Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Munetaka Akita' 'Shiro Hikichi' 'Masato Kujime' _publ_contact_author_name 'Prof Munetaka Akita' _publ_contact_author_address ; Chemical Resources Laboratory Tokyo Institute of Technology 4259 Nagatsuta, Midori-ku Yokohama 226-8503 JAPAN ; _publ_contact_author_email MAKITA@RES.TITECH.AC.JP _publ_section_title ; Interaction of Hydroperoxopalladium Complexes, (TpR)(py)Pd-OOH, with Hydroxonickel and -cobalt Complexes, [(u-OH)(MTpR')]2 (M=Ni, Co), Leading to Oxidative Dehydrogenation of the Saturated Hydrocarbyl Moiety in the Ancillary Ligand (TpiPr2) ; data_compound_5a(Ni) _database_code_CSD 198038 _audit_creation_date 'Fri Jul 18 16:36:09 2003' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C62 H106 B2 N16 O3 Ni Pd ' _chemical_formula_moiety 'C62 H106 B2 N16 O3 Ni Pd ' _chemical_formula_weight 1310.34 _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 15.8998(4) _cell_length_b 23.5702(8) _cell_length_c 20.0482(6) _cell_angle_alpha 90 _cell_angle_beta 104.810(1) _cell_angle_gamma 90 _cell_volume 7263.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 64560 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 52663 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15842 _reflns_number_gt 12893 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1865 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 12893 _refine_ls_number_parameters 778 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0050 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.74 _refine_diff_density_min -2.04 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 0.18490(1) 0.19800(1) 0.03536(1) 0.03769(9) Uani 1.00 d . . . Ni(1) Ni 0.32834(3) 0.17067(2) 0.16800(2) 0.0401(1) Uani 1.00 d . . . O(1) O 0.2934(1) 0.2323(1) 0.0970(1) 0.0441(5) Uani 1.00 d . . . O(2) O 0.2317(1) 0.1318(1) 0.0968(1) 0.0471(5) Uani 1.00 d . . . O(3) O 0.2043(3) 0.3491(3) 0.0996(3) 0.132(2) Uani 1.00 d . . . N(11) N 0.3184(2) 0.1117(1) 0.2401(1) 0.0432(6) Uani 1.00 d . . . N(12) N 0.3938(2) 0.0921(1) 0.2831(1) 0.0399(6) Uani 1.00 d . . . N(21) N 0.4106(2) 0.2160(1) 0.2477(1) 0.0437(6) Uani 1.00 d . . . N(22) N 0.4756(2) 0.1842(1) 0.2910(1) 0.0415(6) Uani 1.00 d . . . N(31) N 0.4326(2) 0.1293(1) 0.1496(1) 0.0443(6) Uani 1.00 d . . . N(32) N 0.4951(2) 0.1107(1) 0.2061(1) 0.0428(6) Uani 1.00 d . . . N(41) N 0.0801(2) 0.1574(1) -0.0221(1) 0.0417(6) Uani 1.00 d . . . N(42) N 0.0025(2) 0.1862(1) -0.0454(2) 0.0419(6) Uani 1.00 d . . . N(51) N 0.1476(2) 0.2669(1) -0.0243(1) 0.0412(6) Uani 1.00 d . . . N(52) N 0.0625(2) 0.2849(1) -0.0386(2) 0.0439(6) Uani 1.00 d . . . N(61) N 0.0596(2) 0.2844(2) 0.1010(2) 0.0578(8) Uani 1.00 d . . . N(62) N -0.0012(2) 0.2506(1) 0.0585(1) 0.0443(6) Uani 1.00 d . . . N(71) N 0.6399(5) 0.0806(3) 0.9542(5) 0.161(3) Uani 1.00 d . . . N(72) N 0.8626(5) 0.0173(3) 0.6009(4) 0.138(2) Uani 1.00 d . . . N(73) N 0.6554(4) 0.1614(3) 0.6620(4) 0.143(3) Uani 1.00 d . . . N(74) N 0.164(2) 0.455(2) 0.062(2) 0.3194(2) Uiso 0.50 d P . . N(75) N 0.275(1) 0.5793(9) 0.077(1) 0.17249(8) Uiso 0.50 d P . . C(11) C 0.2529(2) 0.0808(2) 0.2548(2) 0.0510(8) Uani 1.00 d . . . C(12) C 0.2874(2) 0.0416(2) 0.3067(2) 0.0557(9) Uani 1.00 d . . . C(13) C 0.3748(2) 0.0495(2) 0.3230(2) 0.0453(7) Uani 1.00 d . . . C(14) C 0.1591(2) 0.0917(2) 0.2232(2) 0.0596(10) Uani 1.00 d . . . C(15) C 0.1308(3) 0.1457(2) 0.2072(3) 0.072(1) Uani 1.00 d . . . C(16) C 0.1013(3) 0.0423(3) 0.2150(3) 0.088(2) Uani 1.00 d . . . C(17) C 0.4433(3) 0.0180(2) 0.3752(2) 0.061(1) Uani 1.00 d . . . C(18) C 0.4886(3) -0.0247(2) 0.3415(3) 0.083(1) Uani 1.00 d . . . C(19) C 0.4020(4) -0.0131(3) 0.4280(3) 0.089(2) Uani 1.00 d . . . C(21) C 0.4238(2) 0.2695(2) 0.2692(2) 0.0487(8) Uani 1.00 d . . . C(22) C 0.4973(2) 0.2735(2) 0.3252(2) 0.0541(9) Uani 1.00 d . . . C(23) C 0.5280(2) 0.2190(2) 0.3377(2) 0.0470(7) Uani 1.00 d . . . C(24) C 0.3645(3) 0.3172(2) 0.2355(2) 0.0583(10) Uani 1.00 d . . . C(25) C 0.3366(4) 0.3533(2) 0.2895(3) 0.090(2) Uani 1.00 d . . . C(26) C 0.4069(4) 0.3525(3) 0.1922(4) 0.105(2) Uani 1.00 d . . . C(27) C 0.6038(2) 0.1972(2) 0.3932(2) 0.0572(10) Uani 1.00 d . . . C(28) C 0.6771(3) 0.2403(3) 0.4093(3) 0.104(2) Uani 1.00 d . . . C(29) C 0.5742(4) 0.1808(3) 0.4571(3) 0.091(2) Uani 1.00 d . . . C(31) C 0.4604(2) 0.1168(2) 0.0940(2) 0.0514(8) Uani 1.00 d . . . C(32) C 0.5413(3) 0.0907(2) 0.1142(2) 0.0564(9) Uani 1.00 d . . . C(33) C 0.5623(2) 0.0874(2) 0.1853(2) 0.0504(8) Uani 1.00 d . . . C(34) C 0.4070(3) 0.1314(2) 0.0218(2) 0.0598(10) Uani 1.00 d . . . C(35) C 0.3925(4) 0.0781(3) -0.0247(3) 0.086(2) Uani 1.00 d . . . C(36) C 0.4507(4) 0.1781(2) -0.0084(3) 0.083(1) Uani 1.00 d . . . C(37) C 0.6443(2) 0.0658(2) 0.2349(2) 0.066(1) Uani 1.00 d . . . C(38) C 0.6803(6) 0.0159(4) 0.2054(4) 0.170(4) Uani 1.00 d . . . C(39) C 0.7088(3) 0.1138(4) 0.2571(4) 0.121(3) Uani 1.00 d . . . C(41) C 0.0722(2) 0.1069(2) -0.0529(2) 0.0425(7) Uani 1.00 d . . . C(42) C -0.0112(2) 0.1022(2) -0.0966(2) 0.0487(8) Uani 1.00 d . . . C(43) C -0.0531(2) 0.1525(2) -0.0919(2) 0.0451(7) Uani 1.00 d . . . C(44) C 0.1442(2) 0.0640(2) -0.0384(2) 0.0477(7) Uani 1.00 d . . . C(45) C 0.1246(3) 0.0177(2) 0.0090(3) 0.077(1) Uani 1.00 d . . . C(46) C 0.1564(3) 0.0370(2) -0.1049(2) 0.079(1) Uani 1.00 d . . . C(47) C -0.1428(2) 0.1712(2) -0.1303(2) 0.0510(8) Uani 1.00 d . . . C(48) C -0.1418(3) 0.2087(2) -0.1918(3) 0.071(1) Uani 1.00 d . . . C(49) C -0.2017(3) 0.1197(2) -0.1541(3) 0.080(1) Uani 1.00 d . . . C(51) C 0.1921(2) 0.3048(2) -0.0518(2) 0.0443(7) Uani 1.00 d . . . C(52) C 0.1362(2) 0.3472(2) -0.0838(2) 0.0567(9) Uani 1.00 d . . . C(53) C 0.0552(2) 0.3334(2) -0.0753(2) 0.0559(9) Uani 1.00 d . . . C(54) C 0.2874(2) 0.2989(2) -0.0470(2) 0.0519(9) Uani 1.00 d . . . C(55) C 0.3387(3) 0.3492(3) -0.0101(3) 0.093(2) Uani 1.00 d . . . C(56) C 0.3037(3) 0.2941(3) -0.1177(2) 0.072(1) Uani 1.00 d . . . C(57) C -0.0298(3) 0.3655(2) -0.0988(4) 0.094(2) Uani 1.00 d . . . C(58) C -0.0423(7) 0.4034(5) -0.0441(6) 0.210(6) Uani 1.00 d . . . C(59) C -0.0335(4) 0.3993(3) -0.1628(4) 0.117(3) Uani 1.00 d . . . C(61) C 0.0410(2) 0.2845(2) 0.1626(2) 0.0580(9) Uani 1.00 d . . . C(62) C -0.0334(2) 0.2518(2) 0.1598(2) 0.0575(9) Uani 1.00 d . . . C(63) C -0.0591(2) 0.2310(2) 0.0929(2) 0.0463(7) Uani 1.00 d . . . C(64) C 0.0942(3) 0.3197(3) 0.2207(3) 0.075(1) Uani 1.00 d . . . C(65) C 0.0642(6) 0.3802(3) 0.2156(4) 0.132(3) Uani 1.00 d . . . C(66) C 0.0969(3) 0.2954(3) 0.2914(3) 0.087(2) Uani 1.00 d . . . C(67) C -0.1328(3) 0.1921(2) 0.0618(2) 0.0546(9) Uani 1.00 d . . . C(68) C -0.2112(3) 0.2034(2) 0.0918(3) 0.078(1) Uani 1.00 d . . . C(69) C -0.1068(3) 0.1305(2) 0.0700(3) 0.075(1) Uani 1.00 d . . . C(71) C 0.6365(4) 0.0502(3) 0.9101(4) 0.099(2) Uani 1.00 d . . . C(72) C 0.6365(4) 0.0082(3) 0.8568(4) 0.104(2) Uani 1.00 d . . . C(73) C 0.8472(4) 0.0657(4) 0.5955(4) 0.106(2) Uani 1.00 d . . . C(74) C 0.8268(5) 0.1257(4) 0.5877(6) 0.145(3) Uani 1.00 d . . . C(75) C 0.6214(4) 0.2035(3) 0.6634(3) 0.085(1) Uani 1.00 d . . . C(76) C 0.5799(6) 0.2553(3) 0.6655(4) 0.126(3) Uani 1.00 d . . . C(77) C 0.2351(8) 0.4807(6) 0.0763(6) 0.17194(5) Uiso 1.00 d . . . C(78) C 0.2728(7) 0.5286(6) 0.0752(6) 0.16380(5) Uiso 1.00 d . . . B(1) B 0.4810(2) 0.1198(2) 0.2794(2) 0.0422(8) Uani 1.00 d . . . B(2) B -0.0084(2) 0.2472(2) -0.0203(2) 0.0438(8) Uani 1.00 d . . . H(01) H 0.2792 0.2641 0.1102 0.1010 Uiso 1.00 calc . . . H(1) H 0.5280 0.1037 0.3133 0.0514 Uiso 1.00 calc . . . H(02) H 0.1783 0.1185 0.1098 0.0698 Uiso 1.00 calc . . . H(2) H -0.0692 0.2654 -0.0474 0.0437 Uiso 1.00 calc . . . H(03A) H 0.1510 0.3254 0.0999 0.0698 Uiso 1.00 calc . . . H(12) H 0.2557 0.0146 0.3264 0.0684 Uiso 1.00 calc . . . H(15A) H 0.0718 0.1529 0.1899 0.0860 Uiso 1.00 calc . . . H(15B) H 0.1706 0.1754 0.2135 0.0860 Uiso 1.00 calc . . . H(16A) H 0.0419 0.0547 0.2014 0.0879 Uiso 1.00 calc . . . H(16B) H 0.1116 0.0222 0.2580 0.0879 Uiso 1.00 calc . . . H(16C) H 0.1127 0.0177 0.1802 0.0879 Uiso 1.00 calc . . . H(17) H 0.4856 0.0450 0.4005 0.0738 Uiso 1.00 calc . . . H(18A) H 0.4480 -0.0535 0.3200 0.0835 Uiso 1.00 calc . . . H(18B) H 0.5353 -0.0417 0.3756 0.0835 Uiso 1.00 calc . . . H(18C) H 0.5114 -0.0063 0.3072 0.0835 Uiso 1.00 calc . . . H(19A) H 0.3730 0.0141 0.4500 0.0887 Uiso 1.00 calc . . . H(19B) H 0.4469 -0.0317 0.4622 0.0887 Uiso 1.00 calc . . . H(19C) H 0.3608 -0.0407 0.4043 0.0887 Uiso 1.00 calc . . . H(22) H 0.5204 0.3072 0.3499 0.0649 Uiso 1.00 calc . . . H(24) H 0.3128 0.3012 0.2057 0.0710 Uiso 1.00 calc . . . H(25A) H 0.3861 0.3733 0.3168 0.0904 Uiso 1.00 calc . . . H(25B) H 0.3130 0.3292 0.3188 0.0904 Uiso 1.00 calc . . . H(25C) H 0.2932 0.3801 0.2668 0.0904 Uiso 1.00 calc . . . H(26A) H 0.4548 0.3728 0.2213 0.1047 Uiso 1.00 calc . . . H(26B) H 0.3654 0.3790 0.1661 0.1047 Uiso 1.00 calc . . . H(26C) H 0.4278 0.3285 0.1612 0.1047 Uiso 1.00 calc . . . H(27) H 0.6260 0.1635 0.3762 0.0696 Uiso 1.00 calc . . . H(28A) H 0.7221 0.2275 0.4480 0.1041 Uiso 1.00 calc . . . H(28B) H 0.6551 0.2761 0.4201 0.1041 Uiso 1.00 calc . . . H(28C) H 0.7005 0.2446 0.3699 0.1041 Uiso 1.00 calc . . . H(29A) H 0.5541 0.2140 0.4761 0.0907 Uiso 1.00 calc . . . H(29B) H 0.6220 0.1644 0.4908 0.0907 Uiso 1.00 calc . . . H(29C) H 0.5277 0.1537 0.4447 0.0907 Uiso 1.00 calc . . . H(32) H 0.5760 0.0772 0.0848 0.0666 Uiso 1.00 calc . . . H(34) H 0.3502 0.1447 0.0254 0.0715 Uiso 1.00 calc . . . H(35A) H 0.3603 0.0504 -0.0064 0.0865 Uiso 1.00 calc . . . H(35B) H 0.4478 0.0626 -0.0261 0.0865 Uiso 1.00 calc . . . H(35C) H 0.3605 0.0884 -0.0705 0.0865 Uiso 1.00 calc . . . H(36A) H 0.5055 0.1647 -0.0140 0.0833 Uiso 1.00 calc . . . H(36B) H 0.4601 0.2102 0.0220 0.0833 Uiso 1.00 calc . . . H(36C) H 0.4142 0.1890 -0.0525 0.0833 Uiso 1.00 calc . . . H(37) H 0.6279 0.0525 0.2749 0.0803 Uiso 1.00 calc . . . H(38A) H 0.6406 -0.0154 0.2008 0.1699 Uiso 1.00 calc . . . H(38B) H 0.7353 0.0054 0.2355 0.1699 Uiso 1.00 calc . . . H(38C) H 0.6881 0.0256 0.1608 0.1699 Uiso 1.00 calc . . . H(39A) H 0.7535 0.1022 0.2967 0.1210 Uiso 1.00 calc . . . H(39B) H 0.6793 0.1464 0.2686 0.1210 Uiso 1.00 calc . . . H(39C) H 0.7345 0.1231 0.2201 0.1210 Uiso 1.00 calc . . . H(42) H -0.0351 0.0706 -0.1247 0.0573 Uiso 1.00 calc . . . H(44) H 0.1977 0.0824 -0.0146 0.0580 Uiso 1.00 calc . . . H(45A) H 0.1105 0.0350 0.0481 0.0769 Uiso 1.00 calc . . . H(45B) H 0.1748 -0.0061 0.0244 0.0769 Uiso 1.00 calc . . . H(45C) H 0.0763 -0.0047 -0.0158 0.0769 Uiso 1.00 calc . . . H(46A) H 0.1023 0.0208 -0.1305 0.0787 Uiso 1.00 calc . . . H(46B) H 0.1998 0.0078 -0.0936 0.0787 Uiso 1.00 calc . . . H(46C) H 0.1746 0.0655 -0.1324 0.0787 Uiso 1.00 calc . . . H(47) H -0.1673 0.1935 -0.0993 0.0618 Uiso 1.00 calc . . . H(48A) H -0.1062 0.2415 -0.1763 0.0712 Uiso 1.00 calc . . . H(48B) H -0.2000 0.2207 -0.2138 0.0712 Uiso 1.00 calc . . . H(48C) H -0.1185 0.1878 -0.2241 0.0712 Uiso 1.00 calc . . . H(49A) H -0.2598 0.1323 -0.1754 0.0798 Uiso 1.00 calc . . . H(49B) H -0.2022 0.0962 -0.1151 0.0798 Uiso 1.00 calc . . . H(49C) H -0.1800 0.0982 -0.1869 0.0798 Uiso 1.00 calc . . . H(52) H 0.1504 0.3796 -0.1079 0.0690 Uiso 1.00 calc . . . H(54) H 0.3081 0.2650 -0.0215 0.0625 Uiso 1.00 calc . . . H(55A) H 0.3992 0.3443 -0.0082 0.0929 Uiso 1.00 calc . . . H(55B) H 0.3314 0.3516 0.0359 0.0929 Uiso 1.00 calc . . . H(55C) H 0.3178 0.3834 -0.0347 0.0929 Uiso 1.00 calc . . . H(56A) H 0.2703 0.2631 -0.1423 0.0722 Uiso 1.00 calc . . . H(56B) H 0.3644 0.2873 -0.1131 0.0722 Uiso 1.00 calc . . . H(56C) H 0.2867 0.3287 -0.1427 0.0722 Uiso 1.00 calc . . . H(57) H -0.0775 0.3391 -0.1094 0.1096 Uiso 1.00 calc . . . H(58A) H -0.0063 0.4364 -0.0419 0.2097 Uiso 1.00 calc . . . H(58B) H -0.0266 0.3839 -0.0006 0.2097 Uiso 1.00 calc . . . H(58C) H -0.1022 0.4147 -0.0539 0.2097 Uiso 1.00 calc . . . H(59A) H 0.0113 0.4277 -0.1531 0.1165 Uiso 1.00 calc . . . H(59B) H -0.0893 0.4173 -0.1778 0.1165 Uiso 1.00 calc . . . H(59C) H -0.0247 0.3746 -0.1985 0.1165 Uiso 1.00 calc . . . H(62) H -0.0600 0.2445 0.1970 0.0675 Uiso 1.00 calc . . . H(64) H 0.1525 0.3200 0.2155 0.0916 Uiso 1.00 calc . . . H(65A) H 0.1023 0.4022 0.2511 0.1316 Uiso 1.00 calc . . . H(65B) H 0.0060 0.3820 0.2211 0.1316 Uiso 1.00 calc . . . H(65C) H 0.0651 0.3952 0.1712 0.1316 Uiso 1.00 calc . . . H(66A) H 0.0406 0.2991 0.3002 0.0873 Uiso 1.00 calc . . . H(66B) H 0.1390 0.3158 0.3260 0.0873 Uiso 1.00 calc . . . H(66C) H 0.1128 0.2561 0.2926 0.0873 Uiso 1.00 calc . . . H(67) H -0.1502 0.1999 0.0130 0.0664 Uiso 1.00 calc . . . H(68A) H -0.2306 0.2418 0.0820 0.0781 Uiso 1.00 calc . . . H(68B) H -0.1944 0.1977 0.1408 0.0781 Uiso 1.00 calc . . . H(68C) H -0.2576 0.1778 0.0713 0.0781 Uiso 1.00 calc . . . H(69A) H -0.1530 0.1075 0.0430 0.0752 Uiso 1.00 calc . . . H(69B) H -0.0958 0.1199 0.1177 0.0752 Uiso 1.00 calc . . . H(69C) H -0.0551 0.1248 0.0544 0.0752 Uiso 1.00 calc . . . H(72A) H 0.6692 -0.0240 0.8764 0.1040 Uiso 1.00 calc . . . H(72B) H 0.6603 0.0252 0.8223 0.1040 Uiso 1.00 calc . . . H(72C) H 0.5768 -0.0028 0.8359 0.1040 Uiso 1.00 calc . . . H(74A) H 0.8806 0.1467 0.5947 0.1437 Uiso 1.00 calc . . . H(74B) H 0.7967 0.1371 0.6208 0.1437 Uiso 1.00 calc . . . H(74C) H 0.7919 0.1325 0.5419 0.1437 Uiso 1.00 calc . . . H(76A) H 0.6180 0.2815 0.6931 0.1264 Uiso 1.00 calc . . . H(76B) H 0.5298 0.2489 0.6839 0.1264 Uiso 1.00 calc . . . H(76C) H 0.5589 0.2696 0.6189 0.1264 Uiso 1.00 calc . . . 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) 0.0341(1) 0.0420(2) 0.0367(1) -0.00127(9) 0.00875(9) 0.00065(9) Ni(1) 0.0457(2) 0.0419(2) 0.0318(2) 0.0029(2) 0.0083(2) 0.0010(2) O(1) 0.044(1) 0.043(1) 0.044(1) -0.0055(9) 0.0088(9) 0.004(1) O(2) 0.044(1) 0.043(1) 0.049(1) -0.0080(9) 0.0044(9) 0.002(1) O(3) 0.118(3) 0.152(5) 0.137(4) -0.044(3) 0.054(3) -0.023(4) N(11) 0.045(1) 0.046(2) 0.034(1) 0.004(1) 0.002(1) 0.002(1) N(12) 0.038(1) 0.044(1) 0.036(1) 0.000(1) 0.0070(10) 0.005(1) N(21) 0.051(1) 0.044(2) 0.036(1) -0.001(1) 0.010(1) -0.002(1) N(22) 0.040(1) 0.045(1) 0.038(1) -0.001(1) 0.009(1) -0.002(1) N(31) 0.049(1) 0.047(2) 0.039(1) 0.004(1) 0.015(1) -0.001(1) N(32) 0.042(1) 0.045(2) 0.042(1) 0.002(1) 0.014(1) -0.002(1) N(41) 0.035(1) 0.046(2) 0.044(1) 0.002(1) 0.009(1) 0.001(1) N(42) 0.033(1) 0.050(2) 0.042(1) 0.001(1) 0.008(1) -0.001(1) N(51) 0.035(1) 0.050(2) 0.040(1) 0.002(1) 0.012(1) 0.002(1) N(52) 0.035(1) 0.049(2) 0.050(2) 0.005(1) 0.016(1) 0.004(1) N(61) 0.049(2) 0.071(2) 0.059(2) -0.012(1) 0.024(1) -0.016(2) N(62) 0.041(1) 0.054(2) 0.042(1) 0.000(1) 0.017(1) -0.006(1) N(71) 0.164(6) 0.148(6) 0.208(8) -0.042(5) 0.115(6) -0.081(6) N(72) 0.151(6) 0.115(5) 0.146(6) 0.011(4) 0.037(5) 0.040(5) N(73) 0.115(4) 0.113(5) 0.187(7) 0.019(4) 0.015(4) -0.016(5) C(11) 0.044(2) 0.054(2) 0.052(2) -0.005(1) 0.008(1) -0.008(2) C(12) 0.053(2) 0.047(2) 0.068(2) -0.009(2) 0.016(2) 0.003(2) C(13) 0.052(2) 0.040(2) 0.045(2) 0.000(1) 0.015(1) 0.004(1) C(14) 0.050(2) 0.075(3) 0.057(2) -0.004(2) 0.019(2) 0.006(2) C(15) 0.048(2) 0.072(3) 0.092(3) 0.011(2) 0.008(2) 0.003(3) C(16) 0.064(3) 0.091(4) 0.103(4) -0.019(3) 0.011(3) 0.003(3) C(17) 0.074(2) 0.048(2) 0.056(2) 0.002(2) 0.007(2) 0.014(2) C(18) 0.084(3) 0.077(3) 0.091(4) 0.022(3) 0.023(3) 0.018(3) C(19) 0.103(4) 0.086(4) 0.075(3) -0.006(3) 0.021(3) 0.035(3) C(21) 0.060(2) 0.043(2) 0.044(2) -0.002(2) 0.015(1) -0.002(1) C(22) 0.058(2) 0.050(2) 0.055(2) -0.013(2) 0.015(2) -0.008(2) C(23) 0.043(2) 0.053(2) 0.047(2) -0.006(1) 0.014(1) -0.005(2) C(24) 0.077(3) 0.044(2) 0.048(2) -0.003(2) 0.007(2) -0.001(2) C(25) 0.095(4) 0.077(3) 0.087(4) 0.023(3) 0.002(3) -0.018(3) C(26) 0.103(4) 0.082(4) 0.131(5) 0.002(3) 0.034(4) 0.051(4) C(27) 0.043(2) 0.068(3) 0.059(2) -0.008(2) 0.009(2) -0.011(2) C(28) 0.073(3) 0.110(5) 0.108(4) -0.035(3) -0.016(3) 0.002(4) C(29) 0.076(3) 0.127(5) 0.064(3) 0.025(3) 0.010(2) 0.013(3) C(31) 0.058(2) 0.056(2) 0.044(2) 0.002(2) 0.021(1) 0.000(2) C(32) 0.060(2) 0.063(2) 0.056(2) 0.004(2) 0.033(2) -0.005(2) C(33) 0.046(2) 0.052(2) 0.057(2) 0.001(1) 0.020(2) -0.003(2) C(34) 0.063(2) 0.076(3) 0.045(2) 0.005(2) 0.022(2) 0.002(2) C(35) 0.109(4) 0.098(4) 0.052(2) -0.012(3) 0.019(2) -0.012(3) C(36) 0.108(4) 0.078(3) 0.072(3) 0.016(3) 0.040(3) 0.019(3) C(37) 0.048(2) 0.082(3) 0.071(3) 0.016(2) 0.021(2) 0.009(2) C(38) 0.178(8) 0.163(8) 0.137(7) 0.121(7) -0.017(6) -0.031(6) C(39) 0.060(3) 0.150(7) 0.144(6) -0.009(3) 0.009(3) 0.030(5) C(41) 0.040(1) 0.044(2) 0.044(2) 0.000(1) 0.012(1) -0.003(1) C(42) 0.046(2) 0.054(2) 0.045(2) -0.005(1) 0.008(1) -0.007(2) C(43) 0.035(1) 0.057(2) 0.044(2) -0.005(1) 0.010(1) -0.001(2) C(44) 0.048(2) 0.047(2) 0.048(2) 0.004(1) 0.011(1) -0.001(2) C(45) 0.083(3) 0.062(3) 0.084(3) 0.002(2) 0.019(3) 0.010(2) C(46) 0.083(3) 0.092(4) 0.062(3) 0.023(3) 0.021(2) -0.015(3) C(47) 0.037(2) 0.072(3) 0.043(2) 0.000(2) 0.008(1) 0.003(2) C(48) 0.055(2) 0.093(4) 0.063(3) 0.002(2) 0.010(2) 0.018(2) C(49) 0.047(2) 0.090(4) 0.089(3) -0.017(2) -0.006(2) 0.012(3) C(51) 0.041(2) 0.055(2) 0.039(2) 0.002(1) 0.012(1) 0.011(1) C(52) 0.048(2) 0.056(2) 0.071(2) 0.004(2) 0.024(2) 0.017(2) C(53) 0.049(2) 0.052(2) 0.073(2) 0.010(2) 0.027(2) 0.013(2) C(54) 0.037(2) 0.068(2) 0.053(2) 0.001(1) 0.016(1) 0.018(2) C(55) 0.065(3) 0.122(5) 0.098(4) -0.033(3) 0.031(3) -0.016(4) C(56) 0.054(2) 0.112(4) 0.058(2) 0.015(2) 0.028(2) 0.017(2) C(57) 0.055(2) 0.070(3) 0.164(6) 0.021(2) 0.044(3) 0.047(4) C(58) 0.23(1) 0.21(1) 0.23(1) 0.158(9) 0.126(10) 0.033(9) C(59) 0.070(3) 0.122(5) 0.149(6) 0.028(3) 0.014(3) 0.063(5) C(61) 0.050(2) 0.075(3) 0.052(2) -0.004(2) 0.018(2) -0.014(2) C(62) 0.055(2) 0.075(3) 0.049(2) -0.002(2) 0.028(2) -0.005(2) C(63) 0.041(2) 0.053(2) 0.050(2) 0.004(1) 0.020(1) -0.001(2) C(64) 0.071(3) 0.099(4) 0.058(2) -0.021(3) 0.022(2) -0.026(3) C(65) 0.202(8) 0.101(5) 0.075(4) -0.031(5) 0.005(4) -0.028(4) C(66) 0.067(3) 0.129(5) 0.061(3) 0.007(3) 0.006(2) -0.025(3) C(67) 0.052(2) 0.065(2) 0.051(2) -0.010(2) 0.020(2) 0.002(2) C(68) 0.059(2) 0.102(4) 0.083(3) -0.015(2) 0.034(2) 0.001(3) C(69) 0.084(3) 0.064(3) 0.077(3) -0.015(2) 0.020(2) 0.000(2) C(71) 0.089(4) 0.094(4) 0.131(5) -0.023(3) 0.057(4) -0.028(4) C(72) 0.117(4) 0.098(5) 0.099(4) -0.043(4) 0.033(4) -0.018(4) C(73) 0.081(4) 0.113(5) 0.130(6) -0.001(4) 0.038(4) 0.023(5) C(74) 0.125(6) 0.113(6) 0.188(9) 0.032(5) 0.025(6) -0.017(6) C(75) 0.085(3) 0.088(4) 0.081(4) 0.002(3) 0.024(3) -0.010(3) C(76) 0.182(7) 0.097(5) 0.129(6) 0.033(5) 0.092(6) 0.017(5) B(1) 0.043(2) 0.046(2) 0.037(2) 0.000(1) 0.009(1) 