C32 0.034(10) 0.039(10) 0.043(12) 0.007(9) -0.002(8) -0.004(8) C33 0.030(10) 0.037(10) 0.040(11) -0.002(8) -0.005(9) 0.013(8) C34 0.026(9) 0.044(11) 0.044(11) -0.018(9) 0.004(8) 0.008(8) C35 0.041(11) 0.036(10) 0.042(12) 0.004(9) 0.017(9) -0.002(8) C36 0.024(9) 0.052(12) 0.050(12) 0.016(9) 0.014(8) 0.004(8) C37 0.026(9) 0.050(11) 0.033(10) -0.002(9) 0.000(8) -0.004(8) N20 0.031(8) 0.041(9) 0.040(9) 0.002(7) -0.009(7) 0.003(6) N21 0.044(9) 0.041(9) 0.030(8) 0.002(7) -0.009(7) 0.007(7) N22 0.035(9) 0.042(9) 0.040(9) -0.003(7) -0.004(7) 0.001(7) N23 0.029(8) 0.042(9) 0.040(9) -0.008(7) -0.009(6) -0.005(7) N24 0.027(8) 0.043(9) 0.033(8) -0.007(7) 0.000(6) -0.008(6) N25 0.026(8) 0.031(8) 0.059(10) 0.000(7) -0.006(7) 0.007(6) N26 0.023(7) 0.042(9) 0.036(9) -0.004(7) -0.007(6) 0.001(6) N27 0.018(7) 0.038(8) 0.055(10) -0.001(7) 0.006(7) -0.001(6) N28 0.027(7) 0.036(8) 0.034(8) 0.007(7) -0.005(6) -0.005(6) N29 0.017(7) 0.042(8) 0.024(7) 0.000(6) 0.001(6) -0.005(6) N30 0.041(8) 0.041(9) 0.021(8) 0.004(6) 0.002(6) 0.012(7) N31 0.024(8) 0.040(8) 0.053(10) -0.019(7) -0.017(7) 0.006(6) O20 0.042(8) 0.063(9) 0.056(9) 0.004(7) -0.011(7) 0.026(7) O21 0.021(7) 0.050(8) 0.065(9) 0.005(6) -0.012(6) -0.002(5) O22 0.034(7) 0.057(8) 0.044(8) -0.001(6) -0.003(6) -0.011(6) O23 0.027(7) 0.047(8) 0.045(8) 0.007(6) -0.004(6) 0.004(5) O24 0.055(8) 0.044(8) 0.054(9) 0.014(7) -0.036(7) 0.002(6) O25 0.043(8) 0.051(8) 0.051(8) -0.002(7) -0.016(7) 0.010(6) Cl10 0.135(9) 0.229(14) 0.219(13) 0.008(11) 0.016(9) -0.019(9) Cl11 0.189(12) 0.201(13) 0.247(16) 0.031(11) 0.023(12) -0.020(10) _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 W1 O2 2.176(12) . ? W1 O1 2.202(12) . ? W1 O3 2.248(12) . ? W1 S1 2.328(4) . ? W1 S2 2.341(5) . ? W1 S3 2.343(5) . ? W1 W2 2.699(2) . ? W1 W3 2.729(2) . ? W1 Pd1 2.883(3) . ? W2 O5 2.182(11) . ? W2 O4 2.196(11) . ? W2 S4 2.338(5) . ? W2 S3 2.349(5) . ? W2 S2 2.355(5) . ? W2 Cl1 2.469(7) . ? W2 W3 2.725(2) . ? W2 Pd1 2.873(2) . ? W3 O7 2.182(11) . ? W3 O6 2.185(12) . ? W3 S4 2.337(5) . ? W3 S1 2.342(5) . ? W3 S2 2.359(5) . ? W3 Cl2 2.510(5) . ? W3 Pd1 2.874(2) . ? Pd1 P1 2.257(5) . ? Pd1 S4 2.371(5) . ? Pd1 S1 2.392(5) . ? Pd1 S3 2.406(5) . ? P1 O11 1.592(13) . ? P1 O10 1.596(12) . ? P1 C50 1.76(2) . ? C50 C51 1.46(3) . ? C50 C55 1.49(3) . ? C51 C52 1.39(3) . ? C52 C53 1.41(4) . ? C53 C54 1.31(4) . ? C54 C55 1.38(3) . ? C20 N20 1.41(2) . ? C20 N31 1.46(2) 5_566 ? C21 O20 1.22(2) . ? C21 N20 1.34(2) . ? C21 N21 1.38(2) . ? C22 N22 1.41(2) . ? C22 N21 1.47(2) . ? C23 O21 1.220(18) . ? C23 N22 1.37(2) . ? C23 N23 1.38(2) . ? C24 N24 1.44(2) . ? C24 N23 1.45(2) . ? C25 O22 1.256(19) . ? C25 N25 1.34(2) . ? C25 N24 1.35(2) . ? C26 N26 1.46(2) . ? C26 N20 1.47(2) . ? C26 C27 1.55(2) . ? C27 N27 1.431(19) . ? C27 N21 1.463(19) . ? C28 N22 1.44(2) . ? C28 N28 1.462(19) . ? C28 C29 1.50(2) . ? C29 N23 1.41(2) . ? C29 N29 1.44(2) . ? C30 N24 1.46(2) . ? C30 N30 1.47(2) . ? C30 C31 1.53(2) . ? C31 N31 1.40(2) . ? C31 N25 1.44(2) . ? C32 N26 1.45(2) . ? C32 N25 1.46(2) 5_566 ? C33 O23 1.194(19) . ? C33 N26 1.39(2) . ? C33 N27 1.40(2) . ? C34 N28 1.41(2) . ? C34 N27 1.45(2) . ? C35 O24 1.24(2) . ? C35 N28 1.36(2) . ? C35 N29 1.36(2) . ? C36 N30 1.42(2) . ? C36 N29 1.46(2) . ? C37 O25 1.25(2) . ? C37 N30 1.35(2) . ? C37 N31 1.35(2) . ? N25 C32 1.46(2) 5_566 ? N31 C20 1.46(2) 5_566 ? 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 W1 O1 76.4(5) . . ? O2 W1 O3 81.4(5) . . ? O1 W1 O3 78.7(5) . . ? O2 W1 S1 88.1(3) . . ? O1 W1 S1 159.3(4) . . ? O3 W1 S1 85.7(3) . . ? O2 W1 S2 82.6(4) . . ? O1 W1 S2 85.3(4) . . ? O3 W1 S2 159.5(3) . . ? S1 W1 S2 106.42(17) . . ? O2 W1 S3 160.2(4) . . ? O1 W1 S3 87.4(4) . . ? O3 W1 S3 84.5(4) . . ? S1 W1 S3 104.62(16) . . ? S2 W1 S3 107.52(17) . . ? O2 W1 W2 137.8(3) . . ? O1 W1 W2 98.2(4) . . ? O3 W1 W2 139.5(3) . . ? S1 W1 W2 102.47(12) . . ? S2 W1 W2 55.16(12) . . ? S3 W1 W2 54.99(12) . . ? O2 W1 W3 97.1(4) . . ? O1 W1 W3 140.0(4) . . ? O3 W1 W3 140.1(3) . . ? S1 W1 W3 54.49(12) . . ? S2 W1 W3 54.80(13) . . ? S3 W1 W3 102.59(13) . . ? W2 W1 W3 60.24(3) . . ? O2 W1 Pd1 141.4(3) . . ? O1 W1 Pd1 141.0(3) . . ? O3 W1 Pd1 95.3(3) . . ? S1 W1 Pd1 53.37(11) . . ? S2 W1 Pd1 105.19(12) . . ? S3 W1 Pd1 53.62(11) . . ? W2 W1 Pd1 61.86(3) . . ? W3 W1 Pd1 61.53(4) . . ? O5 W2 O4 77.5(4) . . ? O5 W2 S4 87.1(3) . . ? O4 W2 S4 159.8(3) . . ? O5 W2 S3 161.6(3) . . ? O4 W2 S3 87.8(3) . . ? S4 W2 S3 104.45(16) . . ? O5 W2 S2 82.9(3) . . ? O4 W2 S2 84.6(3) . . ? S4 W2 S2 106.48(18) . . ? S3 W2 S2 106.84(17) . . ? O5 W2 Cl1 81.5(4) . . ? O4 W2 Cl1 78.2(4) . . ? S4 W2 Cl1 86.8(2) . . ? S3 W2 Cl1 84.9(2) . . ? S2 W2 Cl1 158.91(18) . . ? O5 W2 W1 137.5(3) . . ? O4 W2 W1 97.9(3) . . ? S4 W2 W1 102.32(12) . . ? S3 W2 W1 54.78(11) . . ? S2 W2 W1 54.67(12) . . ? Cl1 W2 W1 139.63(17) . . ? O5 W2 W3 95.8(3) . . ? O4 W2 W3 139.4(3) . . ? S4 W2 W3 54.33(11) . . ? S3 W2 W3 102.57(13) . . ? S2 W2 W3 54.75(12) . . ? Cl1 W2 W3 141.10(17) . . ? W1 W2 W3 60.42(6) . . ? O5 W2 Pd1 140.0(3) . . ? O4 W2 Pd1 141.5(3) . . ? S4 W2 Pd1 52.93(12) . . ? S3 W2 Pd1 53.72(11) . . ? S2 W2 Pd1 105.09(13) . . ? Cl1 W2 Pd1 95.99(16) . . ? W1 W2 Pd1 62.21(7) . . ? W3 W2 Pd1 61.70(5) . . ? O7 W3 O6 78.4(5) . . ? O7 W3 S4 160.0(3) . . ? O6 W3 S4 86.0(3) . . ? O7 W3 S1 88.4(3) . . ? O6 W3 S1 163.9(4) . . ? S4 W3 S1 104.55(16) . . ? O7 W3 S2 84.2(3) . . ? O6 W3 S2 82.6(4) . . ? S4 W3 S2 106.41(17) . . ? S1 W3 S2 105.36(16) . . ? O7 W3 Cl2 79.4(3) . . ? O6 W3 Cl2 82.3(4) . . ? S4 W3 Cl2 86.12(18) . . ? S1 W3 Cl2 86.32(16) . . ? S2 W3 Cl2 159.61(16) . . ? O7 W3 W2 138.8(3) . . ? O6 W3 W2 94.7(4) . . ? S4 W3 W2 54.37(13) . . ? S1 W3 W2 101.33(13) . . ? S2 W3 W2 54.63(11) . . ? Cl2 W3 W2 140.47(12) . . ? O7 W3 W1 98.5(3) . . ? O6 W3 W1 136.7(4) . . ? S4 W3 W1 101.47(13) . . ? S1 W3 W1 53.98(11) . . ? S2 W3 W1 54.19(12) . . ? Cl2 W3 W1 140.28(12) . . ? W2 W3 W1 59.33(6) . . ? O7 W3 Pd1 141.8(3) . . ? O6 W3 Pd1 138.9(3) . . ? S4 W3 Pd1 52.93(12) . . ? S1 W3 Pd1 53.42(11) . . ? S2 W3 Pd1 104.99(14) . . ? Cl2 W3 Pd1 95.40(14) . . ? W2 W3 Pd1 61.70(5) . . ? W1 W3 Pd1 61.87(7) . . ? P1 Pd1 S4 114.69(17) . . ? P1 Pd1 S1 114.65(16) . . ? S4 