Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_kata-10-Pd-complex-230k _database_code_CSD 188014 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Iki, Nobuhiko' 'Katagiri, Hiroshi' 'Matsunaga, Yoshiaki' 'Miyano, Sotaro' _publ_contact_author_name 'Dr Nobuhiko Iki' _publ_contact_author_address ; Biomolecular Engineering Tohoku University Aramaki-Aoba07 Aoba-ku Sendai 980-8579 JAPAN ; _publ_contact_author_email 'IKI@ORGSYNTH.CHE.TOHOKU.AC.JP' _publ_requested_journal 'Chemical Communications' _publ_section_title ; gThiacalix[4]anilineh as a highly specific extractant for Au(III) and Pd(II) ions ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C83.50 H103.50 Cl10.50 N8 Pd2 S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 2060.83 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 16.0963(4) _cell_length_b 35.1851(4) _cell_length_c 17.7567(9) _cell_angle_alpha 90 _cell_angle_beta 104.0085(4) _cell_angle_gamma 90 _cell_volume 9757.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16008 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 230.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.840 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64044 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9277 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9277 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 4.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 4.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 20744 _reflns_number_gt 9970 _reflns_threshold_expression F^2^>4.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.0497 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9970 _refine_ls_number_parameters 883 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.0029 _refine_diff_density_max 0.64 _refine_diff_density_min -0.57 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Pd(1) Pd 0.65157(3) 0.72934(1) 0.83669(3) 0.0313(1) Uani 1.00 d . . . Pd(2) Pd 0.71341(3) 0.74837(1) 0.53809(3) 0.0294(1) Uani 1.00 d . . . Cl(1) Cl 0.8664 0.5414 1.1157 0.1891 Uani 1.00 d . . . Cl(2) Cl 0.7389 0.4890 1.0631 0.2401 Uani 1.00 d . . . Cl(3) Cl 0.8569 0.5033 0.9749 0.1919 Uani 1.00 d . . . Cl(4) Cl 0.1025 0.7579 0.3491 0.1998 Uani 1.00 d . . . Cl(5) Cl 0.0838 0.7406 0.4983 0.1831 Uani 1.00 d . . . Cl(6) Cl 0.2477 0.7318 0.4661 0.3546 Uani 1.00 d . . . Cl(7) Cl 0.9015 0.9764 0.9470 0.1313 Uani 1.00 d . . . Cl(8) Cl 0.7899 0.9718 0.7962 0.1764 Uani 1.00 d . . . Cl(9) Cl 0.7369 1.0098 0.9149 0.2304 Uani 1.00 d . . . Cl(10) Cl 0.5702 0.9979 1.0784 0.1491 Uiso 0.50 d P . . Cl(11) Cl 0.5689 0.9606 0.9557 0.1308 Uiso 0.50 d P . . Cl(12) Cl 0.4344 1.0058 0.9430 0.3582 Uiso 0.50 d P . . S(1) S 0.6763(1) 0.89217(5) 0.5568(1) 0.0415(5) Uani 1.00 d . . . S(2) S 0.6061(1) 0.87216(5) 0.84582(10) 0.0445(5) Uani 1.00 d . . . S(3) S 0.5084(1) 0.72454(5) 0.77912(9) 0.0345(4) Uani 1.00 d . . . S(4) S 0.5695(1) 0.74584(5) 0.48360(8) 0.0293(4) Uani 1.00 d . . . S(5) S 0.6943(1) 0.58633(5) 0.8308(1) 0.0436(5) Uani 1.00 d . . . S(6) S 0.7447(1) 0.60420(5) 0.53385(10) 0.0449(5) Uani 1.00 d . . . S(7) S 0.8581(1) 0.75055(5) 0.59391(8) 0.0312(4) Uani 1.00 d . . . S(8) S 0.7955(1) 0.73400(5) 0.89157(8) 0.0315(4) Uani 1.00 d . . . N(1) N 0.6787(4) 0.8493(2) 0.7075(3) 0.047(2) Uani 1.00 d . . . N(2) N 0.6327(3) 0.7851(2) 0.8317(3) 0.033(1) Uani 1.00 d . . . N(3) N 0.5878(3) 0.7664(2) 0.6569(3) 0.038(2) Uani 1.00 d . . . N(4) N 0.6950(3) 0.8041(1) 0.5469(3) 0.033(1) Uani 1.00 d . . . N(5) N 0.6859(4) 0.6281(2) 0.6761(3) 0.049(2) Uani 1.00 d . . . N(6) N 0.7309(3) 0.6921(2) 0.5357(3) 0.040(2) Uani 1.00 d . . . N(7) N 0.7826(3) 0.7090(1) 0.7198(3) 0.036(1) Uani 1.00 d . . . N(8) N 0.6734(3) 0.6732(1) 0.8343(3) 0.037(2) Uani 1.00 d . . . C(1) C 0.6388(4) 0.8845(2) 0.7004(4) 0.039(2) Uani 1.00 d . . . C(2) C 0.6319(4) 0.9073(2) 0.6351(4) 0.038(2) Uani 1.00 d . . . C(3) C 0.5869(5) 0.9417(2) 0.6274(4) 0.043(2) Uani 1.00 d . . . C(4) C 0.5487(5) 0.9555(2) 0.6839(4) 0.047(2) Uani 1.00 d . . . C(5) C 0.5583(5) 0.9331(2) 0.7497(4) 0.047(2) Uani 1.00 d . . . C(6) C 0.6010(4) 