Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Paul Beer' _publ_contact_author_address ; Department of Chemistry University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email PAUL.BEER@CHEM.OX.AC.UK _publ_section_title ; Transition metal-directed self-assembly of calix[4]arene based dithiocarbamate ligands ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; loop_ _publ_author_name 'Paul Beer' 'Michael G. B. Drew' 'Richard Hibbert' 'Philip R. A. Webber' data_19 _database_code_depnum_ccdc_archive 'CCDC 229318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H180 Cl6 N8 Ni2 O13 S8' _chemical_formula_weight 2625.40 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' Ni Ni 0.3393 1.1124 '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' _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 12.365(15) _cell_length_b 15.106(17) _cell_length_c 22.60(3) _cell_angle_alpha 78.907(10) _cell_angle_beta 75.256(10) _cell_angle_gamma 67.410(10) _cell_volume 3749(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description black _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1394 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 1.000 _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_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10707 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.06 _reflns_number_total 10707 _reflns_number_gt 4040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10707 _refine_ls_number_parameters 737 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.2708 _refine_ls_R_factor_gt 0.1267 _refine_ls_wR_factor_ref 0.4060 _refine_ls_wR_factor_gt 0.3489 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.425 _refine_ls_shift/su_mean 0.025 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.13552(12) -0.24146(11) -0.05454(6) 0.0856(6) Uani 1 d . . . C11 C -0.5985(8) 0.1415(8) 0.2257(4) 0.065(3) Uani 1 d . . . C12 C -0.6537(9) 0.0858(9) 0.2684(5) 0.083(3) Uani 1 d . . . H12 H -0.7350 0.1136 0.2842 0.100 Uiso 1 calc R . . C13 C -0.5949(12) -0.0102(10) 0.2894(5) 0.098(4) Uani 1 d . . . C14 C -0.4742(9) -0.0477(9) 0.2659(5) 0.086(3) Uani 1 d . . . H14 H -0.4320 -0.1108 0.2797 0.103 Uiso 1 calc R . . C15 C -0.4128(8) 0.0028(7) 0.2232(4) 0.066(3) Uani 1 d . . . C16 C -0.4744(9) 0.0952(9) 0.2029(4) 0.075(3) Uani 1 d . . . C17 C -0.2787(8) -0.0409(8) 0.2008(4) 0.076(3) Uani 1 d . . . H17A H -0.2569 -0.1096 0.1997 0.092 Uiso 1 calc R . . H17B H -0.2581 -0.0129 0.1590 0.092 Uiso 1 calc R . . C21 C -0.2063(8) -0.0260(7) 0.2400(4) 0.067(3) Uani 1 d . . . C22 C -0.1942(9) -0.0819(8) 0.2963(5) 0.082(3) Uani 1 d . . . H22 H -0.2258 -0.1309 0.3069 0.098 Uiso 1 calc R . . C23 C -0.1369(10) -0.0676(10) 0.3373(5) 0.097(4) Uani 1 d . . . C24 C -0.0921(9) 0.0090(8) 0.3225(5) 0.083(3) Uani 1 d . . . H24 H -0.0547 0.0208 0.3495 0.100 Uiso 1 calc R . . C25 C -0.1052(8) 0.0656(7) 0.2673(4) 0.064(3) Uani 1 d . . . C26 C -0.1573(7) 0.0474(7) 0.2259(4) 0.060(2) Uani 1 d . . . C27 C -0.0664(8) 0.1530(8) 0.2556(4) 0.074(3) Uani 1 d . . . H27A H 0.0018 0.1378 0.2744 0.089 Uiso 1 calc R . . H27B H -0.0417 0.1675 0.2117 0.089 Uiso 1 calc R . . C31 C -0.1650(9) 0.2394(8) 0.2811(4) 0.073(3) Uani 1 d . . . C32 C -0.1766(10) 0.2576(9) 0.3443(4) 0.081(3) Uani 1 d . . . H32 H -0.1185 0.2173 0.3663 0.097 Uiso 1 calc R . . C33 C -0.2687(10) 0.3310(9) 0.3720(5) 0.089(3) Uani 1 d . . . C34 C -0.3520(9) 0.3891(8) 0.3375(4) 0.082(3) Uani 1 d . . . H34 H -0.4146 0.4402 0.3557 0.099 Uiso 1 calc R . . C35 C -0.3503(8) 0.3781(7) 0.2787(4) 0.066(2) Uani 1 d . . . C36 C -0.2550(8) 0.3037(7) 0.2512(4) 0.062(2) Uani 1 d . . . C37 C -0.4526(8) 0.4438(6) 0.2463(4) 0.071(3) Uani 1 d . . . H37A H -0.4800 0.5083 0.2583 0.085 Uiso 1 calc R . . H37B H -0.4228 0.4471 0.2022 0.085 Uiso 1 calc R . . C41 C -0.5554(7) 0.4094(7) 0.2613(4) 0.057(2) Uani 1 d . . . C47 C -0.6677(8) 0.2445(8) 0.2061(5) 0.075(3) Uani 1 d . . . H47A H -0.6370 0.2593 0.1629 0.090 Uiso 1 calc R . . H47B H -0.7506 0.2515 0.2104 0.090 Uiso 1 calc R . . C42 C -0.6420(9) 0.4319(7) 0.3158(4) 0.074(3) Uani 1 d . . . H42 H -0.6356 0.4714 0.3406 0.089 Uiso 1 calc R . . C44 C -0.7420(8) 0.3384(8) 0.2971(5) 0.074(3) Uani 1 d . . . H44 H -0.8016 0.3117 0.3097 0.089 Uiso 1 calc R . . C43 C -0.7375(9) 0.3974(8) 0.3344(4) 0.079(3) Uani 1 d . . . C45 C -0.6630(8) 0.3156(7) 0.2414(4) 0.062(3) Uani 1 d . . . C46 C -0.5760(7) 0.3555(7) 0.2252(4) 0.058(2) Uani 1 d . . . O250 O -0.1630(5) 0.1051(4) 0.1692(2) 0.0672(17) Uani 1 d . . . C251 C -0.0644(8) 0.0660(7) 0.1185(4) 0.068(3) Uani 1 d . . . H25A H -0.0495 -0.0016 0.1175 0.082 Uiso 1 calc R . . H25B H 0.0082 0.0725 0.1230 0.082 Uiso 1 calc R . . C252 C -0.1034(10) 0.1242(8) 0.0609(4) 0.087(3) Uani 1 d . . . H25C H -0.1160 0.1914 0.0618 0.104 Uiso 1 calc R . . H25D H -0.0420 0.1011 0.0252 0.104 Uiso 1 calc R . . N253 N -0.2161(7) 0.1146(6) 0.0567(3) 0.071(2) Uani 1 d . . . H253 H -0.2745 0.1264 0.0879 0.085 Uiso 1 calc R . . C254 C -0.2314(9) 0.0891(7) 0.0080(5) 0.072(3) Uani 1 d . . . O255 O -0.1631(7) 0.0812(6) -0.0419(3) 0.100(2) Uani 1 d . . . C256 C -0.3518(10) 0.0737(9) 0.0192(5) 0.093(3) Uani 1 d . . . H25E H -0.3631 0.0351 0.0583 0.112 Uiso 1 calc R . . H25F H -0.4167 0.1355 0.0211 0.112 Uiso 1 calc R . . N257 N -0.3546(9) 0.0236(9) -0.0316(4) 0.098(3) Uani 1 d . . . C258 C -0.2885(9) -0.0639(9) -0.0361(5) 0.080(3) Uani 1 d . . . S259 S -0.2073(3) -0.1390(3) 0.01544(13) 0.0945(10) Uani 1 d . . . S260 S -0.2734(3) -0.1242(3) -0.09761(15) 0.1068(11) Uani 1 d . . . O450 O -0.4910(5) 0.3341(5) 0.1690(3) 0.0678(17) Uani 1 d . . . C451 C -0.5250(8) 0.4049(7) 0.1162(4) 