Pd1 S1 101.97(17) . . ? P1 Pd1 S3 120.41(17) . . ? S4 Pd1 S3 101.71(17) . . ? S1 Pd1 S3 100.78(16) . . ? P1 Pd1 W2 149.18(13) . . ? S4 Pd1 W2 51.87(12) . . ? S1 Pd1 W2 96.01(12) . . ? S3 Pd1 W2 51.93(12) . . ? P1 Pd1 W3 142.60(13) . . ? S4 Pd1 W3 51.84(12) . . ? S1 Pd1 W3 51.85(11) . . ? S3 Pd1 W3 96.99(13) . . ? W2 Pd1 W3 56.60(4) . . ? P1 Pd1 W1 148.75(14) . . ? S4 Pd1 W1 96.35(12) . . ? S1 Pd1 W1 51.34(10) . . ? S3 Pd1 W1 51.64(11) . . ? W2 Pd1 W1 55.93(6) . . ? W3 Pd1 W1 56.61(5) . . ? W1 S1 W3 71.53(13) . . ? W1 S1 Pd1 75.29(14) . . ? W3 S1 Pd1 74.73(14) . . ? W1 S2 W2 70.17(14) . . ? W1 S2 W3 71.01(13) . . ? W2 S2 W3 70.62(14) . . ? W1 S3 W2 70.23(14) . . ? W1 S3 Pd1 74.74(15) . . ? W2 S3 Pd1 74.34(15) . . ? W3 S4 W2 71.30(14) . . ? W3 S4 Pd1 75.23(14) . . ? W2 S4 Pd1 75.20(15) . . ? O11 P1 O10 105.4(7) . . ? O11 P1 C50 98.1(9) . . ? O10 P1 C50 102.2(8) . . ? O11 P1 Pd1 116.4(6) . . ? O10 P1 Pd1 115.9(5) . . ? C50 P1 Pd1 116.3(7) . . ? C51 C50 C55 114.5(19) . . ? C51 C50 P1 124.8(17) . . ? C55 C50 P1 120.6(14) . . ? C52 C51 C50 121(2) . . ? C51 C52 C53 122(3) . . ? C54 C53 C52 117(3) . . ? C53 C54 C55 127(3) . . ? C54 C55 C50 118(2) . . ? N20 C20 N31 116.0(14) . 5_566 ? O20 C21 N20 127.0(18) . . ? O20 C21 N21 124.4(18) . . ? N20 C21 N21 108.6(16) . . ? N22 C22 N21 115.1(14) . . ? O21 C23 N22 126.3(16) . . ? O21 C23 N23 127.9(17) . . ? N22 C23 N23 105.7(13) . . ? N24 C24 N23 114.4(14) . . ? O22 C25 N25 124.7(16) . . ? O22 C25 N24 126.4(15) . . ? N25 C25 N24 108.9(14) . . ? N26 C26 N20 114.0(14) . . ? N26 C26 C27 103.6(13) . . ? N20 C26 C27 103.8(14) . . ? N27 C27 N21 116.5(14) . . ? N27 C27 C26 103.5(13) . . ? N21 C27 C26 102.2(13) . . ? N22 C28 N28 115.3(14) . . ? N22 C28 C29 105.0(13) . . ? N28 C28 C29 103.8(13) . . ? N23 C29 N29 114.0(14) . . ? N23 C29 C28 103.1(13) . . ? N29 C29 C28 104.4(13) . . ? N24 C30 N30 114.1(14) . . ? N24 C30 C31 103.3(13) . . ? N30 C30 C31 102.8(13) . . ? N31 C31 N25 119.2(15) . . ? N31 C31 C30 103.8(14) . . ? N25 C31 C30 103.1(13) . . ? N26 C32 N25 114.3(14) . 5_566 ? O23 C33 N26 128.0(16) . . ? O23 C33 N27 125.9(16) . . ? N26 C33 N27 106.1(14) . . ? N28 C34 N27 114.4(13) . . ? O24 C35 N28 123.9(16) . . ? O24 C35 N29 127.7(16) . . ? N28 C35 N29 108.4(16) . . ? N30 C36 N29 113.7(13) . . ? O25 C37 N30 124.8(16) . . ? O25 C37 N31 126.2(16) . . ? N30 C37 N31 109.0(15) . . ? C21 N20 C20 122.4(15) . . ? C21 N20 C26 112.4(15) . . ? C20 N20 C26 123.8(15) . . ? C21 N21 C27 112.7(15) . . ? C21 N21 C22 124.7(15) . . ? C27 N21 C22 121.8(14) . . ? C23 N22 C22 122.8(15) . . ? C23 N22 C28 111.7(14) . . ? C22 N22 C28 124.8(15) . . ? C23 N23 C29 114.3(14) . . ? C23 N23 C24 119.3(14) . . ? C29 N23 C24 125.6(14) . . ? C25 N24 C24 121.9(14) . . ? C25 N24 C30 111.6(14) . . ? C24 N24 C30 125.7(14) . . ? C25 N25 C31 113.0(14) . . ? C25 N25 C32 124.3(14) . 5_566 ? C31 N25 C32 122.2(14) . 5_566 ? C33 N26 C32 123.3(13) . . ? C33 N26 C26 112.8(14) . . ? C32 N26 C26 123.0(14) . . ? C33 N27 C27 113.8(14) . . ? C33 N27 C34 122.9(13) . . ? C27 N27 C34 122.5(15) . . ? C35 N28 C34 122.5(14) . . ? C35 N28 C28 111.4(14) . . ? C34 N28 C28 125.6(14) . . ? C35 N29 C29 111.9(14) . . ? C35 N29 C36 120.4(14) . . ? C29 N29 C36 126.6(14) . . ? C37 N30 C36 123.3(15) . . ? C37 N30 C30 110.7(14) . . ? C36 N30 C30 124.7(14) . . ? C37 N31 C31 113.3(14) . . ? C37 N31 C20 122.3(14) . 5_566 ? C31 N31 C20 124.4(14) . 5_566 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.920 _refine_diff_density_min -2.391 _refine_diff_density_rms 0.271 # Attachment 'B613790C_cif6_revised.cif' data_[W3S4Pd(H2O)9]2(pts)8+27H2O _database_code_depnum_ccdc_archive 'CCDC 621861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'H36 O18 Pd2 S8 W6, 8(C7 H7 O3 S), 19(H2 O)' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C56 H130 O61 Pd2 S16 W6' _chemical_formula_iupac ? _chemical_formula_weight 3608.46 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.7390(10) _cell_length_b 14.8360(10) _cell_length_c 33.410(2) _cell_angle_alpha 98.463(10) _cell_angle_beta 100.082(10) _cell_angle_gamma 101.608(10) _cell_volume 5510.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Least Squares Treatment of 25 SET4 setting angles. ; _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.115 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.175 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3492 _exptl_absorpt_coefficient_mu 6.952 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.704 _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD Bruker-Nonius Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 100861 _diffrn_reflns_av_R_equivalents 0.1192 _diffrn_reflns_av_sigmaI/netI 0.1515 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 0.63 _diffrn_reflns_theta_max 28.50 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measured_fraction_theta_full 0.932 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 26017 # number of observed reflections (> n sig(I)) _reflns_number_gt 16717 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR2002 (Altomare et al., 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Refinement on F^2 for ALL reflections except those 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 _refine_ls_weighting_details 'CALC W=1/[\S^2^(FO^2^)+(0.0772P)^2^+33.6050P] WHERE P=(FO^2^+2FC^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 26017 _refine_ls_number_parameters 1276 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1377 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.2181 _refine_ls_wR_factor_gt 0.1897 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.353 _refine_diff_density_min -5.186 _refine_diff_density_rms 0.675 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 W1 W 0.32517(6) 0.72989(4) -0.030089(19) 0.02423(16) Uani 1 1 d . . . W2 W 0.45302(6) 0.81515(4) 0.047197(18) 0.02328(16) Uani 1 1 d . . . W3 W 0.57071(6) 0.79336(4) -0.016180(18) 0.02291(16) Uani 1 1 d . . . Pd1 Pd 0.41635(11) 0.91921(8) -0.01927(4) 0.0272(3) Uani 1 1 d . . . S1 S 0.4665(4) 0.6706(3) 0.01076(11) 0.0249(9) Uani 1 1 d . . . S2 S 0.2743(4) 0.8446(3) 0.01528(12) 0.0291(9) Uani 