0.001(2) B(2) 0.038(2) 0.050(2) 0.046(2) 0.004(1) 0.016(1) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _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) O(1) 2.017(2) . . yes Pd(1) O(2) 2.009(2) . . yes Pd(1) N(41) 2.009(2) . . yes Pd(1) N(51) 2.014(3) . . yes Ni(1) O(1) 2.009(2) . . yes Ni(1) O(2) 2.030(2) . . yes Ni(1) N(11) 2.039(3) . . yes Ni(1) N(21) 2.082(3) . . yes Ni(1) N(31) 2.037(3) . . yes N(11) N(12) 1.367(3) . . yes N(11) C(11) 1.364(5) . . yes N(12) C(13) 1.364(5) . . yes N(12) B(1) 1.550(5) . . yes N(21) N(22) 1.388(4) . . yes N(21) C(21) 1.333(5) . . yes N(22) C(23) 1.358(4) . . yes N(22) B(1) 1.542(5) . . yes N(31) N(32) 1.374(4) . . yes N(31) C(31) 1.332(5) . . yes N(32) C(33) 1.359(5) . . yes N(32) B(1) 1.557(5) . . yes N(41) N(42) 1.381(4) . . yes N(41) C(41) 1.331(4) . . yes N(42) C(43) 1.364(4) . . yes N(42) B(2) 1.548(5) . . yes N(51) N(52) 1.377(4) . . yes N(51) C(51) 1.342(5) . . yes N(52) C(53) 1.348(5) . . yes N(52) B(2) 1.550(5) . . yes N(61) N(62) 1.370(4) . . yes N(61) C(61) 1.342(6) . . yes N(62) C(63) 1.365(5) . . yes N(62) B(2) 1.557(5) . . yes N(71) C(71) 1.13(1) . . yes N(72) C(73) 1.17(1) . . yes N(73) C(75) 1.132(10) . . yes N(74) C(77) 1.26(4) . . yes N(75) C(78) 1.20(3) . . yes C(11) C(12) 1.397(5) . . yes C(11) C(14) 1.485(5) . . yes C(12) C(13) 1.357(5) . . yes C(13) C(17) 1.501(5) . . yes C(14) C(15) 1.362(7) . . yes C(14) C(16) 1.466(7) . . yes C(17) C(18) 1.495(8) . . yes C(17) C(19) 1.564(8) . . yes C(21) C(22) 1.402(5) . . yes C(21) C(24) 1.512(5) . . yes C(22) C(23) 1.374(5) . . yes C(23) C(27) 1.507(5) . . yes C(24) C(25) 1.528(8) . . yes C(24) C(26) 1.482(9) . . yes C(27) C(28) 1.519(7) . . yes C(27) C(29) 1.523(8) . . yes C(31) C(32) 1.390(5) . . yes C(31) C(34) 1.519(5) . . yes C(32) C(33) 1.380(6) . . yes C(33) C(37) 1.511(5) . . yes C(34) C(35) 1.546(7) . . yes C(34) C(36) 1.508(8) . . yes C(37) C(38) 1.50(1) . . yes C(37) C(39) 1.515(8) . . yes C(41) C(42) 1.395(4) . . yes C(41) C(44) 1.500(5) . . yes C(42) C(43) 1.376(5) . . yes C(43) C(47) 1.503(4) . . yes C(44) C(45) 1.529(7) . . yes C(44) C(46) 1.534(7) . . yes C(47) C(48) 1.522(7) . . yes C(47) C(49) 1.533(6) . . yes C(51) C(52) 1.382(5) . . yes C(51) C(54) 1.499(5) . . yes C(52) C(53) 1.382(6) . . yes C(53) C(57) 1.515(6) . . yes C(54) C(55) 1.520(7) . . yes C(54) C(56) 1.509(6) . . yes C(57) C(58) 1.47(1) . . yes C(57) C(59) 1.50(1) . . yes C(61) C(62) 1.402(6) . . yes C(61) C(64) 1.503(6) . . yes C(62) C(63) 1.387(5) . . yes C(63) C(67) 1.493(5) . . yes C(64) C(65) 1.498(10) . . yes C(64) C(66) 1.519(8) . . yes C(67) C(68) 1.539(7) . . yes C(67) C(69) 1.508(7) . . yes C(71) C(72) 1.46(1) . . yes C(73) C(74) 1.45(1) . . yes C(75) C(76) 1.39(1) . . yes C(77) C(78) 1.28(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 O(1) Pd(1) O(2) 79.08(9) . . . yes O(1) Pd(1) N(41) 175.0(1) . . . yes O(1) Pd(1) N(51) 96.74(9) . . . yes O(2) Pd(1) N(41) 95.97(10) . . . yes O(2) Pd(1) N(51) 175.48(9) . . . yes N(41) Pd(1) N(51) 88.2(1) . . . yes O(1) Ni(1) O(2) 78.78(9) . . . yes O(1) Ni(1) N(11) 159.5(1) . . . yes O(1) Ni(1) N(21) 100.3(1) . . . yes O(1) Ni(1) N(31) 107.9(1) . . . yes O(2) Ni(1) N(11) 90.5(1) . . . yes O(2) Ni(1) N(21) 170.3(1) . . . yes O(2) Ni(1) N(31) 99.3(1) . . . yes N(11) Ni(1) N(21) 87.3(1) . . . yes N(11) Ni(1) N(31) 90.9(1) . . . yes N(21) Ni(1) N(31) 90.2(1) . . . yes Pd(1) O(1) Ni(1) 100.5(1) . . . yes Pd(1) O(2) Ni(1) 100.1(1) . . . yes Ni(1) N(11) N(12) 117.7(2) . . . yes Ni(1) N(11) C(11) 135.9(2) . . . yes N(12) N(11) C(11) 106.1(3) . . . yes N(11) N(12) C(13) 109.2(3) . . . yes N(11) N(12) B(1) 118.6(3) . . . yes C(13) N(12) B(1) 132.2(3) . . . yes Ni(1) N(21) N(22) 115.1(2) . . . yes Ni(1) N(21) C(21) 138.6(2) . . . yes N(22) N(21) C(21) 106.2(2) . . . yes N(21) N(22) C(23) 109.4(3) . . . yes N(21) N(22) B(1) 119.9(2) . . . yes C(23) N(22) B(1) 130.6(3) . . . yes Ni(1) N(31) N(32) 117.0(2) . . . yes Ni(1) N(31) C(31) 135.8(2) . . . yes N(32) N(31) C(31) 107.1(3) . . . yes N(31) N(32) C(33) 109.6(3) . . . yes N(31) N(32) B(1) 119.1(3) . . . yes C(33) N(32) B(1) 131.3(3) . . . yes Pd(1) N(41) N(42) 119.9(2) . . . yes Pd(1) N(41) C(41) 131.1(2) . . . yes N(42) N(41) C(41) 108.2(2) . . . yes N(41) N(42) C(43) 108.2(3) . . . yes N(41) N(42) B(2) 120.8(2) . . . yes C(43) N(42) B(2) 130.9(3) . . . yes Pd(1) N(51) N(52) 119.7(2) . . . yes Pd(1) N(51) C(51) 132.4(2) . . . yes N(52) N(51) C(51) 107.7(3) . . . yes N(51) N(52) C(53) 108.5(3) . . . yes N(51) N(52) B(2) 120.7(3) . . . yes C(53) N(52) B(2) 130.4(3) . . . yes N(62) N(61) C(61) 106.7(3) . . . yes N(61) N(62) C(63) 110.0(3) . . . yes N(61) N(62) B(2) 121.2(3) . . . yes C(63) N(62) B(2) 127.8(3) . . . yes N(11) C(11) C(12) 109.8(3) . . . yes N(11) C(11) C(14) 123.7(3) . . . yes C(12) C(11) C(14) 126.3(4) . . . yes C(11) C(12) C(13) 105.7(4) . . . yes N(12) C(13) C(12) 109.1(3) . . . yes N(12) C(13) C(17) 122.9(3) . . . yes C(12) C(13) C(17) 128.0(4) . . . yes C(11) C(14) C(15) 119.8(4) . . . yes C(11) C(14) C(16) 116.4(4) . . . yes C(15) C(14) C(16) 123.8(4) . . . yes C(13) C(17) C(18) 111.4(4) . . . yes C(13) C(17) C(19) 110.4(4) . . . yes C(18) C(17) C(19) 109.0(4) . . . yes N(21) C(21) C(22) 110.7(3) . . . yes N(21) C(21) C(24) 122.1(3) . . . yes C(22) C(21) C(24) 127.3(3) . . . yes C(21) C(22) C(23) 105.5(3) . . . yes N(22) C(23) C(22) 108.3(3) . . . yes N(22) C(23) C(27) 122.4(3) . . . yes C(22) C(23) C(27) 129.3(3) . . . yes C(21) C(24) C(25) 110.9(4) . . . yes C(21) C(24) C(26) 110.7(4) . . . yes C(25) C(24) C(26) 111.1(4) . . . yes C(23) C(27) C(28) 110.7(4) . . . yes C(23) C(27) C(29) 110.3(4) . . . yes C(28) C(27) C(29) 112.1(4) . . . yes N(31) C(31) C(32) 109.6(3) . . . yes N(31) C(31) C(34) 121.5(3) . . . yes C(32) C(31) C(34) 128.9(4) . . . yes C(31) C(32) C(33) 106.7(4) . . . yes N(32) C(33) C(32) 107.0(3) . . . yes N(32) C(33) C(37) 123.2(4) . . . yes C(32) C(33) C(37) 129.7(4) . . . yes C(31) C(34) C(35) 110.6(4) . . . yes C(31) C(34) C(36) 110.2(3) . . . yes C(35) C(34) C(36) 111.2(4) . . . yes C(33) C(37) C(38) 110.9(4) . . . yes C(33) C(37) C(39) 110.4(4) . . . yes C(38) C(37) C(39) 113.9(5) . . . yes N(41) C(41) C(42) 109.0(3) . . . yes N(41) C(41) C(44) 122.4(3) . . . yes C(42) C(41) C(44) 128.6(3) . . . yes C(41) C(42) C(43) 106.7(3) . . . yes N(42) C(43) C(42) 107.9(3) . . . yes N(42) C(43) C(47) 123.0(3) . . . yes C(42) C(43) C(47) 129.0(3) . . . yes C(41) C(44) C(45) 109.6(3) . . . yes C(41) C(44) C(46) 111.7(3) . . . yes C(45) C(44) C(46) 109.6(4) . . . yes C(43) C(47) C(48) 112.3(3) . . . yes C(43) C(47) C(49) 110.6(3) . . . yes C(48) C(47) C(49) 109.9(3) . . . yes N(51) C(51) C(52) 109.1(3) . . . yes N(51) C(51) C(54) 122.8(3) . . . yes C(52) C(51) C(54) 128.0(4) . . . yes C(51) C(52) C(53) 106.3(4) . . . yes N(52) C(53) C(52) 108.3(3) . . . yes N(52) C(53) C(57) 122.6(4) . . . yes C(52) C(53) C(57) 129.0(4) . . . yes C(51) C(54) C(55) 111.5(4) . . . yes C(51) C(54) C(56) 111.2(3) . . . yes C(55) C(54) C(56) 108.4(4) . . . yes C(53) C(57) C(58) 110.6(6) . . . yes C(53) C(57) C(59) 111.7(5) . . . yes C(58) C(57) C(59) 109.4(6) . . . yes N(61) C(61) C(62) 110.2(3) . . . yes N(61) C(61) C(64) 120.1(4) . . . yes C(62) C(61) C(64) 129.6(4) . . . yes C(61) C(62) C(63) 105.7(4) . . . yes N(62) C(63) C(62) 107.4(3) . . . yes N(62) C(63) C(67) 123.7(3) . . . yes C(62) C(63) C(67) 128.8(4) . . . yes C(61) C(64) C(65) 111.5(4) . . . yes C(61) C(64) C(66) 113.0(5) . . . yes C(65) C(64) C(66) 110.8(5) . . . yes C(63) C(67) C(68) 111.0(4) . . . yes C(63) C(67) C(69) 112.5(3) . . . yes C(68) C(67) C(69) 110.6(4) . . . yes N(71) C(71) C(72) 175.7(7) . . . yes N(72) C(73) C(74) 179.0(8) . . . yes N(73) C(75) C(76) 179.7(7) . . . yes N(74) C(77) C(78) 145(1) . . . yes N(75) C(78) C(77) 153(1) . . . yes N(12) B(1) N(22) 108.8(3) . . . yes N(12) B(1) N(32) 109.4(2) . . . yes N(22) B(1) N(32) 107.8(3) . . . yes N(42) B(2) N(52) 107.9(3) . . . yes N(42) B(2) N(62) 113.0(3) . . . yes N(52) B(2) N(62) 109.9(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(21) C(56) 3.546(6) . 4_555 ? N(21) C(76) 3.56(1) . 4_554 ? N(31) C(72) 3.414(8) . 3_656 ? N(31) C(76) 3.551(9) . 4_554 ? N(32) C(72) 3.530(7) . 3_656 ? N(72) N(74) 3.51(4) . 2_645 ? N(72) C(77) 3.60(1) . 2_645 ? N(75) C(27) 3.34(2) . 2_655 ? N(75) C(39) 3.37(2) . 2_655 ? N(75) C(74) 3.47(2) . 2_655 ? N(75) C(73) 3.53(2) . 2_655 ? N(75) C(29) 3.57(2) . 2_655 ? C(18) C(26) 3.489(9) . 2_645 ? C(31) C(72) 3.578(8) . 3_656 ? C(49) C(71) 3.556(9) . 1_454 ? C(73) C(78) 3.57(1) . 2_645 ? Pd(1) N(52) 2.951(3) . . ? Pd(1) N(42) 2.951(2) . . ? Pd(1) Ni(1) 3.0963(4) . . ? Pd(1) N(61) 3.345(4) . . ? Ni(1) N(32) 2.928(3) . . ? Ni(1) N(12) 2.935(3) . . ? Ni(1) N(22) 2.952(2) . . ? O(1) O(2) 2.563(3) . . ? O(1) N(51) 3.013(3) . . ? O(1) O(3) 3.104(6) . . ? O(1) N(21) 3.140(3) . . ? O(1) N(31) 3.272(4) . . ? O(2) N(11) 2.890(3) . . ? O(2) N(41) 2.985(3) . . ? O(2) N(31) 3.098(3) . . ? O(3) N(61) 2.767(6) . . ? O(3) N(51) 3.098(6) . . ? O(3) N(52) 3.443(6) . . ? N(11) N(21) 2.844(4) . . ? N(11) N(31) 2.905(4) . . ? N(11) N(22) 2.983(4) . . ? N(11) N(32) 3.054(4) . . ? N(12) N(22) 2.514(4) . . ? N(12) N(32) 2.537(4) . . ? N(12) N(31) 3.026(4) . . ? N(12) N(21) 3.033(4) . . ? N(21) N(31) 2.919(4) . . ? N(21) N(32) 3.039(4) . . ? N(22) N(32) 2.503(4) . . ? N(22) N(31) 3.032(4) . . ? N(41) N(51) 2.800(4) . . ? N(41) N(52) 3.029(4) . . ? N(42) N(52) 2.505(4) . . ? N(42) N(51) 2.936(4) . . ? N(51) N(61) 3.199(5) . . ? N(52) N(61) 2.809(5) . . ? #------------------------------------------------------------------------------ #===END data_compound_5b(Ni) _database_code_CSD 213632 _audit_creation_date 'Thu Jul 17 20:22:46 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C50 H80 B2 N16 O2 Ni Pd ' _chemical_formula_moiety 'C50 H80 B2 N16 O2 Ni Pd ' _chemical_formula_weight 1124.01 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.254(1) _cell_length_b 21.125(2) _cell_length_c 12.1299(8) _cell_angle_alpha 101.662(4) _cell_angle_beta 112.767(3) _cell_angle_gamma 89.006(5) _cell_volume 3060.0(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9023 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.937 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 22208 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12561 _reflns_number_gt 8286 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2083 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8286 _refine_ls_number_parameters 657 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.60 _refine_diff_density_min -2.00 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 0.71737(3) 0.23837(2) 0.30881(4) 0.0363(1) Uani 1.00 d . . . Ni(1) Ni 0.49129(6) 0.16345(3) 0.21912(6) 0.0372(2) Uani 1.00 d . . . O(1) O 0.6389(3) 0.1803(2) 0.3654(3) 0.0415(9) Uani 1.00 d . . . O(2) O 0.5647(3) 0.2370(2) 0.1807(4) 0.0450(9) Uani 1.00 d . . . N(11) N 0.3531(4) 0.1478(2) 0.0527(4) 0.039(1) Uani 1.00 d . . . N(12) N 0.2552(4) 0.1314(2) 0.0571(4) 0.042(1) Uani 1.00 d . . . N(21) N 0.4347(4) 0.0849(2) 0.2655(4) 0.039(1) Uani 1.00 d . . . N(22) N 0.3244(4) 0.0785(2) 0.2370(4) 0.039(1) Uani 1.00 d . . . N(31) N 0.3965(4) 0.2206(2) 0.3009(4) 0.043(1) Uani 1.00 d . . . N(32) N 0.2903(4) 0.1964(2) 0.2669(4) 0.040(1) Uani 1.00 d . . . N(41) N 0.7913(4) 0.2918(2) 0.2382(4) 0.042(1) Uani 1.00 d . . . N(42) N 0.8718(4) 0.3400(2) 0.3145(4) 0.041(1) Uani 1.00 d . . . N(51) N 0.8663(4) 0.2354(2) 0.4388(4) 0.042(1) Uani 1.00 d . . . N(52) N 0.9332(4) 0.2914(2) 0.4976(4) 0.042(1) Uani 1.00 d . . . N(61) N 0.8109(5) 0.3832(3) 0.6008(5) 0.057(1) Uani 1.00 d . . . N(62) N 0.8049(4) 0.3840(3) 0.4845(5) 0.053(1) Uani 1.00 d . . . N(71) N 0.5760(4) 0.0981(2) 0.1273(5) 0.048(1) Uani 1.00 d . . . N(81) N 0.068(1) 0.2683(7) 0.001(1) 0.151(5) Uani 1.00 d . . . N(82) N 1.2331(7) 0.1080(4) 0.5433(8) 0.096(2) Uani 1.00 d . . . N(83) N 0.6864(9) 0.1665(6) 0.6393(8) 0.148(5) Uani 1.00 d . . . C(11) C 0.3349(5) 0.1454(3) -0.0638(5) 0.048(1) Uani 1.00 d . . . C(12) C 0.2238(6) 0.1269(4) -0.1372(6) 0.061(2) Uani 1.00 d . . . C(13) C 0.1759(5) 0.1188(3) -0.0584(6) 0.055(2) Uani 1.00 d . . . C(14) C 0.4216(6) 0.1613(4) -0.1054(6) 0.061(2) Uani 1.00 d . . . C(15) C 0.0589(6) 0.0988(4) -0.0861(7) 0.074(2) Uani 1.00 d . . . C(21) C 0.4807(5) 0.0351(3) 0.3146(6) 0.044(1) Uani 1.00 d . . . C(22) C 0.3986(6) -0.0048(3) 0.3174(6) 0.052(2) Uani 1.00 d . . . C(23) C 0.3015(5) 0.0239(3) 0.2686(6) 0.049(1) Uani 1.00 d . . . C(24) C 0.6007(5) 0.0261(3) 0.3574(7) 0.055(2) Uani 1.00 d . . . C(25) C 0.1881(6) 0.0019(4) 0.2489(7) 0.065(2) Uani 1.00 d . . . C(31) C 0.4087(6) 0.2768(3) 0.3796(6) 0.054(2) Uani 1.00 d . . . C(32) C 0.3117(6) 0.2893(3) 0.3966(7) 0.060(2) Uani 1.00 d . . . C(33) C 0.2380(5) 0.2376(3) 0.3237(6) 0.048(1) Uani 1.00 d . . . C(34) C 0.5140(6) 0.3166(4) 0.4376(8) 0.077(2) Uani 1.00 d . . . C(35) C 0.1221(6) 0.2266(4) 0.3073(7) 0.062(2) Uani 1.00 d . . . C(41) C 0.7903(5) 0.2844(3) 0.1252(5) 0.049(2) Uani 1.00 d . . . C(42) C 0.8688(6) 0.3277(3) 0.1284(6) 0.060(2) Uani 1.00 d . . . C(43) C 0.9196(6) 0.3621(3) 0.2472(6) 0.056(2) Uani 1.00 d . . . C(44) C 0.7188(6) 0.2326(4) 0.0202(6) 0.067(2) Uani 1.00 d . . . C(45) C 0.7868(9) 0.1811(4) -0.0172(8) 0.091(3) Uani 1.00 d . . . C(46) C 0.6483(7) 0.2635(5) -0.0850(7) 0.081(3) Uani 1.00 d . . . C(47) C 1.0098(7) 0.4153(4) 0.3016(7) 0.077(3) Uani 1.00 d . . . C(48) C 1.085(1) 0.4021(6) 0.220(1) 0.073(4) Uani 0.63 d P . . C(48A) C 1.106(2) 0.403(1) 0.350(2) 0.06934(7) Uiso 0.37 d P . . C(49) C 0.981(1) 0.4758(5) 0.323(1) 0.078(4) Uani 0.63 d P . . C(49A) C 0.977(2) 0.466(1) 0.205(2) 0.08767(9) Uiso 0.37 d P . . C(51) C 0.9244(5) 0.1856(3) 0.4759(6) 0.045(1) Uani 1.00 d . . . C(52) C 1.0278(5) 0.2082(3) 0.5598(6) 0.047(1) Uani 1.00 d . . . C(53) C 1.0320(5) 0.2748(3) 0.5725(5) 0.049(1) Uani 1.00 d . . . C(54) C 0.8786(5) 0.1163(3) 0.4228(6) 0.051(2) Uani 1.00 d . . . C(55) C 0.9182(9) 0.0855(4) 0.3237(8) 0.091(3) Uani 1.00 d . . . C(56) C 0.9045(8) 0.0774(4) 0.5201(8) 0.078(2) Uani 1.00 d . . . C(57) C 1.1246(6) 0.3243(3) 0.6545(6) 0.061(2) Uani 1.00 d . . . C(58) C 1.2326(7) 0.2926(5) 0.6973(8) 0.087(3) Uani 1.00 d . . . C(59) C 1.1005(7) 0.3614(4) 0.7623(7) 0.081(3) Uani 1.00 d . . . C(61) C 0.7402(7) 0.4257(4) 0.6201(8) 0.069(2) Uani 1.00 d . . . C(62) C 0.6913(7) 0.4542(4) 0.5230(10) 0.080(3) Uani 1.00 d . . . C(63) C 0.7342(7) 0.4294(3) 0.4401(8) 0.068(2) Uani 1.00 d . . . C(64) C 0.730(1) 0.4370(7) 0.741(1) 0.127(5) Uani 1.00 d . . . C(65) C 0.643(2) 0.468(1) 0.754(2) 0.27(1) Uani 1.00 d . . . C(66) C 0.815(2) 0.4172(7) 0.845(1) 0.172(7) Uani 1.00 d . . . C(67) C 0.7039(8) 0.4473(5) 0.3153(10) 0.090(3) Uani 1.00 d . . . C(68) C 0.703(1) 0.5203(6) 0.328(1) 0.161(6) Uani 1.00 d . . . C(69) C 0.595(1) 0.4134(6) 0.218(1) 0.122(4) Uani 1.00 d . . . C(71) C 0.6198(5) 0.0649(3) 0.0792(6) 0.050(1) Uani 1.00 d . . . C(72) C 0.6763(6) 0.0206(3) 0.0153(7) 0.067(2) Uani 1.00 d . . . C(81) C 0.159(1) 0.2868(7) 0.033(1) 0.117(4) Uani 1.00 d . . . C(82) C 0.274(1) 0.3099(6) 0.076(1) 0.109(3) Uani 1.00 d . . . C(83) C 1.3110(8) 0.1274(4) 0.5470(8) 0.070(2) Uani 1.00 d . . . C(84) C 1.4171(8) 0.1517(4) 0.5559(7) 0.080(2) Uani 1.00 d . . . C(85) C 0.7623(9) 0.2031(5) 0.6800(8) 0.087(3) Uani 1.00 d . . . C(86) C 0.854(1) 0.2484(5) 0.7252(9) 0.106(4) Uani 1.00 d . . . B(1) B 0.2501(5) 0.1289(3) 0.1798(6) 0.041(1) Uani 1.00 d . . . B(2) B 0.9007(6) 0.3546(3) 0.4530(6) 0.043(1) Uani 1.00 d . . . H(1) H 0.1760 0.1183 0.1686 0.0499 Uiso 1.00 calc . . . H(01) H 0.6544 0.1782 0.4512 0.0049 Uiso 1.00 calc . . . H(2) H 0.1893 0.1210 -0.2240 0.0748 Uiso 1.00 calc . . . H(02) H 0.5325 0.2760 0.1978 0.0932 Uiso 1.00 calc . . . H(3) H 0.4436 0.1221 -0.1427 0.0619 Uiso 1.00 calc . . . H(4) H 0.4836 0.1837 -0.0362 0.0619 Uiso 1.00 calc . . . H(5) H 0.3934 0.1886 -0.1636 0.0619 Uiso 1.00 calc . . . H(6) H 0.0355 0.1255 -0.0272 0.0748 Uiso 1.00 calc . . . H(7) H 0.0536 0.0543 -0.0813 0.0748 Uiso 1.00 calc . . . H(8) H 0.0131 0.1042 -0.1666 0.0748 Uiso 1.00 calc . . . H(9) H 0.4081 -0.0437 0.3487 0.0654 Uiso 1.00 calc . . . H(10) H 0.6212 0.0005 0.4188 0.0557 Uiso 1.00 calc . . . H(11) H 0.6408 0.0676 0.3913 0.0557 Uiso 1.00 calc . . . H(12) H 0.6175 0.0044 0.2895 0.0557 Uiso 1.00 calc . . . H(13) H 0.1587 0.0348 0.2928 0.0659 Uiso 1.00 calc . . . H(14) H 0.1905 -0.0373 0.2780 0.0659 Uiso 1.00 calc . . . H(15) H 0.1427 -0.0059 0.1632 0.0659 Uiso 1.00 calc . . . H(16) H 0.2995 0.3269 0.4500 0.0724 Uiso 1.00 calc . . . H(17) H 0.5630 0.2997 0.5052 0.0778 Uiso 1.00 calc . . . H(18) H 0.5014 0.3605 0.4657 0.0778 Uiso 1.00 calc . . . H(19) H 0.5464 0.3151 0.3784 0.0778 Uiso 1.00 calc . . . H(20) H 0.1033 0.2625 0.3574 0.0629 Uiso 1.00 calc . . . H(21) H 0.1138 0.1874 0.3320 0.0629 Uiso 1.00 calc . . . H(22) H 0.0749 0.2237 0.2233 0.0629 Uiso 1.00 calc . . . H(23) H 0.9632 0.3853 0.4924 0.0509 Uiso 1.00 calc . . . H(24) H 0.8848 0.3327 0.0590 0.0718 Uiso 1.00 calc . . . H(25) H 0.6699 0.2125 0.0459 0.0818 Uiso 1.00 calc . . . H(26) H 0.7392 0.1466 -0.0801 0.0914 Uiso 1.00 calc . . . H(27) H 0.8306 0.1636 0.0526 0.0914 Uiso 1.00 calc . . . H(28) H 0.8339 0.1993 -0.0475 0.0914 Uiso 1.00 calc . . . H(29) H 0.6043 0.2945 -0.0572 0.0811 Uiso 1.00 calc . . . H(30) H 0.6012 0.2308 -0.1512 0.0811 Uiso 1.00 calc . . . H(31) H 0.6946 0.2854 -0.1116 0.0811 Uiso 1.00 calc . . . H(32) H 1.0856 0.1830 0.6029 0.0575 Uiso 1.00 calc . . . H(33) H 0.7998 0.1160 0.3847 0.0622 Uiso 1.00 calc . . . H(34) H 0.8813 0.0432 0.2841 0.0926 Uiso 1.00 calc . . . H(35) H 0.9959 0.0813 0.3594 0.0926 Uiso 1.00 calc . . . H(36) H 0.9024 0.1120 0.2643 0.0926 Uiso 1.00 calc . . . H(37) H 0.8758 0.0971 0.5795 0.0789 Uiso 1.00 calc . . . H(38) H 0.9830 0.0764 0.5604 0.0789 Uiso 1.00 calc . . . H(39) H 0.8727 0.0340 0.4841 0.0789 Uiso 1.00 calc . . . H(40) H 1.1307 0.3553 0.6079 0.0735 Uiso 1.00 calc . . . H(41) H 1.2282 0.2609 0.7416 0.0895 Uiso 1.00 calc . . . H(42) H 1.2904 0.3250 0.7490 0.0895 Uiso 1.00 calc . . . H(43) H 1.2478 0.2721 0.6273 0.0895 Uiso 1.00 calc . . . H(44) H 1.1573 0.3953 0.8096 0.0822 Uiso 1.00 calc . . . H(45) H 1.0980 0.3325 0.8126 0.0822 Uiso 1.00 calc . . . H(46) H 1.0312 0.3803 0.7322 0.0822 Uiso 1.00 calc . . . H(47) H 0.6365 0.4859 0.5154 0.0942 Uiso 1.00 calc . . . H(48) H 0.6379 0.4836 0.8295 0.2816 Uiso 1.00 calc . . . H(49) H 0.5893 0.4803 0.6813 0.2816 Uiso 1.00 calc . . . H(50) H 0.7865 0.4091 0.9021 0.1724 Uiso 1.00 calc . . . H(51) H 0.8738 0.4514 0.8857 0.1724 Uiso 1.00 calc . . . H(52) H 0.8463 0.3786 0.8169 0.1724 Uiso 1.00 calc . . . H(53) H 0.7593 0.4329 0.2855 0.1072 Uiso 1.00 calc . . . H(54) H 0.7750 0.5404 0.3775 0.1646 Uiso 1.00 calc . . . H(55) H 0.6531 0.5370 0.3660 0.1646 Uiso 1.00 calc . . . H(56) H 0.6785 0.5309 0.2485 0.1646 Uiso 1.00 calc . . . H(57) H 0.5351 0.4303 0.2367 0.1248 Uiso 1.00 calc . . . H(58) H 0.5953 0.3676 0.2130 0.1248 Uiso 1.00 calc . . . H(59) H 0.5867 0.4215 0.1384 0.1248 Uiso 1.00 calc . . . H(60) H 0.6784 -0.0210 0.0370 0.0679 Uiso 1.00 calc . . . H(61) H 0.7505 0.0378 0.0399 0.0679 Uiso 1.00 calc . . . H(62) H 0.6386 0.0156 -0.0712 0.0679 Uiso 1.00 calc . . . H(63) H 0.3195 0.2796 0.1202 0.1110 Uiso 1.00 calc . . . H(64) H 0.2860 0.3514 0.1312 0.1110 Uiso 1.00 calc . . . H(65) H 0.2919 0.3132 0.0090 0.1110 Uiso 1.00 calc . . . H(66) H 1.4744 0.1383 0.6222 0.0806 Uiso 1.00 calc . . . H(67) H 1.4201 0.1981 0.5697 0.0806 Uiso 1.00 calc . . . H(68) H 1.4258 0.1343 0.4807 0.0806 Uiso 1.00 calc . . . H(69) H 0.8857 0.2568 0.8126 0.1059 Uiso 1.00 calc . . . H(70) H 0.8308 0.2883 0.6988 0.1059 Uiso 1.00 calc . . . H(71) H 0.9076 0.2315 0.6937 0.1059 Uiso 1.00 calc . . . 