0.075(3) Uani 1 d . . . H45A H -0.5535 0.4700 0.1274 0.089 Uiso 1 calc R . . H45B H -0.5879 0.3961 0.1022 0.089 Uiso 1 calc R . . C452 C -0.4117(9) 0.3867(9) 0.0656(4) 0.089(4) Uani 1 d . . . H45C H -0.3738 0.3180 0.0627 0.106 Uiso 1 calc R . . H45D H -0.4343 0.4173 0.0266 0.106 Uiso 1 calc R . . N453 N -0.3273(7) 0.4223(6) 0.0762(3) 0.071(2) Uani 1 d . . . H453 H -0.2829 0.3894 0.1023 0.085 Uiso 1 calc R . . O150 O -0.4164(6) 0.1490(5) 0.1589(3) 0.079(2) Uani 1 d . . . H150 H -0.3466 0.1151 0.1474 0.095 Uiso 1 calc R . . O350 O -0.2495(6) 0.2935(5) 0.1894(3) 0.0739(19) Uani 1 d . . . H350 H -0.1991 0.2412 0.1803 0.089 Uiso 1 calc R . . C100 C -0.6659(18) -0.0646(15) 0.3385(10) 0.158(7) Uani 1 d . . . C101 C -0.758(2) -0.0114(16) 0.3818(10) 0.230(13) Uani 1 d . . . H10A H -0.8120 0.0425 0.3611 0.276 Uiso 1 calc R . . H10B H -0.7257 0.0114 0.4075 0.276 Uiso 1 calc R . . H10C H -0.8007 -0.0515 0.4067 0.276 Uiso 1 calc R . . C102 C -0.5910(17) -0.1630(19) 0.3545(15) 0.35(3) Uani 1 d . . . H10D H -0.6234 -0.1852 0.3954 0.425 Uiso 1 calc R . . H10E H -0.5116 -0.1652 0.3529 0.425 Uiso 1 calc R . . H10F H -0.5883 -0.2036 0.3259 0.425 Uiso 1 calc R . . C103 C -0.731(3) -0.093(2) 0.3027(16) 0.34(2) Uani 1 d . . . H10G H -0.6746 -0.1426 0.2776 0.404 Uiso 1 calc R . . H10H H -0.7708 -0.0383 0.2769 0.404 Uiso 1 calc R . . H10I H -0.7883 -0.1177 0.3304 0.404 Uiso 1 calc R . . C200 C -0.1229(11) -0.1360(11) 0.3980(6) 0.111(5) Uani 1 d . . . C201 C -0.016(2) -0.2111(13) 0.3882(8) 0.217(11) Uani 1 d . . . H20A H 0.0114 -0.2168 0.3449 0.260 Uiso 1 calc R . . H20B H -0.0263 -0.2699 0.4091 0.260 Uiso 1 calc R . . H20C H 0.0420 -0.1993 0.4039 0.260 Uiso 1 calc R . . C202 C -0.131(2) -0.0860(13) 0.4496(7) 0.246(15) Uani 1 d . . . H20D H -0.1289 -0.1297 0.4867 0.295 Uiso 1 calc R . . H20E H -0.2048 -0.0319 0.4546 0.295 Uiso 1 calc R . . H20F H -0.0651 -0.0639 0.4414 0.295 Uiso 1 calc R . . C203 C -0.205(3) -0.191(3) 0.4163(13) 0.46(4) Uani 1 d . . . H20G H -0.2000 -0.2223 0.4571 0.554 Uiso 1 calc R . . H20H H -0.1821 -0.2379 0.3882 0.554 Uiso 1 calc R . . H20I H -0.2849 -0.1472 0.4154 0.554 Uiso 1 calc R . . C300 C -0.2771(11) 0.3500(12) 0.4381(5) 0.110(4) Uani 1 d . . . C301 C -0.1854(16) 0.2743(19) 0.4697(7) 0.239(13) Uani 1 d . . . H30A H -0.1963 0.2136 0.4736 0.286 Uiso 1 calc R . . H30B H -0.1934 0.2912 0.5098 0.286 Uiso 1 calc R . . H30C H -0.1071 0.2689 0.4460 0.286 Uiso 1 calc R . . C302 C -0.3965(16) 0.3538(17) 0.4761(6) 0.200(10) Uani 1 d . . . H30D H -0.4072 0.2940 0.4763 0.240 Uiso 1 calc R . . H30E H -0.4581 0.4059 0.4590 0.240 Uiso 1 calc R . . H30F H -0.4010 0.3638 0.5175 0.240 Uiso 1 calc R . . C303 C -0.2764(18) 0.4477(17) 0.4381(8) 0.189(8) Uani 1 d . . . H30G H -0.3053 0.4662 0.4791 0.227 Uiso 1 calc R . . H30H H -0.3270 0.4927 0.4115 0.227 Uiso 1 calc R . . H30I H -0.1963 0.4475 0.4235 0.227 Uiso 1 calc R . . C400 C -0.8287(12) 0.4221(10) 0.3943(6) 0.109(4) Uiso 1 d . . . C401 C -0.946(2) 0.5139(17) 0.3691(10) 0.226(10) Uiso 1 d . . . H40A H -0.9375 0.5744 0.3693 0.271 Uiso 1 calc R . . H40B H -1.0195 0.5127 0.3959 0.271 Uiso 1 calc R . . H40C H -0.9467 0.5061 0.3281 0.271 Uiso 1 calc R . . C402 C -0.8828(15) 0.3514(13) 0.4216(8) 0.166(6) Uiso 1 d . . . H40D H -0.8217 0.2903 0.4292 0.199 Uiso 1 calc R . . H40E H -0.9270 0.3456 0.3941 0.199 Uiso 1 calc R . . H40F H -0.9359 0.3709 0.4597 0.199 Uiso 1 calc R . . C403 C -0.807(3) 0.488(3) 0.4248(16) 0.38(2) Uiso 1 d . . . H40G H -0.7456 0.5093 0.3986 0.460 Uiso 1 calc R . . H40H H -0.7823 0.4555 0.4626 0.460 Uiso 1 calc R . . H40I H -0.8793 0.5424 0.4335 0.460 Uiso 1 calc R . . S460 S 0.0086(3) -0.3569(2) -0.01368(12) 0.0891(9) Uani 1 d . . . S459 S -0.0532(3) -0.3352(2) -0.12944(14) 0.0957(10) Uani 1 d . . . C458 C 0.0479(10) -0.4039(8) -0.0821(5) 0.078(3) Uani 1 d . . . N457 N 0.1480(9) -0.4769(7) -0.1003(4) 0.088(3) Uani 1 d . . . C456 C 0.2211(10) -0.5354(9) -0.0549(5) 0.092(3) Uani 1 d . . . H45E H 0.2588 -0.6008 -0.0661 0.111 Uiso 1 calc R . . H45F H 0.1680 -0.5374 -0.0152 0.111 Uiso 1 calc R . . C455 C 0.3147(11) -0.5032(11) -0.0477(5) 0.097(4) Uani 1 d . . . O454 O 0.3837(9) -0.5566(8) -0.0135(5) 0.153(4) Uani 1 d . . . C51 C 0.4380(14) -0.0874(11) 0.0742(7) 0.128(5) Uani 1 d . . . H51A H 0.5161 -0.1190 0.0498 0.154 Uiso 1 calc R . . H51B H 0.4472 -0.0476 0.1002 0.154 Uiso 1 calc R . . C52 C 0.3977(15) -0.1541(13) 0.1096(8) 0.150(6) Uani 1 d . . . H52A H 0.3906 -0.1967 0.0849 0.180 Uiso 1 calc R . . H52B H 0.3205 -0.1245 0.1355 0.180 Uiso 1 calc R . . C53 C 0.5025(19) -0.2142(15) 0.1523(9) 0.193(9) Uani 1 d . . . H53A H 0.5818 -0.2300 0.1265 0.232 Uiso 1 calc R . . H53B H 0.4972 -0.1751 0.1831 0.232 Uiso 1 calc R . . C54 C 0.481(3) -0.2981(18) 0.1805(14) 0.33(2) Uani 1 d . . . H54A H 0.5213 -0.3242 0.2144 0.400 Uiso 1 calc R . . H54B H 0.5100 -0.3445 0.1512 0.400 Uiso 1 calc R . . H54C H 0.3965 -0.2832 0.1952 0.400 Uiso 1 calc R . . C61 C -0.1785(10) 0.5075(10) 0.1619(5) 0.100(4) Uani 1 d . . . H61A H -0.1458 0.4521 0.1903 0.120 Uiso 1 calc R . . H61B H -0.2648 0.5311 0.1752 0.120 Uiso 1 calc R . . C62 C -0.1324(14) 0.5851(11) 0.1650(7) 0.130(5) Uani 1 d D . . H62A H -0.1866 0.6479 0.1519 0.156 Uiso 1 calc R . . H62B H -0.0544 0.5743 0.1384 0.156 Uiso 1 calc R . . C63 C -0.123(2) 0.580(2) 0.2379(17) 0.32(2) Uani 1 d D . . H63A H -0.1021 0.5139 0.2575 0.380 Uiso 1 calc R . . H63B H -0.0656 0.6066 0.2411 0.380 Uiso 1 calc R . . C64 C -0.242(3) 0.637(3) 0.2644(13) 0.36(2) Uani 1 d D . . H64A H -0.2393 0.6814 0.2889 0.429 Uiso 1 calc R . . H64B H -0.2829 0.5963 0.2900 0.429 Uiso 1 calc R . . H64C H -0.2849 0.6730 0.2322 0.429 Uiso 1 calc