1 1 d . . . S3 S 0.4332(4) 0.8051(3) -0.07401(11) 0.0289(9) Uani 1 1 d . . . S4 S 0.6058(4) 0.9294(3) 0.03432(11) 0.0254(9) Uani 1 1 d . . . O1 O 0.2904(10) 0.6010(7) -0.0763(3) 0.039(3) Uani 1 1 d . . . H1A H 0.3340 0.5884 -0.0932 0.058 Uiso 1 1 d R . . H1B H 0.2331 0.5534 -0.0797 0.058 Uiso 1 1 d R . . O2 O 0.1663(10) 0.7313(7) -0.0720(3) 0.035(3) Uani 1 1 d . . . H2A H 0.1191 0.6876 -0.0904 0.052 Uiso 1 1 d R . . H2B H 0.1320 0.7762 -0.0685 0.052 Uiso 1 1 d R . . O3 O 0.1920(9) 0.6311(7) -0.0120(3) 0.036(3) Uani 1 1 d . . . H3A H 0.1836 0.5783 -0.0045 0.054 Uiso 1 1 d R . . H3B H 0.1412 0.6581 -0.0034 0.054 Uiso 1 1 d R . . O4 O 0.4486(10) 0.9219(7) 0.0996(3) 0.034(3) Uani 1 1 d . . . H4A H 0.5121 0.9595 0.0982 0.051 Uiso 1 1 d R . . H4B H 0.4153 0.9507 0.1164 0.051 Uiso 1 1 d R . . O5 O 0.3480(10) 0.7302(7) 0.0812(3) 0.034(3) Uani 1 1 d . . . H5A H 0.3471 0.6731 0.0821 0.051 Uiso 1 1 d R . . H5B H 0.3022 0.7473 0.0964 0.051 Uiso 1 1 d R . . O6 O 0.5869(10) 0.7897(7) 0.0939(3) 0.031(3) Uani 1 1 d . . . H6A H 0.6032 0.7381 0.0982 0.047 Uiso 1 1 d R . . H6B H 0.6442 0.8338 0.1080 0.047 Uiso 1 1 d R . . O7 O 0.6290(9) 0.6852(7) -0.0520(3) 0.033(3) Uani 1 1 d . . . H7A H 0.5931 0.6287 -0.0624 0.049 Uiso 1 1 d R . . H7B H 0.6887 0.6988 -0.0630 0.049 Uiso 1 1 d R . . O8 O 0.7358(10) 0.7752(7) 0.0214(3) 0.033(3) Uani 1 1 d . . . H8A H 0.7607 0.7255 0.0222 0.049 Uiso 1 1 d R . . H8B H 0.7836 0.8187 0.0397 0.049 Uiso 1 1 d R . . O9 O 0.7033(10) 0.8709(7) -0.0426(3) 0.036(3) Uani 1 1 d . . . H9A H 0.6994 0.8994 -0.0629 0.055 Uiso 1 1 d R . . H9B H 0.7749 0.8864 -0.0290 0.055 Uiso 1 1 d R . . W4 W 0.92800(5) 0.33943(4) 0.555011(17) 0.01848(15) Uani 1 1 d . . . W5 W 0.79885(5) 0.24169(4) 0.478419(17) 0.01865(15) Uani 1 1 d . . . W6 W 1.04108(5) 0.28332(4) 0.494034(17) 0.01819(15) Uani 1 1 d . . . Pd2 Pd 0.90627(10) 0.42553(7) 0.48455(3) 0.0213(3) Uani 1 1 d . . . S5 S 0.7545(3) 0.3700(2) 0.51831(11) 0.0203(8) Uani 1 1 d . . . S6 S 0.9217(3) 0.1826(2) 0.52701(11) 0.0207(8) Uani 1 1 d . . . S7 S 0.9194(3) 0.3002(2) 0.43424(11) 0.0207(8) Uani 1 1 d . . . S8 S 1.0976(3) 0.4302(2) 0.53863(11) 0.0205(8) Uani 1 1 d . . . O10 O 0.9406(9) 0.4621(6) 0.6013(3) 0.024(2) Uani 1 1 d . . . H10A H 1.0049 0.5017 0.6134 0.036 Uiso 1 1 d R . . H10B H 0.8844 0.4905 0.6005 0.036 Uiso 1 1 d R . . O11 O 0.8188(9) 0.2780(7) 0.5942(3) 0.030(3) Uani 1 1 d . . . H11A H 0.8224 0.2358 0.6088 0.045 Uiso 1 1 d R . . H11B H 0.7515 0.2913 0.5934 0.045 Uiso 1 1 d R . . O12 O 1.0621(9) 0.3264(7) 0.6059(3) 0.028(3) Uani 1 1 d . . . H12A H 1.1302 0.3638 0.6136 0.041 Uiso 1 1 d R . . H12B H 1.0625 0.2815 0.6191 0.041 Uiso 1 1 d R . . O13 O 0.7738(9) 0.1053(6) 0.4403(3) 0.025(2) Uani 1 1 d . . . H13A H 0.7196 0.0889 0.4184 0.038 Uiso 1 1 d R . . H13B H 0.7970 0.0567 0.4454 0.038 Uiso 1 1 d R . . O14 O 0.6567(8) 0.2468(6) 0.4286(3) 0.022(2) Uani 1 1 d . . . H14A H 0.6642 0.2833 0.4113 0.033 Uiso 1 1 d R . . H14B H 0.5828 0.2283 0.4278 0.033 Uiso 1 1 d R . . O15 O 0.6482(9) 0.1527(6) 0.4924(3) 0.027(2) Uani 1 1 d . . . H15A H 0.6002 0.1730 0.5058 0.040 Uiso 1 1 d R . . H15B H 0.6258 0.0933 0.4867 0.040 Uiso 1 1 d R . . O16 O 1.0519(8) 0.1538(6) 0.4579(3) 0.022(2) Uani 1 1 d . . . H16A H 1.0328 0.1005 0.4645 0.033 Uiso 1 1 d R . . H16B H 1.0658 0.1451 0.4337 0.033 Uiso 1 1 d R . . O17 O 1.1923(8) 0.2496(6) 0.5304(3) 0.020(2) Uani 1 1 d . . . H17A H 1.2108 0.1990 0.5214 0.030 Uiso 1 1 d R . . H17B H 1.2409 0.2754 0.5531 0.030 Uiso 1 1 d R . . O18 O 1.1853(9) 0.3321(6) 0.4646(3) 0.027(2) Uani 1 1 d . . . H18A H 1.1817 0.3527 0.4421 0.040 Uiso 1 1 d R . . H18B H 1.2583 0.3385 0.4754 0.040 Uiso 1 1 d R . . S20 S 0.7377(4) 0.4359(2) 0.35711(11) 0.0250(9) Uani 1 1 d . . . O20 O 0.8575(9) 0.4209(7) 0.3590(3) 0.031(3) Uani 1 1 d . . . O21 O 0.7374(9) 0.5366(6) 0.3620(3) 0.024(2) Uani 1 1 d . . . O22 O 0.6721(9) 0.3899(7) 0.3850(3) 0.027(2) Uani 1 1 d . . . C21 C 0.6597(12) 0.3847(9) 0.3059(5) 0.021(3) Uani 1 1 d . . . C22 C 0.7143(17) 0.3919(11) 0.2733(5) 0.037(4) Uani 1 1 d . . . H22 H 0.7965 0.4217 0.2788 0.045 Uiso 1 1 calc R . . C23 C 0.6548(18) 0.3575(11) 0.2328(6) 0.045(5) Uani 1 1 d . . . H23 H 0.6958 0.3629 0.2108 0.054 Uiso 1 1 calc R . . C24 C 0.5346(15) 0.3151(10) 0.2246(5) 0.031(4) Uani 1 1 d . . . C25 C 0.4794(14) 0.3063(10) 0.2571(5) 0.034(4) Uani 1 1 d . . . H25 H 0.3982 0.2740 0.2517 0.040 Uiso 1 1 calc R . . C26 C 0.5381(15) 0.3427(10) 0.2971(5) 0.036(4) Uani 1 1 d . . . H26 H 0.4962 0.3395 0.3190 0.043 Uiso 1 1 calc R . . C27 C 0.4697(17) 0.2749(14) 0.1808(5) 0.053(5) Uani 1 1 d . . . H27A H 0.3840 0.2573 0.1798 0.079 Uiso 1 1 calc R . . H27B H 0.4969 0.2194 0.1705 0.079 Uiso 1 1 calc R . . H27C H 0.4856 0.3218 0.1634 0.079 Uiso 1 1 calc R . . S30 S 0.2600(4) 0.3830(3) 0.36707(12) 0.0280(9) Uani 1 1 d . . . O30 O 0.1830(10) 0.4050(7) 0.3957(3) 0.033(3) Uani 1 1 d . . . O31 O 0.2939(9) 0.2965(7) 0.3731(3) 0.030(3) Uani 1 1 d . . . O32 O 0.3608(10) 0.4593(7) 0.3693(3) 0.035(3) Uani 1 1 d . . . C31 C 0.1707(14) 0.3621(10) 0.3170(5) 0.032(4) Uani 1 1 d . . . C32 C 0.2214(16) 0.3784(13) 0.2836(5) 0.046(5) Uani 1 1 d . . . H32 H 0.3038 0.4069 0.2886 0.055 Uiso 1 1 calc R . . C33 C 0.1574(18) 0.3549(13) 0.2437(5) 0.050(5) Uani 1 1 d . . . H33 H 0.1954 0.3672 0.2216 0.060 Uiso 1 1 calc R . . C34 C 0.0380(15) 0.3133(11) 0.2357(5) 0.036(4) Uani 1 1 d . . . C35 C -0.0156(15) 0.2997(12) 0.2693(6) 0.043(5) Uani 1 1 d . . . H35 H -0.0993 0.2762 0.2645 0.052 Uiso 1 1 calc R . . C36 C 0.0512(15) 0.3199(10) 0.3099(5) 0.034(4) Uani 1 1 d . . . H36 H 0.0150 0.3048 0.3321 0.041 Uiso 1 1 calc R . . C37 C -0.0405(19) 0.2851(13) 0.1915(6) 0.061(6) Uani 1 1 d . . . H37A H -0.0243 0.2280 0.1772 0.092 Uiso 1 1 calc R . . H37B H -0.0224 0.3358 0.1762 0.092 Uiso 1 1 calc R . . H37C H -0.1246 0.2735 0.1932 0.092 Uiso 1 1 calc R . . S40 S 0.5135(4) 0.5505(3) 0.11533(12) 0.0298(9) Uani 1 1 d . . . O40 O 0.6135(10) 0.6224(7) 0.1114(3) 0.034(3) Uani 1 1 d . . . O41 O 0.3972(10) 0.5614(7) 0.0946(3) 0.033(3) Uani 1 1 d . . . O42 O 0.5311(10) 0.4560(7) 0.1010(4) 0.040(3) Uani 1 1 d . . . C41 C 0.5144(15) 0.5620(10) 0.1692(5) 0.031(4) Uani 1 1 d . . . C42 C 