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) 0.0315(2) 0.0414(2) 0.0360(2) -0.0075(2) 0.0128(2) 0.0082(2) Ni(1) 0.0303(4) 0.0439(4) 0.0366(4) -0.0066(3) 0.0127(3) 0.0070(3) O(1) 0.035(2) 0.050(2) 0.038(2) -0.010(2) 0.011(2) 0.014(2) O(2) 0.042(2) 0.049(2) 0.044(2) -0.010(2) 0.016(2) 0.011(2) N(11) 0.031(2) 0.050(3) 0.032(2) -0.010(2) 0.007(2) 0.009(2) N(12) 0.028(2) 0.054(3) 0.039(2) -0.006(2) 0.008(2) 0.007(2) N(21) 0.033(2) 0.040(2) 0.043(2) -0.007(2) 0.014(2) 0.006(2) N(22) 0.033(2) 0.044(2) 0.043(2) -0.010(2) 0.018(2) 0.008(2) N(31) 0.035(3) 0.046(3) 0.046(3) -0.006(2) 0.016(2) 0.004(2) N(32) 0.031(2) 0.047(3) 0.043(2) -0.005(2) 0.018(2) 0.005(2) N(41) 0.041(3) 0.043(3) 0.039(2) -0.010(2) 0.013(2) 0.004(2) N(42) 0.039(3) 0.041(2) 0.045(3) -0.017(2) 0.019(2) 0.005(2) N(51) 0.037(3) 0.040(2) 0.047(3) -0.008(2) 0.016(2) 0.005(2) N(52) 0.036(3) 0.043(3) 0.039(2) -0.009(2) 0.007(2) 0.006(2) N(61) 0.057(4) 0.057(3) 0.057(3) -0.006(3) 0.029(3) -0.003(3) N(62) 0.047(3) 0.051(3) 0.058(3) -0.010(2) 0.022(3) 0.006(3) N(71) 0.045(3) 0.051(3) 0.051(3) 0.005(2) 0.028(2) 0.001(2) N(81) 0.124(10) 0.20(1) 0.129(9) 0.000(9) 0.029(8) 0.065(8) N(82) 0.072(5) 0.105(6) 0.111(6) 0.008(4) 0.037(5) 0.025(5) N(83) 0.132(9) 0.22(1) 0.081(6) -0.070(9) 0.041(6) -0.003(7) C(11) 0.042(3) 0.059(4) 0.037(3) -0.010(3) 0.011(3) 0.009(3) C(12) 0.042(4) 0.088(5) 0.042(3) -0.012(3) 0.004(3) 0.014(3) C(13) 0.040(3) 0.069(4) 0.047(3) -0.008(3) 0.010(3) 0.006(3) C(14) 0.053(4) 0.085(5) 0.047(4) -0.010(3) 0.022(3) 0.014(3) C(15) 0.040(4) 0.114(6) 0.055(4) -0.022(4) 0.004(3) 0.016(4) C(21) 0.037(3) 0.047(3) 0.050(3) -0.003(2) 0.015(3) 0.019(3) C(22) 0.055(4) 0.046(3) 0.061(4) -0.006(3) 0.027(3) 0.016(3) C(23) 0.044(4) 0.049(3) 0.057(4) -0.011(3) 0.023(3) 0.008(3) C(24) 0.046(4) 0.055(4) 0.067(4) 0.004(3) 0.021(3) 0.024(3) C(25) 0.046(4) 0.071(4) 0.083(5) -0.017(3) 0.029(4) 0.022(4) C(31) 0.053(4) 0.045(3) 0.058(4) -0.009(3) 0.023(3) -0.008(3) C(32) 0.057(4) 0.054(4) 0.074(5) 0.003(3) 0.036(4) 0.004(4) C(33) 0.038(3) 0.050(3) 0.058(4) 0.005(3) 0.023(3) 0.010(3) C(34) 0.052(5) 0.076(5) 0.088(6) -0.017(4) 0.029(4) -0.018(4) C(35) 0.051(4) 0.070(4) 0.077(5) 0.008(3) 0.037(4) 0.018(4) C(41) 0.053(4) 0.064(4) 0.032(3) -0.020(3) 0.017(3) 0.010(3) C(42) 0.066(5) 0.067(4) 0.048(3) -0.025(3) 0.025(3) 0.007(3) C(43) 0.060(4) 0.059(4) 0.050(4) -0.022(3) 0.020(3) 0.016(3) C(44) 0.064(5) 0.085(5) 0.048(4) -0.040(4) 0.021(3) 0.000(4) C(45) 0.128(8) 0.065(5) 0.080(6) -0.022(5) 0.053(6) -0.010(4) C(46) 0.078(6) 0.113(7) 0.045(4) -0.027(5) 0.018(4) 0.009(4) C(47) 0.092(6) 0.075(5) 0.063(4) -0.050(4) 0.032(4) 0.006(4) C(48) 0.061(7) 0.073(7) 0.100(9) -0.023(6) 0.056(7) 0.003(7) C(49) 0.071(8) 0.042(6) 0.12(1) -0.020(5) 0.052(8) -0.003(7) C(51) 0.035(3) 0.049(3) 0.051(3) -0.001(2) 0.017(3) 0.013(3) C(52) 0.033(3) 0.053(3) 0.055(4) -0.001(2) 0.013(3) 0.021(3) C(53) 0.042(3) 0.056(3) 0.042(3) -0.014(3) 0.009(3) 0.013(3) C(54) 0.042(3) 0.042(3) 0.068(4) -0.006(2) 0.019(3) 0.012(3) C(55) 0.128(8) 0.060(5) 0.075(5) -0.020(5) 0.040(6) -0.009(4) C(56) 0.097(7) 0.054(4) 0.092(6) 0.000(4) 0.041(5) 0.027(4) C(57) 0.051(4) 0.064(4) 0.050(4) -0.021(3) -0.002(3) 0.013(3) C(58) 0.046(4) 0.106(7) 0.081(6) -0.026(4) -0.005(4) 0.017(5) C(59) 0.083(6) 0.076(5) 0.055(4) -0.015(4) 0.001(4) 0.002(4) C(61) 0.065(5) 0.066(5) 0.080(5) -0.011(4) 0.044(4) -0.007(4) C(62) 0.067(5) 0.046(4) 0.119(7) 0.001(3) 0.044(5) -0.013(5) C(63) 0.070(5) 0.045(4) 0.080(5) -0.008(3) 0.020(4) 0.013(4) C(64) 0.111(9) 0.13(1) 0.14(1) -0.032(7) 0.090(9) -0.036(9) C(65) 0.18(2) 0.42(3) 0.17(2) 0.12(2) 0.10(1) -0.04(2) C(66) 0.30(2) 0.15(1) 0.12(1) 0.04(1) 0.14(1) 0.039(10) C(67) 0.068(6) 0.093(6) 0.121(8) 0.021(5) 0.036(6) 0.050(6) C(68) 0.16(1) 0.095(8) 0.20(1) -0.026(8) 0.01(1) 0.092(9) C(69) 0.111(9) 0.101(8) 0.131(10) -0.002(7) 0.018(8) 0.034(7) C(71) 0.044(4) 0.056(4) 0.045(3) -0.013(3) 0.014(3) 0.009(3) C(72) 0.073(5) 0.055(4) 0.073(5) -0.006(3) 0.043(4) -0.018(4) C(81) 0.13(1) 0.14(1) 0.102(9) 0.037(9) 0.044(9) 0.062(8) C(82) 0.105(9) 0.129(9) 0.094(7) 0.031(7) 0.031(7) 0.042(7) C(83) 0.072(6) 0.068(5) 0.067(5) 0.018(4) 0.025(4) 0.017(4) C(84) 0.086(6) 0.099(6) 0.055(4) 0.007(5) 0.024(4) 0.024(4) C(85) 0.092(7) 0.108(8) 0.060(5) -0.009(6) 0.033(5) 0.011(5) C(86) 0.15(1) 0.098(7) 0.090(7) -0.033(7) 0.069(7) 0.002(6) B(1) 0.021(3) 0.055(4) 0.045(3) -0.005(2) 0.011(3) 0.007(3) B(2) 0.045(4) 0.033(3) 0.043(3) -0.012(3) 0.013(3) -0.002(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement SHELXL97 _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) O(1) 1.998(5) . . yes Pd(1) O(2) 2.015(4) . . yes Pd(1) N(41) 2.012(6) . . yes Pd(1) N(51) 2.004(4) . . yes Ni(1) O(1) 2.046(3) . . yes Ni(1) O(2) 2.068(5) . . yes Ni(1) N(11) 2.105(4) . . yes Ni(1) N(21) 2.093(5) . . yes Ni(1) N(31) 2.109(5) . . yes Ni(1) N(71) 2.168(6) . . yes N(11) N(12) 1.372(8) . . yes N(11) C(11) 1.329(8) . . yes N(12) C(13) 1.362(7) . . yes N(12) B(1) 1.527(10) . . yes N(21) N(22) 1.368(7) . . yes N(21) C(21) 1.335(8) . . yes N(22) C(23) 1.361(9) . . yes N(22) B(1) 1.524(8) . . yes N(31) N(32) 1.380(7) . . yes N(31) C(31) 1.333(8) . . yes N(32) C(33) 1.349(9) . . yes N(32) B(1) 1.553(7) . . yes N(41) N(42) 1.387(6) . . yes N(41) C(41) 1.342(9) . . yes N(42) C(43) 1.36(1) . . yes N(42) B(2) 1.537(9) . . yes N(51) N(52) 1.378(6) . . yes N(51) C(51) 1.340(8) . . yes N(52) C(53) 1.362(7) . . yes N(52) B(2) 1.535(8) . . yes N(61) N(62) 1.386(9) . . yes N(61) C(61) 1.34(1) . . yes N(62) C(63) 1.368(9) . . yes N(62) B(2) 1.55(1) . . yes N(71) C(71) 1.119(9) . . yes N(81) C(81) 1.16(2) . . yes N(82) C(83) 1.10(1) . . yes N(83) C(85) 1.16(2) . . yes C(11) C(12) 1.407(8) . . yes C(11) C(14) 1.49(1) . . yes C(12) C(13) 1.37(1) . . yes C(13) C(15) 1.50(1) . . yes C(21) C(22) 1.40(1) . . yes C(21) C(24) 1.492(9) . . yes C(22) C(23) 1.380(9) . . yes C(23) C(25) 1.49(1) . . yes C(31) C(32) 1.39(1) . . yes C(31) C(34) 1.48(1) . . yes C(32) C(33) 1.382(8) . . yes C(33) C(35) 1.49(1) . . yes C(41) C(42) 1.38(1) . . yes C(41) C(44) 1.502(8) . . yes C(42) C(43) 1.378(8) . . yes C(43) C(47) 1.50(1) . . yes C(44) C(45) 1.51(1) . . yes C(44) C(46) 1.52(1) . . yes C(47) C(48) 1.64(2) . . yes C(47) C(48A) 1.23(2) . . yes C(47) C(49) 1.33(1) . . yes C(47) C(49A) 1.68(3) . . yes C(48) C(48A) 1.48(3) . . yes C(49) C(49A) 1.38(4) . . yes C(51) C(52) 1.374(7) . . yes C(51) C(54) 1.507(8) . . yes C(52) C(53) 1.383(9) . . yes C(53) C(57) 1.507(8) . . yes C(54) C(55) 1.52(1) . . yes C(54) C(56) 1.50(1) . . yes C(57) C(58) 1.52(1) . . yes C(57) C(59) 1.52(1) . . yes C(61) C(62) 1.36(1) . . yes C(61) C(64) 1.49(2) . . yes C(62) C(63) 1.35(2) . . yes C(63) C(67) 1.53(2) . . yes C(64) C(65) 1.36(3) . . yes C(64) C(66) 1.46(2) . . yes C(67) C(68) 1.52(2) . . yes C(67) C(69) 1.54(1) . . yes C(71) C(72) 1.47(1) . . yes C(81) C(82) 1.46(2) . . yes C(83) C(84) 1.46(1) . . yes C(85) C(86) 1.42(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 O(1) Pd(1) O(2) 80.8(2) . . . yes O(1) Pd(1) N(41) 175.3(2) . . . yes O(1) Pd(1) N(51) 96.1(2) . . . yes O(2) Pd(1) N(41) 96.5(2) . . . yes O(2) Pd(1) N(51) 176.7(2) . . . yes N(41) Pd(1) N(51) 86.7(2) . . . yes O(1) Ni(1) O(2) 78.4(2) . . . yes O(1) Ni(1) N(11) 171.3(2) . . . yes O(1) Ni(1) N(21) 96.4(2) . . . yes O(1) Ni(1) N(31) 98.4(2) . . . yes O(1) Ni(1) N(71) 85.6(2) . . . yes O(2) Ni(1) N(11) 95.0(2) . . . yes O(2) Ni(1) N(21) 173.5(2) . . . yes O(2) Ni(1) N(31) 98.2(2) . . . yes O(2) Ni(1) N(71) 86.0(2) . . . yes N(11) Ni(1) N(21) 89.8(2) . . . yes N(11) Ni(1) N(31) 88.1(2) . . . yes N(11) Ni(1) N(71) 88.3(2) . . . yes N(21) Ni(1) N(31) 86.4(2) . . . yes N(21) Ni(1) N(71) 89.7(2) . . . yes N(31) Ni(1) N(71) 174.7(2) . . . yes Pd(1) O(1) Ni(1) 100.1(2) . . . yes Pd(1) O(2) Ni(1) 98.8(2) . . . yes Ni(1) N(11) N(12) 116.5(4) . . . yes Ni(1) N(11) C(11) 135.9(4) . . . yes N(12) N(11) C(11) 107.4(4) . . . yes N(11) N(12) C(13) 109.3(6) . . . yes N(11) N(12) B(1) 119.8(4) . . . yes C(13) N(12) B(1) 130.9(6) . . . yes Ni(1) N(21) N(22) 116.7(3) . . . yes Ni(1) N(21) C(21) 135.1(4) . . . yes N(22) N(21) C(21) 108.1(5) . . . yes N(21) N(22) C(23) 109.0(5) . . . yes N(21) N(22) B(1) 120.0(5) . . . yes C(23) N(22) B(1) 131.0(5) . . . yes Ni(1) N(31) N(32) 115.8(3) . . . yes Ni(1) N(31) C(31) 137.9(5) . . . yes N(32) N(31) C(31) 106.3(5) . . . yes N(31) N(32) C(33) 110.1(4) . . . yes N(31) N(32) B(1) 119.9(5) . . . yes C(33) N(32) B(1) 130.0(5) . . . yes Pd(1) N(41) N(42) 120.3(4) . . . yes Pd(1) N(41) C(41) 131.3(4) . . . yes N(42) N(41) C(41) 107.6(5) . . . yes N(41) N(42) C(43) 108.8(5) . . . yes N(41) N(42) B(2) 119.7(5) . . . yes C(43) N(42) B(2) 131.2(5) . . . yes Pd(1) N(51) N(52) 120.1(3) . . . yes Pd(1) N(51) C(51) 131.7(3) . . . yes N(52) N(51) C(51) 107.8(4) . . . yes N(51) N(52) C(53) 107.9(5) . . . yes N(51) N(52) B(2) 120.2(4) . . . yes C(53) N(52) B(2) 130.2(5) . . . yes N(62) N(61) C(61) 105.3(6) . . . yes N(61) N(62) C(63) 108.3(6) . . . yes N(61) N(62) B(2) 115.8(5) . . . yes C(63) N(62) B(2) 132.0(7) . . . yes Ni(1) N(71) C(71) 179.1(6) . . . yes N(11) C(11) C(12) 109.5(7) . . . yes N(11) C(11) C(14) 123.4(5) . . . yes C(12) C(11) C(14) 127.1(6) . . . yes C(11) C(12) C(13) 105.9(6) . . . yes N(12) C(13) C(12) 107.8(6) . . . yes N(12) C(13) C(15) 123.0(7) . . . yes C(12) C(13) C(15) 129.2(6) . . . yes N(21) C(21) C(22) 108.9(5) . . . yes N(21) C(21) C(24) 123.3(6) . . . yes C(22) C(21) C(24) 127.8(6) . . . yes C(21) C(22) C(23) 106.2(6) . . . yes N(22) C(23) C(22) 107.9(6) . . . yes N(22) C(23) C(25) 123.0(6) . . . yes C(22) C(23) C(25) 129.1(7) . . . yes N(31) C(31) C(32) 110.1(6) . . . yes N(31) C(31) C(34) 121.7(7) . . . yes C(32) C(31) C(34) 128.2(6) . . . yes C(31) C(32) C(33) 106.2(6) . . . yes N(32) C(33) C(32) 107.3(6) . . . yes N(32) C(33) C(35) 124.3(5) . . . yes C(32) C(33) C(35) 128.4(7) . . . yes N(41) C(41) C(42) 108.7(5) . . . yes N(41) C(41) C(44) 122.4(7) . . . yes C(42) C(41) C(44) 128.8(7) . . . yes C(41) C(42) C(43) 107.9(7) . . . yes N(42) C(43) C(42) 107.1(6) . . . yes N(42) C(43) C(47) 122.6(6) . . . yes C(42) C(43) C(47) 130.3(8) . . . yes C(41) C(44) C(45) 111.0(6) . . . yes C(41) C(44) C(46) 109.4(6) . . . yes C(45) C(44) C(46) 112.6(7) . . . yes C(43) C(47) C(48) 106.6(7) . . . yes C(43) C(47) C(48A) 121(1) . . . yes C(43) C(47) C(49) 117.5(9) . . . yes C(43) C(47) C(49A) 106.4(9) . . . yes C(48) C(47) C(48A) 60(1) . . . yes C(48) C(47) C(49) 115(1) . . . yes C(48) C(47) C(49A) 71(1) . . . yes C(48A) C(47) C(49) 119(1) . . . yes C(48A) C(47) C(49A) 118(1) . . . yes C(49) C(47) C(49A) 53(1) . . . yes C(47) C(48) C(48A) 45(1) . . . yes C(47) C(48A) C(48) 73(1) . . . yes C(47) C(49) C(49A) 76(1) . . . yes C(47) C(49A) C(49) 50(1) . . . yes N(51) C(51) C(52) 109.7(5) . . . yes N(51) C(51) C(54) 121.9(5) . . . yes C(52) C(51) C(54) 128.3(6) . . . yes C(51) C(52) C(53) 106.3(5) . . . yes N(52) C(53) C(52) 108.3(5) . . . yes N(52) C(53) C(57) 122.5(6) . . . yes C(52) C(53) C(57) 129.2(5) . . . yes C(51) C(54) C(55) 110.7(7) . . . yes C(51) C(54) C(56) 111.8(5) . . . yes C(55) C(54) C(56) 111.6(6) . . . yes C(53) C(57) C(58) 110.8(6) . . . yes C(53) C(57) C(59) 110.5(7) . . . yes C(58) C(57) C(59) 111.5(6) . . . yes N(61) C(61) C(62) 111.5(9) . . . yes N(61) C(61) C(64) 118.2(8) . . . yes C(62) C(61) C(64) 130.2(9) . . . yes C(61) C(62) C(63) 106.3(8) . . . yes N(62) C(63) C(62) 108.4(8) . . . yes N(62) C(63) C(67) 126.3(8) . . . yes C(62) C(63) C(67) 125.2(8) . . . yes C(61) C(64) C(65) 119(1) . . . yes C(61) C(64) C(66) 119(1) . . . yes C(65) C(64) C(66) 120(1) . . . yes C(63) C(67) C(68) 110.8(9) . . . yes C(63) C(67) C(69) 113.6(10) . . . yes C(68) C(67) C(69) 111.0(9) . . . yes N(71) C(71) C(72) 179.2(7) . . . yes N(81) C(81) C(82) 178(1) . . . yes N(82) C(83) C(84) 177.6(10) . . . yes N(83) C(85) C(86) 177(1) . . . yes N(12) B(1) N(22) 110.2(5) . . . yes N(12) B(1) N(32) 108.7(5) . . . yes N(22) B(1) N(32) 108.8(4) . . . yes N(42) B(2) N(52) 107.7(5) . . . yes N(42) B(2) N(62) 111.7(5) . . . yes N(52) B(2) N(62) 112.2(6) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . yes ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(11) C(72) 3.479(8) . 2_655 ? N(12) C(72) 3.359(9) . 2_655 ? N(21) C(72) 3.450(8) . 2_655 ? N(22) C(72) 3.337(9) . 2_655 ? N(22) C(84) 3.582(9) . 1_455 ? N(31) C(84) 3.59(1) . 1_455 ? N(32) C(84) 3.567(10) . 1_455 ? N(81) C(86) 3.40(1) . 1_454 ? N(81) C(48) 3.41(2) . 1_455 ? N(83) C(84) 3.31(2) . 1_455 ? C(13) C(72) 3.52(1) . 2_655 ? C(15) C(25) 3.561(10) . 2_555 ? C(23) C(72) 3.51(1) . 2_655 ? C(23) C(83) 3.59(1) . 1_455 ? C(32) C(48A) 3.56(2) . 1_455 ? C(48) C(81) 3.39(2) . 1_655 ? Pd(1) N(52) 2.947(4) . . ? Pd(1) N(42) 2.964(5) . . ? Pd(1) Ni(1) 3.1004(9) . . ? Ni(1) N(22) 2.971(5) . . ? Ni(1) N(32) 2.980(6) . . ? Ni(1) N(12) 2.981(4) . . ? O(1) O(2) 2.600(6) . . ? O(1) N(51) 2.976(6) . . ? O(1) N(21) 3.086(6) . . ? O(1) N(31) 3.145(6) . . ? O(2) N(41) 3.003(7) . . ? O(2) N(11) 3.076(6) . . ? O(2) N(31) 3.156(8) . . ? N(11) N(31) 2.929(7) . . ? N(11) N(21) 2.963(7) . . ? N(11) N(32) 3.010(8) . . ? N(11) N(22) 3.048(8) . . ? N(12) N(22) 2.502(7) . . ? N(12) N(32) 2.503(7) . . ? N(12) N(21) 3.048(6) . . ? N(12) N(31) 3.064(6) . . ? N(21) N(31) 2.877(6) . . ? N(21) N(32) 3.010(7) . . ? N(22) N(32) 2.502(6) . . ? N(22) N(31) 3.019(6) . . ? N(41) N(51) 2.756(7) . . ? N(41) N(52) 2.978(6) . . ? N(42) N(51) 2.933(8) . . ? N(51) N(61) 3.565(7) . . ? N(52) N(61) 2.905(8) . . ? #------------------------------------------------------------------------------ #===END data_compound_5c(Ni) _database_code_CSD 213633 _audit_creation_date 'Thu Jul 17 21:27:12 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C46 H74 B2 N14 O2 Ni Pd ' _chemical_formula_moiety 'C46 H74 B2 N14 O2 Ni Pd ' _chemical_formula_weight 1041.90 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 22.458(3) _cell_length_b 9.007(1) _cell_length_c 26.689(4) _cell_angle_alpha 90 _cell_angle_beta 94.160(2) _cell_angle_gamma 90 _cell_volume 5384(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9680 _cell_measurement_theta_min 0.8 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.964 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11219 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7556 _reflns_number_gt 3583 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.2352 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3583 _refine_ls_number_parameters 612 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0330 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.50 _refine_diff_density_min -1.