R . . C71 C 0.1327(11) -0.2504(11) 0.1339(6) 0.1938(15) Uiso 0.616(7) d PD A 1 H71 H 0.1677 -0.2041 0.1084 0.233 Uiso 0.616(7) calc PR A 1 Cl71 Cl -0.0136(5) -0.2220(4) 0.1192(3) 0.1938(15) Uiso 0.616(7) d PD A 1 Cl72 Cl 0.2139(8) -0.3634(7) 0.1095(5) 0.1938(15) Uiso 0.616(7) d PD A 1 Cl73 Cl 0.1003(8) -0.2288(8) 0.2112(4) 0.1938(15) Uiso 0.616(7) d PD A 1 C81 C 0.1327(11) -0.2504(11) 0.1339(6) 0.1938(15) Uiso 0.384(7) d PD A 2 H81 H 0.1479 -0.1912 0.1332 0.233 Uiso 0.384(7) calc PR A 2 Cl81 Cl -0.0136(5) -0.2220(4) 0.1192(3) 0.1938(15) Uiso 0.384(7) d PD A 2 Cl82 Cl 0.2510(11) -0.3289(12) 0.0778(6) 0.1938(15) Uiso 0.384(7) d PD A 2 Cl83 Cl 0.1495(12) -0.3224(12) 0.2059(5) 0.1938(15) Uiso 0.384(7) d PD A 2 O91 O 0.5612(18) 0.1649(15) 0.3537(9) 0.140(6) Uiso 0.50 d PD . . H91 H 0.572(6) 0.107(3) 0.345(2) 0.00(2) Uiso 0.50 d PD . . C921 C 0.493(3) 0.129(2) 0.4034(12) 0.198(16) Uiso 0.25 d PD B 1 H92A H 0.4094 0.1636 0.4012 0.238 Uiso 0.25 calc PR B 1 H92B H 0.5050 0.1439 0.4405 0.238 Uiso 0.25 calc PR B 1 C931 C 0.515(4) 0.022(2) 0.4101(18) 0.095(13) Uiso 0.25 d PD B 1 H93A H 0.4409 0.0117 0.4270 0.114 Uiso 0.25 calc PR B 1 H93B H 0.5701 -0.0112 0.4372 0.114 Uiso 0.25 calc PR B 1 H93C H 0.5481 -0.0015 0.3705 0.114 Uiso 0.25 calc PR B 1 C922 C 0.493(3) 0.129(2) 0.4034(12) 0.198(16) Uiso 0.25 d PD B 2 H92C H 0.4899 0.0700 0.3941 0.238 Uiso 0.25 calc PR B 2 H92D H 0.4118 0.1753 0.4103 0.238 Uiso 0.25 calc PR B 2 C932 C 0.543(6) 0.108(5) 0.4627(13) 0.18(3) Uiso 0.25 d PD B 2 H93D H 0.6163 0.1206 0.4534 0.217 Uiso 0.25 calc PR B 2 H93E H 0.5576 0.0419 0.4788 0.217 Uiso 0.25 calc PR B 2 H93F H 0.4860 0.1491 0.4927 0.217 Uiso 0.25 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0802(10) 0.0988(12) 0.0942(10) -0.0059(8) -0.0286(7) -0.0445(8) C11 0.070(6) 0.088(8) 0.048(5) -0.014(5) 0.000(5) -0.045(6) C12 0.069(6) 0.101(9) 0.088(7) -0.007(7) -0.006(6) -0.045(7) C13 0.111(10) 0.114(11) 0.079(7) -0.006(7) 0.015(7) -0.076(9) C14 0.062(6) 0.099(9) 0.096(8) 0.005(7) -0.008(6) -0.041(6) C15 0.068(6) 0.054(6) 0.072(6) -0.007(5) -0.013(5) -0.019(5) C16 0.070(7) 0.109(10) 0.064(6) -0.021(6) -0.007(5) -0.048(7) C17 0.072(6) 0.085(8) 0.077(6) -0.016(5) -0.003(5) -0.038(6) C21 0.049(5) 0.064(7) 0.067(6) -0.012(5) 0.001(5) -0.004(5) C22 0.079(7) 0.074(7) 0.090(8) 0.012(6) -0.018(6) -0.035(6) C23 0.068(7) 0.099(10) 0.087(8) 0.003(7) -0.013(6) 0.002(7) C24 0.081(7) 0.063(7) 0.099(8) 0.013(6) -0.026(6) -0.022(6) C25 0.065(6) 0.072(7) 0.060(6) 0.005(5) -0.012(5) -0.037(5) C26 0.045(5) 0.061(6) 0.065(6) 0.004(5) -0.011(4) -0.012(5) C27 0.053(5) 0.101(9) 0.062(6) -0.004(6) -0.022(4) -0.015(6) C31 0.076(7) 0.082(8) 0.075(6) -0.002(6) -0.023(5) -0.041(6) C32 0.084(7) 0.108(9) 0.070(7) 0.003(6) -0.032(6) -0.051(7) C33 0.085(7) 0.116(10) 0.077(7) -0.020(7) -0.025(6) -0.037(7) C34 0.082(7) 0.102(9) 0.073(7) -0.023(6) -0.022(6) -0.032(6) C35 0.068(6) 0.069(7) 0.071(6) -0.010(5) -0.014(5) -0.035(6) C36 0.064(6) 0.062(6) 0.059(6) 0.013(5) -0.013(5) -0.032(5) C37 0.086(7) 0.046(6) 0.074(6) -0.001(5) -0.029(5) -0.011(5) C41 0.053(5) 0.066(6) 0.061(5) -0.015(5) -0.014(4) -0.023(5) C47 0.054(5) 0.093(8) 0.080(6) -0.007(6) -0.013(5) -0.030(6) C42 0.070(6) 0.067(7) 0.085(7) -0.026(5) -0.020(6) -0.012(6) C44 0.051(5) 0.081(8) 0.087(7) -0.011(6) -0.016(5) -0.016(5) C43 0.058(6) 0.097(8) 0.070(6) -0.030(6) -0.006(5) -0.009(6) C45 0.046(5) 0.074(7) 0.067(6) -0.019(5) -0.014(5) -0.015(5) C46 0.047(5) 0.061(6) 0.055(5) -0.010(4) -0.007(4) -0.007(5) O250 0.069(4) 0.070(4) 0.057(4) -0.001(3) -0.005(3) -0.026(3) C251 0.062(5) 0.090(7) 0.058(6) -0.021(5) 0.006(5) -0.039(5) C252 0.095(8) 0.101(9) 0.074(7) -0.030(6) 0.017(6) -0.054(7) N253 0.067(5) 0.082(6) 0.066(5) -0.020(4) 0.002(4) -0.033(4) C254 0.072(7) 0.085(8) 0.065(7) -0.025(6) -0.002(5) -0.033(6) O255 0.093(5) 0.148(7) 0.068(4) -0.033(5) 0.001(4) -0.052(5) C256 0.092(8) 0.105(9) 0.095(8) -0.018(7) -0.019(6) -0.045(7) N257 0.105(7) 0.127(9) 0.076(6) -0.016(6) -0.038(5) -0.040(7) C258 0.073(7) 0.078(8) 0.094(7) -0.014(6) -0.022(6) -0.025(6) S259 0.0925(19) 0.121(3) 0.0845(19) -0.0079(17) -0.0313(15) -0.0463(19) S260 0.117(2) 0.111(3) 0.108(2) -0.0263(19) -0.0569(19) -0.029(2) O450 0.064(4) 0.077(4) 0.066(4) -0.001(3) -0.014(3) -0.030(3) C451 0.072(6) 0.083(7) 0.069(6) 0.006(5) -0.031(5) -0.024(5) C452 0.094(7) 0.136(10) 0.049(5) 0.014(6) -0.017(5) -0.064(8) N453 0.068(5) 0.078(6) 0.074(5) 0.010(5) -0.026(4) -0.034(5) O150 0.065(4) 0.099(5) 0.068(4) -0.014(4) 0.009(3) -0.035(4) O350 0.074(4) 0.085(5) 0.061(4) -0.004(3) -0.020(3) -0.024(4) C100 0.136(14) 0.148(16) 0.196(18) 0.017(14) -0.004(14) -0.093(13) C101 0.22(2) 0.21(2) 0.22(2) -0.041(18) 0.126(19) -0.122(19) C102 0.122(15) 0.26(3) 0.46(4) 0.24(3) 0.05(2) -0.027(16) C103 0.29(3) 0.30(4) 0.46(5) 0.10(4) -0.02(4) -0.26(3) C200 0.085(8) 0.121(11) 0.092(9) 0.045(9) -0.015(7) -0.028(8) C201 0.26(3) 0.143(15) 0.135(14) 0.060(12) -0.040(15) 0.010(17) C202 0.44(4) 0.124(15) 0.075(10) 0.029(10) -0.050(15) -0.010(18) C203 0.45(5) 0.83(8) 0.31(3) 0.43(5) -0.29(3) -0.54(6) C300 0.096(9) 0.179(15) 0.089(8) -0.048(9) -0.020(7) -0.067(9) C301 0.154(14) 0.41(4) 0.115(12) -0.099(17) -0.071(11) -0.004(19) C302 0.175(16) 0.33(3) 0.072(9) -0.053(12) -0.028(10) -0.041(17) C303 0.21(2) 0.26(3) 0.156(15) -0.102(15) -0.033(13) -0.118(19) S460 0.0938(19) 0.106(2) 0.0806(18) -0.0004(16) -0.0253(15) -0.0495(18) S459 0.092(2) 0.108(2) 0.104(2) -0.0115(18) -0.0400(17) -0.0399(18) C458 0.081(7) 0.087(8) 0.082(7) 0.008(6) -0.031(6) -0.046(7) N457 0.098(7) 0.087(7) 0.090(7) 0.002(5) -0.034(6) -0.041(6) C456 0.095(8) 0.086(8) 0.110(8) 0.016(7) -0.035(7) -0.051(7) C455 