0.4124(17) 0.5279(14) 0.1824(6) 0.053(5) Uani 1 1 d . . . H42 H 0.3415 0.4954 0.1630 0.063 Uiso 1 1 calc R . . C43 C 0.4147(16) 0.5414(14) 0.2237(5) 0.045(5) Uani 1 1 d . . . H43 H 0.3424 0.5221 0.2325 0.055 Uiso 1 1 calc R . . C44 C 0.5163(16) 0.5816(12) 0.2533(5) 0.038(4) Uani 1 1 d . . . C45 C 0.6200(16) 0.6102(13) 0.2392(5) 0.044(5) Uani 1 1 d . . . H45 H 0.6923 0.6379 0.2588 0.053 Uiso 1 1 calc R . . C46 C 0.6202(16) 0.5994(14) 0.1980(6) 0.054(5) Uani 1 1 d . . . H46 H 0.6925 0.6173 0.1890 0.065 Uiso 1 1 calc R . . C47 C 0.5164(17) 0.5914(12) 0.2968(5) 0.047(5) Uani 1 1 d . . . H47A H 0.4636 0.5359 0.3018 0.071 Uiso 1 1 calc R . . H47B H 0.4883 0.6473 0.3059 0.071 Uiso 1 1 calc R . . H47C H 0.5974 0.5976 0.3124 0.071 Uiso 1 1 calc R . . S50 S 0.0181(4) 0.5149(3) 0.11413(13) 0.0348(10) Uani 1 1 d . . . O50 O 0.1231(11) 0.5771(8) 0.1073(4) 0.052(4) Uani 1 1 d . . . O51 O -0.0931(10) 0.5305(8) 0.0916(3) 0.039(3) Uani 1 1 d . . . O52 O 0.0210(10) 0.4162(8) 0.1057(3) 0.041(3) Uani 1 1 d . . . C51 C 0.0166(16) 0.5420(11) 0.1676(5) 0.032(4) Uani 1 1 d . . . C52 C -0.0904(18) 0.5258(14) 0.1810(6) 0.066(7) Uani 1 1 d . . . H52 H -0.1638 0.5030 0.1615 0.079 Uiso 1 1 calc R . . C53 C -0.0886(17) 0.5432(13) 0.2223(5) 0.045(5) Uani 1 1 d . . . H53 H -0.1621 0.5315 0.2310 0.054 Uiso 1 1 calc R . . C54 C 0.0172(16) 0.5777(10) 0.2526(5) 0.033(4) Uani 1 1 d . . . C55 C 0.1193(17) 0.5928(14) 0.2377(6) 0.055(6) Uani 1 1 d . . . H55 H 0.1932 0.6133 0.2570 0.067 Uiso 1 1 calc R . . C56 C 0.1206(16) 0.5796(13) 0.1954(5) 0.050(5) Uani 1 1 d . . . H56 H 0.1930 0.5967 0.1864 0.060 Uiso 1 1 calc R . . C57 C 0.0123(19) 0.5942(13) 0.2974(5) 0.056(6) Uani 1 1 d . . . H57A H 0.0810 0.6437 0.3129 0.084 Uiso 1 1 calc R . . H57B H 0.0137 0.5363 0.3081 0.084 Uiso 1 1 calc R . . H57C H -0.0612 0.6136 0.3007 0.084 Uiso 1 1 calc R . . S60 S 0.7418(4) 0.0065(3) 0.16108(13) 0.0388(11) Uani 1 1 d . . . O60 O 0.8565(12) 0.0315(12) 0.1504(4) 0.080(5) Uani 1 1 d . . . O61 O 0.6487(11) 0.0406(7) 0.1377(3) 0.044(3) Uani 1 1 d . . . O62 O 0.7015(12) -0.0956(8) 0.1602(3) 0.055(4) Uani 1 1 d . . . C61 C 0.7569(14) 0.0568(10) 0.2127(5) 0.033(4) Uani 1 1 d . . . C62 C 0.8493(14) 0.0388(10) 0.2421(5) 0.031(4) Uani 1 1 d . . . H62 H 0.9053 0.0061 0.2335 0.037 Uiso 1 1 calc R . . C63 C 0.8547(16) 0.0714(11) 0.2845(5) 0.040(5) Uani 1 1 d . . . H63 H 0.9157 0.0607 0.3047 0.048 Uiso 1 1 calc R . . C64 C 0.7732(17) 0.1184(10) 0.2971(5) 0.034(4) Uani 1 1 d . . . C65 C 0.6878(17) 0.1366(11) 0.2673(5) 0.039(5) Uani 1 1 d . . . H65 H 0.6342 0.1720 0.2757 0.047 Uiso 1 1 calc R . . C66 C 0.6785(14) 0.1053(11) 0.2261(5) 0.032(4) Uani 1 1 d . . . H66 H 0.6169 0.1171 0.2065 0.038 Uiso 1 1 calc R . . C67 C 0.7813(18) 0.1524(13) 0.3427(5) 0.051(5) Uani 1 1 d . . . H67A H 0.7533 0.2103 0.3464 0.077 Uiso 1 1 calc R . . H67B H 0.8642 0.1644 0.3575 0.077 Uiso 1 1 calc R . . H67C H 0.7318 0.1044 0.3535 0.077 Uiso 1 1 calc R . . S70 S 1.0453(4) 0.8773(3) 0.34607(12) 0.0278(9) Uani 1 1 d . . . O70 O 1.0471(10) 0.9788(7) 0.3573(3) 0.038(3) Uani 1 1 d . . . O71 O 1.1604(10) 0.8585(7) 0.3601(3) 0.034(3) Uani 1 1 d . . . O72 O 0.9482(10) 0.8200(7) 0.3597(3) 0.035(3) Uani 1 1 d . . . C71 C 1.0140(15) 0.8488(11) 0.2927(5) 0.036(2) Uani 1 1 d . . . C72 C 1.1059(16) 0.8592(11) 0.2692(5) 0.036(2) Uani 1 1 d . . . H72 H 1.1869 0.8811 0.2832 0.043 Uiso 1 1 calc R . . C73 C 1.0780(16) 0.8381(13) 0.2272(5) 0.042(5) Uani 1 1 d . . . H73 H 1.1398 0.8446 0.2121 0.050 Uiso 1 1 calc R . . C74 C 0.9583(18) 0.8066(11) 0.2054(5) 0.039(5) Uani 1 1 d . . . C75 C 0.8754(16) 0.7992(12) 0.2281(6) 0.048(5) Uani 1 1 d . . . H75 H 0.7945 0.7781 0.2140 0.058 Uiso 1 1 calc R . . C76 C 0.8986(15) 0.8195(10) 0.2697(5) 0.036(2) Uani 1 1 d . . . H76 H 0.8342 0.8135 0.2836 0.043 Uiso 1 1 calc R . . C77 C 0.9294(17) 0.7786(13) 0.1589(5) 0.049(5) Uani 1 1 d . . . H77A H 0.8850 0.8209 0.1469 0.073 Uiso 1 1 calc R . . H77B H 0.8811 0.7142 0.1508 0.073 Uiso 1 1 calc R . . H77C H 1.0034 0.7825 0.1488 0.073 Uiso 1 1 calc R . . S80 S 0.5619(4) 0.8748(3) 0.37630(13) 0.0303(10) Uani 1 1 d . . . O80 O 0.6744(9) 0.8477(7) 0.3863(3) 0.034(3) Uani 1 1 d . . . O81 O 0.5739(9) 0.9749(7) 0.3922(3) 0.035(3) Uani 1 1 d . . . O82 O 0.4680(9) 0.8158(7) 0.3895(3) 0.034(3) Uani 1 1 d . . . C81 C 0.5239(14) 0.8560(9) 0.3228(5) 0.025(4) Uani 1 1 d . . . C82 C 0.6059(17) 0.8800(12) 0.2996(5) 0.044(5) Uani 1 1 d . . . H82 H 0.6858 0.9081 0.3135 0.053 Uiso 1 1 calc R . . C83 C 0.5786(18) 0.8654(12) 0.2570(6) 0.049(5) Uani 1 1 d . . . H83 H 0.6387 0.8862 0.2426 0.058 Uiso 1 1 calc R . . C84 C 0.4645(19) 0.8209(12) 0.2349(6) 0.046(5) Uani 1 1 d . . . C85 C 0.3835(17) 0.7936(13) 0.2575(6) 0.047(5) Uani 1 1 d . . . H85 H 0.3062 0.7588 0.2433 0.057 Uiso 1 1 calc R . . C86 C 0.4083(14) 0.8142(10) 0.3007(5) 0.030(4) Uani 1 1 d . . . H86 H 0.3461 0.7997 0.3151 0.036 Uiso 1 1 calc R . . C87 C 0.432(2) 0.7994(15) 0.1879(5) 0.065(6) Uani 1 1 d . . . H87A H 0.3572 0.8178 0.1785 0.097 Uiso 1 1 calc R . . H87B H 0.4210 0.7321 0.1780 0.097 Uiso 1 1 calc R . . H87C H 0.4951 0.8344 0.1768 0.097 Uiso 1 1 calc R . . S90 S 0.1964(4) 0.0339(3) 0.12341(12) 0.0316(10) Uani 1 1 d . . . O90 O 0.1179(10) -0.0614(8) 0.1086(3) 0.041(3) Uani 1 1 d . . . O91 O 0.3072(10) 0.0412(7) 0.1085(3) 0.034(3) Uani 1 1 d . . . O92 O 0.1320(9) 0.1041(8) 0.1120(3) 0.038(3) Uani 1 1 d . . . C91 C 0.2350(14) 0.0510(10) 0.1768(5) 0.027(4) Uani 1 1 d . . . C92 C 0.1625(15) 0.0865(11) 0.1999(5) 0.035(4) Uani 1 1 d . . . H92 H 0.0924 0.1020 0.1868 0.042 Uiso 1 1 calc R . . C93 C 0.1948(18) 0.0997(11) 0.2446(5) 0.044(5) Uani 1 1 d . . . H93 H 0.1464 0.1258 0.2608 0.052 Uiso 1 1 calc R . . C94 C 0.2957(16) 0.0747(12) 0.2642(5) 0.038(4) Uani 1 1 d . . . C95 C 0.3619(17) 0.0383(11) 0.2395(5) 0.040(5) Uani 1 1 d . . . H95 H 0.4309 0.0210 0.2524 0.049 Uiso 1 1 calc R . . C96 C 0.3362(17) 0.0252(12) 0.1976(5) 0.042(5) Uani 1 1 d . . . H96 H 0.3860 -0.0013 0.1821 0.051 Uiso 1 1 calc R . . C97 C 0.3289(17) 0.0902(14) 0.3113(5) 0.056(5) Uani 1 1 d . . . H97A H 0.3368 0.1564 0.3229 0.083 Uiso 1 1 calc R . . H97B H 0.4046 0.0730 0.3198 0.083 Uiso 1 1 calc R . . H97C H 0.2665 