0.8985(2) 0.7588(4) 0.039(2) Uani 1.00 d . . . C(7) C 0.4959(6) 0.9922(2) 0.6754(4) 0.053(2) Uani 1.00 d . . . C(8) C 0.5329(10) 1.0191(3) 0.7411(6) 0.128(5) Uani 1.00 d . . . C(9) C 0.4052(8) 0.9820(3) 0.6794(9) 0.127(5) Uani 1.00 d . . . C(10) C 0.4910(8) 1.0119(3) 0.5994(6) 0.097(4) Uani 1.00 d . . . C(11) C 0.6162(4) 0.8193(2) 0.5144(3) 0.030(2) Uani 1.00 d . . . C(12) C 0.5472(4) 0.7954(2) 0.4847(3) 0.031(2) Uani 1.00 d . . . C(13) C 0.4647(4) 0.8084(2) 0.4517(3) 0.037(2) Uani 1.00 d . . . C(14) C 0.4467(5) 0.8471(2) 0.4452(4) 0.040(2) Uani 1.00 d . . . C(15) C 0.5151(5) 0.8714(2) 0.4752(4) 0.041(2) Uani 1.00 d . . . C(16) C 0.5963(4) 0.8588(2) 0.5106(4) 0.034(2) Uani 1.00 d . . . C(17) C 0.3591(5) 0.8631(2) 0.4027(4) 0.052(2) Uani 1.00 d . . . C(18) C 0.3324(6) 0.8946(3) 0.4507(7) 0.098(4) Uani 1.00 d . . . C(19) C 0.3665(6) 0.8799(3) 0.3260(6) 0.098(4) Uani 1.00 d . . . C(20) C 0.2901(6) 0.8333(3) 0.3893(6) 0.087(4) Uani 1.00 d . . . C(21) C 0.5397(4) 0.7355(2) 0.6314(3) 0.032(2) Uani 1.00 d . . . C(22) C 0.5008(4) 0.7133(2) 0.6792(3) 0.033(2) Uani 1.00 d . . . C(23) C 0.4573(4) 0.6799(2) 0.6535(4) 0.041(2) Uani 1.00 d . . . C(24) C 0.4474(4) 0.6665(2) 0.5779(4) 0.042(2) Uani 1.00 d . . . C(25) C 0.4798(4) 0.6896(2) 0.5285(3) 0.037(2) Uani 1.00 d . . . C(26) C 0.5236(4) 0.7230(2) 0.5535(3) 0.032(2) Uani 1.00 d . . . C(27) C 0.4027(6) 0.6286(2) 0.5508(5) 0.058(3) Uani 1.00 d . . . C(28) C 0.418(1) 0.6160(4) 0.4806(9) 0.199(8) Uani 1.00 d . . . C(29) C 0.3088(9) 0.6325(4) 0.543(1) 0.219(9) Uani 1.00 d . . . C(30) C 0.428(2) 0.5996(3) 0.6104(8) 0.217(8) Uani 1.00 d . . . C(31) C 0.8275(4) 0.7412(2) 0.7428(3) 0.031(2) Uani 1.00 d . . . C(32) C 0.8393(4) 0.7552(2) 0.8188(3) 0.032(2) Uani 1.00 d . . . C(33) C 0.8784(4) 0.7902(2) 0.8403(3) 0.037(2) Uani 1.00 d . . . C(34) C 0.9102(4) 0.8126(2) 0.7895(4) 0.038(2) Uani 1.00 d . . . C(35) C 0.9049(4) 0.7975(2) 0.7160(4) 0.038(2) Uani 1.00 d . . . C(36) C 0.8654(4) 0.7627(2) 0.6930(3) 0.033(2) Uani 1.00 d . . . C(37) C 0.9480(5) 0.8521(2) 0.8116(4) 0.053(2) Uani 1.00 d . . . C(38) C 0.918(1) 0.8688(3) 0.8756(9) 0.168(7) Uani 1.00 d . . . C(39) C 0.925(1) 0.8788(3) 0.7469(7) 0.177(7) Uani 1.00 d . . . C(40) C 1.0408(9) 0.8490(4) 0.836(2) 0.252(10) Uani 1.00 d . . . C(41) C 0.8113(4) 0.6774(2) 0.5604(3) 0.032(2) Uani 1.00 d . . . C(42) C 0.8804(4) 0.7011(2) 0.5917(3) 0.034(2) Uani 1.00 d . . . C(43) C 0.9642(4) 0.6882(2) 0.6193(4) 0.042(2) Uani 1.00 d . . . C(44) C 0.9821(5) 0.6493(2) 0.6190(4) 0.047(2) Uani 1.00 d . . . C(45) C 0.9131(5) 0.6250(2) 0.5908(4) 0.046(2) Uani 1.00 d . . . C(46) C 0.8301(4) 0.6379(2) 0.5622(3) 0.036(2) Uani 1.00 d . . . C(47) C 1.0723(6) 0.6330(3) 0.6509(5) 0.067(3) Uani 1.00 d . . . C(48) C 1.0966(7) 0.6085(4) 0.5889(8) 0.132(5) Uani 1.00 d . . . C(49) C 1.1397(6) 0.6637(4) 0.6734(7) 0.104(4) Uani 1.00 d . . . C(50) C 1.0733(8) 0.6095(4) 0.7212(8) 0.141(6) Uani 1.00 d . . . C(51) C 0.7233(4) 0.5930(2) 0.6824(4) 0.039(2) Uani 1.00 d . . . C(52) C 0.7339(4) 0.5708(2) 0.7500(4) 0.040(2) Uani 1.00 d . . . C(53) C 0.7747(5) 0.5356(2) 0.7555(4) 0.043(2) Uani 1.00 d . . . C(54) C 0.8067(5) 0.5210(2) 0.6957(4) 0.048(2) Uani 1.00 d . . . C(55) C 0.7947(5) 0.5430(2) 0.6288(4) 0.046(2) Uani 1.00 d . . . C(56) C 0.7550(4) 0.5785(2) 0.6220(4) 0.041(2) Uani 1.00 d . . . C(57) C 0.8523(6) 0.4825(2) 0.7006(5) 0.067(3) Uani 1.00 d . . . C(58) C 0.803(1) 0.4558(3) 0.6408(7) 0.142(5) Uani 1.00 d . . . C(59) C 0.9391(9) 0.4885(4) 0.6849(9) 0.147(6) Uani 1.00 d . . . C(60) C 0.8652(8) 0.4644(3) 0.7790(6) 0.096(4) Uani 1.00 d . . . C(61) C 0.7524(4) 0.6599(2) 0.8675(3) 0.032(2) Uani 1.00 d . . . C(62) C 0.7737(4) 0.6204(2) 0.8725(4) 0.036(2) Uani 1.00 d . . . C(63) C 0.8567(5) 0.6090(2) 0.9038(4) 0.044(2) Uani 1.00 d . . . C(64) C 0.9238(5) 0.6340(2) 0.9313(4) 0.046(2) Uani 1.00 d . . . C(65) C 0.9039(4) 0.6726(2) 0.9258(4) 0.040(2) Uani 1.00 d . . . C(66) C 0.8213(4) 0.6846(2) 0.8944(3) 0.031(2) Uani 1.00 d . . . C(67) C 1.0150(5) 0.6199(2) 0.9697(5) 0.063(3) Uani 1.00 d . . . C(68) C 1.0218(7) 0.6150(5) 1.0544(7) 0.153(6) Uani 