0.109(9) 0.119(11) 0.079(7) 0.028(7) -0.045(7) -0.060(9) O454 0.172(9) 0.152(9) 0.176(9) 0.082(8) -0.109(8) -0.102(8) C51 0.137(12) 0.096(11) 0.142(12) 0.002(9) -0.043(10) -0.027(9) C52 0.157(14) 0.143(15) 0.142(13) -0.007(12) -0.044(11) -0.039(12) C53 0.22(2) 0.149(17) 0.207(19) 0.053(15) -0.128(16) -0.049(15) C54 0.50(5) 0.15(2) 0.42(4) 0.04(3) -0.29(4) -0.08(3) C61 0.092(8) 0.113(10) 0.089(8) -0.008(7) -0.018(6) -0.032(7) C62 0.148(12) 0.120(12) 0.170(14) -0.052(10) -0.034(10) -0.082(10) C63 0.33(4) 0.35(4) 0.38(5) -0.24(4) 0.10(4) -0.26(4) C64 0.35(5) 0.39(5) 0.43(6) -0.20(4) -0.14(4) -0.12(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S459 2.202(4) . ? Ni1 S260 2.203(4) . ? Ni1 S259 2.204(4) . ? Ni1 S460 2.213(4) . ? C11 C12 1.379(13) . ? C11 C16 1.422(13) . ? C11 C47 1.501(13) . ? C12 C13 1.399(15) . ? C13 C14 1.375(15) . ? C13 C100 1.545(19) . ? C14 C15 1.371(13) . ? C15 C16 1.361(13) . ? C15 C17 1.517(13) . ? C16 O150 1.392(11) . ? C17 C21 1.509(14) . ? C21 C22 1.392(13) . ? C21 C26 1.407(13) . ? C22 C23 1.391(16) . ? C23 C24 1.416(16) . ? C23 C200 1.555(15) . ? C24 C25 1.379(13) . ? C25 C26 1.382(13) . ? C25 C27 1.526(14) . ? C26 O250 1.407(10) . ? C27 C31 1.494(14) . ? C31 C36 1.392(13) . ? C31 C32 1.468(13) . ? C32 C33 1.361(15) . ? C33 C34 1.376(14) . ? C33 C300 1.546(15) . ? C34 C35 1.364(12) . ? C35 C36 1.385(13) . ? C35 C37 1.532(12) . ? C36 O350 1.416(10) . ? C37 C41 1.490(13) . ? C41 C46 1.383(12) . ? C41 C42 1.411(12) . ? C47 C45 1.481(13) . ? C42 C43 1.407(14) . ? C44 C43 1.364(14) . ? C44 C45 1.394(12) . ? C43 C400 1.528(15) . ? C45 C46 1.368(13) . ? C46 O450 1.429(10) . ? O250 C251 1.464(9) . ? C251 C252 1.502(13) . ? C252 N253 1.482(13) . ? N253 C254 1.312(12) . ? C254 O255 1.220(10) . ? C254 C256 1.545(15) . ? C256 N257 1.505(14) . ? N257 C258 1.267(13) . ? N257 C51 1.519(16) 2 ? C258 S259 1.692(11) . ? C258 S260 1.738(12) . ? O450 C451 1.471(10) . ? C451 C452 1.534(13) . ? C452 N453 1.429(13) . ? N453 C455 1.313(14) 2 ? C100 C101 1.39(2) . ? C100 C102 1.45(2) . ? C100 C103 1.49(4) . ? C200 C201 1.372(19) . ? C200 C202 1.47(2) . ? C200 C203 1.47(3) . ? C300 C301 1.49(2) . ? C300 C303 1.48(2) . ? C300 C302 1.493(19) . ? C400 C402 1.432(19) . ? C400 C403 1.45(4) . ? C400 C401 1.71(2) . ? S460 C458 1.704(12) . ? S459 C458 1.744(10) . ? C458 N457 1.336(13) . ? N457 C456 1.470(12) . ? N457 C61 1.464(14) 2 ? C456 C455 1.470(16) . ? C455 O454 1.242(12) . ? C455 N453 1.313(14) 2 ? C51 C52 1.333(18) . ? C51 N257 1.519(16) 2 ? C52 C53 1.68(2) . ? C53 C54 1.40(3) . ? C61 N457 1.464(14) 2 ? C61 C62 1.506(17) . ? C62 C63 1.67(4) . ? C63 C64 1.432(18) . ? C71 Cl72 1.729(14) . ? C71 Cl73 1.755(13) . ? C71 Cl71 1.795(12) . ? C81 Cl83 1.787(15) . ? C81 Cl81 1.795(12) . ? C81 Cl82 1.859(14) . ? O91 C922 1.379(14) . ? O91 C921 1.379(14) . ? C921 C931 1.512(19) . ? C922 C932 1.55(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S459 Ni1 S260 99.56(14) . . ? S459 Ni1 S259 174.39(13) . . ? S260 Ni1 S259 79.56(14) . . ? S459 Ni1 S460 79.89(14) . . ? S260 Ni1 S460 177.64(14) . . ? S259 Ni1 S460 100.77(14) . . ? C12 C11 C16 115.6(10) . . ? C12 C11 C47 120.7(9) . . ? C16 C11 C47 123.7(9) . . ? C11 C12 C13 124.0(10) . . ? C14 C13 C12 116.0(10) . . ? C14 C13 C100 124.7(14) . . ? C12 C13 C100 119.2(13) . . ? C13 C14 C15 123.6(11) . . ? C16 C15 C14 118.3(9) . . ? C16 C15 C17 120.3(9) . . ? C14 C15 C17 121.3(9) . . ? C15 C16 O150 120.5(9) . . ? C15 C16 C11 122.4(10) . . ? O150 C16 C11 117.0(10) . . ? C21 C17 C15 113.9(8) . . ? C22 C21 C26 116.6(10) . . ? C22 C21 C17 119.3(11) . . ? C26 C21 C17 123.9(9) . . ? C23 C22 C21 122.9(11) . . ? C22 C23 C24 119.1(10) . . ? C22 C23 C200 119.5(13) . . ? C24 C23 C200 121.4(13) . . ? C25 C24 C23 118.5(11) . . ? C24 C25 C26 121.6(10) . . ? C24 C25 C27 117.1(10) . . ? C26 C25 C27 121.3(8) . . ? C25 C26 O250 118.8(9) . . ? C25 C26 C21 121.3(8) . . ? O250 C26 C21 119.9(8) . . ? C31 C27 C25 111.6(8) . . ? C36 C31 C32 114.8(9) . . ? C36 C31 C27 125.5(9) . . ? C32 C31 C27 119.5(9) . . ? C33 C32 C31 122.9(10) . . ? C32 C33 C34 116.5(10) . . ? C32 C33 C300 121.8(11) . . ? C34 C33 C300 121.7(11) . . ? C35 C34 C33 125.4(10) . . ? C34 C35 C36 117.1(9) . . ? C34 C35 C37 120.6(9) . . ? C36 C35 C37 122.3(8) . . ? C35 C36 C31 123.3(9) . . ? C35 C36 O350 117.8(8) . . ? C31 C36 O350 118.9(8) . . ? C41 C37 C35 112.6(7) . . ? C46 C41 C42 114.6(9) . . ? C46 C41 C37 125.2(8) . . ? C42 C41 C37 120.2(9) . . ? C45 C47 C11 114.3(8) . . ? C41 C42 C43 123.1(10) . . ? C43 C44 C45 124.2(10) . . ? C44 C43 C42 116.3(9) . . ? C44 C43 C400 121.9(12) . . ? C42 C43 C400 121.7(11) . . ? C46 C45 C44 115.8(9) . . ? C46 C45 C47 123.2(8) . . ? C44 C45 C47 120.8(10) . . ? C45 C46 C41 125.6(8) . . ? C45 C46 O450 118.6(8) . . ? C41 C46 O450 115.5(9) . . ? C26 O250 C251 115.0(7) . . ? O250 C251 C252 105.7(7) . . ? N253 C252 C251 108.8(8) . . ? C254 N253 C252 123.5(8) . . ? O255 C254 N253 125.8(10) . . ? O255 C254 C256 121.9(10) . . ? N253 C254 C256 112.2(9) . . ? N257 C256 C254 110.7(9) . . ? C258 N257 C51 126.3(10) . 