0.0513 0.3215 0.083 Uiso 1 1 calc R . . O1W O 0.5351(9) 0.4624(7) 0.4400(3) 0.034(3) Uani 1 1 d . . . O2W O 0.4158(9) 0.3720(7) 0.5008(3) 0.032(3) Uani 1 1 d . . . O3W O 0.4757(9) 0.2051(7) 0.5266(3) 0.030(3) Uani 1 1 d . . . O4W O 0.4280(9) 0.2081(7) 0.4271(3) 0.033(3) Uani 1 1 d . . . O5W O 0.6412(9) 0.6656(7) 0.4067(3) 0.034(3) Uani 1 1 d . . . O6W O 0.3458(10) 0.0175(7) 0.4900(3) 0.033(3) Uani 1 1 d . . . O7W O 0.1415(9) 0.0609(7) 0.5115(3) 0.035(3) Uani 1 1 d . . . O8W O 0.8826(11) 0.9801(7) 0.4114(4) 0.043(3) Uani 1 1 d . . . O9W O 0.3134(10) 0.6380(8) 0.3660(4) 0.041(3) Uani 1 1 d . . . O10W O 0.3512(10) 0.0092(8) 0.4080(3) 0.036(3) Uani 1 1 d . . . O11W O 0.7438(11) 0.6146(8) 0.0483(4) 0.049(3) Uani 1 1 d . . . O12W O 0.8810(12) 0.9028(9) 0.0810(4) 0.061(4) Uani 1 1 d . . . O13W O 0.1200(12) 0.1578(8) 0.3899(4) 0.068(5) Uani 1 1 d . . . O14W O 0.2064(12) 0.4899(9) 0.0268(4) 0.074(5) Uani 1 1 d . . . O15W O 0.9025(12) 0.1164(9) 0.0856(4) 0.061(4) Uani 1 1 d . . . O16W O 0.0069(12) 0.3350(9) 0.0007(5) 0.073(5) Uani 1 1 d . . . O17W O 0.8844(12) 0.9878(10) 0.0080(5) 0.073(5) Uani 1 1 d . . . O18W O 0.1968(13) 0.2926(10) 0.0940(5) 0.072(5) Uani 1 1 d . . . O19W O 0.126(2) 0.7466(15) 0.0818(8) 0.036(9) Uani 0.51(4) 1 d P . . O20W O 0.188(2) 0.7787(18) 0.1154(11) 0.057(11) Uani 0.49(4) 1 d P . . 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 W1 0.0226(4) 0.0228(3) 0.0252(3) 0.0021(3) 0.0036(3) 0.0036(3) W2 0.0260(4) 0.0217(3) 0.0216(3) 0.0036(2) 0.0053(3) 0.0045(3) W3 0.0226(4) 0.0223(3) 0.0229(3) 0.0038(2) 0.0053(3) 0.0029(3) Pd1 0.0296(8) 0.0221(6) 0.0284(6) 0.0050(5) 0.0041(5) 0.0044(5) S1 0.027(2) 0.0214(19) 0.0250(19) 0.0038(15) 0.0059(17) 0.0029(17) S2 0.032(3) 0.028(2) 0.028(2) 0.0026(17) 0.0090(18) 0.0100(18) S3 0.031(2) 0.032(2) 0.0216(19) 0.0064(16) 0.0030(17) 0.0047(18) S4 0.028(2) 0.023(2) 0.0214(19) 0.0027(15) 0.0055(17) -0.0007(17) O1 0.038(8) 0.030(6) 0.041(7) -0.014(5) 0.007(6) 0.007(5) O2 0.037(7) 0.037(6) 0.031(6) 0.000(5) 0.005(5) 0.017(5) O3 0.027(7) 0.030(6) 0.047(7) 0.006(5) 0.007(6) -0.001(5) O4 0.048(8) 0.026(6) 0.026(6) -0.005(5) 0.017(5) 0.005(5) O5 0.043(8) 0.036(6) 0.026(6) 0.007(5) 0.016(5) 0.006(5) O6 0.043(7) 0.021(5) 0.028(6) -0.001(4) 0.008(5) 0.007(5) O7 0.025(7) 0.033(6) 0.041(7) 0.002(5) 0.011(5) 0.009(5) O8 0.044(8) 0.034(6) 0.022(5) 0.004(5) 0.006(5) 0.012(5) O9 0.036(7) 0.042(7) 0.031(6) 0.015(5) 0.010(5) 0.000(5) W4 0.0188(3) 0.0171(3) 0.0194(3) 0.0033(2) 0.0041(2) 0.0040(2) W5 0.0166(3) 0.0167(3) 0.0218(3) 0.0031(2) 0.0031(2) 0.0032(2) W6 0.0165(3) 0.0167(3) 0.0211(3) 0.0029(2) 0.0038(2) 0.0037(2) Pd2 0.0209(7) 0.0178(6) 0.0248(6) 0.0049(5) 0.0037(5) 0.0039(5) S5 0.020(2) 0.0191(18) 0.0227(18) 0.0033(14) 0.0058(16) 0.0065(15) S6 0.025(2) 0.0146(17) 0.0217(18) 0.0038(14) 0.0009(16) 0.0059(15) S7 0.019(2) 0.0221(19) 0.0189(18) 0.0029(14) 0.0019(15) 0.0034(16) S8 0.017(2) 0.0178(18) 0.0257(19) 0.0055(15) 0.0040(16) 0.0003(15) O10 0.016(6) 0.018(5) 0.039(6) 0.007(4) 0.007(5) 0.006(4) O11 0.035(7) 0.026(6) 0.036(6) 0.022(5) 0.010(5) 0.011(5) O12 0.028(6) 0.026(6) 0.025(5) 0.017(4) -0.005(5) -0.003(5) O13 0.020(6) 0.026(6) 0.027(6) 0.008(4) -0.002(5) 0.005(5) O14 0.011(5) 0.030(6) 0.028(5) 0.010(4) 0.000(4) 0.008(4) O15 0.020(6) 0.018(5) 0.042(6) 0.001(5) 0.014(5) -0.001(4) O16 0.023(6) 0.014(5) 0.027(5) -0.003(4) 0.008(5) -0.001(4) O17 0.015(6) 0.027(5) 0.022(5) 0.001(4) 0.002(4) 0.015(4) O18 0.022(6) 0.033(6) 0.022(5) 0.005(4) 0.004(5) 0.000(5) S20 0.030(2) 0.0208(19) 0.0228(19) 0.0021(15) 0.0029(17) 0.0050(17) O20 0.023(7) 0.034(6) 0.031(6) -0.003(5) 0.002(5) 0.003(5) O21 0.024(6) 0.017(5) 0.029(6) 0.001(4) 0.003(5) 0.006(4) O22 0.023(6) 0.033(6) 0.022(5) 0.008(4) -0.005(5) 0.009(5) C21 0.009(8) 0.017(7) 0.035(9) 0.001(6) 0.001(7) 0.006(6) C22 0.042(12) 0.041(10) 0.031(9) 0.004(8) 0.016(9) 0.012(9) C23 0.057(14) 0.028(9) 0.045(11) 0.002(8) 0.005(10) 0.011(9) C24 0.035(11) 0.027(9) 0.026(8) -0.003(7) -0.005(8) 0.011(8) C25 0.018(9) 0.025(9) 0.050(11) 0.001(8) -0.007(8) 0.004(7) C26 0.035(11) 0.029(9) 0.034(9) 0.003(7) -0.005(8) 0.001(8) C27 0.052(14) 0.074(14) 0.024(9) 0.011(9) 0.003(9) -0.002(11) S30 0.031(2) 0.027(2) 0.030(2) 0.0075(17) 0.0097(18) 0.0115(18) O30 0.041(7) 0.037(6) 0.030(6) 0.011(5) 0.017(5) 0.018(5) O31 0.026(6) 0.024(6) 0.041(6) 0.010(5) 0.002(5) 0.008(5) O32 0.038(7) 0.024(6) 0.039(6) 0.007(5) 0.000(6) 0.006(5) C31 0.020(9) 0.017(8) 0.054(11) 0.012(7) -0.006(8) -0.001(7) C32 0.024(10) 0.065(13) 0.037(10) 0.000(9) 0.015(8) -0.014(9) C33 0.060(15) 0.061(13) 0.028(10) 0.008(9) 0.012(10) 0.011(11) C34 0.027(10) 0.038(10) 0.039(10) 0.006(8) -0.008(8) 0.012(8) C35 0.015(9) 0.048(11) 0.062(13) 0.013(10) -0.009(9) 0.009(8) C36 0.027(10) 0.030(9) 0.045(10) 0.005(8) 0.010(8) 0.004(8) C37 0.076(17) 0.048(12) 0.057(13) 0.007(10) 0.014(12) 0.010(11) S40 0.030(3) 0.027(2) 0.033(2) 0.0038(17) 0.0109(19) 0.0052(18) O40 0.034(7) 0.019(5) 0.051(7) 0.007(5) 0.015(6) 0.009(5) O41 0.031(7) 0.027(6) 0.039(6) 0.011(5) 0.003(5) 0.003(5) O42 0.029(7) 0.027(6) 0.058(8) -0.009(5) 0.006(6) 0.004(5) C41 0.029(10) 0.022(8) 0.039(9) 0.008(7) 0.006(8) 0.002(7) C42 0.034(12) 0.065(13) 0.053(12) 0.006(10) 0.002(10) 0.005(10) C43 0.028(11) 0.083(14) 0.022(9) 0.016(9) 0.003(8) 0.003(10) C44 0.041(12) 0.041(10) 0.034(10) 0.005(8) 0.006(9) 0.021(9) C45 0.027(11) 0.066(13) 0.034(10) 0.003(9) -0.004(8) 0.011(9) C46 0.016(10) 0.068(14) 0.066(14) 0.002(11) -0.001(10) -0.001(9) C47 0.054(14) 0.050(11) 0.043(11) 0.015(9) 0.024(10) 0.006(10) S50 0.030(3) 0.037(2) 0.035(2) 0.0084(19) 0.006(2) 0.001(2) O50 0.033(8) 0.053(8) 0.069(9) 0.010(7) 0.021(7) -0.002(6) O51 0.024(7) 0.042(7) 0.047(7) 0.009(6) -0.005(6) 0.005(5) O52 0.027(7) 0.045(7) 0.043(7) -0.001(6) 0.007(6) 0.000(6) C51 0.039(11) 0.027(9) 0.031(9) 0.003(7) 0.003(8) 0.013(8) C52 0.040(13) 0.074(15) 0.062(14) 0.009(12) 0.003(11) -0.027(11) C53 0.036(12) 0.070(13) 0.025(9) 0.011(9) 0.005(8) 0.004(10) C54 0.041(12) 0.020(8) 0.040(10) 0.006(7) 0.002(9) 0.013(8) C55 0.029(12) 0.071(14) 0.045(12) -0.009(10) -0.008(9) -0.010(10) C56 0.022(11) 0.071(13) 0.042(11) -0.009(10) 0.007(9) -0.007(9) C57 0.075(16) 0.055(12) 