1.00 d . . . C(69) C 1.0821(6) 0.6482(3) 0.9585(7) 0.097(4) Uani 1.00 d . . . C(70) C 1.0325(7) 0.5828(3) 0.934(1) 0.154(6) Uani 1.00 d . . . C(71) C 0.5488(4) 0.7986(2) 0.8098(3) 0.033(2) Uani 1.00 d . . . C(72) C 0.5250(5) 0.8376(2) 0.8108(4) 0.038(2) Uani 1.00 d . . . C(73) C 0.4410(5) 0.8487(2) 0.7810(4) 0.048(2) Uani 1.00 d . . . C(74) C 0.3759(5) 0.8231(2) 0.7487(4) 0.048(2) Uani 1.00 d . . . C(75) C 0.3973(4) 0.7850(2) 0.7493(4) 0.042(2) Uani 1.00 d . . . C(76) C 0.4826(4) 0.7737(2) 0.7790(3) 0.035(2) Uani 1.00 d . . . C(77) C 0.2846(6) 0.8374(3) 0.7123(6) 0.077(3) Uani 1.00 d . . . C(78) C 0.2273(9) 0.8090(4) 0.681(2) 0.266(10) Uani 1.00 d . . . C(79) C 0.2887(9) 0.8653(7) 0.651(1) 0.24(1) Uani 1.00 d . . . C(80) C 0.2524(9) 0.8614(6) 0.766(1) 0.205(9) Uani 1.00 d . . . C(101) C 0.7981 0.5215 1.0345 0.1036 Uani 1.00 d . . . C(102) C 0.1572 0.7545 0.4488 0.1537 Uani 1.00 d . . . C(103) C 0.7943 0.9723 0.8929 0.1020 Uani 1.00 d . . . C(104) C 0.5457 0.9996 0.9960 0.0935 Uiso 0.50 d P . . H(1) H 0.5851 0.9571 0.5821 0.0485 Uiso 1.00 calc . . . H(2) H 0.5328 0.9423 0.7909 0.0520 Uiso 1.00 calc . . . H(3) H 0.4168 0.7905 0.4322 0.0387 Uiso 1.00 calc . . . H(4) H 0.5054 0.8983 0.4740 0.0475 Uiso 1.00 calc . . . H(5) H 0.4316 0.6652 0.6876 0.0471 Uiso 1.00 calc . . . H(6) H 0.4712 0.6823 0.4737 0.0426 Uiso 1.00 calc . . . H(7) H 0.8836 0.8003 0.8931 0.0417 Uiso 1.00 calc . . . H(8) H 0.9288 0.8120 0.6801 0.0381 Uiso 1.00 calc . . . H(9) H 0.7814 0.5207 0.8029 0.0543 Uiso 1.00 calc . . . H(10) H 0.8147 0.5337 0.5862 0.0551 Uiso 1.00 calc . . . H(11) H 0.8682 0.5822 0.9072 0.0491 Uiso 1.00 calc . . . H(12) H 0.9474 0.6905 0.9439 0.0484 Uiso 1.00 calc . . . H(13) H 0.9816 0.5958 1.0628 0.1384 Uiso 1.00 calc . . . H(14) H 1.0782 0.6059 1.0800 0.1384 Uiso 1.00 calc . . . H(15) H 1.0108 0.6376 1.0785 0.1384 Uiso 1.00 calc . . . H(16) H 0.8117 0.4593 0.7920 0.0978 Uiso 1.00 calc . . . H(17) H 0.8972 0.4416 0.7835 0.0978 Uiso 1.00 calc . . . H(18) H 0.8966 0.4819 0.8189 0.0978 Uiso 1.00 calc . . . H(19) H 0.7434 0.4517 0.6495 0.1198 Uiso 1.00 calc . . . H(20) H 0.7905 0.4660 0.5884 0.1198 Uiso 1.00 calc . . . H(21) H 0.8261 0.4315 0.6406 0.1198 Uiso 1.00 calc . . . H(22) H 0.9742 0.4662 0.6910 0.1277 Uiso 1.00 calc . . . H(23) H 0.9399 0.5006 0.6379 0.1277 Uiso 1.00 calc . . . H(24) H 0.9740 0.5065 0.7267 0.1277 Uiso 1.00 calc . . . H(25) H 0.4084 0.8992 0.3324 0.1008 Uiso 1.00 calc . . . H(26) H 0.3809 0.8604 0.2925 0.1008 Uiso 1.00 calc . . . H(27) H 0.3122 0.8907 0.2974 0.1008 Uiso 1.00 calc . . . H(28) H 0.2349 0.8433 0.3639 0.0932 Uiso 1.00 calc . . . H(29) H 0.3024 0.8128 0.3575 0.0932 Uiso 1.00 calc . . . H(30) H 0.2853 0.8224 0.4377 0.0932 Uiso 1.00 calc . . . H(31) H 0.3761 0.9160 0.4582 0.1050 Uiso 1.00 calc . . . H(32) H 0.2800 0.9075 0.4228 0.1050 Uiso 1.00 calc . . . H(33) H 0.3275 0.8876 0.4989 0.1050 Uiso 1.00 calc . . . H(34) H 1.1382 0.6375 0.9800 0.1076 Uiso 1.00 calc . . . H(35) H 1.0775 0.6506 0.9026 0.1076 Uiso 1.00 calc . . . H(36) H 1.0764 0.6714 0.9794 0.1076 Uiso 1.00 calc . . . H(37) H 0.5438 1.0199 0.5920 0.0933 Uiso 1.00 calc . . . H(38) H 0.4636 0.9956 0.5555 0.0933 Uiso 1.00 calc . . . H(39) H 0.4533 1.0345 0.5935 0.0933 Uiso 1.00 calc . . . H(40) H 0.3670 1.0042 0.6739 0.1335 Uiso 1.00 calc . . . H(41) H 0.3767 0.9652 0.6364 0.1335 Uiso 1.00 calc . . . H(42) H 0.4007 0.9695 0.7260 0.1335 Uiso 1.00 calc . . . H(43) H 0.5360 1.0068 0.7903 0.1129 Uiso 1.00 calc . . . H(44) H 0.5919 1.0249 0.7399 0.1129 Uiso 1.00 calc . . . H(45) H 0.5021 1.0415 0.7380 0.1129 Uiso 1.00 calc . . . H(46) H 0.3950 0.5896 0.4658 0.1424 Uiso 1.00 calc . . . H(47) H 0.4012 0.6309 0.4367 0.1424 Uiso 1.00 calc . . . H(48) H 0.4822 0.6108 0.4856 0.1424 Uiso 1.00 calc . . . H(49) H 0.4335 0.6026 0.6635 0.1521 Uiso 1.00 calc . . . H(50) H 0.4157 0.5722 0.5982 0.1521 Uiso 1.00 calc . . . H(51) H 0.5026 0.5936 0.6185 0.1521 Uiso 1.00 calc . . . H(52) H 0.1684 0.8189 0.6583 0.1655 Uiso 1.00 calc . . . H(53) H 0.2414 0.7914 0.6505 0.1655 Uiso 1.00 calc . . . H(54) H 0.2145 0.7942 0.7285 0.1655 