2 ? C258 N257 C256 119.5(9) . . ? C51 N257 C256 114.2(11) 2 . ? N257 C258 S259 126.6(9) . . ? N257 C258 S260 122.9(8) . . ? S259 C258 S260 110.6(7) . . ? C258 S259 Ni1 85.0(4) . . ? C258 S260 Ni1 84.0(4) . . ? C46 O450 C451 113.7(6) . . ? O450 C451 C452 106.1(7) . . ? N453 C452 C451 113.5(9) . . ? C455 N453 C452 122.8(9) 2 . ? C101 C100 C102 122(2) . . ? C101 C100 C103 103(2) . . ? C102 C100 C103 94(2) . . ? C101 C100 C13 117.6(18) . . ? C102 C100 C13 111.6(15) . . ? C103 C100 C13 103.7(18) . . ? C201 C200 C202 110.6(16) . . ? C201 C200 C203 99(2) . . ? C202 C200 C203 109.8(19) . . ? C201 C200 C23 109.0(11) . . ? C202 C200 C23 112.6(14) . . ? C203 C200 C23 114.6(13) . . ? C301 C300 C303 112.4(14) . . ? C301 C300 C302 107.1(14) . . ? C303 C300 C302 103.7(15) . . ? C301 C300 C33 113.4(13) . . ? C303 C300 C33 110.3(13) . . ? C302 C300 C33 109.4(11) . . ? C402 C400 C403 128.0(19) . . ? C402 C400 C43 114.8(14) . . ? C403 C400 C43 111.5(18) . . ? C402 C400 C401 101.2(13) . . ? C403 C400 C401 90.7(19) . . ? C43 C400 C401 102.4(10) . . ? C458 S460 Ni1 85.0(4) . . ? C458 S459 Ni1 84.4(4) . . ? N457 C458 S460 125.6(8) . . ? N457 C458 S459 123.6(8) . . ? S460 C458 S459 110.6(7) . . ? C458 N457 C456 118.9(9) . . ? C458 N457 C61 121.6(9) . 2 ? C456 N457 C61 119.1(10) . 2 ? N457 C456 C455 116.6(9) . . ? O454 C455 N453 120.4(11) . 2 ? O454 C455 C456 117.1(12) . . ? N453 C455 C456 122.5(10) 2 . ? C52 C51 N257 112.3(14) . 2 ? C51 C52 C53 103.6(15) . . ? C54 C53 C52 107(2) . . ? N457 C61 C62 113.2(10) 2 . ? C61 C62 C63 106.9(14) . . ? C64 C63 C62 102(2) . . ? Cl72 C71 Cl73 122.7(10) . . ? Cl72 C71 Cl71 104.6(8) . . ? Cl73 C71 Cl71 102.0(7) . . ? Cl83 C81 Cl81 111.2(9) . . ? Cl83 C81 Cl82 103.0(9) . . ? Cl81 C81 Cl82 111.8(8) . . ? C922 O91 C921 0(3) . . ? O91 C921 C931 117(2) . . ? O91 C922 C932 112.2(19) . . ? _refine_diff_density_max 1.408 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.107 #===END data_21 _database_code_depnum_ccdc_archive 'CCDC 229319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H180 N8 O14 Pd2 S8' _chemical_formula_weight 2500.06 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' Pd Pd -0.9988 1.0072 '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' _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 12.190(17) _cell_length_b 14.032(17) _cell_length_c 23.53(3) _cell_angle_alpha 77.276(10) _cell_angle_beta 74.902(10) _cell_angle_gamma 68.497(10) _cell_volume 3581(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12023 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.8989 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12023 _reflns_number_gt 2503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12023 _refine_ls_number_parameters 649 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.3427 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2472 _refine_ls_wR_factor_gt 0.2045 _refine_ls_goodness_of_fit_ref 0.727 _refine_ls_restrained_S_all 0.731 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.006 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 Pd1 Pd 0.07252(7) 0.23046(7) 0.04663(4) 0.0759(4) Uani 1 1 d . . . S159 S 0.0064(3) 0.0911(2) 0.08728(15) 0.0941(11) Uani 1 1 d . . . S160 S 0.1786(3) 0.1087(2) -0.01783(15) 0.0829(10) Uani 1 1 d . . . S360 S -0.0218(2) 0.3419(2) 0.11864(14) 0.0785(9) Uani 1 1 d . . . S359 S 0.1432(2) 0.3702(2) 0.01073(13) 0.0794(10) Uani 1 1 d . . . C11 C 0.2599(14) 0.0208(16) 0.2432(8) 0.121(5) Uani 1 1 d . . . C12 C 0.259(2) -0.0580(17) 0.2851(9) 0.155(8) Uani 1 1 d . . . H12 H 0.1860 -0.0677 0.3048 0.186 Uiso 1 1 calc R . . C13 C 0.3595(18) -0.1228(14) 0.2991(6) 0.158(7) Uani 1 1 d D . . C14 C 0.4740(13) -0.1207(11) 0.2614(7) 0.100(4) Uani 1 1 d . . . H14 H 0.5440 -0.1740 0.2682 0.120 Uiso 1 1 calc R . . C15 C 0.4806(14) -0.0419(13) 0.2161(6) 0.088(4) Uani 1 1 d . . . C16 C 0.3772(15) 0.0285(12) 0.2001(7) 0.087(4) Uani 1 1 d . . . C17 C 0.6038(10) -0.0464(8) 0.1844(5) 0.083(4) Uani 1 1 d . . . H17A H 0.6016 -0.0082 0.1448 0.100 Uiso 1 1 calc R . . H17B H 0.6533 -0.1177 0.1808 0.100 Uiso 1 1 calc R . . C21 C 0.6612(10) 0.0027(11) 0.2202(5) 0.070(3) Uani 1 1 d . . . C22 C 0.7157(9) -0.0576(9) 0.2668(6) 0.080(4) Uani 1 1 d . . . H22 H 0.7279 -0.1282 0.2727 0.096 Uiso 1 1 calc R . . C23 C 0.7522(10) -0.0204(11) 0.3041(5) 0.088(4) Uani 1 1 d D . . C24 C 0.7437(11) 0.0773(13) 0.2932(6) 0.095(4) Uani 1 1 d . . . H24 H 0.7720 0.1033 0.3175 0.114 Uiso 1 1 calc R . . C25 C 0.6931(10) 0.1440(11) 0.2460(6) 0.075(3) Uani 1 1 d . . . C26 C 0.6477(10) 0.1060(10) 0.2109(6) 0.073(3) Uani 1 1 d . . . C27 C 0.6668(11) 0.2602(12) 0.2368(5) 0.109(5) Uani 1 1 d . . . H27A H 0.6716 0.2848 0.1946 0.130 Uiso 1 1 calc R . . H27B H 0.7297 0.2735 0.2487 0.130 Uiso 1 1 calc R . . C31 C 0.5428(12) 0.3256(9) 0.2707(6) 0.084(4) Uani 1 1 d . . . C32 C 0.5342(13) 0.3301(10) 0.3293(7) 0.110(5) Uani 1 1 d . . . H32 H 0.6037 0.3088 0.3447 0.132 Uiso 1 1 calc R . . C33 C 0.4175(14) 0.3679(11) 0.3677(5) 0.129(5) Uani 1 1 d D . . C34 C 0.3185(11) 0.4144(9) 0.3381(6) 0.103(4) Uani 1 1 d . . . H34 H 0.2434 0.4482 0.3595 0.124 Uiso 1 1 calc R . . C35 C 0.3312(13) 0.4106(9) 0.2780(6) 0.088(4) Uani 1 1 d . . . C36 C 0.4447(13) 0.3677(10) 0.2436(6) 0.082(4) Uani 1 1 d . . . C37 C 0.2107(10) 0.4479(9) 0.2530(5) 0.095(4) Uani 1 1 d . . . H37A H 0.1573 0.5123 0.2673 0.114 Uiso 1 1 calc R . . H37B H 0.2295 0.4607 0.2100 0.114 Uiso 1 1 calc R . . C41 C 0.1490(12) 0.3689(11) 0.2722(7) 0.097(4) Uani 1 1 d . . . C42 C 0.0651(13) 0.3643(13) 0.3290(6) 0.116(5) Uani 1 1 d . . . H42 H 0.0400 0.4179 0.3516 0.140 Uiso 1 1 calc R . . C43 C 0.0225(11) 0.2818(13) 0.3497(5) 0.131(6) Uani 1 1 d D . . C44 C 0.0520(12) 0.2004(14) 0.3141(8) 0.144(6) Uani 1 1 d . . . H44 H 0.0275 0.1425 0.3281 0.172 Uiso 1 1 calc R . . C45 C 0.1212(10) 0.2158(12) 0.2561(6) 0.082(4) Uani 1 1 d . . . C46 C 0.1726(11) 0.2919(12) 0.2365(7) 0.086(4) Uani 1 1 d . . . C47 C 0.1487(10) 0.1225(11) 0.2239(5) 0.102(4) Uani 1 1 d . . . H47A H 0.1681 0.1434 0.1814 0.122 Uiso 1 1 calc R . . H47B H 0.0769 0.1032 0.2321 0.122 Uiso 1 1 calc R . . O150 O 0.3883(6) 0.1014(6) 0.1539(4) 0.079(2) Uani 1 1 d . . . C151 C 0.3838(13) 0.0806(12) 0.0947(7) 