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 0.18104(4) 0.4224(1) 0.86296(3) 0.0381(2) Uani 1.00 d . . . Ni(1) Ni 0.17721(6) 0.4050(2) 0.74592(4) 0.0384(4) Uani 1.00 d . . . O(1) O 0.1549(3) 0.2850(9) 0.8056(3) 0.048(2) Uani 1.00 d . . . O(2) O 0.2125(3) 0.5326(9) 0.8041(2) 0.045(2) Uani 1.00 d . . . N(11) N 0.1825(4) 0.567(1) 0.6915(3) 0.044(2) Uani 1.00 d . . . N(12) N 0.1993(4) 0.521(1) 0.6452(3) 0.043(2) Uani 1.00 d . . . N(21) N 0.1234(4) 0.288(1) 0.6925(3) 0.045(2) Uani 1.00 d . . . N(22) N 0.1468(4) 0.277(1) 0.6451(3) 0.043(2) Uani 1.00 d . . . N(31) N 0.2503(4) 0.300(1) 0.7244(3) 0.041(2) Uani 1.00 d . . . N(32) N 0.2577(4) 0.292(1) 0.6726(3) 0.039(2) Uani 1.00 d . . . N(41) N 0.2069(4) 0.571(1) 0.9174(3) 0.045(2) Uani 1.00 d . . . N(42) N 0.1702(4) 0.5931(10) 0.9562(3) 0.041(2) Uani 1.00 d . . . N(51) N 0.1501(4) 0.289(1) 0.9155(3) 0.046(2) Uani 1.00 d . . . N(52) N 0.1138(4) 0.352(1) 0.9513(3) 0.040(2) Uani 1.00 d . . . N(61) N 0.0691(4) 0.738(1) 0.9063(3) 0.051(3) Uani 1.00 d . . . N(62) N 0.0663(4) 0.589(1) 0.9130(3) 0.045(2) Uani 1.00 d . . . N(71) N 0.039(2) 0.168(5) 0.393(1) 0.22(2) Uani 1.00 d . . . N(72) N 0.0825(10) 0.323(3) 0.2745(9) 0.159(9) Uani 1.00 d . . . C(11) C 0.1767(5) 0.718(1) 0.6880(4) 0.049(3) Uani 1.00 d . . . C(12) C 0.1898(5) 0.765(1) 0.6406(4) 0.053(3) Uani 1.00 d . . . C(13) C 0.2041(6) 0.640(1) 0.6148(4) 0.053(3) Uani 1.00 d . . . C(14) C 0.1594(7) 0.810(2) 0.7312(5) 0.065(4) Uani 1.00 d . . . C(15) C 0.1807(8) 0.957(2) 0.7335(6) 0.099(6) Uani 1.00 d . . . C(16) C 0.1097(6) 0.762(2) 0.7581(4) 0.075(4) Uani 1.00 d . . . C(17) C 0.2279(6) 0.623(1) 0.5622(4) 0.055(3) Uani 1.00 d . . . C(18) C 0.2081(9) 0.755(2) 0.5306(5) 0.100(6) Uani 1.00 d . . . C(19) C 0.2948(7) 0.609(2) 0.5659(5) 0.079(4) Uani 1.00 d . . . C(21) C 0.0713(6) 0.217(2) 0.6895(4) 0.056(3) Uani 1.00 d . . . C(22) C 0.0587(5) 0.163(2) 0.6401(4) 0.060(4) Uani 1.00 d . . . C(23) C 0.1071(5) 0.202(1) 0.6145(4) 0.045(3) Uani 1.00 d . . . C(24) C 0.0320(6) 0.206(2) 0.7315(4) 0.064(4) Uani 1.00 d . . . C(25) C -0.0153(7) 0.094(2) 0.7280(5) 0.077(4) Uani 1.00 d . . . C(26) C 0.0115(7) 0.356(2) 0.7487(5) 0.085(5) Uani 1.00 d . . . C(27) C 0.1169(6) 0.175(2) 0.5595(4) 0.074(5) Uani 1.00 d . . . C(28) C 0.0821(7) 0.039(2) 0.5404(5) 0.083(5) Uani 1.00 d . . . C(29) C 0.0977(8) 0.315(2) 0.5299(6) 0.099(6) Uani 1.00 d . . . C(31) C 0.2986(4) 0.233(1) 0.7467(3) 0.037(3) Uani 1.00 d . . . C(32) C 0.3353(4) 0.180(1) 0.7103(4) 0.039(3) Uani 1.00 d . . . C(33) C 0.3083(5) 0.217(1) 0.6646(4) 0.051(3) Uani 1.00 d . . . C(34) C 0.3072(5) 0.218(1) 0.8032(4) 0.049(3) Uani 1.00 d . . . C(35) C 0.3572(5) 0.324(1) 0.8225(4) 0.054(3) Uani 1.00 d . . . C(36) C 0.3228(6) 0.062(2) 0.8195(4) 0.070(4) Uani 1.00 d . . . C(37) C 0.3286(5) 0.182(1) 0.6131(4) 0.052(3) Uani 1.00 d . . . C(38) C 0.3924(7) 0.227(3) 0.6085(6) 0.120(8) Uani 1.00 d . . . C(39) C 0.315(1) 0.036(2) 0.5978(6) 0.138(9) Uani 1.00 d . . . C(41) C 0.2565(5) 0.654(1) 0.9250(4) 0.043(3) Uani 1.00 d . . . C(42) C 0.2505(6) 0.731(1) 0.9706(5) 0.054(3) Uani 1.00 d . . . C(43) C 0.1967(6) 0.692(1) 0.9883(4) 0.051(3) Uani 1.00 d . . . C(44) C 0.3061(6) 0.660(2) 0.8918(5) 0.072(4) Uani 1.00 d . . . C(45) C 0.1706(7) 0.746(2) 1.0352(5) 0.079(4) Uani 1.00 d . . . C(51) C 0.1481(5) 0.144(1) 0.9206(4) 0.039(2) Uani 1.00 d . . . C(52) C 0.1134(6) 0.111(1) 0.9605(4) 0.057(3) Uani 1.00 d . . . C(53) C 0.0935(5) 0.241(1) 0.9781(4) 0.046(3) Uani 1.00 d . . . C(54) C 0.1829(6) 0.038(1) 0.8914(5) 0.064(4) Uani 1.00 d . . . C(55) C 0.0506(7) 0.267(2) 1.0218(5) 0.084(5) Uani 1.00 d . . . C(61) C 0.0247(5) 0.767(2) 0.8722(4) 0.054(3) Uani 1.00 d . . . C(62) C -0.0072(6) 0.643(2) 0.8579(4) 0.056(3) Uani 1.00 d . . . C(63) C 0.0194(5) 0.529(2) 0.8844(4) 0.053(3) Uani 1.00 d . . . C(64) C 0.0123(6) 0.927(2) 0.8580(5) 0.065(4) Uani 1.00 d . . . C(65) C 0.0001(7) 0.370(2) 0.8858(6) 0.070(4) Uani 1.00 d . . . C(71) C 0.003(3) 0.279(7) 0.382(2) 0.31(5) Uani 1.00 d . . . C(72) C -0.026(2) 0.392(3) 0.380(2) 0.33(4) Uani 1.00 d . . . C(73) C 0.1234(10) 0.238(2) 0.2794(7) 0.095(5) Uani 1.00 d . . . C(74) C 0.1669(9) 0.131(3) 0.2840(8) 0.121(8) Uani 1.00 d . . . B(1) B 0.2063(6) 0.352(2) 0.6363(4) 0.046(3) Uani 1.00 d . . . B(2) B 0.1106(6) 0.521(2) 0.9561(4) 0.050(4) Uani 1.00 d . . . H(3) H 0.2157 0.3348 0.6020 0.0494 Uiso 1.00 calc . . . H(4) H 0.1896 0.8693 0.6285 0.0626 Uiso 1.00 calc . . . H(5) H 0.1610 1.0280 0.7538 0.1245 Uiso 1.00 calc . . . H(6) H 0.2129 0.9866 0.7156 0.1245 Uiso 1.00 calc . . . H(7) H 0.1037 0.8310 0.7848 0.0751 Uiso 1.00 calc . . . H(8) H 0.1177 0.6654 0.7720 0.0751 Uiso 1.00 calc . . . H(9) H 0.0744 0.7587 0.7356 0.0751 Uiso 1.00 calc . . . H(10) H 0.2103 0.5355 0.5469 0.0712 Uiso 1.00 calc . . . H(11) H 0.2191 0.8447 0.5484 0.1004 Uiso 1.00 calc . . . H(12) H 0.1655 0.7521 0.5239 0.1004 Uiso 1.00 calc . . . H(13) H 0.2270 0.7523 0.4995 0.1004 Uiso 1.00 calc . . . H(14) H 0.3059 0.5115 0.5778 0.0788 Uiso 1.00 calc . . . H(15) H 0.3118 0.6820 0.5889 0.0788 Uiso 1.00 calc . . . H(16) H 0.3094 0.6244 0.5333 0.0788 Uiso 1.00 calc . . . H(17) H 0.0228 0.1142 0.6267 0.0706 Uiso 1.00 calc . . . H(18) H 0.0582 0.1741 0.7592 0.0751 Uiso 1.00 calc . . . H(19) H -0.0319 0.0836 0.7599 0.0766 Uiso 1.00 calc . . . H(20) H 0.0012 0.0002 0.7185 0.0766 Uiso 1.00 calc . . . H(21) H -0.0461 0.1233 0.7031 0.0766 Uiso 1.00 calc . . . H(22) H 0.0449 0.4230 0.7520 0.0846 Uiso 1.00 calc . . . H(23) H -0.0054 0.3463 0.7806 0.0846 Uiso 1.00 calc . . . H(24) H -0.0182 0.3952 0.7245 0.0846 Uiso 1.00 calc . . . H(25) H 0.1585 0.1585 0.5558 0.0919 Uiso 1.00 calc . . . H(26) H 0.0406 0.0524 0.5458 0.0827 Uiso 1.00 calc . . . H(27) H 0.0971 -0.0472 0.5581 0.0827 Uiso 1.00 calc . . . H(28) H 0.0866 0.0273 0.5051 0.0827 Uiso 1.00 calc . . . H(29) H 0.1212 0.3981 0.5425 0.0993 Uiso 1.00 calc . . . H(30) H 0.0562 0.3349 0.5338 0.0993 Uiso 1.00 calc . . . H(31) H 0.1036 0.3010 0.4950 0.0993 Uiso 1.00 calc . . . H(32) H 0.3726 0.1277 0.7175 0.0501 Uiso 1.00 calc . . . H(33) H 0.2709 0.2498 0.8179 0.0636 Uiso 1.00 calc . . . H(34) H 0.3555 0.3383 0.8580 0.0544 Uiso 1.00 calc . . . H(35) H 0.3522 0.4180 0.8057 0.0544 Uiso 1.00 calc . . . H(36) H 0.3952 0.2825 0.8158 0.0544 Uiso 1.00 calc . . . H(37) H 0.2926 -0.0050 0.8059 0.0699 Uiso 1.00 calc . . . H(38) H 0.3253 0.0563 0.8555 0.0699 Uiso 1.00 calc . . . H(39) H 0.3606 0.0350 0.8074 0.0699 Uiso 1.00 calc . . . H(40) H 0.3042 0.2418 0.5891 0.0627 Uiso 1.00 calc . . . H(41) H 0.4176 0.1789 0.6342 0.1201 Uiso 1.00 calc . . . H(42) H 0.3960 0.3329 0.6124 0.1201 Uiso 1.00 calc . . . H(43) H 0.4045 0.1989 0.5761 0.1201 Uiso 1.00 calc . . . H(44) H 0.2788 0.0049 0.6124 0.1381 Uiso 1.00 calc . . . H(45) H 0.3468 -0.0290 0.6086 0.1381 Uiso 1.00 calc . . . H(46) H 0.3084 0.0328 0.5618 0.1381 Uiso 1.00 calc . . . H(47) H 0.2802 0.8000 0.9860 0.0715 Uiso 1.00 calc . . . H(48) H 0.3364 0.5899 0.9033 0.0716 Uiso 1.00 calc . . . H(49) H 0.3228 0.7580 0.8923 0.0716 Uiso 1.00 calc . . . H(50) H 0.2915 0.6351 0.8581 0.0716 Uiso 1.00 calc . . . H(51) H 0.1983 0.8123 1.0529 0.0785 Uiso 1.00 calc . . . H(52) H 0.1628 0.6632 1.0562 0.0785 Uiso 1.00 calc . . . H(53) H 0.1340 0.7982 1.0264 0.0785 Uiso 1.00 calc . . . H(54) H 0.1036 0.0094 0.9723 0.0691 Uiso 1.00 calc . . . H(55) H 0.1630 -0.0564 0.8895 0.0640 Uiso 1.00 calc . . . H(56) H 0.2221 0.0258 0.9078 0.0640 Uiso 1.00 calc . . . H(57) H 0.1861 0.0760 0.8581 0.0640 Uiso 1.00 calc . . . H(58) H 0.0667 0.3435 1.0438 0.0836 Uiso 1.00 calc . . . H(59) H 0.0472 0.1764 1.0404 0.0836 Uiso 1.00 calc . . . H(60) H 0.0119 0.2962 1.0076 0.0836 Uiso 1.00 calc . . . H(61) H -0.0419 0.6349 0.8336 0.0706 Uiso 1.00 calc . . . H(62) H 0.0493 0.9803 0.8582 0.0650 Uiso 1.00 calc . . . H(63) H -0.0126 0.9708 0.8817 0.0650 Uiso 1.00 calc . . . H(64) H -0.0077 0.9308 0.8250 0.0650 Uiso 1.00 calc . . . H(65) H -0.0113 0.3464 0.9189 0.0698 Uiso 1.00 calc . . . H(66) H 0.0324 0.3070 0.8776 0.0698 Uiso 1.00 calc . . . H(67) H -0.0334 0.3550 0.8619 0.0698 Uiso 1.00 calc . . . H(68) H 0.0941 0.5444 0.9880 0.0617 Uiso 1.00 calc . . . H(72) H 0.1685 0.0896 0.3177 0.1220 Uiso 1.00 calc . . . H(73) H 0.2049 0.1736 0.2785 0.1220 Uiso 1.00 calc . . . H(74) H 0.1579 0.0529 0.2603 0.1220 Uiso 1.00 calc . . . 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) 0.0472(5) 0.0442(5) 0.0234(4) 0.0007(5) 0.0057(3) -0.0017(4) Ni(1) 0.0439(8) 0.0488(9) 0.0233(6) -0.0028(7) 0.0081(5) -0.0037(6) O(1) 0.058(5) 0.050(5) 0.038(4) -0.007(4) 0.014(4) -0.011(3) O(2) 0.058(5) 0.053(5) 0.024(3) -0.005(4) 0.006(3) -0.003(3) N(11) 0.056(6) 0.053(6) 0.025(4) -0.001(5) 0.009(4) 0.002(4) N(12) 0.059(6) 0.048(6) 0.024(4) 0.005(5) 0.014(4) -0.008(4) N(21) 0.044(5) 0.060(7) 0.032(5) -0.006(5) 0.010(4) -0.013(4) N(22) 0.055(5) 0.062(7) 0.012(4) -0.008(5) 0.008(4) 0.002(4) N(31) 0.048(5) 0.051(6) 0.024(4) 0.009(5) 0.009(4) 0.001(4) N(32) 0.043(5) 0.066(7) 0.011(4) 0.002(5) 0.007(3) -0.005(4) N(41) 0.072(6) 0.042(6) 0.023(4) 0.005(5) 0.006(4) -0.013(4) N(42) 0.063(6) 0.037(5) 0.023(4) 0.009(5) 0.003(4) -0.007(4) N(51) 0.052(6) 0.066(7) 0.021(4) 0.017(5) 0.005(4) -0.009(4) N(52) 0.050(5) 0.042(6) 0.029(4) 0.001(4) 0.015(4) 0.000(4) N(61) 0.049(6) 0.065(7) 0.040(5) 0.004(5) 0.011(4) 0.001(5) N(62) 0.063(6) 0.044(6) 0.030(4) -0.004(5) 0.007(4) -0.002(4) N(71) 0.22(3) 0.28(4) 0.17(3) -0.08(3) 0.04(2) -0.08(3) N(72) 0.14(2) 0.14(2) 0.20(2) 0.03(1) 0.00(2) -0.01(2) C(11) 0.054(7) 0.062(9) 0.030(6) 0.010(6) 0.013(5) 0.002(5) C(12) 0.058(7) 0.059(9) 0.042(6) 0.010(6) 0.012(6) 0.004(6) C(13) 0.080(9) 0.048(8) 0.033(6) 0.006(7) 0.018(6) 0.006(5) C(14) 0.09(1) 0.061(9) 0.047(7) 0.003(8) 0.016(7) 0.003(6) C(15) 0.14(2) 0.08(1) 0.09(1) -0.04(1) 0.07(1) -0.040(9) C(16) 0.083(10) 0.11(1) 0.031(6) 0.011(9) 0.028(6) -0.025(7) C(17) 0.087(9) 0.048(8) 0.032(6) -0.009(7) 0.027(6) -0.001(5) C(18) 0.18(2) 0.10(1) 0.032(7) 0.02(1) 0.021(9) 0.013(8) C(19) 0.10(1) 0.08(1) 0.062(8) -0.007(9) 0.044(8) -0.018(8) C(21) 0.055(7) 0.08(1) 0.028(6) 0.006(7) -0.001(5) -0.013(6) C(22) 0.051(7) 0.09(1) 0.036(6) -0.021(7) -0.001(5) -0.025(6) C(23) 0.039(6) 0.067(9) 0.030(5) -0.012(6) 0.014(4) -0.008(5) C(24) 0.057(8) 0.10(1) 0.033(6) -0.028(8) 0.014(6) -0.013(7) C(25) 0.09(1) 0.10(1) 0.043(7) 0.012(10) 0.026(7) 0.014(8) C(26) 0.08(1) 0.12(1) 0.053(9) 0.00(1) 0.013(8) 0.006(9) C(27) 0.066(9) 0.13(1) 0.025(6) -0.010(9) 0.004(6) -0.016(7) C(28) 0.09(1) 0.11(1) 0.049(8) -0.014(10) 0.008(7) -0.036(8) C(29) 0.12(1) 0.13(2) 0.047(9) -0.01(1) -0.016(9) -0.011(9) C(31) 0.042(6) 0.057(7) 0.014(4) 0.004(5) 0.017(4) -0.004(4) C(32) 0.031(5) 0.040(7) 0.046(6) 0.015(5) 0.009(4) -0.006(5) C(33) 0.055(7) 0.064(9) 0.032(6) 0.000(7) 0.008(5) -0.007(6) C(34) 0.061(7) 0.059(8) 0.029(6) 0.007(7) 0.012(5) 0.008(5) C(35) 0.067(8) 0.063(9) 0.033(6) 0.012(7) -0.001(6) -0.009(5) C(36) 0.076(9) 0.10(1) 0.041(6) 0.005(8) 0.019(6) 0.020(7) C(37) 0.052(7) 0.068(9) 0.038(6) 0.004(6) 0.019(5) -0.010(6) C(38) 0.07(1) 0.22(3) 0.07(1) 0.01(1) 0.029(9) -0.02(1) C(39) 0.25(3) 0.09(1) 0.09(1) -0.03(2) 0.11(1) -0.03(1) C(41) 0.034(6) 0.055(7) 0.038(6) -0.007(5) -0.004(5) 0.002(5) C(42) 0.062(8) 0.056(8) 0.043(7) -0.005(7) -0.009(6) -0.013(6) C(43) 0.071(9) 0.043(7) 0.034(6) 0.001(6) -0.019(6) -0.009(5) C(44) 0.055(8) 0.08(1) 0.074(9) -0.012(7) 0.000(7) -0.041(8) C(45) 0.10(1) 0.09(1) 0.042(7) 0.003(10) 0.006(7) -0.010(8) C(51) 0.051(7) 0.024(6) 0.042(6) 0.006(5) 0.013(5) 0.010(5) C(52) 0.076(9) 0.054(9) 0.040(6) -0.001(7) 0.003(6) 0.018(6) C(53) 0.059(7) 0.051(8) 0.029(5) 0.014(6) 0.014(5) 0.000(5) C(54) 0.080(9) 0.043(8) 0.072(9) 0.016(7) 0.027(7) -0.006(6) C(55) 0.09(1) 0.12(1) 0.049(8) 0.010(10) 0.033(8) 0.013(8) C(61) 0.040(7) 0.075(10) 0.049(7) 0.012(7) 0.010(5) 0.013(7) C(62) 0.064(8) 0.075(10) 0.029(6) 0.022(7) 0.001(5) 0.003(6) C(63) 0.050(7) 0.072(10) 0.037(6) 0.009(6) 0.012(5) -0.004(6) C(64) 0.066(8) 0.08(1) 0.048(7) 0.009(8) 0.019(6) 0.015(7) C(65) 0.076(10) 0.057(9) 0.073(9) -0.001(8) -0.019(8) 0.003(7) C(71) 0.40(8) 0.39(8) 0.16(4) -0.33(7) 0.23(5) -0.19(5) C(72) 0.19(3) 0.10(2) 0.7(1) 0.05(2) -0.17(5) -0.10(4) C(73) 0.11(2) 0.08(1) 0.10(1) 0.00(1) 0.03(1) -0.01(1) C(74) 0.11(1) 0.13(2) 0.12(2) 0.04(1) -0.03(1) -0.04(1) B(1) 0.047(7) 0.075(10) 0.020(5) -0.005(7) 0.026(5) -0.007(6) B(2) 0.037(7) 0.09(1) 0.022(6) -0.009(7) 0.004(5) -0.003(6) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL97 _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) O(1) 2.022(7) . . yes Pd(1) O(2) 2.029(7) . . yes Pd(1) N(41) 2.031(8) . . yes Pd(1) N(51) 2.006(9) . . yes Ni(1) O(1) 2.018(8) . . yes Ni(1) O(2) 2.045(7) . . yes Ni(1) N(11) 2.070(9) . . yes Ni(1) N(21) 2.089(9) . . yes Ni(1) N(31) 2.013(9) . . yes N(11) N(12) 1.38(1) . . yes N(11) C(11) 1.37(2) . . yes N(12) C(13) 1.35(2) . . yes N(12) B(1) 1.55(2) . . yes N(21) N(22) 1.41(1) . . yes N(21) C(21) 1.33(2) . . yes N(22) C(23) 1.35(1) . . yes N(22) B(1) 1.53(2) . . yes N(31) N(32) 1.41(1) . . yes N(31) C(31) 1.35(1) . . yes N(32) C(33) 1.35(2) . . yes N(32) B(1) 1.55(1) . . yes N(41) N(42) 1.38(1) . . yes N(41) C(41) 1.34(1) . . yes N(42) C(43) 1.35(1) . . yes N(42) B(2) 1.49(2) . . yes N(51) N(52) 1.42(1) . . yes N(51) C(51) 1.32(1) . . yes N(52) C(53) 1.33(2) . . yes N(52) B(2) 1.53(2) . . yes N(61) N(62) 1.36(1) . . yes N(61) C(61) 1.33(1) . . yes N(62) C(63) 1.37(1) . . yes N(62) B(2) 1.58(2) . . yes N(71) C(71) 1.30(8) . . yes N(72) C(73) 1.19(3) . . yes C(11) C(12) 1.38(2) . . yes C(11) C(14) 1.49(2) . . yes C(12) C(13) 1.37(2) . . yes C(13) C(17) 1.55(2) . . yes C(14) C(15) 1.41(2) . . yes C(14) C(16) 1.44(2) . . yes C(17) C(18) 1.50(2) . . yes C(17) C(19) 1.50(2) . . yes C(21) C(22) 1.41(2) . . yes C(21) C(24) 1.48(2) . . yes C(22) C(23) 1.37(2) . . yes C(23) C(27) 1.52(2) . . yes C(24) C(25) 1.47(2) . . yes C(24) C(26) 1.51(2) . . yes C(27) C(28) 1.51(2) . . yes C(27) C(29) 1.54(2) . . yes C(31) C(32) 1.40(1) . . yes C(31) C(34) 1.51(1) . . yes C(32) C(33) 1.36(1) . . yes C(33) C(37) 1.51(2) . . yes C(34) C(35) 1.53(2) . . yes C(34) C(36) 1.51(2) . . yes C(37) C(38) 1.50(2) . . yes C(37) C(39) 1.40(2) . . yes C(41) C(42) 1.41(2) . . yes C(41) C(44) 1.47(2) . . yes C(42) C(43) 1.37(2) . . yes C(43) C(45) 1.50(2) . . yes C(51) C(52) 1.40(2) . . yes C(51) C(54) 1.49(2) . . yes C(52) C(53) 1.35(2) . . yes C(53) C(55) 1.58(2) . . yes C(61) C(62) 1.37(2) . . yes C(61) C(64) 1.51(2) . . yes C(62) C(63) 1.36(2) . . yes C(63) C(65) 1.49(2) . . yes C(71) C(72) 1.21(7) . . yes C(73) C(74) 1.38(3) . . 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 O(1) Pd(1) O(2) 79.1(3) . . . yes O(1) Pd(1) N(41) 176.4(3) . . . yes O(1) Pd(1) N(51) 93.9(3) . . . yes O(2) Pd(1) N(41) 97.7(3) . . . yes O(2) Pd(1) N(51) 172.5(3) . . . yes N(41) Pd(1) N(51) 89.4(4) . . . yes O(1) Ni(1) O(2) 78.9(3) . . . yes O(1) Ni(1) N(11) 164.2(3) . . . yes O(1) Ni(1) N(21) 96.0(3) . . . yes O(1) Ni(1) N(31) 103.2(3) . . . yes O(2) Ni(1) N(11) 95.5(3) . . . yes O(2) Ni(1) N(21) 167.5(3) . . . yes O(2) Ni(1) N(31) 101.6(3) . . . yes N(11) Ni(1) N(21) 86.5(4) . . . yes N(11) Ni(1) N(31) 92.4(4) . . . yes N(21) Ni(1) N(31) 90.6(4) . . . yes Pd(1) O(1) Ni(1) 101.2(3) . . . yes Pd(1) O(2) Ni(1) 100.1(3) . . . yes Ni(1) N(11) N(12) 116.5(7) . . . yes Ni(1) N(11) C(11) 137.7(7) . . . yes N(12) N(11) C(11) 105.7(8) . . . yes N(11) N(12) C(13) 109.5(9) . . . yes N(11) N(12) B(1) 118.2(8) . . . yes C(13) N(12) B(1) 132.3(9) . . . yes Ni(1) N(21) N(22) 114.4(7) . . . yes Ni(1) N(21) C(21) 138.3(7) . . . yes N(22) N(21) C(21) 107.4(8) . . . yes N(21) N(22) C(23) 107.8(8) . . . yes N(21) N(22) B(1) 119.7(8) . . . yes C(23) N(22) B(1) 132.4(8) . . . yes Ni(1) N(31) N(32) 117.6(6) . . . yes Ni(1) N(31) C(31) 137.2(6) . . . yes N(32) N(31) C(31) 105.2(8) . . . yes N(31) N(32) C(33) 110.1(8) . . . yes N(31) N(32) B(1) 117.3(8) . . . yes C(33) N(32) B(1) 132.3(8) . . . yes Pd(1) N(41) N(42) 118.2(7) . . . yes Pd(1) N(41) C(41) 131.8(7) . . . yes N(42) N(41) C(41) 109.9(8) . . . yes N(41) N(42) C(43) 108.0(9) . . . yes N(41) N(42) B(2) 121.6(8) . . . yes C(43) N(42) B(2) 130.2(10) . . . yes Pd(1) N(51) N(52) 118.7(7) . . . yes Pd(1) N(51) C(51) 133.0(7) . . . yes N(52) N(51) C(51) 107.4(9) . . . yes N(51) N(52) C(53) 107.6(9) . . . yes N(51) N(52) B(2) 118.9(9) . . . yes C(53) N(52) B(2) 133.0(9) . . . yes N(62) N(61) C(61) 104.2(10) . . . yes N(61) N(62) C(63) 110.9(9) . . . yes N(61) N(62) B(2) 116.3(9) . . . yes C(63) N(62) B(2) 132(1) . . . yes N(11) C(11) C(12) 109(1) . . . yes N(11) C(11) C(14) 121(1) . . . yes C(12) C(11) C(14) 128(1) . . . yes C(11) C(12) C(13) 106(1) . . . yes N(12) C(13) C(12) 108(1) . . . yes N(12) C(13) C(17) 121(1) . . . yes C(12) C(13) C(17) 130(1) . . . yes C(11) C(14) C(15) 116(1) . . . yes C(11) C(14) C(16) 118(1) . . . yes C(15) C(14) C(16) 122(1) . . . yes C(13) C(17) C(18) 108(1) . . . yes C(13) C(17) C(19) 111.0(10) . . . yes C(18) C(17) C(19) 110(1) . . . yes N(21) C(21) C(22) 109(1) . . . yes N(21) C(21) C(24) 123(1) . . . yes C(22) C(21) C(24) 126(1) . . . yes C(21) C(22) C(23) 105(1) . . . yes N(22) C(23) C(22) 109.7(9) . . . yes N(22) C(23) C(27) 122(1) . . . yes C(22) C(23) C(27) 128(1) . . . yes C(21) C(24) C(25) 117(1) . . . yes C(21) C(24) C(26) 112(1) . . . yes C(25) C(24) C(26) 113(1) . . . yes C(23) C(27) C(28) 110(1) . . . yes C(23) C(27) C(29) 107(1) . . . yes C(28) C(27) C(29) 111(1) . . . yes N(31) C(31) C(32) 110.0(8) . . . yes N(31) C(31) C(34) 121.5(9) . . . yes C(32) C(31) C(34) 128.6(9) . . . yes C(31) C(32) C(33) 106.9(9) . . . yes N(32) C(33) C(32) 107.8(9) . . . yes N(32) C(33) C(37) 124.1(9) . . . yes C(32) C(33) C(37) 127(1) . . . yes C(31) C(34) C(35) 108.5(9) . . . yes C(31) C(34) C(36) 112.3(10) . . . yes C(35) C(34) C(36) 109.6(10) . . . yes C(33) C(37) C(38) 111(1) . . . yes C(33) C(37) C(39) 112(1) . . . yes C(38) C(37) C(39) 115(1) . . . yes N(41) C(41) C(42) 105.7(10) . . . yes N(41) C(41) C(44) 125(1) . . . yes C(42) C(41) C(44) 128(1) . . . yes C(41) C(42) C(43) 108(1) . . . yes N(42) C(43) C(42) 107(1) . . . yes N(42) C(43) C(45) 124(1) . . . yes C(42) C(43) C(45) 127(1) . . . yes N(51) C(51) C(52) 108.5(10) . . . yes N(51) C(51) C(54) 124(1) . . . yes C(52) C(51) C(54) 127(1) . . . yes C(51) C(52) C(53) 107(1) . . . yes N(52) C(53) C(52) 109(1) . . . yes N(52) C(53) C(55) 122(1) . . . yes C(52) C(53) C(55) 127(1) . . . yes N(61) C(61) C(62) 112(1) . . . yes N(61) C(61) C(64) 118(1) . . . yes C(62) C(61) C(64) 128(1) . . . yes C(61) C(62) C(63) 105(1) . . . yes N(62) C(63) C(62) 106(1) . . . yes N(62) C(63) C(65) 125(1) . . . yes C(62) C(63) C(65) 128(1) . . . yes N(71) C(71) C(72) 168(5) . . . yes N(72) C(73) C(74) 174(2) . . . yes N(12) B(1) N(22) 107.9(10) . . . yes N(12) B(1) N(32) 109.1(9) . . . yes N(22) B(1) N(32) 111.8(9) . . . yes N(42) B(2) N(52) 112(1) . . . yes N(42) B(2) N(62) 110(1) . . . yes N(52) B(2) N(62) 110.6(9) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . yes ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(15) 3.59(2) . 1_545 ? N(11) C(74) 3.44(2) . 2_556 ? N(12) C(74) 3.57(2) . 2_556 ? N(21) C(15) 3.39(2) . 1_545 ? N(31) C(15) 3.47(2) . 1_545 ? N(31) C(74) 3.53(2) . 2_556 ? N(61) C(55) 3.42(2) . 3_567 ? N(62) C(55) 3.51(2) . 3_567 ? C(15) C(21) 3.53(2) . 1_565 ? C(55) C(61) 3.41(2) . 3_567 ? C(55) C(62) 3.52(2) . 3_567 ? C(55) C(63) 3.56(2) . 3_567 ? Pd(1) N(42) 2.949(8) . . ? Pd(1) N(52) 2.960(9) . . ? Pd(1) Ni(1) 3.123(1) . . ? Ni(1) N(32) 2.942(8) . . ? Ni(1) N(12) 2.958(9) . . ? Ni(1) N(22) 2.960(8) . . ? O(1) O(2) 2.58(1) . . ? O(1) N(51) 2.94(1) . . ? O(1) N(21) 3.05(1) . . ? O(1) N(31) 3.16(1) . . ? O(2) N(11) 3.05(1) . . ? O(2) N(41) 3.06(1) . . ? O(2) N(31) 3.14(1) . . ? N(11) N(21) 2.85(1) . . ? N(11) N(31) 2.95(1) . . ? N(11) N(22) 2.98(1) . . ? N(11) N(32) 3.07(1) . . ? N(12) N(32) 2.52(1) . . ? N(12) N(21) 3.03(1) . . ? N(12) N(31) 3.06(1) . . ? N(21) N(31) 2.92(1) . . ? N(21) N(32) 3.10(1) . . ? N(22) N(32) 2.55(1) . . ? N(22) N(31) 3.03(1) . . ? N(41) N(51) 2.84(1) . . ? N(41) N(52) 3.06(1) . . ? N(41) N(61) 3.43(1) . . ? N(42) N(52) 2.51(1) . . ? N(42) N(61) 2.86(1) . . ? N(42) N(51) 2.96(1) . . ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_compound_5a(Co) _database_code_CSD 213634 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C62 H106 B2 Co N16 O3 Pd ' _chemical_formula_moiety 'C62 H106 B2 Co N16 O3 Pd ' _chemical_formula_weight 1310.58 _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 15.840(1) _cell_length_b 23.393(2) _cell_length_c 20.111(1) _cell_angle_alpha 90 _cell_angle_beta 104.604(3) _cell_angle_gamma 90 _cell_volume 7211.6(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 35401 _cell_measurement_theta_min 0.