0.037(11) 0.024(9) 0.001(10) 0.013(11) S60 0.036(3) 0.046(3) 0.027(2) -0.0040(19) 0.005(2) 0.004(2) O60 0.040(9) 0.138(14) 0.030(7) -0.014(8) 0.005(7) -0.025(9) O61 0.061(9) 0.031(6) 0.029(6) 0.005(5) -0.010(6) 0.000(6) O62 0.076(10) 0.033(7) 0.035(7) -0.004(5) -0.023(7) 0.002(7) C61 0.023(10) 0.023(8) 0.042(10) -0.005(7) 0.001(8) -0.002(7) C62 0.018(9) 0.028(9) 0.040(10) -0.002(7) -0.006(7) 0.006(7) C63 0.047(12) 0.033(10) 0.034(10) 0.016(8) -0.006(9) 0.003(9) C64 0.055(13) 0.020(8) 0.026(9) -0.001(7) 0.010(9) 0.003(8) C65 0.054(13) 0.029(9) 0.033(10) -0.007(7) 0.022(9) 0.003(9) C66 0.022(9) 0.043(10) 0.035(9) 0.010(8) 0.008(8) 0.015(8) C67 0.067(15) 0.050(12) 0.035(10) 0.003(9) 0.022(10) 0.004(10) S70 0.027(2) 0.022(2) 0.035(2) 0.0066(17) 0.0052(18) 0.0065(17) O70 0.044(8) 0.022(6) 0.045(7) -0.001(5) 0.017(6) 0.000(5) O71 0.026(7) 0.038(6) 0.038(6) 0.013(5) 0.000(5) 0.007(5) O72 0.040(7) 0.027(6) 0.046(7) 0.020(5) 0.015(6) 0.011(5) C71 0.031(6) 0.027(5) 0.053(7) 0.014(5) 0.007(5) 0.010(5) C72 0.031(6) 0.027(5) 0.053(7) 0.014(5) 0.007(5) 0.010(5) C73 0.023(10) 0.067(13) 0.038(10) 0.007(9) 0.006(8) 0.017(9) C74 0.059(14) 0.039(10) 0.041(10) 0.022(8) 0.033(10) 0.029(9) C75 0.029(11) 0.040(11) 0.062(13) 0.016(9) -0.009(10) -0.013(9) C76 0.031(6) 0.027(5) 0.053(7) 0.014(5) 0.007(5) 0.010(5) C77 0.040(12) 0.065(13) 0.036(10) 0.008(9) -0.003(9) 0.012(10) S80 0.028(2) 0.023(2) 0.038(2) 0.0052(17) 0.0081(19) 0.0024(18) O80 0.025(7) 0.025(6) 0.052(7) 0.012(5) 0.003(6) 0.008(5) O81 0.025(7) 0.029(6) 0.042(7) -0.005(5) -0.003(5) 0.003(5) O82 0.014(6) 0.042(7) 0.040(6) 0.009(5) 0.007(5) -0.007(5) C81 0.023(9) 0.016(7) 0.043(9) 0.001(7) 0.016(8) 0.013(7) C82 0.038(12) 0.046(11) 0.043(11) -0.010(9) 0.015(9) 0.007(9) C83 0.053(14) 0.043(11) 0.054(12) 0.007(9) 0.030(11) 0.005(10) C84 0.071(15) 0.035(10) 0.044(11) 0.003(8) 0.042(11) 0.015(10) C85 0.033(12) 0.059(13) 0.047(12) 0.000(10) 0.007(9) 0.014(9) C86 0.013(9) 0.035(9) 0.042(10) 0.008(8) 0.003(7) 0.003(7) C87 0.084(18) 0.084(16) 0.039(11) 0.026(11) 0.030(12) 0.027(13) S90 0.023(2) 0.042(2) 0.029(2) 0.0079(18) 0.0064(18) 0.0053(19) O90 0.035(7) 0.042(7) 0.037(7) -0.003(5) 0.008(6) -0.001(6) O91 0.034(7) 0.033(6) 0.039(6) 0.012(5) 0.010(6) 0.009(5) O92 0.020(7) 0.055(8) 0.042(7) 0.017(6) 0.007(5) 0.011(6) C91 0.028(10) 0.028(8) 0.032(9) 0.009(7) 0.020(8) 0.011(7) C92 0.031(10) 0.035(10) 0.046(10) 0.011(8) 0.014(8) 0.013(8) C93 0.072(15) 0.033(10) 0.037(10) 0.009(8) 0.027(10) 0.021(10) C94 0.036(11) 0.038(10) 0.041(10) 0.014(8) 0.006(9) 0.006(9) C95 0.061(13) 0.031(9) 0.031(9) 0.019(7) 0.000(9) 0.011(9) C96 0.045(12) 0.041(10) 0.037(10) 0.001(8) 0.012(9) 0.002(9) C97 0.043(13) 0.073(14) 0.045(12) 0.005(10) 0.003(10) 0.013(11) O1W 0.027(7) 0.035(6) 0.040(7) 0.005(5) 0.004(5) 0.008(5) O2W 0.029(7) 0.034(6) 0.031(6) 0.006(5) 0.005(5) 0.005(5) O3W 0.027(7) 0.025(6) 0.040(6) 0.000(5) 0.014(5) 0.008(5) O4W 0.016(6) 0.045(7) 0.039(6) 0.016(5) 0.004(5) 0.009(5) O5W 0.023(7) 0.043(7) 0.031(6) 0.001(5) 0.000(5) 0.009(5) O6W 0.034(7) 0.024(6) 0.047(7) 0.012(5) 0.016(6) 0.013(5) O7W 0.028(7) 0.025(6) 0.051(7) 0.002(5) -0.001(6) 0.015(5) O8W 0.046(8) 0.033(7) 0.053(8) 0.009(6) 0.015(6) 0.012(6) O9W 0.026(7) 0.043(7) 0.058(8) 0.014(6) 0.020(6) 0.006(5) O10W 0.033(7) 0.046(7) 0.034(6) 0.012(5) 0.011(5) 0.017(6) O11W 0.059(9) 0.033(7) 0.066(9) 0.020(6) 0.021(7) 0.023(6) O12W 0.060(10) 0.055(8) 0.048(8) -0.016(7) -0.015(7) 0.007(7) O13W 0.077(11) 0.044(8) 0.061(9) -0.029(6) 0.045(8) -0.035(7) O14W 0.058(10) 0.050(8) 0.088(11) 0.033(8) -0.048(8) -0.005(7) O15W 0.050(9) 0.046(8) 0.081(10) 0.022(7) -0.012(8) 0.012(7) O16W 0.038(9) 0.048(8) 0.143(15) 0.009(9) 0.048(9) 0.018(7) O17W 0.037(9) 0.088(11) 0.075(10) -0.005(8) 0.007(8) -0.006(8) O18W 0.057(10) 0.075(10) 0.113(13) 0.042(9) 0.053(10) 0.035(8) O19W 0.041(18) 0.021(13) 0.06(2) 0.009(12) 0.027(15) 0.022(11) O20W 0.030(17) 0.044(16) 0.08(3) -0.013(15) 0.001(16) -0.013(13) _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 W1 O2 2.133(11) . ? W1 O3 2.150(10) . ? W1 O1 2.192(9) . ? W1 S2 2.349(4) . ? W1 S1 2.353(4) . ? W1 S3 2.360(4) . ? W1 W2 2.7271(9) . ? W1 Pd1 2.7424(13) . ? W1 W3 2.7786(9) . ? W2 O6 2.146(11) . ? W2 O5 2.165(10) . ? W2 O4 2.197(9) . ? W2 S2 2.335(4) . ? W2 S4 2.353(4) . ? W2 S1 2.354(4) . ? W2 W3 2.7384(9) . ? W2 Pd1 2.9054(13) . ? W3 O9 2.141(10) . ? W3 O7 2.153(10) . ? W3 O8 2.205(11) . ? W3 S3 2.343(4) . ? W3 S4 2.348(4) . ? W3 S1 2.366(4) . ? W3 Pd1 2.8519(15) . ? Pd1 S3 2.366(4) . ? Pd1 S2 2.376(4) . ? Pd1 S4 2.426(4) 2_675 ? Pd1 S4 2.562(4) . ? Pd1 Pd1 2.752(2) 2_675 ? S4 Pd1 2.426(4) 2_675 ? W4 O11 2.158(10) . ? W4 O12 2.166(9) . ? W4 O10 2.170(9) . ? W4 S5 2.348(4) . ? W4 S6 2.358(3) . ? W4 S8 2.366(4) . ? W4 W6 2.7382(8) . ? W4 W5 2.7594(9) . ? W4 Pd2 2.8362(12) . ? W5 O15 2.150(9) . ? W5 O14 2.163(9) . ? W5 O13 2.163(9) . ? W5 S7 2.356(4) . ? W5 S5 2.359(4) . ? W5 S6 2.365(4) . ? W5 W6 2.7237(9) . ? W5 Pd2 2.7262(12) . ? W6 O16 2.152(9) . ? W6 O18 2.158(9) . ? W6 O17 2.158(9) . ? W6 S7 2.321(4) . ? W6 S8 2.351(3) . ? W6 S6 2.365(4) . ? W6 Pd2 2.9019(13) . ? Pd2 S5 2.347(4) . ? Pd2 S7 2.365(4) . ? Pd2 S8 2.387(4) 2_766 ? Pd2 S8 2.607(4) . ? Pd2 Pd2 2.714(2) 2_766 ? S8 Pd2 2.387(4) 2_766 ? S20 O20 1.459(11) . ? S20 O22 1.468(11) . ? S20 O21 1.479(10) . ? S20 C21 1.771(15) . ? C21 C22 1.36(2) . ? C21 C26 1.40(2) . ? C22 C23 1.38(2) . ? C23 C24 1.39(2) . ? C24 C25 1.37(2) . ? C24 C27 1.50(2) . ? C25 C26 1.37(2) . ? S30 O32 1.446(11) . ? S30 O31 1.449(10) . ? S30 O30 1.474(11) . ? S30 C31 1.759(16) . ? C31 C32 1.38(2) . ? C31 C36 1.38(2) . ? C32 C33 1.37(2) . ? C33 C34 1.37(2) . ? C34 C35 1.40(2) . ? C34 C37 1.54(2) . ? C35 C36 1.40(2) . ? S40 O40 1.458(11) . ? S40 O41 1.469(12) . ? S40 O42 1.480(11) . ? S40 C41 1.779(16) . ? C41 C42 1.38(2) . ? C41 C46 1.39(2) . ? C42 C43 1.36(2) . ? C43 C44 1.37(2) . ? C44 C45 1.39(2) . ? C44 C47 1.44(2) . ? C45 C46 1.36(3) . ? S50 O50 1.458(12) . ? S50 O52 1.459(12) . ? S50 O51 1.468(12) . ? S50 C51 1.776(16) . ? C51 C56 1.36(2) . ? C51 C52 1.39(3) . ? C52 C53 1.36(2) . ? C53 C54 1.41(2) . ? C54 C55 1.37(2) . ? C54 C57 1.50(2) . ? C55 C56 1.40(2) . ? S60 