0.128(6) Uani 1 1 d . . . H15A H 0.4342 0.0105 0.0886 0.154 Uiso 1 1 calc R . . H15B H 0.3020 0.0883 0.0935 0.154 Uiso 1 1 calc R . . C152 C 0.4239(12) 0.1501(11) 0.0508(6) 0.102(5) Uani 1 1 d . . . H15C H 0.4211 0.1371 0.0125 0.122 Uiso 1 1 calc R . . H15D H 0.3703 0.2196 0.0563 0.122 Uiso 1 1 calc R . . N153 N 0.5370(10) 0.1440(7) 0.0507(4) 0.083(3) Uani 1 1 d . . . H153 H 0.5516 0.1491 0.0835 0.100 Uiso 1 1 calc R . . O154 O 0.6195(6) 0.1206(6) -0.0464(3) 0.093(3) Uani 1 1 d . . . C155 C 0.6333(12) 0.1301(9) 0.0014(6) 0.084(4) Uani 1 1 d . . . C156 C 0.7504(9) 0.1214(8) 0.0126(4) 0.058(3) Uani 1 1 d . . . H15E H 0.7499 0.1899 0.0146 0.070 Uiso 1 1 calc R . . H15F H 0.7605 0.0800 0.0509 0.070 Uiso 1 1 calc R . . N157 N 0.8494(7) 0.0766(8) -0.0310(4) 0.062(2) Uani 1 1 d . . . C158 C 0.8779(9) -0.0276(9) -0.0308(5) 0.066(3) Uani 1 1 d . . . O250 O 0.5959(7) 0.1641(6) 0.1649(3) 0.080(2) Uani 1 1 d . . . H250 H 0.6071 0.2201 0.1577 0.095 Uiso 1 1 calc R . . O350 O 0.4573(6) 0.3597(6) 0.1848(4) 0.081(2) Uani 1 1 d . . . C351 C 0.4795(10) 0.4460(11) 0.1465(6) 0.094(4) Uani 1 1 d . . . H35A H 0.5631 0.4409 0.1408 0.113 Uiso 1 1 calc R . . H35B H 0.4289 0.5096 0.1624 0.113 Uiso 1 1 calc R . . C352 C 0.4485(12) 0.4431(10) 0.0868(5) 0.123(5) Uani 1 1 d . . . H35C H 0.4818 0.4892 0.0560 0.148 Uiso 1 1 calc R . . H35D H 0.4888 0.3737 0.0764 0.148 Uiso 1 1 calc R . . N353 N 0.3165(8) 0.4725(9) 0.0858(4) 0.083(3) Uani 1 1 d . . . H353 H 0.2761 0.4350 0.1088 0.100 Uiso 1 1 calc R . . C354 C 0.2605(14) 0.5544(12) 0.0505(7) 0.095(5) Uani 1 1 d . . . O355 O 0.2995(10) 0.6186(9) 0.0211(5) 0.130(4) Uani 1 1 d . . . C356 C 0.1324(10) 0.5694(8) 0.0505(5) 0.081(3) Uani 1 1 d . . . H35E H 0.0846 0.6392 0.0585 0.097 Uiso 1 1 calc R . . H35F H 0.1279 0.5651 0.0106 0.097 Uiso 1 1 calc R . . N357 N 0.0748(8) 0.4977(8) 0.0924(5) 0.090(3) Uani 1 1 d . . . C358 C 0.0546(8) 0.4146(8) 0.0788(4) 0.056(3) Uani 1 1 d . . . O450 O 0.2520(6) 0.2946(6) 0.1833(3) 0.079(2) Uani 1 1 d . . . H450 H 0.2214 0.3448 0.1603 0.095 Uiso 1 1 calc R . . C100 C 0.3523(16) -0.1893(14) 0.3595(8) 0.232(9) Uiso 1 1 d D . . C101 C 0.2529(15) -0.2399(14) 0.3695(8) 0.236(9) Uiso 1 1 d D . . H10A H 0.2769 -0.2898 0.3435 0.325 Uiso 1 1 d . . . H10B H 0.1790 -0.1873 0.3633 0.325 Uiso 1 1 d . . . H10C H 0.2422 -0.2732 0.4105 0.325 Uiso 1 1 d . . . C102 C 0.4746(13) -0.2617(13) 0.3692(8) 0.226(8) Uiso 1 1 d D . . H10D H 0.4664 -0.3139 0.4014 0.325 Uiso 1 1 d . . . H10E H 0.5191 -0.2230 0.3766 0.325 Uiso 1 1 d . . . H10F H 0.5178 -0.2926 0.3332 0.325 Uiso 1 1 d . . . C103 C 0.3012(18) -0.1154(15) 0.4126(8) 0.290(11) Uiso 1 1 d D . . H10G H 0.2960 -0.1550 0.4473 0.325 Uiso 1 1 calc R . . H10H H 0.2329 -0.0618 0.4033 0.325 Uiso 1 1 calc R . . H10I H 0.3666 -0.0829 0.4069 0.325 Uiso 1 1 calc R . . C203 C 0.8099(15) -0.2004(11) 0.3639(8) 0.235(10) Uiso 1 1 d D . . H20A H 0.7709 -0.2251 0.4022 0.282 Uiso 1 1 calc R . . H20B H 0.8942 -0.2392 0.3575 0.282 Uiso 1 1 calc R . . H20C H 0.7754 -0.2085 0.3337 0.282 Uiso 1 1 calc R . . C200 C 0.7930(12) -0.0883(12) 0.3610(7) 0.210(9) Uani 1 1 d D . . C201 C 0.7033(13) -0.0490(14) 0.4181(7) 0.240(10) Uiso 1 1 d D . . H20D H 0.7358 -0.0120 0.4354 0.288 Uiso 1 1 calc R . . H20E H 0.6908 -0.1069 0.4461 0.288 Uiso 1 1 calc R . . H20F H 0.6280 -0.0039 0.4080 0.288 Uiso 1 1 calc R . . C202 C 0.9145(12) -0.0756(13) 0.3643(8) 0.260(10) Uiso 1 1 d D . . H20G H 0.9575 -0.1343 0.3889 0.313 Uiso 1 1 calc R . . H20H H 0.8972 -0.0138 0.3808 0.313 Uiso 1 1 calc R . . H20I H 0.9627 -0.0711 0.3250 0.313 Uiso 1 1 calc R . . C300 C 0.4024(11) 0.3619(12) 0.4383(5) 0.138(6) Uani 1 1 d D . . C301 C 0.4690(12) 0.4322(11) 0.4444(6) 0.184(7) Uiso 1 1 d D . . H30A H 0.5306 0.4351 0.4097 0.221 Uiso 1 1 calc R . . H30B H 0.5050 0.4050 0.4789 0.221 Uiso 1 1 calc R . . H30C H 0.4131 0.5006 0.4486 0.221 Uiso 1 1 calc R . . C302 C 0.2713(11) 0.3984(12) 0.4679(6) 0.202(7) Uiso 1 1 d D . . H30D H 0.2350 0.4695 0.4527 0.242 Uiso 1 1 calc R . . H30E H 0.2646 0.3918 0.5100 0.242 Uiso 1 1 calc R . . H30F H 0.2310 0.3571 0.4598 0.242 Uiso 1 1 calc R . . C303 C 0.4613(15) 0.2468(10) 0.4628(7) 0.236(10) Uiso 1 1 d D . . H30G H 0.5428 0.2351 0.4650 0.283 Uiso 1 1 calc R . . H30H H 0.4605 0.2033 0.4367 0.283 Uiso 1 1 calc R . . H30I H 0.4169 0.2310 0.5017 0.283 Uiso 1 1 calc R . . C400 C -0.0616(14) 0.2678(12) 0.4178(6) 0.253(12) Uani 1 1 d D . . C401 C -0.0279(17) 0.3244(13) 0.4541(8) 0.273(11) Uiso 1 1 d D . . H40A H -0.0595 0.3073 0.4955 0.328 Uiso 1 1 calc R . . H40B H -0.0608 0.3975 0.4425 0.328 Uiso 1 1 calc R . . H40C H 0.0581 0.3044 0.4477 0.328 Uiso 1 1 calc R . . C402 C -0.1894(12) 0.3113(13) 0.4096(8) 0.268(11) Uiso 1 1 d D . . H40D H -0.1936 0.2972 0.3722 0.321 Uiso 1 1 calc R . . H40E H -0.2183 0.3847 0.4100 0.321 Uiso 1 1 calc R . . H40F H -0.2383 0.2799 0.4412 0.321 Uiso 1 1 calc R . . C81 C 0.0076(9) 0.5266(9) 0.1512(5) 0.103(4) Uiso 1 1 d . . . H81A H 0.0518 0.5571 0.1664 0.124 Uiso 1 1 calc R . . H81B H 0.0027 0.4645 0.1781 0.124 Uiso 1 1 calc R . . C82 C -0.1282(10) 0.6078(10) 0.1506(6) 0.130(5) Uiso 1 1 d . . . H82A H -0.1681 0.5843 0.1285 0.156 Uiso 1 1 calc R . . H82B H -0.1241 0.6752 0.1309 0.156 Uiso 1 1 calc R . . C83 C -0.2113(15) 0.6182(15) 0.2235(8) 0.200(7) Uiso 1 1 d . . . H83A H -0.1789 0.6504 0.2446 0.241 Uiso 1 1 calc R . . H83B H -0.2949 0.6590 0.2232 0.241 Uiso 1 1 calc R . . C84 C -0.200(2) 0.5092(18) 0.2521(10) 0.296(12) Uiso 1 1 d . . . H84A H -0.2482 0.5098 0.2915 0.356 Uiso 1 1 calc R . . H84B H -0.1173 0.4712 0.2542 0.356 Uiso 1 1 calc R . . H84C H -0.2270 0.4769 0.2290 0.356 Uiso 1 1 calc R . . C91 C 0.9108(9) 