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_T_max 0.948 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 38840 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15107 _reflns_number_gt 6077 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2218 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6077 _refine_ls_number_parameters 733 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0350 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.59 _refine_diff_density_min -1.14 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 0.18129(3) 0.20090(3) 0.03708(3) 0.0471(2) Uani 1.00 d . . . Co(1) Co 0.32688(6) 0.17107(4) 0.16811(5) 0.0466(3) Uani 1.00 d . . . O(1) O 0.2882(3) 0.2359(2) 0.1006(2) 0.053(1) Uani 1.00 d . . . O(2) O 0.2249(3) 0.1338(2) 0.0986(3) 0.060(1) Uani 1.00 d . . . O(3) O 0.2011(8) 0.3527(7) 0.1007(7) 0.259(7) Uani 1.00 d . . . N(11) N 0.3173(4) 0.1095(3) 0.2410(3) 0.048(1) Uani 1.00 d . . . N(12) N 0.3942(3) 0.0901(2) 0.2842(3) 0.042(1) Uani 1.00 d . . . N(21) N 0.4095(4) 0.2155(3) 0.2510(3) 0.047(1) Uani 1.00 d . . . N(22) N 0.4753(4) 0.1831(2) 0.2936(3) 0.046(1) Uani 1.00 d . . . N(31) N 0.4348(4) 0.1285(3) 0.1528(3) 0.051(2) Uani 1.00 d . . . N(32) N 0.4972(3) 0.1101(3) 0.2089(3) 0.045(1) Uani 1.00 d . . . N(41) N 0.0788(3) 0.1600(3) -0.0209(3) 0.048(1) Uani 1.00 d . . . N(42) N 0.0007(4) 0.1882(2) -0.0454(3) 0.047(1) Uani 1.00 d . . . N(51) N 0.1444(3) 0.2704(3) -0.0220(3) 0.051(2) Uani 1.00 d . . . N(52) N 0.0598(3) 0.2879(3) -0.0380(3) 0.050(2) Uani 1.00 d . . . N(61) N 0.0570(4) 0.2879(3) 0.1002(3) 0.065(2) Uani 1.00 d . . . N(62) N -0.0034(4) 0.2532(3) 0.0580(3) 0.053(2) Uani 1.00 d . . . N(71) N 0.6402(8) 0.0825(6) 0.9503(7) 0.16383(6) Uiso 1.00 d . . . N(72) N 0.8636(7) 0.0177(6) 0.5968(6) 0.14166(5) Uiso 1.00 d . . . N(73) N 0.6594(7) 0.1617(5) 0.6620(6) 0.13705(5) Uiso 1.00 d . . . C(11) C 0.2533(4) 0.0774(4) 0.2569(4) 0.052(2) Uani 1.00 d . . . C(12) C 0.2877(5) 0.0384(3) 0.3075(4) 0.058(2) Uani 1.00 d . . . C(13) C 0.3760(5) 0.0469(3) 0.3239(4) 0.048(2) Uani 1.00 d . . . C(14) C 0.1595(5) 0.0897(4) 0.2256(4) 0.068(2) Uani 1.00 d . . . C(15) C 0.1277(6) 0.1433(4) 0.2133(5) 0.076(3) Uani 1.00 d . . . C(16) C 0.1032(6) 0.0379(4) 0.2161(5) 0.097(3) Uani 1.00 d . . . C(17) C 0.4430(5) 0.0157(4) 0.3772(4) 0.061(2) Uani 1.00 d . . . C(18) C 0.4899(6) -0.0271(4) 0.3437(5) 0.083(3) Uani 1.00 d . . . C(19) C 0.4034(6) -0.0170(4) 0.4273(4) 0.085(3) Uani 1.00 d . . . C(21) C 0.4218(5) 0.2705(4) 0.2740(4) 0.056(2) Uani 1.00 d . . . C(22) C 0.4954(5) 0.2730(4) 0.3305(4) 0.060(2) Uani 1.00 d . . . C(23) C 0.5283(4) 0.2179(3) 0.3409(4) 0.049(2) Uani 1.00 d . . . C(24) C 0.3612(6) 0.3173(3) 0.2421(4) 0.060(2) Uani 1.00 d . . . C(25) C 0.3352(6) 0.3541(4) 0.2954(5) 0.087(3) Uani 1.00 d . . . C(26) C 0.4029(6) 0.3544(5) 0.1969(5) 0.102(3) Uani 1.00 d . . . C(27) C 0.6024(4) 0.1958(4) 0.3961(4) 0.058(2) Uani 1.00 d . . . C(28) C 0.6758(6) 0.2394(4) 0.4141(6) 0.108(4) Uani 1.00 d . . . C(29) C 0.5739(5) 0.1786(4) 0.4602(4) 0.086(3) Uani 1.00 d . . . C(31) C 0.4626(5) 0.1157(3) 0.0975(4) 0.058(2) Uani 1.00 d . . . C(32) C 0.5440(5) 0.0896(3) 0.1176(4) 0.062(2) Uani 1.00 d . . . C(33) C 0.5663(5) 0.0869(3) 0.1892(4) 0.052(2) Uani 1.00 d . . . C(34) C 0.4109(6) 0.1289(4) 0.0258(4) 0.068(2) Uani 1.00 d . . . C(35) C 0.3979(7) 0.0759(4) -0.0207(5) 0.101(3) Uani 1.00 d . . . C(36) C 0.4527(6) 0.1775(4) -0.0040(4) 0.082(3) Uani 1.00 d . . . C(37) C 0.6466(5) 0.0660(4) 0.2379(4) 0.063(2) Uani 1.00 d . . . C(38) C 0.6892(8) 0.0186(5) 0.2086(6) 0.141(5) Uani 1.00 d . . . C(39) C 0.7088(7) 0.1156(5) 0.2615(6) 0.120(4) Uani 1.00 d . . . C(41) C 0.0723(4) 0.1092(3) -0.0525(4) 0.047(2) Uani 1.00 d . . . C(42) C -0.0126(5) 0.1040(3) -0.0971(4) 0.055(2) Uani 1.00 d . . . C(43) C -0.0536(4) 0.1546(3) -0.0920(3) 0.045(2) Uani 1.00 d . . . C(44) C 0.1451(5) 0.0654(3) -0.0375(4) 0.053(2) Uani 1.00 d . . . C(45) C 0.1241(6) 0.0175(4) 0.0085(5) 0.087(3) Uani 1.00 d . . . C(46) C 0.1592(6) 0.0390(5) -0.1028(5) 0.101(3) Uani 1.00 d . . . C(47) C -0.1433(4) 0.1727(3) -0.1308(4) 0.054(2) Uani 1.00 d . . . C(48) C -0.1424(5) 0.2116(4) -0.1918(4) 0.073(3) Uani 1.00 d . . . C(49) C -0.2014(5) 0.1209(4) -0.1550(5) 0.084(3) Uani 1.00 d . . . C(51) C 0.1894(4) 0.3084(3) -0.0498(3) 0.048(2) Uani 1.00 d . . . C(52) C 0.1344(5) 0.3508(3) -0.0838(4) 0.061(2) Uani 1.00 d . . . C(53) C 0.0531(5) 0.3367(4) -0.0756(4) 0.062(2) Uani 1.00 d . . . C(54) C 0.2864(4) 0.3027(4) -0.0433(4) 0.056(2) Uani 1.00 d . . . C(55) C 0.3360(6) 0.3526(4) -0.0048(5) 0.090(3) Uani 1.00 d . . . C(56) C 0.3040(5) 0.2972(4) -0.1129(4) 0.068(2) Uani 1.00 d . . . C(57) C -0.0294(6) 0.3689(4) -0.0998(7) 0.104(4) Uani 1.00 d . . . C(58) C -0.042(1) 0.4084(7) -0.0459(9) 0.23(1) Uani 1.00 d . . . C(59) C -0.0337(6) 0.4017(5) -0.1643(7) 0.135(5) Uani 1.00 d . . . C(61) C 0.0377(5) 0.2861(4) 0.1621(4) 0.069(2) Uani 1.00 d . . . C(62) C -0.0345(5) 0.2523(4) 0.1596(4) 0.060(2) Uani 1.00 d . . . C(63) C -0.0603(4) 0.2317(3) 0.0930(4) 0.050(2) Uani 1.00 d . . . C(64) C 0.0932(6) 0.3225(5) 0.2197(5) 0.094(4) Uani 1.00 d . . . C(65) C 0.0527(9) 0.3839(5) 0.2162(5) 0.129(5) Uani 1.00 d . . . C(66) C 0.0991(6) 0.2952(5) 0.2915(5) 0.095(3) Uani 1.00 d . . . C(67) C -0.1342(5) 0.1922(4) 0.0619(4) 0.058(2) Uani 1.00 d . . . C(68) C -0.2114(5) 0.2021(4) 0.0929(4) 0.078(3) Uani 1.00 d . . . C(69) C -0.1052(6) 0.1291(4) 0.0699(5) 0.081(3) Uani 1.00 d . . . C(71) C 0.6302(7) 0.0530(5) 0.9026(6) 0.10585(5) Uiso 1.00 d . . . C(72) C 0.6324(7) 0.0106(5) 0.8526(6) 0.10879(5) Uiso 1.00 d . . . C(73) C 0.8461(8) 0.0648(6) 0.5921(6) 0.11701(5) Uiso 1.00 d . . . C(74) C 0.8244(9) 0.1247(7) 0.5820(7) 0.14153(6) Uiso 1.00 d . . . C(75) C 0.6249(7) 0.2029(5) 0.6663(5) 0.08927(4) Uiso 1.00 d . . . C(76) C 0.5789(7) 0.2545(5) 0.6698(6) 0.10695(4) Uiso 1.00 d . . . N(74) N 0.145(2) 0.438(1) 0.062(1) 0.1930(1) Uiso 0.50 d P . . N(75) N 0.276(2) 0.576(2) 0.070(2) 0.2103(2) Uiso 0.50 d P . . C(77) C 0.230(1) 0.4745(7) 0.0835(8) 0.15281(7) Uiso 1.00 d . . . C(78) C 0.274(1) 0.5190(9) 0.0785(9) 0.17974(8) Uiso 1.00 d . . . B(1) B 0.4813(5) 0.1186(4) 0.2814(4) 0.047(2) Uani 1.00 d . . . B(2) B -0.0117(6) 0.2508(4) -0.0217(4) 0.054(2) Uani 1.00 d . . . H(1) H 0.5295 0.1019 0.3163 0.0584 Uiso 1.00 calc . . . H(2) H -0.0699 0.2653 -0.0457 0.0645 Uiso 1.00 calc . . . H(12) H 0.2551 0.0113 0.3267 0.0723 Uiso 1.00 calc . . . H(15A) H 0.1650 0.1745 0.2244 0.0927 Uiso 1.00 calc . . . H(15B) H 0.0686 0.1490 0.1936 0.0927 Uiso 1.00 calc . . . H(16A) H 0.0439 0.0486 0.1955 0.0971 Uiso 1.00 calc . . . H(16B) H 0.1070 0.0204 0.2599 0.0971 Uiso 1.00 calc . . . H(16C) H 0.1226 0.0113 0.1867 0.0971 Uiso 1.00 calc . . . H(17) H 0.4874 0.0427 0.4016 0.0781 Uiso 1.00 calc . . . H(18A) H 0.4488 -0.0542 0.3182 0.0835 Uiso 1.00 calc . . . H(18B) H 0.5330 -0.0467 0.3783 0.0835 Uiso 1.00 calc . . . H(18C) H 0.5179 -0.0076 0.3130 0.0835 Uiso 1.00 calc . . . H(19A) H 0.3754 0.0093 0.4515 0.0847 Uiso 1.00 calc . . . H(19B) H 0.4486 -0.0371 0.4596 0.0847 Uiso 1.00 calc . . . H(19C) H 0.3613 -0.0439 0.4025 0.0847 Uiso 1.00 calc . . . H(22) H 0.5191 0.3072 0.3565 0.0704 Uiso 1.00 calc . . . H(24) H 0.3084 0.3005 0.2126 0.0739 Uiso 1.00 calc . . . H(25A) H 0.3850 0.3752 0.3207 0.0875 Uiso 1.00 calc . . . H(25B) H 0.3136 0.3303 0.3263 0.0875 Uiso 1.00 calc . . . H(25C) H 0.2903 0.3803 0.2730 0.0875 Uiso 1.00 calc . . . H(26A) H 0.4525 0.3739 0.2251 0.1020 Uiso 1.00 calc . . . H(26B) H 0.3612 0.3820 0.1731 0.1020 Uiso 1.00 calc . . . H(26C) H 0.4213 0.3308 0.1641 0.1020 Uiso 1.00 calc . . . H(27) H 0.6251 0.1617 0.3791 0.0727 Uiso 1.00 calc . . . H(28A) H 0.7254 0.2227 0.4457 0.1076 Uiso 1.00 calc . . . H(28B) H 0.6566 0.2722 0.4349 0.1076 Uiso 1.00 calc . . . H(28C) H 0.6917 0.2508 0.3730 0.1076 Uiso 1.00 calc . . . H(29A) H 0.5616 0.2122 0.4834 0.0859 Uiso 1.00 calc . . . H(29B) H 0.6198 0.1573 0.4903 0.0859 Uiso 1.00 calc . . . H(29C) H 0.5224 0.1553 0.4472 0.0859 Uiso 1.00 calc . . . H(32) H 0.5802 0.0758 0.0883 0.0761 Uiso 1.00 calc . . . H(34) H 0.3520 0.1414 0.0278 0.0818 Uiso 1.00 calc . . . H(35A) H 0.3740 0.0454 0.0007 0.1012 Uiso 1.00 calc . . . H(35B) H 0.4531 0.0643 -0.0278 0.1012 Uiso 1.00 calc . . . H(35C) H 0.3586 0.0850 -0.0641 0.1012 Uiso 1.00 calc . . . H(36A) H 0.5087 0.1656 -0.0092 0.0821 Uiso 1.00 calc . . . H(36B) H 0.4597 0.2098 0.0262 0.0821 Uiso 1.00 calc . . . H(36C) H 0.4160 0.1879 -0.0481 0.0821 Uiso 1.00 calc . . . H(37) H 0.6303 0.0505 0.2787 0.0789 Uiso 1.00 calc . . . H(38A) H 0.6479 -0.0116 0.1933 0.1414 Uiso 1.00 calc . . . H(38B) H 0.7379 0.0042 0.2433 0.1414 Uiso 1.00 calc . . . H(38C) H 0.7093 0.0327 0.1705 0.1414 Uiso 1.00 calc . . . H(39A) H 0.7577 0.1028 0.2971 0.1202 Uiso 1.00 calc . . . H(39B) H 0.6790 0.1456 0.2789 0.1202 Uiso 1.00 calc . . . H(39C) H 0.7290 0.1297 0.2234 0.1202 Uiso 1.00 calc . . . H(42) H -0.0368 0.0714 -0.1254 0.0646 Uiso 1.00 calc . . . H(44) H 0.1993 0.0849 -0.0125 0.0677 Uiso 1.00 calc . . . H(45A) H 0.1096 0.0341 0.0479 0.0865 Uiso 1.00 calc . . . H(45B) H 0.1741 -0.0069 0.0234 0.0865 Uiso 1.00 calc . . . H(45C) H 0.0756 -0.0045 -0.0171 0.0865 Uiso 1.00 calc . . . H(46A) H 0.1066 0.0203 -0.1273 0.1014 Uiso 1.00 calc . . . H(46B) H 0.2057 0.0116 -0.0912 0.1014 Uiso 1.00 calc . . . H(46C) H 0.1741 0.0684 -0.1311 0.1014 Uiso 1.00 calc . . . H(47) H -0.1692 0.1942 -0.1002 0.0674 Uiso 1.00 calc . . . H(48A) H -0.1094 0.2454 -0.1757 0.0732 Uiso 1.00 calc . . . H(48B) H -0.2012 0.2220 -0.2148 0.0732 Uiso 1.00 calc . . . H(48C) H -0.1162 0.1917 -0.2233 0.0732 Uiso 1.00 calc . . . H(49A) H -0.2594 0.1335 -0.1767 0.0842 Uiso 1.00 calc . . . H(49B) H -0.2025 0.0973 -0.1162 0.0842 Uiso 1.00 calc . . . H(49C) H -0.1786 0.0994 -0.1872 0.0842 Uiso 1.00 calc . . . H(52) H 0.1508 0.3836 -0.1077 0.0710 Uiso 1.00 calc . . . H(54) H 0.3067 0.2680 -0.0172 0.0653 Uiso 1.00 calc . . . H(55A) H 0.3975 0.3463 0.0019 0.0904 Uiso 1.00 calc . . . H(55B) H 0.3227 0.3562 0.0390 0.0904 Uiso 1.00 calc . . . H(55C) H 0.3194 0.3870 -0.0309 0.0904 Uiso 1.00 calc . . . H(56A) H 0.2752 0.2637 -0.1354 0.0680 Uiso 1.00 calc . . . H(56B) H 0.3657 0.2939 -0.1080 0.0680 Uiso 1.00 calc . . . H(56C) H 0.2822 0.3304 -0.1399 0.0680 Uiso 1.00 calc . . . H(57) H -0.0785 0.3428 -0.1117 0.1175 Uiso 1.00 calc . . . H(58A) H -0.0027 0.4402 -0.0425 0.2273 Uiso 1.00 calc . . . H(58B) H -0.0302 0.3887 -0.0027 0.2273 Uiso 1.00 calc . . . H(58C) H -0.1010 0.4220 -0.0575 0.2273 Uiso 1.00 calc . . . H(59A) H 0.0038 0.4344 -0.1541 0.1348 Uiso 1.00 calc . . . H(59B) H -0.0926 0.4140 -0.1837 0.1348 Uiso 1.00 calc . . . H(59C) H -0.0151 0.3777 -0.1966 0.1348 Uiso 1.00 calc . . . H(62) H -0.0619 0.2459 0.1975 0.0693 Uiso 1.00 calc . . . H(64) H 0.1519 0.3270 0.2127 0.1163 Uiso 1.00 calc . . . H(65A) H 0.0897 0.4079 0.2501 0.1292 Uiso 1.00 calc . . . H(65B) H -0.0040 0.3817 0.2250 0.1292 Uiso 1.00 calc . . . H(65C) H 0.0476 0.3998 0.1714 0.1292 Uiso 1.00 calc . . . H(66A) H 0.0419 0.2933 0.2994 0.0950 Uiso 1.00 calc . . . H(66B) H 0.1362 0.3181 0.3266 0.0950 Uiso 1.00 calc . . . H(66C) H 0.1228 0.2573 0.2927 0.0950 Uiso 1.00 calc . . . H(67) H -0.1547 0.2004 0.0123 0.0721 Uiso 1.00 calc . . . H(68A) H -0.2261 0.2420 0.0903 0.0783 Uiso 1.00 calc . . . H(68B) H -0.1961 0.1902 0.1401 0.0783 Uiso 1.00 calc . . . H(68C) H -0.2605 0.1803 0.0679 0.0783 Uiso 1.00 calc . . . H(69A) H -0.1493 0.1056 0.0411 0.0807 Uiso 1.00 calc . . . H(69B) H -0.0967 0.1176 0.1169 0.0807 Uiso 1.00 calc . . . H(69C) H -0.0514 0.1248 0.0565 0.0807 Uiso 1.00 calc . . . H(72A) H 0.6577 -0.0237 0.8750 0.1089 Uiso 1.00 calc . . . H(72B) H 0.6677 0.0243 0.8231 0.1089 Uiso 1.00 calc . . . H(72C) H 0.5746 0.0033 0.8257 0.1089 Uiso 1.00 calc . . . H(74A) H 0.8756 0.1472 0.6008 0.1412 Uiso 1.00 calc . . . H(74B) H 0.7801 0.1341 0.6052 0.1412 Uiso 1.00 calc . . . H(74C) H 0.8036 0.1325 0.5340 0.1412 Uiso 1.00 calc . . . H(76A) H 0.6121 0.2860 0.6604 0.1073 Uiso 1.00 calc . . . H(76B) H 0.5706 0.2581 0.7156 0.1073 Uiso 1.00 calc . . . H(76C) H 0.5234 0.2530 0.6373 0.1073 Uiso 1.00 calc . . . 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) 0.0450(3) 0.0568(4) 0.0404(3) -0.0035(3) 0.0124(2) 0.0004(3) Co(1) 0.0543(6) 0.0524(6) 0.0318(5) 0.0009(5) 0.0084(4) 0.0007(5) O(1) 0.044(3) 0.065(3) 0.047(3) -0.002(2) 0.007(2) 0.005(3) O(2) 0.056(3) 0.065(4) 0.056(3) -0.006(3) 0.012(2) 0.005(3) O(3) 0.21(1) 0.37(2) 0.20(1) -0.11(1) 0.057(10) -0.07(1) N(11) 0.052(4) 0.055(4) 0.033(3) 0.009(3) 0.005(3) 0.004(3) N(12) 0.052(3) 0.036(3) 0.039(3) 0.001(3) 0.015(3) 0.005(3) N(21) 0.057(4) 0.046(4) 0.040(3) -0.003(3) 0.017(3) 0.003(3) N(22) 0.054(4) 0.042(4) 0.043(3) -0.005(3) 0.014(3) -0.006(3) N(31) 0.060(4) 0.064(4) 0.030(3) -0.001(3) 0.016(3) -0.004(3) N(32) 0.037(3) 0.064(4) 0.035(3) -0.001(3) 0.010(2) -0.003(3) N(41) 0.039(3) 0.062(4) 0.046(3) 0.002(3) 0.014(3) 0.005(3) N(42) 0.048(3) 0.050(4) 0.047(3) 0.004(3) 0.018(3) 0.000(3) N(51) 0.037(3) 0.078(5) 0.039(3) -0.007(3) 0.014(3) 0.003(3) N(52) 0.038(3) 0.067(5) 0.050(3) 0.003(3) 0.023(3) 0.004(3) N(61) 0.059(4) 0.083(5) 0.058(4) -0.019(3) 0.026(3) -0.030(4) N(62) 0.045(3) 0.075(5) 0.045(3) 0.000(3) 0.024(3) -0.008(3) C(11) 0.042(4) 0.070(5) 0.045(4) -0.007(4) 0.014(3) -0.004(4) C(12) 0.056(5) 0.052(5) 0.069(5) -0.003(4) 0.019(4) -0.001(4) C(13) 0.060(5) 0.042(4) 0.044(4) 0.007(3) 0.017(3) 0.001(3) C(14) 0.068(6) 0.079(7) 0.057(5) -0.004(5) 0.019(4) -0.004(5) C(15) 0.068(6) 0.072(6) 0.090(7) 0.020(5) 0.022(5) 0.013(5) C(16) 0.069(6) 0.101(9) 0.112(8) -0.006(6) 0.007(6) -0.012(7) C(17) 0.071(5) 0.062(6) 0.053(5) 0.011(4) 0.021(4) 0.017(4) C(18) 0.068(6) 0.097(8) 0.082(7) 0.012(5) 0.014(5) 0.010(6) C(19) 0.105(7) 0.085(7) 0.067(6) 0.001(6) 0.026(5) 0.025(5) C(21) 0.070(5) 0.059(5) 0.041(4) -0.008(4) 0.015(4) -0.003(4) C(22) 0.073(5) 0.067(6) 0.041(4) -0.012(4) 0.018(4) -0.009(4) C(23) 0.046(4) 0.064(6) 0.039(4) -0.007(3) 0.013(3) -0.012(4) C(24) 0.090(6) 0.054(5) 0.036(4) -0.004(4) 0.017(4) -0.002(4) C(25) 0.099(7) 0.089(7) 0.068(6) 0.012(6) 0.009(5) 0.000(5) C(26) 0.103(8) 0.097(8) 0.100(8) -0.007(6) 0.014(6) 0.032(7) C(27) 0.040(4) 0.075(6) 0.055(4) -0.012(4) 0.005(3) -0.006(4) C(28) 0.080(7) 0.101(8) 0.117(9) -0.030(6) -0.022(6) 0.012(7) C(29) 0.058(5) 0.133(9) 0.060(6) 0.014(5) 0.001(4) 0.009(6) C(31) 0.062(5) 0.058(5) 0.055(5) -0.003(4) 0.013(4) 0.003(4) C(32) 0.068(5) 0.059(5) 0.066(5) -0.003(4) 0.032(4) -0.009(4) C(33) 0.049(4) 0.060(5) 0.052(5) 0.002(4) 0.022(4) -0.001(4) C(34) 0.085(6) 0.091(7) 0.038(4) -0.004(5) 0.034(4) -0.009(4) C(35) 0.152(10) 0.101(8) 0.054(6) -0.013(7) 0.034(6) -0.013(6) C(36) 0.096(7) 0.100(8) 0.052(5) 0.012(6) 0.022(5) 0.018(5) C(37) 0.054(5) 0.082(6) 0.058(5) 0.000(4) 0.023(4) -0.001(5) C(38) 0.14(1) 0.13(1) 0.13(1) 0.074(9) -0.011(8) -0.032(9) C(39) 0.084(8) 0.16(1) 0.119(10) -0.002(7) 0.023(7) 0.005(9) C(41) 0.044(4) 0.058(5) 0.041(4) -0.004(3) 0.018(3) -0.005(4) C(42) 0.055(5) 0.062(5) 0.044(4) -0.009(4) 0.006(3) -0.010(4) C(43) 0.036(4) 0.065(5) 0.035(4) -0.005(3) 0.011(3) 0.001(3) C(44) 0.056(4) 0.061(5) 0.044(4) 0.004(4) 0.014(3) -0.003(4) C(45) 0.086(7) 0.081(7) 0.093(7) 0.007(5) 0.022(5) 0.021(6) C(46) 0.098(8) 0.125(9) 0.078(7) 0.031(7) 0.015(6) -0.016(7) C(47) 0.044(4) 0.067(5) 0.049(4) 0.000(4) 0.009(3) 0.003(4) C(48) 0.055(5) 0.094(7) 0.066(5) 0.005(4) 0.008(4) 0.020(5) C(49) 0.053(5) 0.109(8) 0.080(6) -0.009(5) -0.002(4) 0.011(6) C(51) 0.043(4) 0.066(5) 0.038(4) -0.009(4) 0.018(3) 0.001(4) C(52) 0.056(5) 0.050(5) 0.085(6) 0.010(4) 0.035(4) 0.013(4) C(53) 0.059(5) 0.064(6) 0.072(6) 0.018(4) 0.031(4) 0.015(4) C(54) 0.047(4) 0.073(6) 0.050(4) -0.001(4) 0.019(3) 0.019(4) C(55) 0.073(6) 0.119(9) 0.079(7) -0.026(6) 0.020(5) -0.002(6) C(56) 0.058(5) 0.100(7) 0.053(5) 0.011(5) 0.026(4) 0.010(5) C(57) 0.060(6) 0.083(7) 0.19(1) 0.026(5) 0.064(7) 0.065(8) C(58) 0.26(2) 0.21(2) 0.28(2) 0.17(2) 0.18(2) 0.09(2) C(59) 0.066(7) 0.12(1) 0.21(1) 0.016(6) 0.024(8) 0.08(1) C(61) 0.065(5) 0.090(7) 0.059(5) -0.002(5) 0.026(4) -0.025(5) C(62) 0.056(5) 0.081(6) 0.049(5) -0.011(4) 0.024(4) -0.015(4) C(63) 0.042(4) 0.061(5) 0.051(4) 0.003(3) 0.014(3) -0.008(4) C(64) 0.073(6) 0.14(1) 0.072(7) -0.024(6) 0.032(5) -0.045(7) C(65) 0.20(1) 0.107(10) 0.064(7) -0.022(9) 0.004(8) -0.019(7) C(66) 0.071(6) 0.124(9) 0.076(7) 0.026(6) -0.007(5) -0.020(6) C(67) 0.060(5) 0.069(6) 0.046(4) -0.012(4) 0.017(4) 0.005(4) C(68) 0.072(5) 0.100(7) 0.071(6) -0.011(5) 0.033(5) 0.009(5) C(69) 0.090(7) 0.073(7) 0.079(6) -0.006(5) 0.021(5) -0.002(5) B(1) 0.039(4) 0.061(6) 0.039(4) 0.004(4) 0.005(3) 0.002(4) B(2) 0.049(5) 0.072(7) 0.041(5) -0.003(4) 0.011(4) 0.007(4) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution MITHRIL90 _computing_structure_refinement SHELXL97 _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) O(1) 2.020(4) . . yes Pd(1) O(2) 2.009(5) . . yes Pd(1) N(41) 1.989(5) . . yes Pd(1) N(51) 2.011(6) . . yes Co(1) O(1) 2.024(5) . . yes Co(1) O(2) 2.046(4) . . yes Co(1) N(11) 2.087(6) . . yes Co(1) N(21) 2.114(5) . . yes Co(1) N(31) 2.067(6) . . yes N(11) N(12) 1.382(7) . . yes N(11) C(11) 1.363(10) . . yes N(12) C(13) 1.365(9) . . yes N(12) B(1) 1.55(1) . . yes N(21) N(22) 1.395(7) . . yes N(21) C(21) 1.364(10) . . yes N(22) C(23) 1.368(8) . . yes N(22) B(1) 1.53(1) . . yes N(31) N(32) 1.370(7) . . yes N(31) C(31) 1.33(1) . . yes N(32) C(33) 1.367(10) . . yes N(32) B(1) 1.55(1) . . yes N(41) N(42) 1.378(7) . . yes N(41) C(41) 1.340(10) . . yes N(42) C(43) 1.352(8) . . yes N(42) B(2) 1.57(1) . . yes N(51) N(52) 1.362(7) . . yes N(51) C(51) 1.347(10) . . yes N(52) C(53) 1.36(1) . . yes N(52) B(2) 1.53(1) . . yes N(61) N(62) 1.372(8) . . yes N(61) C(61) 1.35(1) . . yes N(62) C(63) 1.37(1) . . yes N(62) B(2) 1.58(1) . . yes N(71) C(71) 1.16(2) . . yes N(72) C(73) 1.13(2) . . yes N(73) C(75) 1.12(2) . . yes C(11) C(12) 1.37(1) . . yes C(11) C(14) 1.49(1) . . yes C(12) C(13) 1.37(1) . . yes C(13) C(17) 1.495(10) . . yes C(14) C(15) 1.35(1) . . yes C(14) C(16) 1.49(1) . . yes C(17) C(18) 1.50(1) . . yes C(17) C(19) 1.52(1) . . yes C(21) C(22) 1.409(10) . . yes C(21) C(24) 1.49(1) . . yes C(22) C(23) 1.39(1) . . yes C(23) C(27) 1.490(9) . . yes C(24) C(25) 1.51(1) . . yes C(24) C(26) 1.52(1) . . yes C(27) C(28) 1.52(1) . . yes C(27) C(29) 1.52(1) . . yes C(31) C(32) 1.39(1) . . yes C(31) C(34) 1.50(1) . . yes C(32) C(33) 1.39(1) . . yes C(33) C(37) 1.480(10) . . yes C(34) C(35) 1.53(1) . . yes C(34) C(36) 1.51(1) . . yes C(37) C(38) 1.49(2) . . yes C(37) C(39) 1.52(1) . . yes C(41) C(42) 1.421(9) . . yes C(41) C(44) 1.51(1) . . yes C(42) C(43) 1.37(1) . . yes C(43) C(47) 1.500(9) . . yes C(44) C(45) 1.54(1) . . yes C(44) C(46) 1.52(1) . . yes C(47) C(48) 1.53(1) . . yes C(47) C(49) 1.52(1) . . yes C(51) C(52) 1.38(1) . . yes C(51) C(54) 1.515(10) . . yes C(52) C(53) 1.38(1) . . yes C(53) C(57) 1.48(1) . . yes C(54) C(55) 1.51(1) . . yes C(54) C(56) 1.50(1) . . yes C(57) C(58) 1.47(2) . . yes C(57) C(59) 1.49(2) . . yes C(61) C(62) 1.38(1) . . yes C(61) C(64) 1.53(1) . . yes C(62) C(63) 1.38(1) . . yes C(63) C(67) 1.499(10) . . yes C(64) C(65) 1.57(2) . . yes C(64) C(66) 1.56(1) . . yes C(67) C(68) 1.52(1) . . yes C(67) C(69) 1.54(1) . . yes C(71) C(72) 1.42(2) . . yes C(73) C(74) 1.45(2) . . yes C(75) C(76) 1.42(2) . . yes N(74) C(77) 1.56(3) . . yes N(75) C(78) 1.34(4) . . yes C(77) C(78) 1.27(3) . . 