Uiso 1.00 calc . . . H(55) H 0.3304 0.8880 0.6713 0.1792 Uiso 1.00 calc . . . H(56) H 0.3136 0.8565 0.6082 0.1792 Uiso 1.00 calc . . . H(57) H 0.2375 0.8790 0.6257 0.1792 Uiso 1.00 calc . . . H(58) H 0.2898 0.8844 0.7848 0.1774 Uiso 1.00 calc . . . H(59) H 0.1968 0.8756 0.7390 0.1774 Uiso 1.00 calc . . . H(60) H 0.2409 0.8501 0.8085 0.1774 Uiso 1.00 calc . . . H(61) H 1.0550 0.5880 0.5707 0.1254 Uiso 1.00 calc . . . H(62) H 1.0986 0.6227 0.5423 0.1254 Uiso 1.00 calc . . . H(63) H 1.1514 0.5960 0.6057 0.1254 Uiso 1.00 calc . . . H(64) H 1.1958 0.6523 0.6924 0.1005 Uiso 1.00 calc . . . H(65) H 1.1414 0.6793 0.6306 0.1005 Uiso 1.00 calc . . . H(66) H 1.1283 0.6789 0.7143 0.1005 Uiso 1.00 calc . . . H(67) H 1.0615 0.6236 0.7629 0.1376 Uiso 1.00 calc . . . H(68) H 1.0320 0.5886 0.7099 0.1376 Uiso 1.00 calc . . . H(69) H 1.1289 0.5969 0.7414 0.1376 Uiso 1.00 calc . . . H(70) H 0.9366 0.8941 0.8901 0.1356 Uiso 1.00 calc . . . H(71) H 0.8512 0.8726 0.8582 0.1356 Uiso 1.00 calc . . . H(72) H 0.9239 0.8537 0.9205 0.1356 Uiso 1.00 calc . . . H(73) H 0.9524 0.9031 0.7619 0.2100 Uiso 1.00 calc . . . H(74) H 0.9483 0.8695 0.7044 0.2100 Uiso 1.00 calc . . . H(75) H 0.8666 0.8820 0.7297 0.2100 Uiso 1.00 calc . . . H(76) H 1.0563 0.8340 0.8881 0.2010 Uiso 1.00 calc . . . H(77) H 1.0691 0.8390 0.8048 0.2010 Uiso 1.00 calc . . . H(78) H 1.0669 0.8743 0.8565 0.2010 Uiso 1.00 calc . . . H(79) H 0.9950 0.5632 0.9351 0.1381 Uiso 1.00 calc . . . H(80) H 1.0301 0.5871 0.8761 0.1381 Uiso 1.00 calc . . . H(81) H 1.0911 0.5742 0.9535 0.1381 Uiso 1.00 calc . . . H(82) H 1.0094 0.7055 0.6381 0.0489 Uiso 1.00 calc . . . H(83) H 0.9229 0.5982 0.5908 0.0549 Uiso 1.00 calc . . . H(84) H 0.4275 0.8757 0.7833 0.0552 Uiso 1.00 calc . . . H(85) H 0.3540 0.7664 0.7294 0.0500 Uiso 1.00 calc . . . H(86) H 0.6821 0.6762 0.5159 0.0544 Uiso 1.00 calc . . . H(89) H 0.6736 0.8059 0.8524 0.0544 Uiso 1.00 calc . . . H(91) H 0.7398 0.8209 0.5605 0.0544 Uiso 1.00 calc . . . H(92) H 0.6166 0.6577 0.8156 0.0544 Uiso 1.00 calc . . . H(93) H 0.7464 0.6967 0.7484 0.0544 Uiso 1.00 calc . . . H(95) H 0.5985 0.7869 0.6297 0.0544 Uiso 1.00 calc . . . H(96) H 0.6619 0.6369 0.7068 0.0544 Uiso 1.00 calc . . . H(97) H 0.7603 0.6990 0.6651 0.0544 Uiso 1.00 calc . . . H(98) H 0.7605 0.5412 1.0058 0.1210 Uiso 1.00 calc . . . H(99) H 0.1723 0.7816 0.4669 0.1804 Uiso 1.00 calc . . . H(100) H 0.7703 0.9482 0.9072 0.1246 Uiso 1.00 calc . . . H(101) H 0.5776 1.0195 0.9804 0.1083 Uiso 0.50 calc 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0372(3) 0.0343(3) 0.0251(2) 0.0050(2) 0.0129(2) 0.0034(2) Pd(2) 0.0353(3) 0.0309(3) 0.0241(2) 0.0015(2) 0.0114(2) 0.0006(2) Cl(1) 0.2051 0.2048 0.1404 -0.0822 0.0089 -0.0360 Cl(2) 0.1318 0.1426 0.4639 -0.0410 0.1071 -0.0373 Cl(3) 0.3365 0.1248 0.1384 0.1120 0.1039 0.0432 Cl(4) 0.2947 0.1419 0.1879 -0.0607 0.1069 -0.0096 Cl(5) 0.2099 0.1550 0.1814 -0.0304 0.0414 0.0457 Cl(6) 0.1958 0.1496 0.7346 0.0724 0.1440 0.0950 Cl(7) 0.1086 0.1698 0.1181 -0.0119 0.0327 -0.0193 Cl(8) 0.1650 0.2353 0.1220 0.0262 0.0211 -0.0597 Cl(9) 0.2195 0.3147 0.1486 0.1562 0.0285 -0.0458 S(1) 0.049(1) 0.0332(9) 0.0466(10) -0.0032(8) 0.0202(8) -0.0033(8) S(2) 0.062(1) 0.0395(10) 0.0291(8) 0.0096(9) 0.0053(8) -0.0025(7) S(3) 0.0387(9) 0.0426(9) 0.0255(8) 0.0004(8) 0.0143(7) 0.0042(7) S(4) 0.0366(9) 0.0323(8) 0.0203(7) 0.0000(7) 0.0095(6) -0.0005(6) S(5) 0.050(1) 0.0342(9) 0.050(1) -0.0040(8) 0.0193(9) 0.0015(8) S(6) 0.063(1) 0.0328(9) 0.0347(9) 0.0049(8) 0.0032(8) -0.0012(7) S(7) 0.0349(9) 0.0371(8) 0.0244(7) -0.0008(8) 0.0127(6) -0.0007(7) S(8) 0.0397(10) 0.0343(9) 0.0217(7) 0.0013(7) 0.0099(7) 0.0004(6) N(1) 0.060(4) 0.033(3) 0.049(4) 0.013(3) 0.015(3) 0.002(3) N(2) 0.035(3) 0.045(3) 0.021(2) -0.003(2) 0.011(2) 0.002(2) N(3) 0.047(3) 0.035(3) 0.038(3) -0.009(3) 0.022(3) 0.004(2) N(4) 0.036(3) 0.034(3) 0.029(3) -0.006(2) 0.003(2) 0.000(2) N(5) 0.064(4) 0.035(3) 0.050(4) 0.016(3) 0.018(3) 0.003(3) N(6) 0.034(3) 0.039(3) 0.042(3) 0.000(3) 0.002(3) 0.001(3) N(7) 0.042(3) 0.039(3) 0.029(3) -0.013(3) 0.012(2) 0.001(2) N(8) 0.035(3) 0.034(3) 