0.1406(9) -0.0752(5) 0.089(3) Uiso 1 1 d . . . H91A H 0.9891 0.0971 -0.0933 0.107 Uiso 1 1 calc R . . H91B H 0.9230 0.1893 -0.0560 0.107 Uiso 1 1 calc R . . C92 C 0.8377(14) 0.1998(13) -0.1234(7) 0.184(7) Uiso 1 1 d . . . H92A H 0.7558 0.2246 -0.1014 0.221 Uiso 1 1 calc R . . H92B H 0.8620 0.2608 -0.1377 0.221 Uiso 1 1 calc R . . C93 C 0.8251 0.1743 -0.1735 0.271 Uiso 1 1 d . . . H93A H 0.7993 0.1142 -0.1581 0.325 Uiso 1 1 calc R . . H93B H 0.9079 0.1469 -0.1939 0.325 Uiso 1 1 calc R . . C94 C 0.7575 0.2265 -0.2262 0.611 Uiso 1 1 d . . . H94A H 0.7046 0.2947 -0.2191 0.733 Uiso 1 1 calc R . . H94B H 0.7115 0.1858 -0.2294 0.733 Uiso 1 1 calc R . . H94C H 0.8150 0.2310 -0.2625 0.733 Uiso 1 1 calc R . . C403 C -0.0226 0.1503 0.4371 0.464 Uiso 1 1 d D . . H40G H 0.0376 0.1306 0.4608 0.557 Uiso 1 1 calc R . . H40H H 0.0098 0.1155 0.4026 0.557 Uiso 1 1 calc R . . H40I H -0.0909 0.1313 0.4601 0.557 Uiso 1 1 calc R . . C900 C 0.2786 0.1119 0.3997 0.264 Uiso 0.50 1 d P . . H90A H 0.2814 0.1052 0.4408 0.316 Uiso 0.50 1 calc PR . . H90B H 0.2519 0.0589 0.3940 0.316 Uiso 0.50 1 calc PR . . H90C H 0.2237 0.1786 0.3881 0.316 Uiso 0.50 1 calc PR . . O901 O 0.3969 0.1016 0.3639 0.373 Uiso 0.50 1 d P . . H901 H 0.4449 0.0890 0.3856 0.448 Uiso 0.50 1 calc PR . . O951 O 0.5285 0.6761 0.1164 0.335 Uiso 0.50 1 d P . . H951 H 0.4986 0.6909 0.0869 0.402 Uiso 0.50 1 calc PR . . C950 C 0.6081 0.7425 0.1101 0.361 Uiso 0.50 1 d P . . H95A H 0.6856 0.7120 0.0864 0.434 Uiso 0.50 1 calc PR . . H95B H 0.6175 0.7462 0.1487 0.434 Uiso 0.50 1 calc PR . . H95C H 0.5710 0.8110 0.0913 0.434 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0772(6) 0.0650(7) 0.0870(7) -0.0188(6) -0.0271(5) -0.0130(5) S159 0.082(2) 0.070(2) 0.134(3) -0.051(2) -0.030(2) -0.0007(18) S160 0.096(2) 0.045(2) 0.111(3) -0.033(2) -0.0398(19) -0.0018(18) S360 0.085(2) 0.047(2) 0.104(3) -0.025(2) -0.0249(18) -0.0095(17) S359 0.093(2) 0.0345(19) 0.103(2) -0.0174(19) -0.0491(19) 0.0127(16) C11 0.098(12) 0.157(19) 0.126(15) -0.056(14) -0.022(12) -0.043(14) C12 0.18(2) 0.17(2) 0.135(17) 0.042(15) -0.059(15) -0.099(18) C13 0.151(16) 0.24(2) 0.094(14) 0.000(14) -0.040(13) -0.073(17) C14 0.112(12) 0.084(11) 0.110(12) 0.011(11) -0.031(10) -0.045(9) C15 0.120(14) 0.090(12) 0.070(10) -0.011(10) -0.030(10) -0.046(11) C16 0.115(13) 0.065(12) 0.107(13) -0.019(10) -0.052(12) -0.033(10) C17 0.081(9) 0.076(9) 0.102(10) -0.032(8) -0.023(7) -0.023(7) C21 0.086(8) 0.058(10) 0.059(8) 0.016(8) -0.022(6) -0.023(8) C22 0.069(8) 0.067(10) 0.106(11) -0.016(10) -0.004(7) -0.032(7) C23 0.082(9) 0.070(11) 0.120(12) -0.014(10) -0.049(8) -0.014(8) C24 0.109(10) 0.083(12) 0.096(11) -0.021(10) -0.043(8) -0.013(9) C25 0.095(9) 0.069(11) 0.084(10) -0.009(9) -0.021(7) -0.052(8) C26 0.085(8) 0.046(10) 0.080(10) -0.001(9) -0.011(7) -0.019(8) C27 0.105(11) 0.157(16) 0.095(10) -0.023(11) -0.016(8) -0.079(11) C31 0.111(12) 0.085(10) 0.064(10) -0.014(8) -0.019(9) -0.038(9) C32 0.121(12) 0.118(12) 0.105(12) -0.023(10) -0.051(10) -0.031(10) C33 0.124(13) 0.154(15) 0.127(14) -0.056(12) -0.040(12) -0.036(11) C34 0.100(10) 0.120(12) 0.086(11) -0.031(9) -0.018(8) -0.023(9) C35 0.110(11) 0.082(10) 0.078(10) -0.021(8) -0.036(9) -0.020(8) C36 0.086(10) 0.087(11) 0.076(11) -0.005(9) -0.030(9) -0.024(8) C37 0.115(10) 0.075(10) 0.092(10) -0.030(8) -0.053(8) 0.004(8) C41 0.090(10) 0.090(12) 0.124(13) -0.030(11) -0.019(9) -0.037(9) C42 0.105(11) 0.165(17) 0.093(12) -0.047(11) -0.004(9) -0.053(11) C43 0.088(10) 0.186(19) 0.147(16) -0.076(15) 0.001(9) -0.062(11) C44 0.116(12) 0.199(18) 0.140(15) -0.080(15) -0.006(11) -0.061(12) C45 0.064(8) 0.137(14) 0.059(9) -0.020(9) 0.003(6) -0.055(9) C46 0.065(9) 0.091(12) 0.104(12) -0.033(11) -0.022(8) -0.013(8) C47 0.073(8) 0.166(14) 0.073(9) -0.046(10) -0.005(7) -0.036(9) O150 0.095(5) 0.056(6) 0.086(6) -0.017(5) -0.020(5) -0.021(5) C151 0.125(12) 0.159(17) 0.126(14) -0.091(13) -0.033(10) -0.029(11) C152 0.090(11) 0.133(15) 0.074(11) -0.030(10) -0.007(8) -0.025(9) N153 0.082(7) 0.108(9) 0.071(8) -0.029(6) -0.032(6) -0.023(6) O154 0.095(6) 0.131(8) 0.063(5) -0.018(5) -0.029(5) -0.037(5) C155 0.102(11) 0.056(9) 0.076(11) 0.007(8) -0.033(10) -0.006(7) C156 0.055(7) 0.059(8) 0.058(7) -0.003(6) -0.012(6) -0.018(6) N157 0.062(6) 0.058(7) 0.072(7) -0.006(6) -0.019(5) -0.024(6) C158 0.081(8) 0.034(8) 0.090(9) 0.002(8) -0.031(6) -0.022(7) O250 0.095(5) 0.081(6) 0.066(5) -0.001(5) -0.025(4) -0.032(5) O350 0.096(6) 0.084(7) 0.069(6) -0.004(5) -0.031(5) -0.033(5) C351 0.093(9) 0.110(12) 0.094(10) 0.003(10) -0.054(8) -0.035(8) C352 0.129(13) 0.130(13) 0.097(11) 0.013(10) 0.009(9) -0.065(10) N353 0.052(6) 0.122(10) 0.085(8) -0.034(8) -0.006(5) -0.035(6) C354 0.114(14) 0.057(12) 0.108(14) -0.008(10) -0.075(11) 0.015(10) O355 0.138(9) 0.105(10) 0.140(10) -0.013(8) -0.041(7) -0.026(7) C356 0.095(9) 0.057(9) 0.107(10) 0.023(8) -0.063(7) -0.033(7) N357 0.100(7) 0.063(8) 0.103(9) -0.023(7) -0.025(6) -0.011(6) C358 0.072(7) 0.015(7) 0.063(8) 0.007(6) -0.015(6) 0.001(6) O450 0.084(5) 0.087(7) 0.071(6) -0.007(5) -0.017(4) -0.034(5) C200 0.158(15) 0.21(2) 0.28(2) -0.10(2) -0.155(17) 0.034(14) C300 0.143(12) 0.23(2) 0.073(10) -0.059(12) -0.015(9) -0.077(13) C400 0.27(2) 0.45(4) 0.109(13) -0.111(19) 0.083(15) -0.24(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S159 2.306(4) . ? Pd1 S160 2.322(3) . ? Pd1 S359 2.331(4) . ? Pd1 S360 2.340(4) . ? S159 C158 1.782(11) 2_655 ? S160 C158 1.634(11) 2_655 ? S360 C358 1.614(10) . ? S359 C358 1.779(10) . ? C11 C12 1.311(19) . ? C11 C16 1.547(19) . ? C11 C47 1.643(19) . ? C12 C13 1.31(2) . ? C13 C14 1.453(17) . ? C13 C100 1.520(15) . ? C14 C15 