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 O(1) Pd(1) O(2) 79.9(2) . . . yes O(1) Pd(1) N(41) 174.9(2) . . . yes O(1) Pd(1) N(51) 96.8(2) . . . yes O(2) Pd(1) N(41) 95.1(2) . . . yes O(2) Pd(1) N(51) 176.6(2) . . . yes N(41) Pd(1) N(51) 88.3(2) . . . yes O(1) Co(1) O(2) 78.9(2) . . . yes O(1) Co(1) N(11) 157.6(2) . . . yes O(1) Co(1) N(21) 100.5(2) . . . yes O(1) Co(1) N(31) 112.5(2) . . . yes O(2) Co(1) N(11) 90.1(2) . . . yes O(2) Co(1) N(21) 166.7(2) . . . yes O(2) Co(1) N(31) 103.5(2) . . . yes N(11) Co(1) N(21) 85.7(2) . . . yes N(11) Co(1) N(31) 89.0(2) . . . yes N(21) Co(1) N(31) 89.1(2) . . . yes Pd(1) O(1) Co(1) 100.6(2) . . . yes Pd(1) O(2) Co(1) 100.2(2) . . . yes Co(1) N(11) N(12) 117.3(4) . . . yes Co(1) N(11) C(11) 137.3(4) . . . yes N(12) N(11) C(11) 105.1(5) . . . yes N(11) N(12) C(13) 109.2(5) . . . yes N(11) N(12) B(1) 119.2(5) . . . yes C(13) N(12) B(1) 131.6(5) . . . yes Co(1) N(21) N(22) 115.7(4) . . . yes Co(1) N(21) C(21) 137.6(4) . . . yes N(22) N(21) C(21) 106.5(5) . . . yes N(21) N(22) C(23) 109.6(5) . . . yes N(21) N(22) B(1) 120.2(5) . . . yes C(23) N(22) B(1) 130.1(5) . . . yes Co(1) N(31) N(32) 118.7(4) . . . yes Co(1) N(31) C(31) 134.0(4) . . . yes N(32) N(31) C(31) 107.2(6) . . . yes N(31) N(32) C(33) 110.5(6) . . . yes N(31) N(32) B(1) 118.6(5) . . . yes C(33) N(32) B(1) 130.9(5) . . . yes Pd(1) N(41) N(42) 120.4(4) . . . yes Pd(1) N(41) C(41) 131.2(4) . . . yes N(42) N(41) C(41) 107.5(5) . . . yes N(41) N(42) C(43) 109.0(5) . . . yes N(41) N(42) B(2) 120.6(5) . . . yes C(43) N(42) B(2) 130.3(6) . . . yes Pd(1) N(51) N(52) 120.3(5) . . . yes Pd(1) N(51) C(51) 132.4(4) . . . yes N(52) N(51) C(51) 107.2(6) . . . yes N(51) N(52) C(53) 108.6(6) . . . yes N(51) N(52) B(2) 121.2(6) . . . yes C(53) N(52) B(2) 129.8(6) . . . yes N(62) N(61) C(61) 105.5(6) . . . yes N(61) N(62) C(63) 110.2(6) . . . yes N(61) N(62) B(2) 121.1(6) . . . yes C(63) N(62) B(2) 127.8(6) . . . yes N(11) C(11) C(12) 111.2(6) . . . yes N(11) C(11) C(14) 121.0(7) . . . yes C(12) C(11) C(14) 127.5(7) . . . yes C(11) C(12) C(13) 105.9(7) . . . yes N(12) C(13) C(12) 108.7(6) . . . yes N(12) C(13) C(17) 124.4(7) . . . yes C(12) C(13) C(17) 126.9(7) . . . yes C(11) C(14) C(15) 122.9(8) . . . yes C(11) C(14) C(16) 113.5(7) . . . yes C(15) C(14) C(16) 123.3(8) . . . yes C(13) C(17) C(18) 110.2(6) . . . yes C(13) C(17) C(19) 112.5(7) . . . yes C(18) C(17) C(19) 107.2(7) . . . yes N(21) C(21) C(22) 109.4(7) . . . yes N(21) C(21) C(24) 121.6(6) . . . yes C(22) C(21) C(24) 128.9(7) . . . yes C(21) C(22) C(23) 106.6(7) . . . yes N(22) C(23) C(22) 107.9(5) . . . yes N(22) C(23) C(27) 122.8(7) . . . yes C(22) C(23) C(27) 129.1(7) . . . yes C(21) C(24) C(25) 112.0(6) . . . yes C(21) C(24) C(26) 110.3(8) . . . yes C(25) C(24) C(26) 109.5(7) . . . yes C(23) C(27) C(28) 110.8(7) . . . yes C(23) C(27) C(29) 112.1(6) . . . yes C(28) C(27) C(29) 110.5(7) . . . yes N(31) C(31) C(32) 109.5(7) . . . yes N(31) C(31) C(34) 122.8(7) . . . yes C(32) C(31) C(34) 127.7(8) . . . yes C(31) C(32) C(33) 107.2(8) . . . yes N(32) C(33) C(32) 105.6(6) . . . yes N(32) C(33) C(37) 123.9(7) . . . yes C(32) C(33) C(37) 130.5(8) . . . yes C(31) C(34) C(35) 112.1(7) . . . yes C(31) C(34) C(36) 110.4(7) . . . yes C(35) C(34) C(36) 111.7(8) . . . yes C(33) C(37) C(38) 112.5(7) . . . yes C(33) C(37) C(39) 109.6(7) . . . yes C(38) C(37) C(39) 111.6(8) . . . yes N(41) C(41) C(42) 108.8(6) . . . yes N(41) C(41) C(44) 122.8(5) . . . yes C(42) C(41) C(44) 128.4(7) . . . yes C(41) C(42) C(43) 105.7(6) . . . yes N(42) C(43) C(42) 109.0(5) . . . yes N(42) C(43) C(47) 123.3(7) . . . yes C(42) C(43) C(47) 127.6(6) . . . yes C(41) C(44) C(45) 110.0(7) . . . yes C(41) C(44) C(46) 111.9(6) . . . yes C(45) C(44) C(46) 108.9(7) . . . yes C(43) C(47) C(48) 112.8(6) . . . yes C(43) C(47) C(49) 111.0(6) . . . yes C(48) C(47) C(49) 110.1(6) . . . yes N(51) C(51) C(52) 110.2(6) . . . yes N(51) C(51) C(54) 122.5(6) . . . yes C(52) C(51) C(54) 127.3(7) . . . yes C(51) C(52) C(53) 105.2(7) . . . yes N(52) C(53) C(52) 108.8(6) . . . yes N(52) C(53) C(57) 123.3(8) . . . yes C(52) C(53) C(57) 127.9(8) . . . yes C(51) C(54) C(55) 111.3(7) . . . yes C(51) C(54) C(56) 110.4(5) . . . yes C(55) C(54) C(56) 110.6(7) . . . yes C(53) C(57) C(58) 110.4(10) . . . yes C(53) C(57) C(59) 112.9(10) . . . yes C(58) C(57) C(59) 109(1) . . . yes N(61) C(61) C(62) 111.2(7) . . . yes N(61) C(61) C(64) 117.4(8) . . . yes C(62) C(61) C(64) 131.3(8) . . . yes C(61) C(62) C(63) 105.8(7) . . . yes N(62) C(63) C(62) 107.3(6) . . . yes N(62) C(63) C(67) 123.9(6) . . . yes C(62) C(63) C(67) 128.8(7) . . . yes C(61) C(64) C(65) 109.0(7) . . . yes C(61) C(64) C(66) 111.3(9) . . . yes C(65) C(64) C(66) 110.2(9) . . . yes C(63) C(67) C(68) 111.0(7) . . . yes C(63) C(67) C(69) 111.5(6) . . . yes C(68) C(67) C(69) 110.6(7) . . . yes N(71) C(71) C(72) 168(1) . . . yes N(72) C(73) C(74) 176(1) . . . yes N(73) C(75) C(76) 178(1) . . . yes N(74) C(77) C(78) 151(1) . . . yes N(75) C(78) C(77) 148(2) . . . yes N(12) B(1) N(22) 109.1(6) . . . yes N(12) B(1) N(32) 109.7(5) . . . yes N(22) B(1) N(32) 107.9(6) . . . yes N(42) B(2) N(52) 108.1(7) . . . yes N(42) B(2) N(62) 110.9(6) . . . yes N(52) B(2) N(62) 108.8(6) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . yes ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(11) C(72) 3.58(1) . 3_656 ? N(12) C(72) 3.57(1) . 3_656 ? N(21) C(76) 3.54(1) . 4_554 ? N(21) C(56) 3.56(1) . 4_555 ? N(31) C(72) 3.42(1) . 3_656 ? N(31) C(76) 3.52(1) . 4_554 ? N(32) C(72) 3.53(1) . 3_656 ? N(32) C(76) 3.58(1) . 4_554 ? C(18) C(26) 3.45(1) . 2_645 ? C(27) N(75) 3.38(3) . 2_645 ? C(29) N(75) 3.54(4) . 2_645 ? C(31) C(72) 3.57(1) . 3_656 ? C(39) N(75) 3.47(3) . 2_645 ? C(49) C(71) 3.54(2) . 1_454 ? C(73) N(75) 3.35(3) . 2_645 ? C(74) N(75) 3.27(3) . 2_645 ? Pd(1) N(42) 2.938(5) . . ? Pd(1) N(52) 2.944(5) . . ? Pd(1) Co(1) 3.112(1) . . ? Pd(1) N(61) 3.300(7) . . ? Co(1) N(32) 2.978(5) . . ? Co(1) N(12) 2.986(5) . . ? Co(1) N(22) 2.996(5) . . ? O(1) O(2) 2.586(7) . . ? O(1) N(51) 3.015(6) . . ? O(1) O(3) 3.06(2) . . ? O(1) N(21) 3.183(7) . . ? O(1) N(31) 3.401(7) . . ? O(2) N(11) 2.925(7) . . ? O(2) N(41) 2.950(7) . . ? O(2) N(31) 3.230(7) . . ? O(3) N(61) 2.74(2) . . ? O(3) N(51) 3.08(2) . . ? O(3) N(52) 3.46(1) . . ? N(11) N(21) 2.858(8) . . ? N(11) N(31) 2.911(9) . . ? N(11) N(22) 3.000(8) . . ? N(11) N(32) 3.076(8) . . ? N(12) N(22) 2.508(8) . . ? N(12) N(32) 2.532(9) . . ? N(12) N(31) 3.010(8) . . ? N(12) N(21) 3.032(8) . . ? N(21) N(31) 2.932(8) . . ? N(21) N(32) 3.052(8) . . ? N(22) N(31) 3.023(8) . . ? N(41) N(51) 2.786(9) . . ? N(41) N(52) 3.019(9) . . ? N(42) N(52) 2.504(8) . . ? N(42) N(51) 2.926(8) . . ? N(51) N(61) 3.138(10) . . ? N(52) N(61) 2.792(9) . . ? #------------------------------------------------------------------------------ #===END data_compound_6b(Co) _database_code_CSD 213635 _audit_creation_date 'Fri Jun 13 18:29:55 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C50 H82 B2 Co N16 O2 Pd ' _chemical_formula_moiety 'C50 H82 B2 Co N16 O2 Pd ' _chemical_formula_weight 1126.26 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.324(3) _cell_length_b 20.964(5) _cell_length_c 12.165(2) _cell_angle_alpha 101.75(1) _cell_angle_beta 112.935(6) _cell_angle_gamma 88.301(8) _cell_volume 3059(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8651 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.940 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 15957 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10718 _reflns_number_gt 4652 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.2198 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4652 _refine_ls_number_parameters 631 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0050 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.45 _refine_diff_density_min -1.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 0.71312(5) 0.23994(3) 0.31130(6) 0.0438(2) Uani 1.00 d . . . Co(1) Co 0.48859(9) 0.16570(6) 0.2229(1) 0.0464(3) Uani 1.00 d . . . O(1) O 0.6345(4) 0.1806(3) 0.3658(5) 0.050(1) Uani 1.00 d . . . O(2) O 0.5622(4) 0.2396(3) 0.1844(5) 0.048(1) Uani 1.00 d . . . N(11) N 0.3487(6) 0.1505(3) 0.0542(6) 0.049(2) Uani 1.00 d . . . N(12) N 0.2508(5) 0.1323(4) 0.0566(6) 0.048(2) Uani 1.00 d . . . N(21) N 0.4301(5) 0.0847(3) 0.2658(6) 0.048(2) Uani 1.00 d . . . N(22) N 0.3194(6) 0.0780(3) 0.2372(7) 0.048(2) Uani 1.00 d . . . N(31) N 0.3874(6) 0.2220(4) 0.3024(7) 0.052(2) Uani 1.00 d . . . N(32) N 0.2826(6) 0.1966(4) 0.2687(6) 0.049(2) Uani 1.00 d . . . N(41) N 0.7857(6) 0.2941(4) 0.2411(7) 0.053(2) Uani 1.00 d . . . N(42) N 0.8663(6) 0.3425(4) 0.3184(7) 0.058(2) Uani 1.00 d . . . N(51) N 0.8612(5) 0.2350(3) 0.4382(6) 0.047(2) Uani 1.00 d . . . N(52) N 0.9294(6) 0.2904(3) 0.4983(6) 0.045(2) Uani 1.00 d . . . N(61) N 0.8061(7) 0.3759(4) 0.6037(8) 0.071(2) Uani 1.00 d . . . N(62) N 0.8025(6) 0.3841(3) 0.4917(7) 0.056(2) Uani 1.00 d . . . N(71) N 0.5767(6) 0.0984(4) 0.1280(7) 0.060(2) Uani 1.00 d . . . N(81) N 0.067(1) 0.2712(8) 0.009(2) 0.17396(8) Uiso 1.00 d . . . N(82) N 1.2290(9) 0.1075(5) 0.5418(10) 0.09643(4) Uiso 1.00 d . . . N(83) N 0.6798(9) 0.1743(6) 0.640(1) 0.11001(4) Uiso 1.00 d . . . C(11) C 0.3297(7) 0.1477(5) -0.0623(8) 0.056(2) Uani 1.00 d . . . C(12) C 0.2223(8) 0.1284(5) -0.1359(9) 0.068(3) Uani 1.00 d . . . C(13) C 0.1737(7) 0.1217(5) -0.0574(9) 0.059(2) Uani 1.00 d . . . C(14) C 0.4181(8) 0.1632(5) -0.1016(9) 0.066(3) Uani 1.00 d . . . C(15) C 0.0571(8) 0.1006(7) -0.0867(9) 0.089(4) Uani 1.00 d . . . C(21) C 0.4759(7) 0.0327(4) 0.3144(8) 0.052(2) Uani 1.00 d . . . C(22) C 0.3942(8) -0.0071(4) 0.3163(9) 0.058(2) Uani 1.00 d . . . C(23) C 0.2975(8) 0.0233(5) 0.2676(9) 0.057(2) Uani 1.00 d . . . C(24) C 0.5975(8) 0.0240(5) 0.3577(9) 0.063(3) Uani 1.00 d . . . C(25) C 0.1852(8) 0.0003(5) 0.2478(10) 0.067(3) Uani 1.00 d . . . C(31) C 0.3953(8) 0.2779(5) 0.3803(9) 0.061(3) Uani 1.00 d . . . C(32) C 0.2975(8) 0.2906(5) 0.3964(10) 0.064(3) Uani 1.00 d . . . C(33) C 0.2277(7) 0.2373(5) 0.3245(9) 0.056(2) Uani 1.00 d . . . C(34) C 0.5004(9) 0.3187(5) 0.441(1) 0.083(3) Uani 1.00 d . . . C(35) C 0.1114(8) 0.2254(5) 0.3084(9) 0.067(3) Uani 1.00 d . . . C(41) C 0.7836(7) 0.2867(5) 0.1275(9) 0.055(2) Uani 1.00 d . . . C(42) C 0.8595(9) 0.3327(6) 0.1327(9) 0.078(3) Uani 1.00 d . . . C(43) C 0.9101(9) 0.3662(6) 0.2491(10) 0.076(3) Uani 1.00 d . . . C(44) C 0.7128(9) 0.2367(6) 0.0238(9) 0.070(3) Uani 1.00 d . . . C(45) C 0.781(1) 0.1834(6) -0.013(1) 0.090(4) Uani 1.00 d . . . C(46) C 0.6429(10) 0.2675(6) -0.083(1) 0.087(3) Uani 1.00 d . . . C(47) C 1.024(3) 0.407(1) 0.304(3) 0.07(1) Uani 0.59 d P . . C(47A) C 0.983(4) 0.431(2) 0.308(3) 0.05(1) Uani 0.41 d P . . C(48) C 1.091(2) 0.4002(9) 0.231(2) 0.077(5) Uani 0.59 d P . . C(48A) C 1.099(3) 0.409(2) 0.355(4) 0.10(1) Uani 0.41 d P . . C(49) C 0.983(2) 0.478(1) 0.324(2) 0.082(7) Uani 0.59 d P . . C(49A) C 0.953(3) 0.476(1) 0.214(3) 0.11(1) Uani 0.41 d P . . C(51) C 0.9186(7) 0.1837(4) 0.4740(8) 0.051(2) Uani 1.00 d . . . C(52) C 1.0219(7) 0.2062(4) 0.5603(8) 0.050(2) Uani 1.00 d . . . C(53) C 1.0278(7) 0.2722(4) 0.5720(8) 0.050(2) Uani 1.00 d . . . C(54) C 0.8721(7) 0.1143(4) 0.4188(9) 0.056(2) Uani 1.00 d . . . C(55) C 0.9163(10) 0.0820(5) 0.325(1) 0.082(3) Uani 1.00 d . . . C(56) C 0.8987(9) 0.0737(5) 0.518(1) 0.074(3) Uani 1.00 d . . . C(57) C 1.1196(8) 0.3216(5) 0.6549(9) 0.066(3) Uani 1.00 d . . . C(58) C 1.2296(9) 0.2897(6) 0.696(1) 0.094(4) Uani 1.00 d . . . C(59) C 1.0967(9) 0.3564(6) 0.764(1) 0.084(3) Uani 1.00 d . . . C(61) C 0.7399(10) 0.4165(7) 0.634(1) 0.087(4) Uani 1.00 d . . . C(62) C 0.6888(9) 0.4514(5) 0.545(2) 0.089(4) Uani 1.00 d . . . C(63) C 0.7293(9) 0.4311(5) 0.453(1) 0.076(3) Uani 1.00 d . . . C(64) C 0.724(1) 0.4188(9) 0.752(2) 0.123(6) Uani 1.00 d . . . C(65) C 0.826(2) 0.4342(9) 0.856(2) 0.153(7) Uani 1.00 d . . . C(66) C 0.639(2) 0.460(2) 0.767(2) 0.30(2) Uani 1.00 d . . . C(67) C 0.707(1) 0.4550(6) 0.340(1) 0.106(4) Uani 1.00 d . . . C(68) C 0.701(1) 0.5278(7) 0.355(2) 0.165(9) Uani 1.00 d . . . C(69) C 0.603(2) 0.4224(7) 0.238(1) 0.139(6) Uani 1.00 d . . . C(71) C 0.6204(8) 0.0638(5) 0.0787(9) 0.055(2) Uani 1.00 d . . . C(72) C 0.6758(9) 0.0190(5) 0.0158(10) 0.077(3) Uani 1.00 d . . . C(81) C 0.158(2) 0.2881(10) 0.038(2) 0.15565(9) Uiso 1.00 d . . . C(82) C 0.267(1) 0.3126(7) 0.080(1) 0.10091(5) Uiso 1.00 d . . . C(83) C 1.3094(9) 0.1282(5) 0.5476(10) 0.07196(4) Uiso 1.00 d . . . C(84) C 1.4117(9) 0.1513(6) 0.555(1) 0.08332(4) Uiso 1.00 d . . . C(85) C 0.7605(10) 0.2079(6) 0.685(1) 0.08130(4) Uiso 1.00 d . . . C(86) C 0.8604(9) 0.2468(6) 0.734(1) 0.07915(4) Uiso 1.00 d . . . B(1) B 0.2463(8) 0.1296(6) 0.1810(10) 0.054(3) Uani 1.00 d . . . B(2) B 0.8959(9) 0.3561(5) 0.458(1) 0.053(3) Uani 1.00 d . . . H(1) H 0.1719 0.1194 0.1692 0.0662 Uiso 1.00 calc . . . H(01) H 0.6451 0.2032 0.4560 0.0493 Uiso 1.00 calc . . . H(2) H 0.1879 0.1203 -0.2248 0.0803 Uiso 1.00 calc . . . H(02) H 0.5143 0.2729 0.1903 0.0493 Uiso 1.00 calc . . . H(3) H 0.4841 0.1431 -0.0592 0.0654 Uiso 1.00 calc . . . H(4) H 0.4331 0.2098 -0.0835 0.0654 Uiso 1.00 calc . . . H(5) H 0.3961 0.1471 -0.1882 0.0654 Uiso 1.00 calc . . . H(6) H 0.0239 0.1346 -0.0485 0.0893 Uiso 1.00 calc . . . H(7) H 0.0562 0.0618 -0.0552 0.0893 Uiso 1.00 calc . . . H(8) H 0.0164 0.0911 -0.1729 0.0893 Uiso 1.00 calc . . . H(9) H 0.4029 -0.0475 0.3449 0.0678 Uiso 1.00 calc . . . H(10) H 0.6218 0.0064 0.4304 0.0633 Uiso 1.00 calc . . . H(11) H 0.6354 0.0654 0.3755 0.0633 Uiso 1.00 calc . . . H(12) H 0.6131 -0.0055 0.2955 0.0633 Uiso 1.00 calc . . . H(13) H 0.1595 0.0296 0.3016 0.0650 Uiso 1.00 calc . . . H(14) H 0.1867 -0.0428 0.2642 0.0650 Uiso 1.00 calc . . . H(15) H 0.1363 -0.0008 0.1646 0.0650 Uiso 1.00 calc . . . H(16) H 0.2818 0.3284 0.4474 0.0785 Uiso 1.00 calc . . . H(17) H 0.5611 0.2914 0.4606 0.0820 Uiso 1.00 calc . . . H(18) H 0.5022 0.3480 0.5132 0.0820 Uiso 1.00 calc . . . H(19) H 0.5065 0.3444 0.3851 0.0820 Uiso 1.00 calc . . . H(20) H 0.0890 0.2618 0.3543 0.0686 Uiso 1.00 calc . . . H(21) H 0.1053 0.1866 0.3376 0.0686 Uiso 1.00 calc . . . H(22) H 0.0637 0.2192 0.2237 0.0686 Uiso 1.00 calc . . . H(23) H 0.9587 0.3868 0.4979 0.0638 Uiso 1.00 calc . . . H(24) H 0.8760 0.3371 0.0617 0.0874 Uiso 1.00 calc . . . H(25) H 0.6621 0.2167 0.0497 0.0847 Uiso 1.00 calc . . . H(26) H 0.7326 0.1488 -0.0737 0.0913 Uiso 1.00 calc . . . H(27) H 0.8252 0.1671 0.0574 0.0913 Uiso 1.00 calc . . . H(28) H 0.8254 0.2013 -0.0459 0.0913 Uiso 1.00 calc . . . H(29) H 0.6096 0.3048 -0.0533 0.0875 Uiso 1.00 calc . . . H(30) H 0.5871 0.2365 -0.1423 0.0875 Uiso 1.00 calc . . . H(31) H 0.6881 0.2814 -0.1199 0.0875 Uiso 1.00 calc . . . H(39) H 1.0794 0.1788 0.6026 0.0611 Uiso 1.00 calc . . . H(40) H 0.7931 0.1154 0.3794 0.0678 Uiso 1.00 calc . . . H(41) H 0.8894 0.0373 0.2960 0.0819 Uiso 1.00 calc . . . H(42) H 0.9942 0.0845 0.3614 0.0819 Uiso 1.00 calc . . . H(43) H 0.8917 0.1041 0.2579 0.0819 Uiso 1.00 calc . . . H(44) H 0.8675 0.0927 0.5748 0.0752 Uiso 1.00 calc . . . H(45) H 0.9763 0.0732 0.5588 0.0752 Uiso 1.00 calc . . . H(46) H 0.8684 0.0300 0.4795 0.0752 Uiso 1.00 calc . . . H(47) H 1.1225 0.3530 0.6082 0.0821 Uiso 1.00 calc . . . H(48) H 1.2261 0.2568 0.7398 0.0943 Uiso 1.00 calc . . . H(49) H 1.2858 0.3223 0.7495 0.0943 Uiso 1.00 calc . . . H(50) H 1.2446 0.2702 0.6267 0.0943 Uiso 1.00 calc . . . H(51) H 1.1566 0.3869 0.8170 0.0845 Uiso 1.00 calc . . . H(52) H 1.0881 0.3251 0.8077 0.0845 Uiso 1.00 calc . . . H(53) H 1.0310 0.3794 0.7368 0.0845 Uiso 1.00 calc . . . H(54) H 0.6329 0.4834 0.5423 0.1052 Uiso 1.00 calc . . . H(55) H 0.7004 0.3728 0.7515 0.1495 Uiso 1.00 calc . . . H(56) H 0.8139 0.4239 0.9236 0.1511 Uiso 1.00 calc . . . H(57) H 0.8444 0.4786 0.8694 0.1511 Uiso 1.00 calc . . . H(58) H 0.8780 0.4070 0.8382 0.1511 Uiso 1.00 calc . . . H(59) H 0.6669 0.5053 0.7926 0.2915 Uiso 1.00 calc . . . H(60) H 0.6180 0.4489 0.8271 0.2915 Uiso 1.00 calc . . . H(61) H 0.5768 0.4554 0.6906 0.2915 Uiso 1.00 calc . . . H(62) H 0.7639 0.4411 0.3073 0.1237 Uiso 1.00 calc . . . H(63) H 0.7691 0.5483 0.4124 0.1683 Uiso 1.00 calc . . . H(64) H 0.6441 0.5416 0.3839 0.1683 Uiso 1.00 calc . . . H(65) H 0.6835 0.5397 0.2776 0.1683 Uiso 1.00 calc . . . H(66) H 0.5418 0.4312 0.2646 0.1395 Uiso 1.00 calc . . . H(67) H 0.6074 0.3754 0.2212 0.1395 Uiso 1.00 calc . . . H(68) H 0.5870 0.4383 0.1662 0.1395 Uiso 1.00 calc . . . H(69) H 0.6689 -0.0236 0.0272 0.0768 Uiso 1.00 calc . . . H(70) H 0.7520 0.0335 0.0484 0.0768 Uiso 1.00 calc . . . H(71) H 0.6443 0.0200 -0.0698 0.0768 Uiso 1.00 calc . . . H(72) H 0.3151 0.2899 0.1397 0.1019 Uiso 1.00 calc . . . H(73) H 0.2739 0.3586 0.1160 0.1019 Uiso 1.00 calc . . . H(74) H 0.2899 0.3068 0.0121 0.1019 Uiso 1.00 calc . . . H(75) H 1.4702 0.1372 0.6208 0.0833 Uiso 1.00 calc . . . H(76) H 1.4157 0.1980 0.5693 0.0833 Uiso 1.00 calc . . . H(77) H 1.4202 0.1337 0.4796 0.0833 Uiso 1.00 calc . . . H(78) H 0.9139 0.2234 0.7115 0.0799 Uiso 1.00 calc . . . H(79) H 0.8855 0.2573 0.8224 0.0799 Uiso 1.00 calc . . . H(80) H 0.8481 0.2867 0.7049 0.0799 Uiso 1.00 calc . . . 