0.042(3) 0.004(2) 0.009(3) 0.000(2) C(1) 0.043(4) 0.030(3) 0.041(4) 0.000(3) 0.005(3) -0.005(3) C(2) 0.042(4) 0.036(4) 0.037(4) 0.001(3) 0.009(3) -0.006(3) C(3) 0.058(5) 0.034(4) 0.038(4) 0.001(3) 0.011(3) 0.003(3) C(4) 0.060(5) 0.032(4) 0.049(4) 0.010(3) 0.013(4) 0.000(3) C(5) 0.057(5) 0.044(4) 0.043(4) 0.009(4) 0.016(4) -0.007(3) C(6) 0.048(4) 0.029(3) 0.039(4) 0.005(3) 0.007(3) -0.002(3) C(7) 0.075(6) 0.038(4) 0.051(4) 0.020(4) 0.024(4) 0.003(3) C(8) 0.23(2) 0.068(7) 0.067(7) 0.066(9) -0.001(8) -0.009(5) C(9) 0.110(10) 0.082(8) 0.21(1) 0.055(7) 0.075(10) 0.057(9) C(10) 0.14(1) 0.073(7) 0.085(7) 0.050(7) 0.048(7) 0.020(6) C(11) 0.040(4) 0.033(3) 0.018(3) 0.002(3) 0.009(3) 0.000(2) C(12) 0.041(4) 0.031(3) 0.022(3) 0.004(3) 0.010(3) 0.003(3) C(13) 0.039(4) 0.047(4) 0.026(3) -0.002(3) 0.009(3) 0.001(3) C(14) 0.047(4) 0.045(4) 0.028(3) 0.011(3) 0.008(3) 0.002(3) C(15) 0.046(4) 0.040(4) 0.039(4) 0.010(3) 0.014(3) 0.006(3) C(16) 0.042(4) 0.032(3) 0.031(3) -0.002(3) 0.015(3) -0.001(3) C(17) 0.040(5) 0.060(5) 0.053(5) 0.019(4) 0.006(4) 0.008(4) C(18) 0.062(7) 0.103(8) 0.124(9) 0.042(6) 0.011(6) -0.020(7) C(19) 0.074(7) 0.14(1) 0.070(6) 0.033(7) 0.005(5) 0.050(7) C(20) 0.038(5) 0.086(7) 0.121(9) 0.014(5) -0.010(5) 0.019(6) C(21) 0.036(4) 0.034(3) 0.026(3) -0.001(3) 0.011(3) 0.003(3) C(22) 0.038(4) 0.035(3) 0.028(3) 0.002(3) 0.013(3) -0.002(3) C(23) 0.044(4) 0.043(4) 0.041(4) -0.007(3) 0.018(3) 0.007(3) C(24) 0.044(4) 0.043(4) 0.040(4) -0.008(3) 0.014(3) -0.003(3) C(25) 0.042(4) 0.039(4) 0.030(3) -0.004(3) 0.010(3) -0.005(3) C(26) 0.038(4) 0.032(3) 0.027(3) 0.001(3) 0.013(3) 0.002(3) C(27) 0.083(6) 0.041(4) 0.056(5) -0.027(4) 0.026(4) -0.013(4) C(28) 0.38(3) 0.12(1) 0.15(1) -0.18(1) 0.16(2) -0.088(10) C(29) 0.080(10) 0.11(1) 0.47(3) -0.061(9) 0.07(1) -0.13(2) C(30) 0.46(3) 0.061(8) 0.091(10) -0.10(1) -0.01(1) 0.001(7) C(31) 0.031(3) 0.041(4) 0.022(3) 0.007(3) 0.007(3) -0.002(2) C(32) 0.036(4) 0.035(3) 0.025(3) -0.003(3) 0.008(3) 0.001(3) C(33) 0.043(4) 0.041(4) 0.026(3) -0.001(3) 0.009(3) -0.004(3) C(34) 0.046(4) 0.032(3) 0.038(4) -0.009(3) 0.010(3) -0.002(3) C(35) 0.040(4) 0.046(4) 0.033(3) -0.005(3) 0.014(3) 0.000(3) C(36) 0.035(4) 0.040(4) 0.026(3) -0.002(3) 0.011(3) 0.001(3) C(37) 0.069(6) 0.043(4) 0.049(4) -0.016(4) 0.015(4) -0.006(4) C(38) 0.31(2) 0.073(8) 0.17(1) -0.11(1) 0.17(1) -0.079(8) C(39) 0.39(3) 0.052(7) 0.078(8) -0.08(1) 0.03(1) -0.003(6) C(40) 0.076(10) 0.09(1) 0.56(4) -0.029(8) 0.00(2) -0.11(2) C(41) 0.042(4) 0.035(4) 0.022(3) 0.013(3) 0.011(3) 0.004(2) C(42) 0.043(4) 0.038(4) 0.023(3) 0.002(3) 0.014(3) 0.002(3) C(43) 0.037(4) 0.056(5) 0.033(3) 0.001(4) 0.010(3) 0.000(3) C(44) 0.046(5) 0.060(5) 0.037(4) 0.014(4) 0.013(3) 0.002(4) C(45) 0.053(5) 0.052(4) 0.033(4) 0.024(4) 0.011(3) 0.004(3) C(46) 0.047(4) 0.039(4) 0.024(3) 0.006(3) 0.009(3) 0.000(3) C(47) 0.048(5) 0.077(6) 0.069(6) 0.022(5) -0.002(4) 0.008(5) C(48) 0.063(7) 0.16(1) 0.16(1) 0.057(8) 0.001(7) -0.06(1) C(49) 0.040(6) 0.122(10) 0.14(1) 0.027(6) -0.009(6) 0.005(8) C(50) 0.080(9) 0.19(1) 0.13(1) 0.023(9) -0.017(7) 0.09(1) C(51) 0.037(4) 0.035(4) 0.043(4) 0.002(3) 0.007(3) -0.002(3) C(52) 0.046(4) 0.034(4) 0.040(4) -0.003(3) 0.012(3) -0.001(3) C(53) 0.049(4) 0.033(4) 0.050(4) -0.001(3) 0.015(4) 0.003(3) C(54) 0.059(5) 0.033(4) 0.051(4) 0.006(3) 0.012(4) 0.003(3) C(55) 0.058(5) 0.036(4) 0.043(4) 0.006(3) 0.012(4) -0.001(3) C(56) 0.049(4) 0.035(4) 0.036(4) 0.003(3) 0.004(3) 0.003(3) C(57) 0.095(7) 0.046(5) 0.067(6) 0.029(5) 0.031(5) 0.014(4) C(58) 0.24(2) 0.044(6) 0.114(10) 0.054(8) -0.01(1) -0.014(6) C(59) 0.14(1) 0.113(10) 0.23(2) 0.097(9) 0.12(1) 0.10(1) C(60) 0.16(1) 0.060(6) 0.083(7) 0.047(7) 0.048(7) 0.030(5) C(61) 0.037(4) 0.032(3) 0.029(3) 0.004(3) 0.014(3) 0.005(3) C(62) 0.044(4) 0.030(3) 0.037(3) 0.001(3) 0.013(3) 0.006(3) C(63) 0.050(5) 0.038(4) 0.043(4) 0.009(3) 0.009(3) 0.006(3) C(64) 0.045(5) 0.048(4) 0.043(4) 0.006(4) 0.007(3) 0.010(3) C(65) 0.041(4) 0.040(4) 0.036(4) 0.002(3) 0.003(3) 0.005(3) C(66) 0.034(4) 0.034(3) 0.024(3) 0.003(3) 0.007(3) 0.004(3) C(67) 0.047(5) 0.058(5) 0.077(6) 0.011(4) -0.003(4) 