1.367(15) . ? C15 C16 1.370(16) . ? C15 C17 1.477(15) . ? C16 O150 1.334(14) . ? C17 C21 1.609(13) . ? C21 C26 1.372(13) . ? C21 C22 1.384(13) . ? C22 C23 1.347(13) . ? C23 C24 1.308(14) . ? C23 C200 1.546(13) . ? C24 C25 1.402(15) . ? C25 C26 1.386(14) . ? C25 C27 1.519(15) . ? C26 O250 1.350(12) . ? C27 C31 1.562(15) . ? C31 C32 1.369(14) . ? C31 C36 1.379(14) . ? C32 C33 1.452(15) . ? C33 C34 1.423(15) . ? C33 C300 1.610(12) . ? C34 C35 1.393(14) . ? C35 C36 1.398(14) . ? C35 C37 1.589(14) . ? C36 O350 1.376(12) . ? C37 C41 1.487(15) . ? C41 C46 1.414(14) . ? C41 C42 1.462(16) . ? C42 C43 1.381(16) . ? C43 C44 1.450(16) . ? C43 C400 1.676(13) . ? C44 C45 1.424(16) . ? C45 C46 1.366(15) . ? C45 C47 1.544(14) . ? C46 O450 1.372(14) . ? O150 C151 1.503(13) . ? C151 C152 1.378(16) . ? C152 N153 1.349(13) . ? N153 C155 1.408(13) . ? O154 C155 1.220(12) . ? C155 C156 1.476(13) . ? C156 N157 1.410(10) . ? N157 C158 1.372(11) . ? N157 C91 1.457(12) . ? C158 S160 1.634(11) 2_655 ? C158 S159 1.782(11) 2_655 ? O350 C351 1.409(12) . ? C351 C352 1.559(14) . ? C352 N353 1.513(13) . ? N353 C354 1.332(14) . ? C354 O355 1.176(15) . ? C354 C356 1.497(17) . ? C356 N357 1.484(12) . ? N357 C358 1.393(12) . ? N357 C81 1.470(12) . ? C100 C102 1.507(15) . ? C100 C101 1.561(15) . ? C100 C103 1.646(15) . ? C203 C200 1.498(14) . ? C200 C201 1.556(14) . ? C200 C202 1.577(13) . ? C300 C302 1.509(12) . ? C300 C301 1.538(12) . ? C300 C303 1.553(13) . ? C400 C402 1.499(15) . ? C400 C401 1.500(14) . ? C400 C403 1.536(15) . ? C81 C82 1.631(14) . ? C82 C83 1.757(18) . ? C83 C84 1.50(2) . ? C91 C92 1.530(16) . ? C92 C93 1.363(15) . ? C93 C94 1.5630 . ? C900 O901 1.4418 . ? O951 C950 1.5355 . ? 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 S159 Pd1 S160 75.31(14) . . ? S159 Pd1 S359 176.62(12) . . ? S160 Pd1 S359 106.37(14) . . ? S159 Pd1 S360 102.75(14) . . ? S160 Pd1 S360 174.01(12) . . ? S359 Pd1 S360 75.27(13) . . ? C158 S159 Pd1 84.4(4) 2_655 . ? C158 S160 Pd1 87.2(4) 2_655 . ? C358 S360 Pd1 86.8(4) . . ? C358 S359 Pd1 83.5(4) . . ? C12 C11 C16 122.2(17) . . ? C12 C11 C47 130.2(18) . . ? C16 C11 C47 107.6(16) . . ? C11 C12 C13 120(2) . . ? C12 C13 C14 120.4(16) . . ? C12 C13 C100 117.4(17) . . ? C14 C13 C100 121.7(15) . . ? C15 C14 C13 121.2(13) . . ? C16 C15 C14 119.7(14) . . ? C16 C15 C17 125.0(15) . . ? C14 C15 C17 115.1(15) . . ? O150 C16 C15 117.7(15) . . ? O150 C16 C11 127.4(16) . . ? C15 C16 C11 114.6(15) . . ? C15 C17 C21 110.0(8) . . ? C26 C21 C22 117.2(11) . . ? C26 C21 C17 122.5(12) . . ? C22 C21 C17 120.0(11) . . ? C23 C22 C21 124.1(11) . . ? C24 C23 C22 118.2(12) . . ? C24 C23 C200 120.4(12) . . ? C22 C23 C200 121.2(13) . . ? C23 C24 C25 121.9(12) . . ? C26 C25 C24 119.1(12) . . ? C26 C25 C27 116.9(13) . . ? C24 C25 C27 123.3(11) . . ? O250 C26 C21 116.9(12) . . ? O250 C26 C25 123.6(12) . . ? C21 C26 C25 119.4(13) . . ? C25 C27 C31 116.5(10) . . ? C32 C31 C36 122.3(13) . . ? C32 C31 C27 117.0(13) . . ? C36 C31 C27 120.4(12) . . ? C31 C32 C33 120.7(12) . . ? C34 C33 C32 115.2(10) . . ? C34 C33 C300 122.5(12) . . ? C32 C33 C300 122.2(12) . . ? C35 C34 C33 121.8(11) . . ? C34 C35 C36 120.3(11) . . ? C34 C35 C37 116.7(13) . . ? C36 C35 C37 122.7(11) . . ? O350 C36 C31 120.3(12) . . ? O350 C36 C35 120.7(11) . . ? C31 C36 C35 118.8(12) . . ? C41 C37 C35 111.1(10) . . ? C46 C41 C42 116.8(13) . . ? C46 C41 C37 120.9(14) . . ? C42 C41 C37 122.3(14) . . ? C43 C42 C41 121.2(13) . . ? C42 C43 C44 121.4(12) . . ? C42 C43 C400 122.3(13) . . ? C44 C43 C400 116.3(13) . . ? C45 C44 C43 114.8(14) . . ? C46 C45 C44 124.5(14) . . ? C46 C45 C47 125.3(12) . . ? C44 C45 C47 109.3(13) . . ? C45 C46 O450 121.9(13) . . ? C45 C46 C41 120.5(14) . . ? O450 C46 C41 117.5(14) . . ? C45 C47 C11 114.0(9) . . ? C16 O150 C151 116.6(10) . . ? C152 C151 O150 108.6(12) . . ? N153 C152 C151 112.8(14) . . ? C152 N153 C155 125.6(10) . . ? O154 C155 N153 120.7(12) . . ? O154 C155 C156 123.3(12) . . ? N153 C155 C156 115.9(11) . . ? N157 C156 C155 113.7(9) . . ? C158 N157 C156 115.9(9) . . ? C158 N157 C91 123.5(9) . . ? C156 N157 C91 120.6(9) . . ? N157 C158 S160 128.3(9) . 2_655 ? N157 C158 S159 120.0(9) . 2_655 ? S160 C158 S159 111.7(7) 2_655 2_655 ? C36 O350 C351 112.2(9) . . ? O350 C351 C352 105.0(10) . . ? N353 C352 C351 116.6(9) . . ? C354 N353 C352 122.5(11) . . ? O355 C354 N353 126.8(16) . . ? O355 C354 C356 116.3(14) . . ? N353 C354 C356 116.7(14) . . ? N357 C356 C354 118.2(10) . . ? C358 N357 C81 113.2(11) . . ? C358 N357 C356 126.6(9) . . ? C81 N357 C356 118.8(9) . . ? N357 C358 S360 130.3(9) . . ? N357 C358 S359 114.7(8) . . ? S360 C358 S359 114.3(6) . . ? C102 C100 C13 111.6(13) . . ? C102 C100 C101 116.1(14) . . ? C13 C100 C101 110.0(13) . . ? C102 C100 C103 105.9(12) . . ? C13 C100 C103 109.9(13) . . ? C101 C100 C103 102.6(12) . . ? C203 C200 C23 113.8(11) . . ? C203 C200 C201 108.3(13) . . ? C23 C200 C201 111.6(10) . . ? C203 C200 C202 109.9(11) . . ? C23 C200 C202 107.9(12) . . ? C201 C200 C202 105.0(10) . . ? C302 C300 C301 111.8(10) . . ? C302 C300 C303 109.5(11) . . ? C301 C300 C303 112.8(10) . . ? C302 C300 C33 111.1(10) . . ? C301 C300 C33 104.5(9) . . ? C303 C300 C33 106.9(10) . . ? C402 C400 C401 115.5(13) . . ? C402 C400 C403 112.0(11) . . ? C401 C400 C403 113.3(12) . . ? C402 C400 C43 105.6(11) . . ? C401 C400 C43 105.0(11) . . ? C403 C400 C43 104.1(10) . . ? N357 C81 C82 113.7(9) . . ? C81 C82 C83 110.5(11) . . ? C84 C83 C82 105.3(15) . . ? N157 C91 C92 111.0(10) . . ? C93 C92 C91 133.5(12) . . ? C92 C93 C94 138.7(7) . . ? _refine_diff_density_max 0.717 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.087