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) 0.0446(4) 0.0450(4) 0.0436(4) -0.0027(3) 0.0151(3) 0.0169(3) Co(1) 0.0472(7) 0.0495(7) 0.0436(7) -0.0051(6) 0.0163(6) 0.0139(6) O(1) 0.045(3) 0.052(4) 0.049(3) -0.008(3) 0.011(3) 0.018(3) O(2) 0.043(3) 0.052(4) 0.043(3) -0.004(3) 0.009(3) 0.011(3) N(11) 0.051(4) 0.050(4) 0.047(4) -0.010(4) 0.024(4) 0.003(4) N(12) 0.039(4) 0.056(5) 0.045(4) -0.006(4) 0.008(3) 0.015(4) N(21) 0.043(4) 0.049(4) 0.043(4) -0.006(4) 0.011(3) 0.000(4) N(22) 0.045(4) 0.046(4) 0.053(4) -0.008(3) 0.020(4) 0.009(4) N(31) 0.053(4) 0.046(4) 0.056(5) 0.000(4) 0.019(4) 0.011(4) N(32) 0.048(4) 0.052(4) 0.049(4) -0.003(4) 0.018(4) 0.015(4) N(41) 0.046(4) 0.067(5) 0.048(5) 0.000(4) 0.016(4) 0.020(4) N(42) 0.065(5) 0.051(5) 0.054(5) -0.008(4) 0.014(4) 0.018(4) N(51) 0.043(4) 0.054(5) 0.050(4) -0.005(4) 0.020(3) 0.019(4) N(52) 0.049(4) 0.039(4) 0.052(4) 0.002(4) 0.023(4) 0.017(4) N(61) 0.065(5) 0.073(6) 0.077(6) -0.002(5) 0.033(5) 0.008(5) N(62) 0.060(5) 0.041(4) 0.060(5) 0.000(4) 0.016(4) 0.009(4) N(71) 0.066(5) 0.066(5) 0.056(5) 0.012(5) 0.027(4) 0.021(4) C(11) 0.059(6) 0.061(6) 0.041(5) -0.006(5) 0.013(5) 0.008(5) C(12) 0.068(6) 0.082(8) 0.045(6) -0.014(6) 0.010(5) 0.018(6) C(13) 0.048(5) 0.063(6) 0.055(6) -0.009(5) 0.006(5) 0.016(5) C(14) 0.065(6) 0.072(7) 0.049(6) -0.020(5) 0.007(5) 0.017(5) C(15) 0.059(6) 0.14(1) 0.051(6) -0.020(7) -0.001(5) 0.039(7) C(21) 0.055(5) 0.049(5) 0.051(6) 0.004(5) 0.018(5) 0.017(5) C(22) 0.068(6) 0.055(6) 0.068(6) 0.004(5) 0.037(5) 0.027(5) C(23) 0.055(6) 0.053(6) 0.067(6) -0.020(5) 0.029(5) 0.009(5) C(24) 0.060(6) 0.058(6) 0.072(7) 0.004(5) 0.016(5) 0.035(6) C(25) 0.071(6) 0.051(6) 0.076(7) -0.011(5) 0.023(6) 0.019(6) C(31) 0.061(6) 0.058(6) 0.058(6) -0.006(5) 0.017(5) 0.013(6) C(32) 0.067(6) 0.063(6) 0.077(7) 0.011(6) 0.041(6) 0.021(6) C(33) 0.045(5) 0.067(6) 0.067(6) 0.014(5) 0.025(5) 0.034(6) C(34) 0.085(8) 0.069(7) 0.097(9) -0.013(7) 0.048(7) -0.005(7) C(35) 0.067(7) 0.076(7) 0.071(7) 0.009(6) 0.037(6) 0.023(6) C(41) 0.058(5) 0.057(6) 0.049(6) -0.016(5) 0.016(5) 0.012(5) C(42) 0.091(8) 0.090(8) 0.046(6) -0.035(7) 0.014(6) 0.021(6) C(43) 0.082(7) 0.094(9) 0.058(7) -0.026(7) 0.022(6) 0.032(7) C(44) 0.078(7) 0.086(8) 0.047(6) -0.026(6) 0.021(5) 0.019(6) C(45) 0.12(1) 0.067(7) 0.074(8) -0.020(8) 0.035(8) 0.008(7) C(46) 0.096(8) 0.100(9) 0.061(7) -0.014(7) 0.030(6) 0.008(7) C(47) 0.11(3) 0.04(2) 0.07(2) -0.03(2) 0.04(2) 0.00(2) C(47A) 0.10(3) 0.03(2) 0.02(1) -0.03(2) 0.01(1) 0.01(2) C(48) 0.08(1) 0.08(1) 0.09(1) -0.03(1) 0.05(1) 0.01(1) C(48A) 0.07(2) 0.11(3) 0.10(3) -0.03(2) 0.00(2) 0.02(2) C(49) 0.09(1) 0.04(1) 0.12(2) -0.02(1) 0.05(1) 0.00(1) C(49A) 0.14(3) 0.07(2) 0.05(2) -0.09(2) -0.03(2) 0.03(2) C(51) 0.058(5) 0.051(5) 0.058(6) 0.012(5) 0.028(5) 0.031(5) C(52) 0.040(5) 0.058(6) 0.053(5) -0.003(4) 0.012(4) 0.023(5) C(53) 0.050(5) 0.049(5) 0.054(6) -0.008(4) 0.020(4) 0.013(5) C(54) 0.057(6) 0.044(5) 0.073(7) -0.001(5) 0.027(5) 0.020(5) C(55) 0.098(8) 0.075(7) 0.090(8) 0.003(7) 0.055(8) 0.021(7) C(56) 0.099(8) 0.060(6) 0.080(8) 0.006(6) 0.044(7) 0.030(6) C(57) 0.076(7) 0.061(6) 0.060(6) -0.005(6) 0.019(6) 0.026(6) C(58) 0.060(7) 0.100(9) 0.110(10) -0.012(7) 0.012(7) 0.035(8) C(59) 0.083(8) 0.076(8) 0.070(7) -0.036(7) 0.010(6) 0.000(7) C(61) 0.073(8) 0.11(1) 0.084(9) -0.007(8) 0.039(7) 0.013(8) C(62) 0.061(7) 0.063(7) 0.15(1) 0.006(6) 0.049(9) 0.028(8) C(63) 0.062(7) 0.055(7) 0.093(9) -0.012(6) 0.010(7) 0.017(7) C(64) 0.084(10) 0.17(2) 0.11(1) 0.01(1) 0.053(9) 0.00(1) C(65) 0.22(2) 0.17(2) 0.13(1) 0.03(2) 0.12(2) 0.06(1) C(66) 0.16(2) 0.56(5) 0.12(2) 0.15(3) 0.07(1) -0.04(2) C(67) 0.12(1) 0.078(9) 0.12(1) 0.027(9) 0.034(10) 0.043(9) C(68) 0.10(1) 0.11(1) 0.27(2) -0.008(9) 0.01(1) 0.13(1) C(69) 0.22(2) 0.070(9) 0.11(1) 0.03(1) 0.04(1) 0.041(9) C(71) 0.053(6) 0.053(6) 0.055(6) -0.004(5) 0.014(5) 0.015(5) C(72) 0.093(8) 0.065(7) 0.073(7) -0.001(7) 0.040(7) 0.001(6) B(1) 0.045(6) 0.066(7) 0.043(6) -0.011(5) 0.004(5) 0.018(6) B(2) 0.055(6) 0.041(6) 0.058(7) -0.011(5) 0.014(5) 0.011(6) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL97 _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) O(1) 2.010(7) . . yes Pd(1) O(2) 2.001(5) . . yes Pd(1) N(41) 2.016(9) . . yes Pd(1) N(51) 1.991(6) . . yes Co(1) O(1) 2.020(5) . . yes Co(1) O(2) 2.080(7) . . yes Co(1) N(11) 2.139(6) . . yes Co(1) N(21) 2.126(8) . . yes Co(1) N(31) 2.145(9) . . yes Co(1) N(71) 2.236(9) . . yes N(11) N(12) 1.38(1) . . yes N(11) C(11) 1.33(1) . . yes N(12) C(13) 1.34(1) . . yes N(12) B(1) 1.55(2) . . yes N(21) N(22) 1.38(1) . . yes N(21) C(21) 1.36(1) . . yes N(22) C(23) 1.35(1) . . yes N(22) B(1) 1.52(1) . . yes N(31) N(32) 1.38(1) . . yes N(31) C(31) 1.33(1) . . yes N(32) C(33) 1.36(1) . . yes N(32) B(1) 1.54(1) . . yes N(41) N(42) 1.397(9) . . yes N(41) C(41) 1.35(1) . . yes N(42) C(43) 1.37(2) . . yes N(42) B(2) 1.55(1) . . yes N(51) N(52) 1.382(9) . . yes N(51) C(51) 1.35(1) . . yes N(52) C(53) 1.36(1) . . yes N(52) B(2) 1.55(1) . . yes N(61) N(62) 1.39(1) . . yes N(61) C(61) 1.31(2) . . yes N(62) C(63) 1.38(1) . . yes N(62) B(2) 1.52(2) . . yes N(71) C(71) 1.14(1) . . yes N(81) C(81) 1.16(3) . . yes N(82) C(83) 1.14(2) . . yes N(83) C(85) 1.17(2) . . yes C(11) C(12) 1.38(1) . . yes C(11) C(14) 1.50(2) . . yes C(12) C(13) 1.38(2) . . yes C(13) C(15) 1.51(1) . . yes C(21) C(22) 1.40(2) . . yes C(21) C(24) 1.51(1) . . yes C(22) C(23) 1.39(1) . . yes C(23) C(25) 1.50(2) . . yes C(31) C(32) 1.40(2) . . yes C(31) C(34) 1.50(1) . . yes C(32) C(33) 1.38(1) . . yes C(33) C(35) 1.51(2) . . yes C(41) C(42) 1.39(2) . . yes C(41) C(44) 1.47(1) . . yes C(42) C(43) 1.35(1) . . yes C(43) C(47) 1.59(4) . . yes C(43) C(47A) 1.56(4) . . yes C(44) C(45) 1.52(2) . . yes C(44) C(46) 1.53(2) . . yes C(47) C(47A) 0.74(6) . . yes C(47) C(48) 1.48(5) . . yes C(47) C(48A) 0.94(5) . . yes C(47) C(49) 1.57(4) . . yes C(47A) C(48A) 1.52(6) . . yes C(47A) C(49) 0.96(4) . . yes C(47A) C(49A) 1.55(5) . . yes C(48) C(48A) 1.44(5) . . yes C(49) C(49A) 1.24(4) . . yes C(51) C(52) 1.39(1) . . yes C(51) C(54) 1.51(1) . . yes C(52) C(53) 1.36(1) . . yes C(53) C(57) 1.51(1) . . yes C(54) C(55) 1.52(2) . . yes C(54) C(56) 1.54(2) . . yes C(57) C(58) 1.53(2) . . yes C(57) C(59) 1.52(2) . . yes C(61) C(62) 1.38(2) . . yes C(61) C(64) 1.52(3) . . yes C(62) C(63) 1.41(2) . . yes C(63) C(67) 1.48(2) . . yes C(64) C(65) 1.44(2) . . yes C(64) C(66) 1.44(3) . . yes C(67) C(68) 1.50(2) . . yes C(67) C(69) 1.52(2) . . yes C(71) C(72) 1.46(2) . . yes C(81) C(82) 1.41(3) . . yes C(83) C(84) 1.43(2) . . yes C(85) C(86) 1.43(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 O(1) Pd(1) O(2) 80.5(2) . . . yes O(1) Pd(1) N(41) 174.7(2) . . . yes O(1) Pd(1) N(51) 96.6(3) . . . yes O(2) Pd(1) N(41) 96.2(3) . . . yes O(2) Pd(1) N(51) 176.6(3) . . . yes N(41) Pd(1) N(51) 86.7(3) . . . yes O(1) Co(1) O(2) 78.4(2) . . . yes O(1) Co(1) N(11) 170.9(3) . . . yes O(1) Co(1) N(21) 97.3(2) . . . yes O(1) Co(1) N(31) 100.8(2) . . . yes O(1) Co(1) N(71) 84.7(2) . . . yes O(2) Co(1) N(11) 95.1(3) . . . yes O(2) Co(1) N(21) 173.5(2) . . . yes O(2) Co(1) N(31) 100.1(3) . . . yes O(2) Co(1) N(71) 85.0(3) . . . yes N(11) Co(1) N(21) 88.7(3) . . . yes N(11) Co(1) N(31) 86.5(3) . . . yes N(11) Co(1) N(71) 88.4(3) . . . yes N(21) Co(1) N(31) 85.4(3) . . . yes N(21) Co(1) N(71) 89.8(3) . . . yes N(31) Co(1) N(71) 173.1(3) . . . yes Pd(1) O(1) Co(1) 100.6(3) . . . yes Pd(1) O(2) Co(1) 98.9(3) . . . yes Co(1) N(11) N(12) 117.1(6) . . . yes Co(1) N(11) C(11) 136.4(7) . . . yes N(12) N(11) C(11) 106.2(6) . . . yes N(11) N(12) C(13) 109.0(8) . . . yes N(11) N(12) B(1) 118.9(6) . . . yes C(13) N(12) B(1) 132.1(8) . . . yes Co(1) N(21) N(22) 117.8(5) . . . yes Co(1) N(21) C(21) 135.2(6) . . . yes N(22) N(21) C(21) 106.9(8) . . . yes N(21) N(22) C(23) 109.3(7) . . . yes N(21) N(22) B(1) 118.9(8) . . . yes C(23) N(22) B(1) 131.8(8) . . . yes Co(1) N(31) N(32) 117.0(5) . . . yes Co(1) N(31) C(31) 138.0(7) . . . yes N(32) N(31) C(31) 105.0(8) . . . yes N(31) N(32) C(33) 110.7(7) . . . yes N(31) N(32) B(1) 119.1(8) . . . yes C(33) N(32) B(1) 130.2(8) . . . yes Pd(1) N(41) N(42) 120.1(6) . . . yes Pd(1) N(41) C(41) 130.8(6) . . . yes N(42) N(41) C(41) 108.3(8) . . . yes N(41) N(42) C(43) 107.9(8) . . . yes N(41) N(42) B(2) 119.7(9) . . . yes C(43) N(42) B(2) 132.3(8) . . . yes Pd(1) N(51) N(52) 120.7(5) . . . yes Pd(1) N(51) C(51) 131.7(5) . . . yes N(52) N(51) C(51) 107.3(6) . . . yes N(51) N(52) C(53) 108.3(7) . . . yes N(51) N(52) B(2) 119.9(6) . . . yes C(53) N(52) B(2) 130.6(7) . . . yes N(62) N(61) C(61) 108.0(9) . . . yes N(61) N(62) C(63) 108.6(10) . . . yes N(61) N(62) B(2) 115.5(8) . . . yes C(63) N(62) B(2) 133(1) . . . yes Co(1) N(71) C(71) 179.2(7) . . . yes N(11) C(11) C(12) 110(1) . . . yes N(11) C(11) C(14) 121.8(7) . . . yes C(12) C(11) C(14) 127.3(9) . . . yes C(11) C(12) C(13) 105.3(8) . . . yes N(12) C(13) C(12) 108.4(8) . . . yes N(12) C(13) C(15) 122(1) . . . yes C(12) C(13) C(15) 129.0(8) . . . yes N(21) C(21) C(22) 109.3(8) . . . yes N(21) C(21) C(24) 121.8(9) . . . yes C(22) C(21) C(24) 129.0(9) . . . yes C(21) C(22) C(23) 105.7(9) . . . yes N(22) C(23) C(22) 108.8(9) . . . yes N(22) C(23) C(25) 123.9(8) . . . yes C(22) C(23) C(25) 127.3(10) . . . yes N(31) C(31) C(32) 111.8(8) . . . yes N(31) C(31) C(34) 120(1) . . . yes C(32) C(31) C(34) 127.8(9) . . . yes C(31) C(32) C(33) 104.9(9) . . . yes N(32) C(33) C(32) 107.5(9) . . . yes N(32) C(33) C(35) 125.2(8) . . . yes C(32) C(33) C(35) 127.3(10) . . . yes N(41) C(41) C(42) 106.9(8) . . . yes N(41) C(41) C(44) 122.9(10) . . . yes C(42) C(41) C(44) 130(1) . . . yes C(41) C(42) C(43) 109(1) . . . yes N(42) C(43) C(42) 107.4(10) . . . yes N(42) C(43) C(47) 123(1) . . . yes N(42) C(43) C(47A) 117(1) . . . yes C(42) C(43) C(47) 125(1) . . . yes C(42) C(43) C(47A) 133(1) . . . yes C(47) C(43) C(47A) 27(2) . . . yes C(41) C(44) C(45) 110.5(9) . . . yes C(41) C(44) C(46) 110.9(9) . . . yes C(45) C(44) C(46) 112.0(10) . . . yes C(43) C(47) C(47A) 73(4) . . . yes C(43) C(47) C(48) 118(2) . . . yes C(43) C(47) C(48A) 146(4) . . . yes C(43) C(47) C(49) 99(2) . . . yes C(47A) C(47) C(48) 129(5) . . . yes C(47A) C(47) C(48A) 129(5) . . . yes C(47A) C(47) C(49) 26(3) . . . yes C(48) C(47) C(48A) 69(4) . . . yes C(48) C(47) C(49) 112(2) . . . yes C(48A) C(47) C(49) 107(3) . . . yes C(43) C(47A) C(47) 79(3) . . . yes C(43) C(47A) C(48A) 104(2) . . . yes C(43) C(47A) C(49) 144(4) . . . yes C(43) C(47A) C(49A) 109(2) . . . yes C(47) C(47A) C(48A) 28(3) . . . yes C(47) C(47A) C(49) 134(6) . . . yes C(47) C(47A) C(49A) 115(6) . . . yes C(48A) C(47A) C(49) 110(4) . . . yes C(48A) C(47A) C(49A) 117(4) . . . yes C(49) C(47A) C(49A) 52(2) . . . yes C(47) C(48) C(48A) 37(1) . . . yes C(47) C(48A) C(47A) 22(2) . . . yes C(47) C(48A) C(48) 73(3) . . . yes C(47A) C(48A) C(48) 86(2) . . . yes C(47) C(49) C(47A) 19(3) . . . yes C(47) C(49) C(49A) 88(2) . . . yes C(47A) C(49) C(49A) 88(3) . . . yes C(47A) C(49A) C(49) 38(1) . . . yes N(51) C(51) C(52) 109.1(7) . . . yes N(51) C(51) C(54) 121.7(7) . . . yes C(52) C(51) C(54) 129.1(8) . . . yes C(51) C(52) C(53) 106.8(8) . . . yes N(52) C(53) C(52) 108.4(7) . . . yes N(52) C(53) C(57) 121.8(8) . . . yes C(52) C(53) C(57) 129.7(8) . . . yes C(51) C(54) C(55) 111.0(10) . . . yes C(51) C(54) C(56) 111.1(7) . . . yes C(55) C(54) C(56) 109.0(8) . . . yes C(53) C(57) C(58) 111.4(8) . . . yes C(53) C(57) C(59) 110.3(10) . . . yes C(58) C(57) C(59) 110.8(9) . . . yes N(61) C(61) C(62) 110(1) . . . yes N(61) C(61) C(64) 121(1) . . . yes C(62) C(61) C(64) 128(1) . . . yes C(61) C(62) C(63) 106(1) . . . yes N(62) C(63) C(62) 105(1) . . . yes N(62) C(63) C(67) 124(1) . . . yes C(62) C(63) C(67) 129(1) . . . yes C(61) C(64) C(65) 110(1) . . . yes C(61) C(64) C(66) 114(1) . . . yes C(65) C(64) C(66) 112(1) . . . yes C(63) C(67) C(68) 114(1) . . . yes C(63) C(67) C(69) 110(1) . . . yes C(68) C(67) C(69) 109(1) . . . yes N(71) C(71) C(72) 179(1) . . . yes N(81) C(81) C(82) 175(2) . . . yes N(82) C(83) C(84) 177(1) . . . yes N(83) C(85) C(86) 177(1) . . . yes N(12) B(1) N(22) 110.4(8) . . . yes N(12) B(1) N(32) 110.1(9) . . . yes N(22) B(1) N(32) 109.7(6) . . . yes N(42) B(2) N(52) 106.4(7) . . . yes N(42) B(2) N(62) 112.5(7) . . . yes N(52) B(2) N(62) 111.9(10) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(11) C(72) 3.48(1) . 2_655 ? N(12) C(72) 3.34(1) . 2_655 ? N(21) C(72) 3.44(1) . 2_655 ? N(22) C(72) 3.35(1) . 2_655 ? N(22) C(84) 3.57(1) . 1_455 ? N(31) C(84) 3.57(2) . 1_455 ? N(32) C(84) 3.54(1) . 1_455 ? N(81) C(48) 3.33(3) . 1_455 ? N(81) C(86) 3.35(2) . 1_454 ? N(83) C(84) 3.33(2) . 1_455 ? C(13) C(72) 3.53(1) . 2_655 ? C(15) C(25) 3.54(1) . 2_555 ? C(23) C(72) 3.53(2) . 2_655 ? C(32) C(48A) 3.53(4) . 1_455 ? C(48) C(81) 3.32(3) . 1_655 ? C(48A) C(68) 3.51(4) . 2_766 ? C(49A) C(59) 3.54(3) . 2_766 ? #------------------------------------------------------------------------------ #===END data_6c(Co) _database_code_CSD 213636 _audit_creation_date 'Thu Jul 17 22:13:15 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C51 H83.50 B2 Co N16.50 O2 Pd ' _chemical_formula_moiety 'C51 H83.50 B2 Co N16.50 O2 Pd ' _chemical_formula_weight 1146.78 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.356(1) _cell_length_b 21.0836(8) _cell_length_c 12.1174(9) _cell_angle_alpha 95.350(4) _cell_angle_beta 114.865(1) _cell_angle_gamma 84.508(4) _cell_volume 3076.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10287 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.941 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 24065 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12688 _reflns_number_gt 11043 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1552 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 11043 _refine_ls_number_parameters 691 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0310 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.88 _refine_diff_density_min -2.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 -0.06448(2) 0.37500(1) -0.19476(2) 0.02829(8) Uani 1.00 d . . . Co(1) Co 0.12609(3) 0.26720(2) -0.13791(4) 0.0317(1) Uani 1.00 d . . . O(1) O -0.0314(2) 0.2826(1) -0.1578(2) 0.0387(5) Uani 1.00 d . . . O(2) O 0.0891(2) 0.3586(1) -0.1855(2) 0.0386(5) Uani 1.00 d . . . N(11) N 0.3011(2) 0.2754(1) -0.0633(2) 0.0334(5) Uani 1.00 d . . . N(12) N 0.3643(2) 0.2206(1) -0.0700(2) 0.0324(5) Uani 1.00 d . . . N(21) N 0.1681(2) 0.1860(1) -0.0295(3) 0.0394(6) Uani 1.00 d . . . N(22) N 0.2483(2) 0.1428(1) -0.0393(3) 0.0422(6) Uani 1.00 d . . . N(31) N 0.1359(2) 0.2076(1) -0.2796(3) 0.0393(6) Uani 1.00 d . . . N(32) N 0.2224(2) 0.1618(1) -0.2528(3) 0.0423(6) Uani 1.00 d . . . N(41) N -0.0803(2) 0.4681(1) -0.2236(2) 0.0326(5) Uani 1.00 d . . . N(42) N -0.1754(2) 0.4957(1) -0.3081(2) 0.0325(5) Uani 1.00 d . . . N(51) N -0.2166(2) 0.3844(1) -0.1971(2) 0.0315(5) Uani 1.00 d . . . N(52) N -0.2990(2) 0.4238(1) -0.2749(2) 0.0340(5) Uani 1.00 d . . . N(61) N -0.2507(2) 0.4445(1) -0.5570(3) 0.0454(6) Uani 1.00 d . . . N(62) N -0.2805(2) 0.4160(1) -0.4784(2) 0.0380(5) Uani 1.00 d . . . N(71) N 0.4055(6) 0.2425(3) 0.5307(6) 0.128(2) Uani 1.00 d . . . N(72) N 0.5691(6) 0.1418(3) 0.2947(7) 0.134(2) Uani 1.00 d . . . N(73) N -0.2087(4) 0.1904(2) -0.2615(5) 0.090(1) Uani 1.00 d . . . N(74) N 0.8667(7) 0.0029(4) 0.7459(7) 0.179(4) Uani 1.00 d . . . N(75) N 1.0000 0.5000 0.5000 0.132(4) Uani 1.00 d S . . C(11) C 0.3725(2) 0.3212(1) -0.0088(3) 0.0348(6) Uani 1.00 d . . . C(12) C 0.4804(3) 0.2962(1) 0.0193(3) 0.0355(6) Uani 1.00 d . . . C(13) C 0.4725(2) 0.2325(1) -0.0195(3) 0.0331(6) Uani 1.00 d . . . C(14) C 0.3364(3) 0.3874(2) 0.0216(4) 0.0461(8) Uani 1.00 d . . . C(15) C 0.4024(4) 0.4373(2) 0.0112(5) 0.070(1) Uani 1.00 d . . . C(16) C 0.3137(5) 0.3937(2) 0.1276(5) 0.084(2) Uani 1.00 d . . . C(17) C 0.5639(3) 0.1829(1) -0.0140(3) 0.0392(6) Uani 1.00 d . . . C(18) C 0.5785(4) 0.1784(2) -0.1321(4) 0.062(1) Uani 1.00 d . . . C(19) C 0.6721(3) 0.1980(2) 0.0945(4) 0.0584(10) Uani 1.00 d . . . C(21) C 0.1364(3) 0.1638(2) 0.0490(4) 0.0513(9) Uani 1.00 d . . . C(22) C 0.1978(4) 0.1071(2) 0.0937(5) 0.068(1) Uani 1.00 d . . . C(23) C 0.2665(3) 0.0950(2) 0.0369(5) 0.061(1) Uani 1.00 d . . . C(24) C 0.0517(4) 0.1986(2) 0.0870(5) 0.064(1) Uani 1.00 d . . . C(25) C 0.1036(6) 0.2421(4) 0.1986(8) 0.145(3) Uani 1.00 d . . . C(26) C -0.0230(6) 0.1557(3) 0.1005(8) 0.113(2) Uani 1.00 d . . . C(27) C 0.3505(5) 0.0398(2) 0.0476(7) 0.089(2) Uani 1.00 d . . . C(28) C 0.3907(6) 0.0098(3) 0.1704(7) 0.121(3) Uani 1.00 d . . . C(29) C 0.2996(7) -0.0110(3) -0.0543(8) 0.147(4) Uani 1.00 d . . . C(31) C 0.0735(3) 0.2012(2) -0.3990(3) 0.0522(8) Uani 1.00 d . . . C(32) C 0.1196(4) 0.1512(2) -0.4501(4) 0.071(1) Uani 1.00 d . . . C(33) C 0.2121(3) 0.1277(2) -0.3567(4) 0.062(1) Uani 1.00 d . . . C(34) C -0.0297(3) 0.2424(2) -0.4601(4) 0.062(1) Uani 1.00 d . . . C(35) C -0.0116(6) 0.2922(4) -0.5280(8) 0.134(3) Uani 1.00 d . . . C(36) C -0.1252(5) 0.2032(3) -0.5412(7) 0.117(3) Uani 1.00 d . . . C(37) C 0.2910(4) 0.0711(3) -0.3616(5) 0.083(2) Uani 1.00 d . . . C(38) C 0.3348(5) 0.0784(3) -0.4537(7) 0.112(3) Uani 1.00 d . . . C(39) C 0.2337(6) 0.0092(3) -0.3898(7) 0.110(2) Uani 1.00 d . . . C(41) C -0.0064(3) 0.5137(1) -0.1733(3) 0.0343(6) Uani 1.00 d . . . C(42) C -0.0558(3) 0.5703(1) -0.2297(3) 0.0402(6) Uani 1.00 d . . . C(43) C -0.1603(3) 0.5575(1) -0.3127(3) 0.0388(6) Uani 1.00 d . . . C(44) C 0.1032(3) 0.5020(2) -0.0731(3) 0.0434(7) Uani 1.00 d . . . C(45) C -0.2473(3) 0.6011(2) -0.3995(4) 0.0524(9) Uani 1.00 d . . . C(51) C -0.2551(2) 0.3614(1) -0.1241(3) 0.0348(6) Uani 1.00 d . . . C(52) C -0.3643(3) 0.3857(2) -0.1562(3) 0.0420(7) Uani 1.00 d . . . C(53) C -0.3890(3) 0.4245(2) -0.2509(3) 0.0393(6) Uani 1.00 d . . . C(54) C -0.1858(3) 0.3196(2) -0.0241(3) 0.0428(7) Uani 1.00 d . . . C(55) C -0.4950(3) 0.4622(2) -0.3204(4) 0.0548(9) Uani 1.00 d . . . C(61) C -0.2793(3) 0.4054(2) -0.6563(3) 0.0489(8) Uani 1.00 d . . . C(62) C -0.3272(3) 0.3525(2) -0.6440(3) 0.0523(8) Uani 1.00 d . . . C(63) C -0.3280(3) 0.3606(2) -0.5311(3) 0.0462(7) Uani 1.00 d . . . C(64) C -0.2551(4) 0.4218(3) -0.7603(4) 0.072(1) Uani 1.00 d . . . C(65) C -0.3707(5) 0.3176(2) -0.4711(4) 0.071(1) Uani 1.00 d . . . C(71) C 0.3688(5) 0.2705(3) 0.5949(5) 0.084(1) Uani 1.00 d . . . C(72) C 0.3277(5) 0.3022(3) 0.6740(5) 0.086(2) Uani 1.00 d . . . C(73) C 0.4978(5) 0.1803(3) 0.2741(5) 0.086(2) Uani 1.00 d . . . C(74) C 0.4097(5) 0.2271(3) 0.2479(5) 0.082(1) Uani 1.00 d . . . C(75) C -0.2762(4) 0.1592(2) -0.3224(5) 0.066(1) Uani 1.00 d . . . C(76) C -0.3636(5) 0.1190(3) -0.4009(5) 0.088(2) Uani 1.00 d . . . C(77) C 0.9309(5) 0.0355(3) 0.7513(6) 0.091(2) Uani 1.00 d . . . C(78) C 1.0077(5) 0.0784(3) 0.7540(8) 0.118(3) Uani 1.00 d . . . C(79) C 1.072(1) 0.4621(5) 0.576(1) 0.079(3) Uani 0.50 d P . . C(80) C 1.129(1) 0.4265(5) 