O60 1.444(14) . ? S60 O61 1.448(13) . ? S60 O62 1.488(12) . ? S60 C61 1.737(16) . ? C61 C66 1.37(2) . ? C61 C62 1.43(2) . ? C62 C63 1.41(2) . ? C63 C64 1.38(2) . ? C64 C65 1.38(2) . ? C64 C67 1.51(2) . ? C65 C66 1.36(2) . ? S70 O71 1.446(11) . ? S70 O72 1.461(11) . ? S70 O70 1.493(11) . ? S70 C71 1.725(18) . ? C71 C76 1.38(2) . ? C71 C72 1.44(2) . ? C72 C73 1.36(2) . ? C73 C74 1.41(2) . ? C74 C75 1.33(2) . ? C74 C77 1.51(2) . ? C75 C76 1.34(2) . ? S80 O82 1.439(10) . ? S80 O80 1.454(11) . ? S80 O81 1.471(11) . ? S80 C81 1.731(16) . ? C81 C82 1.36(2) . ? C81 C86 1.40(2) . ? C82 C83 1.38(2) . ? C83 C84 1.39(3) . ? C84 C85 1.35(2) . ? C84 C87 1.52(2) . ? C85 C86 1.40(2) . ? S90 O92 1.460(12) . ? S90 O91 1.463(11) . ? S90 O90 1.484(11) . ? S90 C91 1.729(16) . ? C91 C92 1.37(2) . ? C91 C96 1.42(2) . ? C92 C93 1.45(2) . ? C93 C94 1.40(2) . ? C94 C95 1.36(2) . ? C94 C97 1.52(2) . ? C95 C96 1.36(2) . ? O19W O20W 1.20(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W1 O3 77.3(4) . . ? O2 W1 O1 75.4(4) . . ? O3 W1 O1 74.7(4) . . ? O2 W1 S2 85.9(3) . . ? O3 W1 S2 85.8(3) . . ? O1 W1 S2 155.4(3) . . ? O2 W1 S1 159.2(3) . . ? O3 W1 S1 86.6(3) . . ? O1 W1 S1 87.9(3) . . ? S2 W1 S1 106.15(14) . . ? O2 W1 S3 87.8(3) . . ? O3 W1 S3 158.7(3) . . ? O1 W1 S3 87.0(3) . . ? S2 W1 S3 108.44(14) . . ? S1 W1 S3 103.75(14) . . ? O2 W1 W2 140.0(3) . . ? O3 W1 W2 97.9(3) . . ? O1 W1 W2 142.4(3) . . ? S2 W1 W2 54.16(10) . . ? S1 W1 W2 54.62(9) . . ? S3 W1 W2 103.23(10) . . ? O2 W1 Pd1 94.3(3) . . ? O3 W1 Pd1 140.6(3) . . ? O1 W1 Pd1 140.9(3) . . ? S2 W1 Pd1 54.98(10) . . ? S1 W1 Pd1 106.47(9) . . ? S3 W1 Pd1 54.64(10) . . ? W2 W1 Pd1 64.17(3) . . ? O2 W1 W3 141.1(3) . . ? O3 W1 W3 140.6(3) . . ? O1 W1 W3 102.8(3) . . ? S2 W1 W3 101.77(11) . . ? S1 W1 W3 54.14(9) . . ? S3 W1 W3 53.50(10) . . ? W2 W1 W3 59.64(2) . . ? Pd1 W1 W3 62.20(3) . . ? O6 W2 O5 77.6(4) . . ? O6 W2 O4 80.0(4) . . ? O5 W2 O4 79.2(4) . . ? O6 W2 S2 160.3(3) . . ? O5 W2 S2 86.4(3) . . ? O4 W2 S2 85.8(3) . . ? O6 W2 S4 86.4(3) . . ? O5 W2 S4 159.6(3) . . ? O4 W2 S4 85.6(3) . . ? S2 W2 S4 106.21(14) . . ? O6 W2 S1 83.6(3) . . ? O5 W2 S1 84.7(3) . . ? O4 W2 S1 159.1(3) . . ? S2 W2 S1 106.56(14) . . ? S4 W2 S1 106.22(13) . . ? O6 W2 W1 138.2(3) . . ? O5 W2 W1 96.9(3) . . ? O4 W2 W1 140.4(3) . . ? S2 W2 W1 54.63(9) . . ? S4 W2 W1 103.47(9) . . ? S1 W2 W1 54.57(10) . . ? O6 W2 W3 96.3(3) . . ? O5 W2 W3 139.4(3) . . ? O4 W2 W3 139.9(3) . . ? S2 W2 W3 103.33(10) . . ? S4 W2 W3 54.28(9) . . ? S1 W2 W3 54.73(9) . . ? W1 W2 W3 61.11(2) . . ? O6 W2 Pd1 143.3(3) . . ? O5 W2 Pd1 138.7(3) . . ? O4 W2 Pd1 99.4(3) . . ? S2 W2 Pd1 52.56(10) . . ? S4 W2 Pd1 57.16(10) . . ? S1 W2 Pd1 101.52(10) . . ? W1 W2 Pd1 58.17(3) . . ? W3 W2 Pd1 60.62(3) . . ? O9 W3 O7 76.9(4) . . ? O9 W3 O8 78.5(4) . . ? O7 W3 O8 72.6(4) . . ? O9 W3 S3 86.2(3) . . ? O7 W3 S3 91.7(3) . . ? O8 W3 S3 160.0(3) . . ? O9 W3 S4 86.3(3) . . ? O7 W3 S4 152.5(3) . . ? O8 W3 S4 82.9(3) . . ? S3 W3 S4 108.93(14) . . ? O9 W3 S1 160.1(3) . . ? O7 W3 S1 85.6(3) . . ? O8 W3 S1 87.5(3) . . ? S3 W3 S1 103.88(14) . . ? S4 W3 S1 106.02(13) . . ? O9 W3 W2 140.7(3) . . ? O7 W3 W2 139.4(3) . . ? O8 W3 W2 96.6(3) . . ? S3 W3 W2 103.35(11) . . ? S4 W3 W2 54.46(9) . . ? S1 W3 W2 54.35(9) . . ? O9 W3 W1 140.0(3) . . ? O7 W3 W1 104.8(3) . . ? O8 W3 W1 140.9(3) . . ? S3 W3 W1 54.06(10) . . ? S4 W3 W1 102.08(10) . . ? S1 W3 W1 53.71(10) . . ? W2 W3 W1 59.24(2) . . ? O9 W3 Pd1 97.0(3) . . ? O7 W3 Pd1 144.8(3) . . ? O8 W3 Pd1 141.0(3) . . ? S3 W3 Pd1 53.10(10) . . ? S4 W3 Pd1 58.08(11) . . ? S1 W3 Pd1 102.79(10) . . ? W2 W3 Pd1 62.59(3) . . ? W1 W3 Pd1 58.28(3) . . ? S3 Pd1 S2 107.33(14) . . ? S3 Pd1 S4 118.03(14) . 2_675 ? S2 Pd1 S4 115.65(15) . 2_675 ? S3 Pd1 S4 101.45(14) . . ? S2 Pd1 S4 98.73(14) . . ? S4 Pd1 S4 113.09(11) 2_675 . ? S3 Pd1 W1 54.42(10) . . ? S2 Pd1 W1 54.07(9) . . ? S4 Pd1 W1 149.12(11) 2_675 . ? S4 Pd1 W1 97.68(9) . . ? S3 Pd1 Pd1 126.80(12) . 2_675 ? S2 Pd1 Pd1 121.53(11) . 2_675 ? S4 Pd1 Pd1 58.91(10) 2_675 2_675 ? S4 Pd1 Pd1 54.18(9) . 2_675 ? W1 Pd1 Pd1 151.77(8) . 2_675 ? S3 Pd1 W3 52.36(10) . . ? S2 Pd1 W3 99.02(11) . . ? S4 Pd1 W3 144.60(11) 2_675 . ? S4 Pd1 W3 51.05(9) . . ? W1 Pd1 W3 59.52(3) . . ? Pd1 Pd1 W3 97.66(6) 2_675 . ? S3 Pd1 W2 97.99(10) . . ? S2 Pd1 W2 51.30(11) . . ? S4 Pd1 W2 143.70(10) 2_675 . ? S4 Pd1 W2 50.50(8) . . ? W1 Pd1 W2 57.66(3) . . ? Pd1 Pd1 W2 96.79(6) 2_675 . ? W3 Pd1 W2 56.79(3) . . ? W1 S1 W2 70.80(11) . . ? W1 S1 W3 72.15(11) . . ? W2 S1 W3 70.92(10) . . ? W2 S2 W1 71.20(12) . . ? W2 S2 Pd1 76.14(13) . . ? W1 S2 Pd1 70.95(12) . . ? W3 S3 W1 72.43(11) . . ? W3 S3 Pd1 74.54(11) . . ? W1 S3 Pd1 70.94(11) . . ? W3 S4 W2 71.27(10) . . ? W3 S4 Pd1 124.21(16) . 2_675 ? W2 S4 Pd1 124.62(18) . 2_675 ? W3 S4 Pd1 70.87(10) . . ? W2 S4 Pd1 72.34(11) . . ? Pd1 S4 Pd1 66.91(11) 2_675 . ? O11 W4 O12 78.7(4) . . ? O11 W4 O10 79.6(4) . . ? O12 W4 O10 77.0(4) . . ? O11 W4 S5 86.9(3) . . ? O12 W4 S5 160.9(3) . . ? O10 W4 S5 88.1(3) . . ? O11 W4 S6 84.3(3) . . ? O12 W4 S6 86.5(3) . . ? O10 W4 S6 158.8(3) . . ? S5 W4 S6 104.74(13) . . ? O11 W4 S8 156.9(3) . . ? O12 W4 S8 81.0(3) . . ? O10 W4 S8 85.0(3) . . ? S5 W4 S8 109.91(13) . . ? S6 W4 S8 105.60(13) . . ? O11 W4 W6 138.9(3) . . ? O12 W4 W6 95.6(3) . . ? O10 W4 W6 139.3(2) . . ? S5 W4 W6 103.49(9) . . ? S6 W4 W6 54.69(9) . . ? S8 W4 W6 54.25(9) . . ? O11 W4 W5 99.9(3) . . ? O12 W4 W5 140.5(3) . . ? O10 W4 W5 142.2(3) . . ? S5 W4 W5 54.28(9) . . ? S6 W4 W5 54.36(9) . . ? S8 W4 W5 102.77(9) . . ? W6 W4 W5 59.40(2) . . ? O11 W4 Pd2 139.7(3) . . ? O12 W4 Pd2 140.4(3) . . ? O10 W4 Pd2 97.7(2) . . ? S5 W4 Pd2 52.83(9) . . ? S6 W4 Pd2 103.44(9) . . ? S8 W4 Pd2 59.32(9) . . ? W6 W4 Pd2 62.71(3) . . ? W5 W4 Pd2 58.29(3) . . ? O15 W5 O14 78.2(4) . . ? O15 W5 O13 73.5(4) . . ? O14 W5 O13 79.6(4) . . ? O15 W5 S7 154.6(3) . . ? O14 W5 S7 82.8(3) . . ? O13 W5 S7 86.6(3) . . ? O15 W5 S5 88.2(3) . . ? O14 W5 S5 88.5(3) . . ? O13 W5 S5 159.9(3) . . ? S7 W5 S5 108.08(12) . . ? O15 W5 S6 87.8(3) . . ? O14 W5 S6 160.8(3) . . ? O13 W5 S6 83.9(3) . . ? S7 W5 S6 106.12(13) . . ? S5 W5 S6 104.21(13) . . ? O15 W5 W6 142.4(3) . . ? O14 W5 W6 