0.021(5) C(68) 0.059(7) 0.28(2) 0.105(10) 0.014(9) -0.007(7) 0.11(1) C(69) 0.041(6) 0.108(9) 0.14(1) 0.018(6) 0.020(6) 0.030(8) C(70) 0.078(8) 0.083(8) 0.27(2) 0.049(7) -0.016(10) -0.04(1) C(71) 0.042(4) 0.040(4) 0.019(3) 0.006(3) 0.011(3) 0.004(3) C(72) 0.048(4) 0.041(4) 0.026(3) 0.008(3) 0.011(3) 0.002(3) C(73) 0.056(5) 0.053(5) 0.035(4) 0.026(4) 0.014(4) 0.005(3) C(74) 0.039(5) 0.066(5) 0.037(4) 0.018(4) 0.004(3) 0.001(4) C(75) 0.038(4) 0.057(5) 0.032(3) 0.008(3) 0.013(3) 0.002(3) C(76) 0.048(4) 0.043(4) 0.015(3) 0.007(3) 0.010(3) 0.001(3) C(77) 0.054(6) 0.094(7) 0.073(6) 0.033(6) -0.006(5) -0.003(6) C(78) 0.078(10) 0.10(1) 0.52(4) 0.036(8) -0.13(2) -0.06(2) C(79) 0.08(1) 0.34(3) 0.26(2) 0.04(1) -0.03(1) 0.21(2) C(80) 0.075(10) 0.27(2) 0.24(2) 0.09(1) -0.01(1) -0.09(2) C(101) 0.0916 0.0650 0.1600 0.0221 0.0417 -0.0068 C(102) 0.1485 0.1378 0.1909 0.0034 0.0726 0.0161 C(103) 0.1061 0.1017 0.1046 0.0005 0.0379 0.0077 #------------------------------------------------------------------------------ _computing_data_collection 'P' _computing_cell_refinement 'P' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) S(3) 2.290(2) . . yes Pd(1) S(8) 2.291(2) . . yes Pd(1) N(2) 1.984(5) . . yes Pd(1) N(8) 2.007(5) . . yes Pd(2) S(4) 2.286(2) . . yes Pd(2) S(7) 2.301(2) . . yes Pd(2) N(4) 1.994(5) . . yes Pd(2) N(6) 2.001(6) . . yes Cl(1) C(101) 1.735 . . yes Cl(2) C(101) 1.646 . . yes Cl(3) C(101) 1.706 . . yes Cl(4) C(102) 1.781 . . yes Cl(5) C(102) 1.706 . . yes Cl(6) C(102) 1.624 . . yes Cl(7) C(103) 1.766 . . yes Cl(8) C(103) 1.702 . . yes Cl(9) C(103) 1.709 . . yes Cl(10) C(104) 1.422 . . yes Cl(11) C(104) 1.632 . . yes Cl(12) C(104) 1.823 . . yes S(1) C(2) 1.792(7) . . yes S(1) C(16) 1.788(7) . . yes S(2) C(6) 1.786(7) . . yes S(2) C(72) 1.783(7) . . yes S(3) C(22) 1.792(6) . . yes S(3) C(76) 1.778(7) . . yes S(4) C(12) 1.783(6) . . yes S(4) C(26) 1.782(6) . . yes S(5) C(52) 1.790(7) . . yes S(5) C(62) 1.777(7) . . yes S(6) C(46) 1.792(7) . . yes S(6) C(56) 1.781(7) . . yes S(7) C(36) 1.786(6) . . yes S(7) C(42) 1.778(7) . . yes S(8) C(32) 1.778(6) . . yes S(8) C(66) 1.783(6) . . yes N(1) C(1) 1.386(8) . . yes N(2) C(71) 1.394(8) . . yes N(3) C(21) 1.350(8) . . yes N(4) C(11) 1.370(8) . . yes N(5) C(51) 1.369(8) . . yes N(6) C(41) 1.365(8) . . yes N(7) C(31) 1.352(8) . . yes N(8) C(61) 1.350(8) . . yes C(1) C(2) 1.392(9) . . yes C(1) C(6) 1.413(9) . . yes C(2) C(3) 1.398(9) . . yes C(3) C(4) 1.384(9) . . yes C(4) C(5) 1.388(10) . . yes C(4) C(7) 1.532(9) . . yes C(5) C(6) 1.388(9) . . yes C(7) C(8) 1.51(1) . . yes C(7) C(9) 1.52(1) . . yes C(7) C(10) 1.50(1) . . yes C(11) C(12) 1.390(9) . . yes C(11) C(16) 1.425(8) . . yes C(12) C(13) 1.391(9) . . yes C(13) C(14) 1.392(9) . . yes C(14) C(15) 1.395(10) . . yes C(14) C(17) 1.536(9) . . yes C(15) C(16) 1.380(9) . . yes C(17) C(18) 1.52(1) . . yes C(17) C(19) 1.51(1) . . yes C(17) C(20) 1.50(1) . . yes C(21) C(22) 1.406(8) . . yes C(21) C(26) 1.415(8) . . yes C(22) C(23) 1.390(9) . . yes C(23) C(24) 1.395(9) . . yes C(24) C(25) 1.386(9) . . yes C(24) C(27) 1.534(9) . . yes C(25) C(26) 1.387(8) . . yes C(27) C(28) 1.40(1) . . yes C(27) C(29) 1.49(2) . . yes C(27) C(30) 1.46(2) . . yes C(31) C(32) 1.405(8) . . yes C(31) C(36) 1.412(8) . . yes C(32) C(33) 1.396(9) . . yes C(33) C(34) 1.384(9) . . yes C(34) C(35) 1.393(9) . . yes C(34) C(37) 1.529(9) . . yes C(35) C(36) 1.395(9) . . yes C(37) C(38) 1.46(1) . . yes C(37) C(39) 1.46(1) . . yes C(37) C(40) 1.46(2) . . yes C(41) C(42) 1.395(9) . . yes C(41) C(46) 1.420(8) . . yes C(42) C(43) 1.395(9) . . yes C(43) C(44) 1.399(10) . . yes C(44) C(45) 1.40(1) . . yes C(44) C(47) 1.54(1) . . yes C(45) C(46) 1.386(9) . . yes C(47) C(48) 1.52(1) . . yes C(47) C(49) 1.51(1) . . yes C(47) C(50) 1.49(1) . . yes C(51) C(52) 1.407(9) . . yes C(51) C(56) 1.391(9) . . yes C(52) C(53) 1.394(9) . . yes C(53) C(54) 1.387(10) . . yes C(54) C(55) 1.392(9) . . yes C(54) C(57) 1.532(10) . . yes C(55) C(56) 1.395(9) . . yes C(57) C(58) 1.50(1) . . yes C(57) C(59) 1.50(1) . . yes C(57) C(60) 1.50(1) . . yes