0.640(1) 0.096(4) Uani 0.50 d P . . B(1) B 0.3071(3) 0.1570(2) -0.1197(4) 0.0381(7) Uani 1.00 d . . . B(2) B -0.2832(3) 0.4599(2) -0.3706(3) 0.0362(7) Uani 1.00 d . . . H(1) H 0.3618 0.1230 -0.1151 0.0450 Uiso 1.00 calc . . . H(2) H 0.5462 0.3192 0.0569 0.0435 Uiso 1.00 calc . . . H(3) H 0.2647 0.3943 -0.0433 0.0561 Uiso 1.00 calc . . . H(4) H 0.4778 0.4310 0.0690 0.0696 Uiso 1.00 calc . . . H(5) H 0.3729 0.4786 0.0276 0.0696 Uiso 1.00 calc . . . H(6) H 0.3993 0.4346 -0.0697 0.0696 Uiso 1.00 calc . . . H(7) H 0.3804 0.3842 0.1981 0.0838 Uiso 1.00 calc . . . H(8) H 0.2594 0.3645 0.1185 0.0838 Uiso 1.00 calc . . . H(9) H 0.2860 0.4366 0.1373 0.0838 Uiso 1.00 calc . . . H(10) H 0.5433 0.1423 -0.0044 0.0462 Uiso 1.00 calc . . . H(11) H 0.6400 0.1489 -0.1251 0.0616 Uiso 1.00 calc . . . H(12) H 0.5921 0.2197 -0.1482 0.0616 Uiso 1.00 calc . . . H(13) H 0.5125 0.1636 -0.1977 0.0616 Uiso 1.00 calc . . . H(14) H 0.7306 0.1688 0.0913 0.0584 Uiso 1.00 calc . . . H(15) H 0.6645 0.1939 0.1689 0.0584 Uiso 1.00 calc . . . H(16) H 0.6891 0.2409 0.0917 0.0584 Uiso 1.00 calc . . . H(17) H 0.1911 0.0822 0.1516 0.0827 Uiso 1.00 calc . . . H(18) H 0.0085 0.2267 0.0246 0.0757 Uiso 1.00 calc . . . H(19) H 0.1578 0.2180 0.2632 0.1447 Uiso 1.00 calc . . . H(20) H 0.0476 0.2612 0.2235 0.1447 Uiso 1.00 calc . . . H(21) H 0.1386 0.2750 0.1807 0.1447 Uiso 1.00 calc . . . H(22) H -0.0764 0.1805 0.1229 0.1126 Uiso 1.00 calc . . . H(23) H 0.0193 0.1267 0.1627 0.1126 Uiso 1.00 calc . . . H(24) H -0.0604 0.1319 0.0246 0.1126 Uiso 1.00 calc . . . H(25) H 0.4137 0.0543 0.0408 0.1076 Uiso 1.00 calc . . . H(26) H 0.3310 -0.0103 0.1745 0.1213 Uiso 1.00 calc . . . H(27) H 0.4163 0.0424 0.2350 0.1213 Uiso 1.00 calc . . . H(28) H 0.4502 -0.0215 0.1786 0.1213 Uiso 1.00 calc . . . H(29) H 0.2378 -0.0270 -0.0472 0.1471 Uiso 1.00 calc . . . H(30) H 0.3540 -0.0454 -0.0483 0.1471 Uiso 1.00 calc . . . H(31) H 0.2751 0.0073 -0.1317 0.1471 Uiso 1.00 calc . . . H(32) H 0.0915 0.1354 -0.5330 0.0866 Uiso 1.00 calc . . . H(33) H -0.0476 0.2653 -0.3970 0.0728 Uiso 1.00 calc . . . H(34) H 0.0580 0.3102 -0.4796 0.1342 Uiso 1.00 calc . . . H(35) H -0.0700 0.3252 -0.5454 0.1342 Uiso 1.00 calc . . . H(36) H -0.0112 0.2733 -0.6031 0.1342 Uiso 1.00 calc . . . H(37) H -0.1908 0.2308 -0.5760 0.1166 Uiso 1.00 calc . . . H(38) H -0.1366 0.1728 -0.4940 0.1166 Uiso 1.00 calc . . . H(39) H -0.1089 0.1811 -0.6052 0.1166 Uiso 1.00 calc . . . H(40) H 0.3532 0.0694 -0.2836 0.1020 Uiso 1.00 calc . . . H(41) H 0.3855 0.0427 -0.4529 0.1123 Uiso 1.00 calc . . . H(42) H 0.3725 0.1172 -0.4347 0.1123 Uiso 1.00 calc . . . H(43) H 0.2747 0.0798 -0.5331 0.1123 Uiso 1.00 calc . . . H(44) H 0.2107 0.0029 -0.3266 0.1097 Uiso 1.00 calc . . . H(45) H 0.2839 -0.0257 -0.3944 0.1097 Uiso 1.00 calc . . . H(46) H 0.1701 0.0111 -0.4664 0.1097 Uiso 1.00 calc . . . H(47) H -0.3432 0.4907 -0.4015 0.0435 Uiso 1.00 calc . . . H(48) H -0.0228 0.6105 -0.2133 0.0483 Uiso 1.00 calc . . . H(49) H 0.1054 0.4624 -0.0385 0.0434 Uiso 1.00 calc . . . H(50) H 0.1166 0.5362 -0.0115 0.0434 Uiso 1.00 calc . . . H(51) H 0.1590 0.4997 -0.1040 0.0434 Uiso 1.00 calc . . . H(52) H -0.2171 0.6412 -0.3955 0.0524 Uiso 1.00 calc . . . H(53) H -0.3090 0.6080 -0.3777 0.0524 Uiso 1.00 calc . . . H(54) H -0.2716 0.5820 -0.4809 0.0524 Uiso 1.00 calc . . . H(55) H -0.4117 0.3765 -0.1200 0.0498 Uiso 1.00 calc . . . H(56) H -0.2097 0.3264 0.0408 0.0428 Uiso 1.00 calc . . . H(57) H -0.1098 0.3295 0.0059 0.0428 Uiso 1.00 calc . . . H(58) H -0.1930 0.2757 -0.0542 0.0428 Uiso 1.00 calc . . . H(59) H -0.4827 0.5070 -0.3065 0.0548 Uiso 1.00 calc . . . H(60) H -0.5500 0.4534 -0.2932 0.0548 Uiso 1.00 calc . . . H(61) H -0.5202 0.4505 -0.4058 0.0548 Uiso 1.00 calc . . . H(62) H -0.3554 0.3177 -0.7021 0.0626 Uiso 1.00 calc . . . H(63) H -0.1838 0.4029 -0.7507 0.0719 Uiso 1.00 calc . . . H(64) H -0.2554 0.4673 -0.7609 0.0719 Uiso 1.00 calc . . . H(65) H -0.3106 0.4056 -0.8357 0.0719 Uiso 1.00 calc . . . H(66) H -0.4363 0.3375 -0.4658 0.0712 Uiso 1.00 calc . . . H(67) H -0.3154 0.3099 -0.3907 0.0712 Uiso 1.00 calc . . . H(68) H -0.3876 0.2778 -0.5184 0.0712 Uiso 1.00 calc . . . H(69) H 0.3869 0.3102 0.7523 0.0862 Uiso 1.00 calc . . . H(70) H 0.2757 0.2765 0.6827 0.0862 Uiso 1.00 calc . . . H(71) H 0.2902 0.3421 0.6420 0.0862 Uiso 1.00 calc . . . H(72) H 0.4342 0.2672 0.2402 0.0821 Uiso 1.00 calc . . . H(73) H 0.3860 0.2313 0.3129 0.0821 Uiso 1.00 calc . . . H(74) H 0.3495 0.2148 0.1730 0.0821 Uiso 1.00 calc . . . H(75) H -0.4335 0.1383 -0.4067 0.0880 Uiso 1.00 calc . . . H(76) H -0.3513 0.0780 -0.3676 0.0880 Uiso 1.00 calc . . . H(77) H -0.3637 0.1140 -0.4806 0.0880 Uiso 1.00 calc . . . H(78) H 1.0799 0.0662 0.8139 0.1174 Uiso 1.00 calc . . . H(79) H 0.9856 0.1207 0.7743 0.1174 Uiso 1.00 calc . . . H(80) H 1.0095 0.0768 0.6753 0.1174 Uiso 1.00 calc . . . H(81) H 1.0894 0.4044 0.6723 0.0971 Uiso 0.50 calc P . . H(82) H 1.1871 0.4486 0.7057 0.0971 Uiso 0.50 calc P . . H(83) H 1.1619 0.3967 0.5978 0.0971 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) 0.0248(1) 0.0284(1) 0.0317(1) -0.00014(7) 0.01204(9) 0.00201(7) Co(1) 0.0268(2) 0.0291(2) 0.0399(2) 0.0012(1) 0.0149(2) 0.0030(1) O(1) 0.031(1) 0.037(1) 0.050(1) 0.0013(8) 0.0181(10) 0.0055(9) O(2) 0.029(1) 0.036(1) 0.051(1) 0.0012(8) 0.0176(10) 0.0048(9) N(11) 0.027(1) 0.032(1) 0.041(1) -0.0004(9) 0.014(1) 0.0009(9) N(12) 0.027(1) 0.033(1) 0.038(1) 0.0031(9) 0.014(1) 0.0025(9) N(21) 0.034(1) 0.034(1) 0.053(2) 0.0034(9) 0.020(1) 0.011(1) N(22) 0.035(1) 0.030(1) 0.063(2) 0.0044(9) 0.022(1) 0.011(1) N(31) 0.032(1) 0.036(1) 0.045(1) 0.0023(9) 0.014(1) -0.0052(10) N(32) 0.028(1) 0.041(1) 0.050(2) 0.0007(10) 0.013(1) -0.010(1) N(41) 0.027(1) 0.038(1) 0.030(1) -0.0018(9) 0.0099(10) 0.0004(9) N(42) 0.030(1) 0.033(1) 0.031(1) 0.0024(9) 0.0095(10) 0.0046(9) N(51) 0.029(1) 0.035(1) 0.031(1) -0.0014(9) 0.0128(10) 0.0019(9) N(52) 0.025(1) 0.040(1) 0.033(1) 0.0033(9) 0.0100(10) 0.0030(9) N(61) 0.040(2) 0.063(2) 0.035(1) -0.008(1) 0.017(1) 0.001(1) N(62) 0.034(1) 0.046(1) 0.031(1) -0.0059(10) 0.011(1) -0.0019(10) N(71) 0.157(6) 0.135(5) 0.117(5) 0.007(4) 0.081(5) 0.026(4) N(72) 0.111(5) 0.137(5) 0.141(6) 0.013(4) 0.039(4) 0.031(4) N(73) 0.074(3) 0.071(3) 0.125(4) -0.020(2) 0.039(3) -0.006(2) N(74) 0.159(7) 0.187(7) 0.168(7) -0.093(6) 0.012(5) 0.084(6) N(75) 0.087(6) 0.21(1) 0.101(7) -0.041(7) 0.047(5) -0.039(7) C(11) 0.031(1) 0.035(1) 0.037(2) -0.001(1) 0.013(1) 0.001(1) C(12) 0.030(1) 0.036(2) 0.038(2) -0.002(1) 0.012(1) 0.002(1) C(13) 0.029(1) 0.036(1) 0.035(1) 0.001(1) 0.014(1) 0.006(1) C(14) 0.033(2) 0.038(2) 0.062(2) -0.004(1) 0.016(2) -0.008(1) C(15) 0.073(3) 0.041(2) 0.095(4) -0.004(2) 0.036(3) 0.000(2) C(16) 0.141(5) 0.053(3) 0.081(3) 0.009(3) 0.073(4) -0.001(2) C(17) 0.028(1) 0.036(2) 0.053(2) 0.004(1) 0.018(1) 0.006(1) C(18) 0.058(2) 0.067(2) 0.068(3) 0.011(2) 0.038(2) 0.002(2) C(19) 0.032(2) 0.063(2) 0.071(3) 0.005(1) 0.014(2) 0.003(2) C(21) 0.042(2) 0.045(2) 0.075(3) 0.006(1) 0.029(2) 0.025(2) C(22) 0.060(2) 0.054(2) 0.109(4) 0.016(2) 0.048(3) 0.046(2) C(23) 0.050(2) 0.038(2) 0.104(3) 0.007(1) 0.038(2) 0.029(2) C(24) 0.062(3) 0.067(3) 0.084(3) 0.019(2) 0.049(2) 0.037(2) C(25) 0.112(6) 0.144(6) 0.197(9) -0.004(5) 0.099(6) -0.063(6) C(26) 0.102(5) 0.104(5) 0.182(8) -0.004(3) 0.108(5) 0.011(4) C(27) 0.084(3) 0.050(3) 0.164(6) 0.027(2) 0.080(4) 0.048(3) C(28) 0.096(5) 0.073(4) 0.158(7) 0.032(3) 0.016(4) 0.049(4) C(29) 0.184(9) 0.089(5) 0.150(7) 0.077(5) 0.065(6) 0.026(4) C(31) 0.038(2) 0.063(2) 0.045(2) 0.002(1) 0.011(2) -0.009(2) C(32) 0.053(2) 0.088(3) 0.053(2) 0.010(2) 0.012(2) -0.026(2) C(33) 0.044(2) 0.068(3) 0.060(2) 0.006(2) 0.016(2) -0.023(2) C(34) 0.043(2) 0.084(3) 0.044(2) 0.012(2) 0.008(2) -0.004(2) C(35) 0.077(4) 0.146(6) 0.168(8) 0.033(4) 0.035(5) 0.081(6) C(36) 0.048(3) 0.112(5) 0.138(6) 0.003(3) -0.009(3) 0.003(4) C(37) 0.061(3) 0.086(3) 0.074(3) 0.019(2) 0.015(2) -0.036(2) C(38) 0.078(4) 0.101(4) 0.175(7) -0.015(3) 0.082(5) -0.058(4) C(39) 0.129(6) 0.073(4) 0.133(6) 0.028(3) 0.070(5) -0.003(3) C(41) 0.034(1) 0.034(1) 0.038(2) -0.006(1) 0.017(1) -0.003(1) C(42) 0.041(2) 0.033(2) 0.044(2) -0.005(1) 0.015(1) 0.003(1) C(43) 0.044(2) 0.035(2) 0.039(2) 0.000(1) 0.018(1) 0.005(1) C(44) 0.036(2) 0.040(2) 0.048(2) -0.006(1) 0.010(1) -0.001(1) C(45) 0.055(2) 0.040(2) 0.051(2) 0.003(1) 0.009(2) 0.013(1) C(51) 0.032(1) 0.041(2) 0.036(2) -0.006(1) 0.019(1) -0.001(1) C(52) 0.033(2) 0.049(2) 0.047(2) -0.003(1) 0.021(1) 0.002(1) C(53) 0.028(1) 0.046(2) 0.041(2) -0.003(1) 0.013(1) 0.001(1) C(54) 0.043(2) 0.048(2) 0.042(2) 0.003(1) 0.022(1) 0.012(1) C(55) 0.028(2) 0.073(2) 0.062(2) 0.008(1) 0.016(2) 0.013(2) C(61) 0.039(2) 0.069(2) 0.036(2) 0.001(1) 0.015(1) -0.002(1) C(62) 0.048(2) 0.060(2) 0.040(2) -0.005(2) 0.012(2) -0.008(1) C(63) 0.047(2) 0.047(2) 0.036(2) -0.009(1) 0.010(1) -0.005(1) C(64) 0.069(3) 0.107(4) 0.045(2) -0.011(2) 0.030(2) -0.007(2) C(65) 0.103(4) 0.059(3) 0.050(2) -0.038(2) 0.026(2) -0.012(2) C(71) 0.087(4) 0.095(4) 0.077(3) -0.003(3) 0.037(3) 0.031(3) C(72) 0.082(4) 0.115(4) 0.063(3) -0.009(3) 0.029(3) 0.030(3) C(73) 0.085(4) 0.093(4) 0.075(4) -0.013(3) 0.024(3) 0.017(3) C(74) 0.078(3) 0.103(4) 0.057(3) 0.000(3) 0.020(3) 0.014(2) C(75) 0.062(3) 0.061(3) 0.082(3) -0.007(2) 0.037(2) -0.001(2) C(76) 0.084(4) 0.100(4) 0.080(4) -0.023(3) 0.035(3) -0.020(3) C(77) 0.088(4) 0.084(4) 0.083(4) -0.026(3) 0.011(3) 0.015(3) C(78) 0.076(4) 0.084(4) 0.198(8) -0.023(3) 0.063(5) -0.016(4) C(79) 0.117(10) 0.063(6) 0.093(8) -0.014(6) 0.077(8) 0.002(5) C(80) 0.17(1) 0.051(6) 0.112(9) 0.009(6) 0.108(10) 0.027(5) B(1) 0.030(2) 0.029(2) 0.054(2) -0.001(1) 0.016(2) 0.000(1) B(2) 0.031(2) 0.041(2) 0.036(2) 0.001(1) 0.014(1) 0.005(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _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) O(1) 2.006(2) . . yes Pd(1) O(2) 2.004(3) . . yes Pd(1) N(41) 2.001(2) . . yes Pd(1) N(51) 2.011(3) . . yes Co(1) O(1) 2.011(3) . . yes Co(1) O(2) 2.019(2) . . yes Co(1) N(11) 2.140(2) . . yes Co(1) N(21) 2.141(3) . . yes Co(1) N(31) 2.073(3) . . yes N(11) N(12) 1.381(3) . . yes N(11) C(11) 1.345(4) . . yes N(12) C(13) 1.350(4) . . yes N(12) B(1) 1.551(4) . . yes N(21) N(22) 1.375(4) . . yes N(21) C(21) 1.328(6) . . yes N(22) C(23) 1.367(6) . . yes N(22) B(1) 1.547(6) . . yes N(31) N(32) 1.379(4) . . yes N(31) C(31) 1.334(4) . . yes N(32) C(33) 1.351(6) . . yes N(32) B(1) 1.538(4) . . yes N(41) N(42) 1.370(3) . . yes N(41) C(41) 1.356(4) . . yes N(42) C(43) 1.346(4) . . yes N(42) B(2) 1.549(4) . . yes N(51) N(52) 1.374(3) . . yes N(51) C(51) 1.339(5) . . yes N(52) C(53) 1.348(5) . . yes N(52) B(2) 1.539(5) . . yes N(61) N(62) 1.378(5) . . yes N(61) C(61) 1.327(4) . . yes N(62) C(63) 1.354(4) . . yes N(62) B(2) 1.541(5) . . yes N(71) C(71) 1.17(1) . . yes N(72) C(73) 1.148(9) . . yes N(73) C(75) 1.119(6) . . yes N(74) C(77) 1.13(1) . . yes N(75) C(79) 1.29(1) . . yes N(75) C(79) 1.29(1) . 2_766 yes C(11) C(12) 1.395(4) . . yes C(11) C(14) 1.497(4) . . yes C(12) C(13) 1.379(4) . . yes C(13) C(17) 1.513(4) . . yes C(14) C(15) 1.482(7) . . yes C(14) C(16) 1.430(8) . . yes C(17) C(18) 1.516(7) . . yes C(17) C(19) 1.526(4) . . yes C(21) C(22) 1.398(5) . . yes C(21) C(24) 1.498(7) . . yes C(22) C(23) 1.354(9) . . yes C(23) C(27) 1.511(7) . . yes C(24) C(25) 1.501(9) . . yes C(24) C(26) 1.477(10) . . yes C(27) C(28) 1.53(1) . . yes C(27) C(29) 1.524(9) . . yes C(31) C(32) 1.396(7) . . yes C(31) C(34) 1.496(5) . . yes C(32) C(33) 1.365(5) . . yes C(33) C(37) 1.528(7) . . yes C(34) C(35) 1.49(1) . . yes C(34) C(36) 1.507(7) . . yes C(37) C(38) 1.49(1) . . yes C(37) C(39) 1.515(8) . . yes C(41) C(42) 1.396(4) . . yes C(41) C(44) 1.473(4) . . yes C(42) C(43) 1.370(4) . . yes C(43) C(45) 1.500(4) . . yes C(51) C(52) 1.399(4) . . yes C(51) C(54) 1.485(4) . . yes C(52) C(53) 1.378(5) . . yes C(53) C(55) 1.502(4) . . yes C(61) C(62) 1.387(6) . . yes C(61) C(64) 1.502(7) . . yes C(62) C(63) 1.367(6) . . yes C(63) C(65) 1.500(7) . . yes C(71) C(72) 1.386(10) . . yes C(73) C(74) 1.408(8) . . yes C(75) C(76) 1.445(7) . . yes C(77) C(78) 1.42(1) . . yes C(79) C(80) 1.11(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 O(1) Pd(1) O(2) 77.6(1) . . . yes O(1) Pd(1) N(41) 173.96(10) . . . yes O(1) Pd(1) N(51) 97.6(1) . . . yes O(2) Pd(1) N(41) 96.9(1) . . . yes O(2) Pd(1) N(51) 175.11(10) . . . yes N(41) Pd(1) N(51) 87.8(1) . . . yes O(1) Co(1) O(2) 77.17(10) . . . yes O(1) Co(1) N(11) 159.31(10) . . . yes O(1) Co(1) N(21) 97.3(1) . . . yes O(1) Co(1) N(31) 111.01(10) . . . yes O(2) Co(1) N(11) 94.25(9) . . . yes O(2) Co(1) N(21) 160.2(1) . . . yes O(2) Co(1) N(31) 110.9(1) . . . yes N(11) Co(1) N(21) 84.4(1) . . . yes N(11) Co(1) N(31) 89.6(1) . . . yes N(21) Co(1) N(31) 88.8(1) . . . yes Pd(1) O(1) Co(1) 102.6(1) . . . yes Pd(1) O(2) Co(1) 102.4(1) . . . yes Co(1) N(11) N(12) 116.4(2) . . . yes Co(1) N(11) C(11) 137.5(2) . . . yes N(12) N(11) C(11) 106.1(2) . . . yes N(11) N(12) C(13) 110.1(2) . . . yes N(11) N(12) B(1) 119.1(2) . . . yes C(13) N(12) B(1) 130.6(2) . . . yes Co(1) N(21) N(22) 116.4(3) . . . yes Co(1) N(21) C(21) 136.9(2) . . . yes N(22) N(21) C(21) 106.7(3) . . . yes N(21) N(22) C(23) 108.9(4) . . . yes N(21) N(22) B(1) 119.4(3) . . . yes C(23) N(22) B(1) 131.5(3) . . . yes Co(1) N(31) N(32) 118.3(2) . . . yes Co(1) N(31) C(31) 134.3(2) . . . yes N(32) N(31) C(31) 107.4(3) . . . yes N(31) N(32) C(33) 108.7(3) . . . yes N(31) N(32) B(1) 118.8(3) . . . yes C(33) N(32) B(1) 132.4(3) . . . yes Pd(1) N(41) N(42) 121.9(2) . . . yes Pd(1) N(41) C(41) 130.2(2) . . . yes N(42) N(41) C(41) 107.8(2) . . . yes N(41) N(42) C(43) 108.9(2) . . . yes N(41) N(42) B(2) 121.8(2) . . . yes C(43) N(42) B(2) 128.8(2) . . . yes Pd(1) N(51) N(52) 121.6(2) . . . yes Pd(1) N(51) C(51) 130.2(2) . . . yes N(52) N(51) C(51) 107.9(3) . . . yes N(51) N(52) C(53) 108.8(3) . . . yes N(51) N(52) B(2) 122.4(3) . . . yes C(53) N(52) B(2) 128.8(2) . . . yes N(62) N(61) C(61) 105.5(3) . . . yes N(61) N(62) C(63) 110.1(3) . . . yes N(61) N(62) B(2) 114.8(3) . . . yes C(63) N(62) B(2) 132.5(3) . . . yes C(79) N(75) C(79) 180.0 . . 2_766 yes N(11) C(11) C(12) 109.9(2) . . . yes N(11) C(11) C(14) 122.5(3) . . . yes C(12) C(11) C(14) 127.5(3) . . . yes C(11) C(12) C(13) 106.2(3) . . . yes N(12) C(13) C(12) 107.7(3) . . . yes N(12) C(13) C(17) 123.6(2) . . . yes C(12) C(13) C(17) 128.7(3) . . . yes C(11) C(14) C(15) 113.4(4) . . . yes C(11) C(14) C(16) 114.7(3) . . . yes C(15) C(14) C(16) 115.9(4) . . . yes C(13) C(17) C(18) 110.4(3) . . . yes C(13) C(17) C(19) 110.9(3) . . . yes C(18) C(17) C(19) 110.8(4) . . . yes N(21) C(21) C(22) 110.1(4) . . . yes N(21) C(21) C(24) 122.9(3) . . . yes C(22) C(21) C(24) 126.9(5) . . . yes C(21) C(22) C(23) 106.1(5) . . . yes N(22) C(23) C(22) 108.2(3) . . . yes N(22) C(23) C(27) 122.0(5) . . . yes C(22) C(23) C(27) 129.8(5) . . . yes C(21) C(24) C(25) 111.9(5) . . . yes C(21) C(24) C(26) 113.0(4) . . . yes C(25) C(24) C(26) 111.9(7) . . . yes C(23) C(27) C(28) 111.4(6) . . . yes C(23) C(27) C(29) 109.9(5) . . . yes C(28) C(27) C(29) 109.0(5) . . . yes N(31) C(31) C(32) 109.1(3) . . . yes N(31) C(31) C(34) 122.1(4) . . . yes C(32) C(31) C(34) 128.8(3) . . . yes C(31) C(32) C(33) 106.4(4) . . . yes N(32) C(33) C(32) 108.4(4) . . . yes N(32) C(33) C(37) 123.5(3) . . . yes C(32) C(33) C(37) 128.0(4) . . . yes C(31) C(34) C(35) 111.3(5) . . . yes C(31) C(34) C(36) 111.4(4) . . . yes C(35) C(34) C(36) 111.5(5) . . . yes C(33) C(37) C(38) 111.6(5) . . . yes C(33) C(37) C(39) 110.6(5) . . . yes C(38) C(37) C(39) 109.5(5) . . . yes N(41) C(41) C(42) 107.8(2) . . . yes N(41) C(41) C(44) 122.9(3) . . . yes C(42) C(41) C(44) 129.2(3) . . . yes C(41) C(42) C(43) 106.9(3) . . . yes N(42) C(43) C(42) 108.5(2) . . . yes N(42) C(43) C(45) 122.7(3) . . . yes C(42) C(43) C(45) 128.9(3) . . . yes N(51) C(51) C(52) 108.6(3) . . . yes N(51) C(51) C(54) 122.6(3) . . . yes C(52) C(51) C(54) 128.8(4) . . . yes C(51) C(52) C(53) 106.3(4) . . . yes N(52) C(53) C(52) 108.3(3) . . . yes N(52) C(53) C(55) 122.9(3) . . . yes C(52) C(53) C(55) 128.8(4) . . . yes N(61) C(61) C(62) 111.1(4) . . . yes N(61) C(61) C(64) 119.2(4) . . . yes C(62) C(61) C(64) 129.7(4) . . . yes C(61) C(62) C(63) 105.9(3) . . . yes N(62) C(63) C(62) 107.4(4) . . . yes N(62) C(63) C(65) 124.2(3) . . . yes C(62) C(63) C(65) 128.4(3) . . . yes N(71) C(71) C(72) 178.0(6) . . . yes N(72) C(73) C(74) 179.4(6) . . . yes N(73) C(75) C(76) 179.8(7) . . . yes N(74) C(77) C(78) 177.2(7) . . . yes N(75) C(79) C(80) 174(1) . . . yes N(12) B(1) N(22) 108.4(3) . . . yes N(12) B(1) N(32) 110.5(3) . . . yes N(22) B(1) N(32) 109.9(3) . . . yes N(42) B(2) N(52) 109.2(2) . . . yes N(42) B(2) N(62) 110.3(3) . . . yes N(52) B(2) N(62) 113.0(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . yes ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(2) C(80) 2.91(2) . 1_454 ? N(11) C(72) 3.451(8) . 1_554 ? N(12) C(72) 3.519(7) . 1_554 ? N(21) C(78) 3.423(7) . 1_454 ? N(22) C(78) 3.447(7) . 1_454 ? N(31) C(78) 3.494(8) . 1_454 ? N(32) C(78) 3.538(9) . 1_454 ? N(61) C(79) 3.32(2) . 2_665 ? N(61) N(75) 3.423(3) . 1_454 ? N(61) C(55) 3.554(4) . 2_464 ? N(71) C(65) 3.52(1) . 1_656 ? N(72) C(76) 3.48(1) . 1_656 ? N(73) C(78) 3.504(9) . 1_454 ? N(73) C(77) 3.585(7) . 1_454 ? N(74) C(22) 3.54(1) . 2_656 ? C(18) C(75) 3.562(9) . 1_655 ? C(35) C(80) 3.52(1) . 1_454 ? C(45) C(71) 3.562(7) . 2_565 ? C(64) C(79) 3.53(1) . 2_665 ? C(72) C(80) 3.47(1) . 1_455 ? C(75) C(77) 3.497(7) . 1_454 ? Pd(1) N(42) 2.963(2) . . ? Pd(1) N(52) 2.971(3) . . ? Pd(1) Co(1) 3.1350(5) . . ? Co(1) N(32) 2.985(3) . . ? Co(1) N(22) 3.015(3) . . ? Co(1) N(12) 3.020(3) . . ? O(1) O(2) 2.513(4) . . ? O(1) N(51) 3.023(3) . . ? O(1) N(21) 3.119(3) . . ? O(1) N(31) 3.366(4) . . ? O(2) N(41) 2.996(3) . . ? O(2) N(11) 3.049(3) . . ? O(2) N(31) 3.371(3) . . ? N(11) N(21) 2.875(4) . . ? N(11) N(31) 2.969(3) . . ? N(11) N(22) 3.015(4) . . ? N(11) N(32) 3.088(3) . . ? N(12) N(22) 2.512(4) . . ? N(12) N(32) 2.538(3) . . ? N(12) N(21) 3.026(4) . . ? N(12) N(31) 3.057(3) . . ? N(21) N(31) 2.949(4) . . ? N(21) N(32) 3.070(5) . . ? N(22) N(32) 2.526(5) . . ? N(22) N(31) 3.044(4) . . ? N(41) N(51) 2.782(4) . . ? N(41) N(52) 2.945(4) . . ? N(42) N(52) 2.517(4) . . ? N(42) N(61) 2.886(4) . . ? N(42) N(51) 3.012(4) . . ? #------------------------------------------------------------------------------ #===END