136.5(3) . . ? O13 W5 W6 96.1(3) . . ? S7 W5 W6 53.78(9) . . ? S5 W5 W6 103.65(9) . . ? S6 W5 W6 54.85(9) . . ? O15 W5 Pd2 142.0(3) . . ? O14 W5 Pd2 92.4(2) . . ? O13 W5 Pd2 141.5(3) . . ? S7 W5 Pd2 54.88(9) . . ? S5 W5 Pd2 54.41(9) . . ? S6 W5 Pd2 106.62(9) . . ? W6 W5 Pd2 64.35(3) . . ? O15 W5 W4 103.8(3) . . ? O14 W5 W4 142.0(2) . . ? O13 W5 W4 138.0(3) . . ? S7 W5 W4 101.58(9) . . ? S5 W5 W4 53.94(9) . . ? S6 W5 W4 54.13(8) . . ? W6 W5 W4 59.92(2) . . ? Pd2 W5 W4 62.26(3) . . ? O16 W6 O18 79.1(3) . . ? O16 W6 O17 77.2(4) . . ? O18 W6 O17 76.3(4) . . ? O16 W6 S7 85.3(3) . . ? O18 W6 S7 84.9(3) . . ? O17 W6 S7 156.3(3) . . ? O16 W6 S8 161.0(3) . . ? O18 W6 S8 87.5(3) . . ? O17 W6 S8 86.6(3) . . ? S7 W6 S8 107.00(13) . . ? O16 W6 S6 83.4(3) . . ? O18 W6 S6 157.8(3) . . ? O17 W6 S6 86.7(3) . . ? S7 W6 S6 107.25(13) . . ? S8 W6 S6 105.85(12) . . ? O16 W6 W5 94.7(3) . . ? O18 W6 W5 139.8(3) . . ? O17 W6 W5 141.5(2) . . ? S7 W6 W5 54.98(9) . . ? S8 W6 W5 104.25(10) . . ? S6 W6 W5 54.83(9) . . ? O16 W6 W4 137.7(2) . . ? O18 W6 W4 142.2(2) . . ? O17 W6 W4 100.5(2) . . ? S7 W6 W4 103.14(10) . . ? S8 W6 W4 54.77(9) . . ? S6 W6 W4 54.44(9) . . ? W5 W6 W4 60.69(2) . . ? O16 W6 Pd2 137.2(3) . . ? O18 W6 Pd2 100.8(3) . . ? O17 W6 Pd2 145.0(2) . . ? S7 W6 Pd2 52.42(9) . . ? S8 W6 Pd2 58.38(10) . . ? S6 W6 Pd2 101.33(10) . . ? W5 W6 Pd2 57.87(3) . . ? W4 W6 Pd2 60.30(3) . . ? S5 Pd2 S7 108.14(13) . . ? S5 Pd2 S8 116.26(14) . 2_766 ? S7 Pd2 S8 115.64(13) . 2_766 ? S5 Pd2 S8 102.22(13) . . ? S7 Pd2 S8 98.00(13) . . ? S8 Pd2 S8 114.32(10) 2_766 . ? S5 Pd2 Pd2 126.32(11) . 2_766 ? S7 Pd2 Pd2 120.94(11) . 2_766 ? S8 Pd2 Pd2 61.06(10) 2_766 2_766 ? S8 Pd2 Pd2 53.26(8) . 2_766 ? S5 Pd2 W5 54.79(9) . . ? S7 Pd2 W5 54.57(9) . . ? S8 Pd2 W5 148.06(10) 2_766 . ? S8 Pd2 W5 97.56(8) . . ? Pd2 Pd2 W5 150.76(7) 2_766 . ? S5 Pd2 W4 52.86(9) . . ? S7 Pd2 W4 99.16(9) . . ? S8 Pd2 W4 144.69(10) 2_766 . ? S8 Pd2 W4 51.32(8) . . ? Pd2 Pd2 W4 96.74(6) 2_766 . ? W5 Pd2 W4 59.44(3) . . ? S5 Pd2 W6 98.78(10) . . ? S7 Pd2 W6 51.06(9) . . ? S8 Pd2 W6 144.76(10) 2_766 . ? S8 Pd2 W6 50.17(8) . . ? Pd2 Pd2 W6 95.92(6) 2_766 . ? W5 Pd2 W6 57.79(3) . . ? W4 Pd2 W6 56.99(3) . . ? Pd2 S5 W4 74.31(12) . . ? Pd2 S5 W5 70.80(11) . . ? W4 S5 W5 71.78(11) . . ? W4 S6 W5 71.51(10) . . ? W4 S6 W6 70.87(10) . . ? W5 S6 W6 70.32(10) . . ? W6 S7 W5 71.23(10) . . ? W6 S7 Pd2 76.53(11) . . ? W5 S7 Pd2 70.55(10) . . ? W6 S8 W4 70.98(10) . . ? W6 S8 Pd2 123.47(16) . 2_766 ? W4 S8 Pd2 121.63(17) . 2_766 ? W6 S8 Pd2 71.45(10) . . ? W4 S8 Pd2 69.36(10) . . ? Pd2 S8 Pd2 65.68(10) 2_766 . ? O20 S20 O22 114.8(6) . . ? O20 S20 O21 111.7(6) . . ? O22 S20 O21 111.5(6) . . ? O20 S20 C21 105.1(6) . . ? O22 S20 C21 107.1(6) . . ? O21 S20 C21 105.9(6) . . ? C22 C21 C26 117.8(15) . . ? C22 C21 S20 120.7(12) . . ? C26 C21 S20 121.3(12) . . ? C21 C22 C23 122.5(17) . . ? C24 C23 C22 119.0(18) . . ? C25 C24 C23 118.9(15) . . ? C25 C24 C27 121.4(16) . . ? C23 C24 C27 119.7(16) . . ? C24 C25 C26 121.7(16) . . ? C25 C26 C21 119.9(16) . . ? O32 S30 O31 112.9(7) . . ? O32 S30 O30 113.6(6) . . ? O31 S30 O30 109.4(6) . . ? O32 S30 C31 107.4(7) . . ? O31 S30 C31 107.2(7) . . ? O30 S30 C31 105.8(7) . . ? C32 C31 C36 118.8(16) . . ? C32 C31 S30 120.5(13) . . ? C36 C31 S30 120.3(13) . . ? C33 C32 C31 122.5(16) . . ? C34 C33 C32 119.9(17) . . ? C33 C34 C35 118.2(15) . . ? C33 C34 C37 123.1(17) . . ? C35 C34 C37 118.7(16) . . ? C36 C35 C34 121.5(16) . . ? C31 C36 C35 118.7(16) . . ? O40 S40 O41 113.8(6) . . ? O40 S40 O42 110.4(7) . . ? O41 S40 O42 111.2(6) . . ? O40 S40 C41 106.4(7) . . ? O41 S40 C41 107.3(7) . . ? O42 S40 C41 107.4(7) . . ? C42 C41 C46 119.6(17) . . ? C42 C41 S40 120.4(13) . . ? C46 C41 S40 119.9(14) . . ? C43 C42 C41 118.9(17) . . ? C42 C43 C44 123.3(17) . . ? C43 C44 C45 116.7(16) . . ? C43 C44 C47 121.8(17) . . ? C45 C44 C47 121.5(17) . . ? C46 C45 C44 121.5(17) . . ? C45 C46 C41 119.7(18) . . ? O50 S50 O52 113.2(7) . . ? O50 S50 O51 112.5(7) . . ? O52 S50 O51 111.1(7) . . ? O50 S50 C51 107.3(8) . . ? O52 S50 C51 105.9(7) . . ? O51 S50 C51 106.3(8) . . ? C56 C51 C52 120.0(16) . . ? C56 C51 S50 119.5(14) . . ? C52 C51 S50 120.6(14) . . ? C53 C52 C51 119.3(18) . . ? C52 C53 C54 123.0(18) . . ? C55 C54 C53 115.1(16) . . ? C55 C54 C57 124.9(17) . . ? C53 C54 C57 120.0(17) . . ? C54 C55 C56 123.5(17) . . ? C51 C56 C55 118.8(17) . . ? O60 S60 O61 114.8(9) . . ? O60 S60 O62 113.1(10) . . ? O61 S60 O62 110.4(7) . . ? O60 S60 C61 107.8(8) . . ? O61 S60 C61 106.2(8) . . ? O62 S60 C61 103.6(7) . . ? C66 C61 C62 119.6(15) . . ? C66 C61 S60 122.9(13) . . ? C62 C61 S60 117.3(13) . . ? C63 C62 C61 117.7(16) . . ? C64 C63 C62 121.4(16) . . ? C63 C64 C65 118.5(15) . . ? C63 C64 C67 120.1(17) . . ? C65 C64 C67 121.3(17) . . ? C66 C65 C64 121.9(17) . . ? C65 C66 C61 120.9(17) . . ? O71 S70 O72 114.0(6) . . ? O71 S70 O70 111.9(7) . . ? O72 S70 O70 110.6(7) . . ? O71 S70 C71 106.6(8) . . ? O72 S70 C71 106.4(7) . . ? O70 S70 C71 106.9(7) . . ? C76 C71 C72 115.6(16) . . ? C76 C71 S70 122.2(14) . . ? C72 C71 S70 122.1(13) . . ? C73 C72 C71 120.6(17) . . ? C72 C73 C74 121.1(17) . . ? C75 C74 C73 116.8(17) . . ? C75 C74 C77 122.9(18) . . ? C73 C74 C77 120.3(16) . . ? C74 C75 C76 124.4(18) . . ? C75 C76 C71 121.5(18) . . ? O82 S80 O80 111.9(7) . . ? O82 S80 O81 112.3(7) . . ? O80 S80 O81 111.6(6) . . ? O82 S80 C81 106.7(7) . . ? O80 S80 C81 105.8(7) . . ? O81 S80 C81 108.0(7) . . ? C82 C81 C86 115.8(15) . . ? C82 C81 S80 121.8(13) . . ? C86 C81 S80 122.4(12) . . ? C81 C82 C83 123.2(18) . . ? C84 C83 C82 121.1(17) . . ? C85 C84 C83 116.2(17) . . ? C85 C84 C87 120.8(19) . . ? C83 C84 C87 123.0(17) . . ? C84 C85 C86 122.9(18) . . ? C81 C86 C85 120.5(16) . . ? O92 S90 O91 112.9(6) . . ? O92 S90 O90 110.0(7) . . ? O91 S90 O90 111.0(6) . . ? O92 S90 C91 108.6(7) . . ? O91 S90 C91 106.7(7) . . ? O90 S90 C91 107.4(7) . . ? C92 C91 C96 118.7(15) . . ? C92 C91 S90 119.2(13) . . ? C96 C91 S90 122.0(12) . . ? C91 C92 C93 118.8(17) . . ? C94 C93 C92 121.3(17) . . ? C95 C94 C93 116.7(16) . . ? C95 C94 C97 122.9(17) . . ? C93 C94 C97 120.4(17) . . ? C96 C95 C94 124.4(19) . . ? C95 C96 C91 120.0(18) . . ?