C(61) C(62) 1.429(8) . . yes C(61) C(66) 1.401(9) . . yes C(62) C(63) 1.378(9) . . yes C(63) C(64) 1.387(10) . . yes C(64) C(65) 1.394(9) . . yes C(64) C(67) 1.54(1) . . yes C(65) C(66) 1.377(9) . . yes C(67) C(68) 1.49(1) . . yes C(67) C(69) 1.52(1) . . yes C(67) C(70) 1.51(1) . . yes C(71) C(72) 1.427(9) . . yes C(71) C(76) 1.386(9) . . yes C(72) C(73) 1.383(10) . . yes C(73) C(74) 1.40(1) . . yes C(74) C(75) 1.385(10) . . yes C(74) C(77) 1.54(1) . . yes C(75) C(76) 1.403(9) . . yes C(77) C(78) 1.38(2) . . yes C(77) C(79) 1.48(2) . . yes C(77) C(80) 1.46(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(3) Pd(1) S(8) 178.70(6) . . . yes S(3) Pd(1) N(2) 85.8(2) . . . yes S(3) Pd(1) N(8) 94.6(2) . . . yes S(8) Pd(1) N(2) 94.4(2) . . . yes S(8) Pd(1) N(8) 85.1(2) . . . yes N(2) Pd(1) N(8) 175.8(2) . . . yes S(4) Pd(2) S(7) 179.44(6) . . . yes S(4) Pd(2) N(4) 85.3(2) . . . yes S(4) Pd(2) N(6) 94.9(2) . . . yes S(7) Pd(2) N(4) 95.0(2) . . . yes S(7) Pd(2) N(6) 84.8(2) . . . yes N(4) Pd(2) N(6) 176.6(2) . . . yes C(2) S(1) C(16) 100.0(3) . . . yes C(6) S(2) C(72) 100.1(3) . . . yes Pd(1) S(3) C(22) 106.2(2) . . . yes Pd(1) S(3) C(76) 98.0(2) . . . yes C(22) S(3) C(76) 104.6(3) . . . yes Pd(2) S(4) C(12) 98.2(2) . . . yes Pd(2) S(4) C(26) 105.7(2) . . . yes C(12) S(4) C(26) 108.4(3) . . . yes C(52) S(5) C(62) 100.4(3) . . . yes C(46) S(6) C(56) 100.8(3) . . . yes Pd(2) S(7) C(36) 104.5(2) . . . yes Pd(2) S(7) C(42) 98.4(2) . . . yes C(36) S(7) C(42) 106.9(3) . . . yes Pd(1) S(8) C(32) 105.0(2) . . . yes Pd(1) S(8) C(66) 98.5(2) . . . yes C(32) S(8) C(66) 107.3(3) . . . yes Pd(1) N(2) C(71) 118.4(4) . . . yes Pd(2) N(4) C(11) 119.4(4) . . . yes Pd(2) N(6) C(41) 119.8(4) . . . yes Pd(1) N(8) C(61) 119.0(4) . . . yes N(1) C(1) C(2) 122.3(6) . . . yes N(1) C(1) C(6) 121.1(6) . . . yes C(2) C(1) C(6) 116.6(6) . . . yes S(1) C(2) C(1) 120.5(5) . . . yes S(1) C(2) C(3) 118.4(5) . . . yes C(1) C(2) C(3) 121.1(6) . . . yes C(2) C(3) C(4) 122.9(6) . . . yes C(3) C(4) C(5) 115.5(6) . . . yes C(3) C(4) C(7) 123.9(6) . . . yes C(5) C(4) C(7) 120.5(6) . . . yes C(4) C(5) C(6) 123.2(6) . . . yes S(2) C(6) C(1) 121.2(5) . . . yes S(2) C(6) C(5) 118.2(5) . . . yes C(1) C(6) C(5) 120.6(6) . . . yes C(4) C(7) C(8) 110.3(7) . . . yes C(4) C(7) C(9) 108.3(7) . . . yes C(4) C(7) C(10) 112.6(6) . . . yes C(8) C(7) C(9) 108.3(9) . . . yes C(8) C(7) C(10) 109.2(8) . . . yes C(9) C(7) C(10) 108.0(9) . . . yes N(4) C(11) C(12) 119.9(6) . . . yes N(4) C(11) C(16) 125.1(6) . . . yes C(12) C(11) C(16) 114.9(6) . . . yes S(4) C(12) C(11) 116.8(5) . . . yes S(4) C(12) C(13) 119.3(5) . . . yes C(11) C(12) C(13) 123.7(6) . . . yes C(12) C(13) C(14) 120.9(6) . . . yes C(13) C(14) C(15) 116.1(6) . . . yes C(13) C(14) C(17) 123.2(7) . . . yes C(15) C(14) C(17) 120.6(6) . . . yes C(14) C(15) C(16) 123.3(6) . . . yes S(1) C(16) C(11) 119.4(5) . . . yes S(1) C(16) C(15) 119.6(5) . . . yes C(11) C(16) C(15) 120.9(6) . . . yes C(14) C(17) C(18) 110.0(7) . . . yes C(14) C(17) C(19) 108.8(7) . . . yes C(14) C(17) C(20) 112.2(7) . . . yes C(18) C(17) C(19) 108.3(8) . . . yes C(18) C(17) C(20) 107.3(8) . . . yes C(19) C(17) C(20) 110.2(8) . . . yes N(3) C(21) C(22) 123.1(5) . . . yes N(3) C(21) C(26) 122.3(5) . . . yes C(22) C(21) C(26) 114.6(5) . . . yes S(3) C(22) C(21) 122.8(5) . . . yes S(3) C(22) C(23) 114.9(5) . . . yes C(21) C(22) C(23) 122.2(5) . . . yes C(22) C(23) C(24) 122.3(6) . . . yes C(23) C(24) C(25) 115.9(6) . . . yes C(23) C(24) C(27) 122.0(6) . . . yes C(25) C(24) C(27) 122.0(6) . . . yes C(24) C(25) C(26) 122.3(6) . . . yes S(4) C(26) C(21) 122.1(5) . . . yes S(4) C(26) C(25) 115.1(4) . . . yes C(21) C(26) C(25) 122.3(5) . . . yes C(24) C(27) C(28) 112.6(7) . . . yes C(24) C(27) C(29) 109.9(8) . . . yes C(24) C(27) C(30) 110.6(8) . . . yes C(28) C(27) C(29) 109(1) . . . yes C(28) C(27) C(30) 110(1) . . . yes C(29) C(27) C(30) 103(1) . . . yes N(7) C(31) C(32) 121.5(5) . . . yes N(7) C(31) C(36) 122.7(5) . . . yes C(32) C(31) C(36) 115.8(6) . . . yes S(8) C(32) C(31) 124.4(5) . . . yes S(8) C(32) C(33) 113.8(4) . . . yes C(31) C(32) C(33) 121.3(5) . . . yes C(32) C(33) C(34) 122.5(5) . . . yes C(33) C(34) C(35) 116.5(6) . . . yes C(33) C(34) C(37) 122.4(6) . . . yes C(35) C(34) C(37) 121.1(6) . . . yes C(34) C(35) C(36) 121.9(6) . . . yes S(7) C(36) C(31) 123.6(5) . . . yes S(7) C(36) C(35) 114.5(4) . . . yes C(31) C(36) C(35) 121.6(5) . . . yes C(34) C(37) C(38) 112.3(7) . . . yes C(34) C(37) C(39) 112.0(7) . . . yes C(34) C(37) C(40) 108.9(8) . . . yes C(38) C(37) C(39) 106(1) . . . yes C(38) C(37) C(40) 107(1) . . . yes C(39) C(37) C(40) 109(1) . . . yes N(6) C(41) C(42) 120.2(6) . . . yes N(6) C(41) C(46) 124.0(6) . . . yes C(42) C(41) C(46) 115.6(6) . . . yes S(7) C(42) C(41) 116.7(5) . . . yes S(7) C(42) C(43) 119.6(5) . . . yes C(41) C(42) C(43) 123.7(6) . . . yes C(42) C(43) C(44) 120.0(7) . . . yes C(43) C(44) C(45) 117.0(7) . . . yes C(43) C(44) C(47) 122.7(7) . . . yes C(45) C(44) C(47) 120.2(7) . . . yes C(44) C(45) C(46) 122.9(7) . . . yes S(6) C(46) C(41) 119.8(5) . . . yes S(6) C(46) C(45) 119.4(5) . . . yes C(41) C(46) C(45) 120.7(7) . . . yes C(44) C(47) C(48) 109.3(7) . . . yes C(44) C(47) C(49) 112.6(8) . . . yes C(44) C(47) C(50) 109.4(8) . . . yes C(48) C(47) C(49) 107.5(9) . . . yes C(48) C(47) C(50) 109(1) . . . yes C(49) C(47) C(50) 108.2(9) . . . yes N(5) C(51) C(52) 122.0(6) . . . yes N(5) C(51) C(56) 120.3(6) . . . yes C(52) C(51) C(56) 117.6(6) . . . yes S(5) C(52) C(51) 121.5(5) . . . yes S(5) C(52) C(53) 117.9(5) . . . yes C(51) C(52) C(53) 120.6(6) . . . yes C(52) C(53) C(54) 122.1(6) . . . yes C(53) C(54) C(55) 116.6(6) . . . yes C(53) C(54) C(57) 123.1(7) . . . yes C(55) C(54) C(57) 120.3(7) . . . yes C(54) C(55) C(56) 122.5(6) . . . yes S(6) C(56) C(51) 121.2(5) . . . yes S(6) C(56) C(55) 118.3(5) . . . yes C(51) C(56) C(55) 120.5(6) . . . yes C(54) C(57) C(58) 110.4(8) . . . yes C(54) C(57) C(59) 108.6(8) . . . yes C(54) C(57) C(60) 112.6(7) . . . yes C(58) C(57) C(59) 108(1) . . . yes C(58) C(57) C(60) 108.9(9) . . . yes C(59) C(57) C(60) 107.8(9) . . . yes N(8) C(61) C(62) 123.5(6) . . . yes N(8) C(61) C(66) 121.1(6) . . . yes C(62) C(61) C(66) 115.2(6) . . . yes S(5) C(62) C(61) 119.5(5) . . . yes S(5) C(62) C(63) 120.1(5) . . . yes C(61) C(62) C(63) 120.2(6) . . . yes C(62) C(63) C(64) 123.6(7) . . . yes C(63) C(64) C(65) 116.6(7) . . . yes C(63) C(64) C(67) 121.8(7) . . . yes C(65) C(64) C(67) 121.5(7) . . . yes C(64) C(65) C(66) 120.7(6) . . . yes S(8) C(66) C(61) 115.9(5) . . . yes S(8) C(66) C(65) 120.4(5) . . . yes C(61) C(66) C(65) 123.6(6) . . . yes C(64) C(67) C(68) 108.2(8) . . . yes C(64) C(67) C(69) 111.3(7) . . . yes C(64) C(67) C(70) 110.2(8) . . . yes C(68) C(67) C(69) 109.1(9) . . . yes C(68) C(67) C(70) 110(1) . . . yes C(69) C(67) C(70) 107.5(10) . . . yes N(2) C(71) C(72) 124.7(6) . . . yes N(2) C(71) C(76) 119.7(6) . . . yes C(72) C(71) C(76) 115.4(6) . . . yes S(2) C(72) C(71) 119.0(5) . . . yes S(2) C(72) C(73) 120.4(6) . . . yes C(71) C(72) C(73) 120.5(7) . . . yes C(72) C(73) C(74) 122.9(7) . . . yes C(73) C(74) C(75) 117.4(6) . . . yes C(73) C(74) C(77) 120.6(7) . . . yes C(75) C(74) C(77) 122.1(8) . . . yes C(74) C(75) C(76) 119.8(7) . . . yes S(3) C(76) C(71) 117.2(5) . . . yes S(3) C(76) C(75) 118.9(5) . . . yes C(71) C(76) C(75) 123.9(6) . . . yes C(74) C(77) C(78) 114.1(9) . . . yes C(74) C(77) C(79) 108.5(10) . . . yes C(74) C(77) C(80) 111.5(9) . . . yes C(78) C(77) C(79) 109(1) . . . yes C(78) C(77) C(80) 111(1) . . . yes C(79) C(77) C(80) 100(1) . . . yes Cl(1) C(101) Cl(2) 108.7996(7) . . . yes Cl(1) C(101) Cl(3) 109.388(1) . . . yes Cl(2) C(101) Cl(3) 112.3281(7) . . . yes Cl(4) C(102) Cl(5) 107.099(1) . . . yes Cl(4) C(102) Cl(6) 115.2299(4) . . . yes Cl(5) C(102) Cl(6) 117.589(1) . . . yes Cl(7) C(103) Cl(8) 110.2519(7) . . . yes Cl(7) C(103) Cl(9) 108.843(1) . . . yes Cl(8) C(103) Cl(9) 110.3 . . . yes Cl(10) C(104) Cl(11) 112.3243(2) . . . yes Cl(10) C(104) Cl(12) 121.9556(3) . . . yes Cl(11) C(104) Cl(12) 100.0803(5) . . . yes #------------------------------------------------------------------------------ #===END