Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_ncw2 _database_code_CSD 169728 #--------------------------------------------------------------------------- #-- _audit_creation_date '1999-10-19' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 2001-07-31 passes checkcif with warnings - see refine_special_details ; #--------------------------------------------------------------------------- _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address ' Justine Bennett' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Geoffrey Salem ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Natalie C. Ward ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Paul Waring ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Kerri Wells ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_requested_journal 'J. Chem. Soc., Dalton ' _publ_requested_category ' FM ' _publ_contact_author_name 'Dr Geoffrey Salem' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email 'GEOFF.SALEM@ANU.EDU.AU' _publ_section_title ; Synthesis of bis[palladium(II)] and bis[platinum(II)] complexes containing chiral, linear quadridentate ligands with a P2N2 donor set ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation (1991-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C. & Guagliardi, A. Burla, M.C., Polidori, G. and Camalli, M. (1994). SIR92. J. Appl. Crystallogr., 27, 435. DIRDIF94: Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., de Gelder, R., Israel, R. and Smits, J.M.M.(1994). The DIRDIF-94 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Molecular Structure Corporation (1991-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rae, A. D. (1996). RAELS96: A Comprehensive Constrained Least-Square Refinement Program. Australian National University, Canberra, A. C. T., Australia. Rae, A. D. (1975). Acta Crystallogr., Section A, A31, 560-570, 570-574. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #--------------------------------------------------------------------------- #-- _cell_length_a 17.622(4) _cell_length_b 21.207(3) _cell_length_c 16.001(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5980(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 46.5 _cell_measurement_theta_max 51.5 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2 ' _symmetry_Int_Tables_number 18 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, +z' '1/2+x,1/2-y, -z' '1/2-x,1/2+y, -z' #--------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1274.07 _chemical_formula_analytical ? _chemical_formula_sum 'C51.5 H65 Cl0.5 F9 N4 O1.5 P3.5 Pd2 ' _chemical_formula_moiety 'C47 H56 N4 P2 Pd2 2+, 0.5(Cl -), 1.5( F6 P -), 1.5(C3 H6 O) ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 6.51 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max .458 _exptl_absorpt_correction_T_min .256 _exptl_special_details ; The scan width was (1.20+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.48 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 2 4 2 2 -4 4 -2 0 _diffrn_reflns_number 9587 _reflns_number_total 8883 _reflns_number_gt 7442 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06617 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 60.11 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03378 _diffrn_orient_matrix_UB_12 0.02923 _diffrn_orient_matrix_UB_13 0.03195 _diffrn_orient_matrix_UB_21 -0.02436 _diffrn_orient_matrix_UB_22 0.03693 _diffrn_orient_matrix_UB_23 -0.02812 _diffrn_orient_matrix_UB_31 -0.03855 _diffrn_orient_matrix_UB_32 0.00228 _diffrn_orient_matrix_UB_33 0.04576 #--------------------------------------------------------------------------- #-- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 206 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 260 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 2 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 36 0.069 0.053 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 16 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 6 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 14 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 8 -0.059 3.934 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom PD1 0.62877(3) 0.16833(3) 0.39242(4) 0.0371(2) 1.0 . Uani d ? PD1' 0.39099(3) 0.18173(3) 0.10105(4) 0.0371(2) 1.0 . Uani d ? P1 0.6599(1) 0.2411(1) 0.3000(1) 0.044(1) 1.0 . Uani d ? C1 0.5850(6) 0.2949(4) 0.2679(7) 0.058(2) 1.0 . Uani d ? C2 0.5135(5) 0.2589(5) 0.2468(7) 0.053(3) 1.0 . Uani d ? C1' 0.4465(6) 0.3010(4) 0.2279(7) 0.058(2) 1.0 . Uani d ? P1' 0.3646(1) 0.2552(1) 0.1943(1) 0.044(1) 1.0 . Uani d ? N1 0.6499(4) 0.1017(3) 0.2931(4) 0.047(2) 1.0 . Uani d ? C3 0.6753(3) 0.1284(4) 0.2155(5) 0.049(2) 1.0 . Uani d ? C4 0.6935(4) 0.0926(5) 0.1462(6) 0.070(3) 1.0 . Uani d ? C5 0.7174(5) 0.1173(7) 0.0730(6) 0.082(3) 1.0 . Uani d ? C6 0.7246(4) 0.1829(7) 0.0655(6) 0.079(3) 1.0 . Uani d ? C7 0.7070(4) 0.2227(5) 0.1335(5) 0.066(2) 1.0 . Uani d ? C8 0.6825(4) 0.1952(4) 0.2082(5) 0.048(2) 1.0 . Uani d ? N1' 0.3674(4) 0.1160(3) 0.2007(4) 0.047(2) 1.0 . Uani d ? C3' 0.3422(3) 0.1433(4) 0.2779(5) 0.049(2) 1.0 . Uani d ? C4' 0.3214(4) 0.1080(5) 0.3468(6) 0.070(3) 1.0 . Uani d ? C5' 0.2977(5) 0.1332(7) 0.4197(6) 0.082(3) 1.0 . Uani d ? C6' 0.2933(4) 0.1990(6) 0.4274(6) 0.079(3) 1.0 . Uani d ? C7' 0.3135(4) 0.2384(5) 0.3598(6) 0.066(2) 1.0 . Uani d ? C8' 0.3378(4) 0.2103(4) 0.2854(5) 0.049(2) 1.0 . Uani d ? C9 0.7435(4) 0.2891(3) 0.3208(2) 0.057(1) 1.0 . Uani d ? C10 0.8075(4) 0.2571(5) 0.3453(5) 0.078(2) 1.0 . Uani d ? C11 0.8732(4) 0.2913(7) 0.3621(5) 0.112(3) 1.0 . Uani d ? C12 0.8723(6) 0.3556(6) 0.3539(4) 0.126(3) 1.0 . Uani d ? C13 0.8083(8) 0.3873(5) 0.3294(6) 0.123(1) 1.0 . Uani d ? C14 0.7423(6) 0.3535(4) 0.3125(5) 0.087(1) 1.0 . Uani d ? C9' 0.2870(4) 0.3107(3) 0.1789(2) 0.059(1) 1.0 . Uani d ? C10' 0.2166(4) 0.2848(5) 0.1654(4) 0.079(2) 1.0 . Uani d ? C11' 0.1551(5) 0.3249(7) 0.1532(5) 0.115(3) 1.0 . Uani d ? C12' 0.1662(6) 0.3889(5) 0.1549(4) 0.133(2) 1.0 . Uani d ? C13' 0.2366(8) 0.4145(5) 0.1684(6) 0.130(2) 1.0 . Uani d ? C14' 0.2984(6) 0.3747(4) 0.1807(5) 0.091(1) 1.0 . Uani d ? C15 0.6112(4) 0.2266(4) 0.4893(5) 0.045(1) 1.0 . Uani d ? C16 0.6011(4) 0.2925(4) 0.4889(6) 0.060(1) 1.0 . Uani d ? C17 0.5853(5) 0.3235(5) 0.5635(7) 0.080(2) 1.0 . Uani d ? C18 0.5791(5) 0.2924(6) 0.6376(7) 0.086(2) 1.0 . Uani d ? C19 0.5894(4) 0.2244(6) 0.6390(6) 0.073(2) 1.0 . Uani d ? C20 0.6049(3) 0.1945(4) 0.5656(5) 0.054(1) 1.0 . Uani d ? C21 0.6158(5) 0.1234(4) 0.5654(6) 0.061(3) 1.0 . Uani d ? N2 0.5941(4) 0.0991(3) 0.4822(4) 0.052(3) 1.0 . Uani d ? C22 0.7011(7) 0.1103(6) 0.5827(8) 0.083(4) 1.0 . Uani d ? C23 0.6211(7) 0.0345(5) 0.4681(7) 0.070(4) 1.0 . Uani d ? C24 0.5108(6) 0.0983(6) 0.4801(8) 0.071(4) 1.0 . Uani d ? C15' 0.4094(3) 0.2394(4) 0.0038(5) 0.045(1) 1.0 . Uani d ? C16' 0.4184(4) 0.3054(4) 0.0029(6) 0.060(1) 1.0 . Uani d ? C17' 0.4320(5) 0.3358(5) -0.0726(7) 0.080(2) 1.0 . Uani d ? C18' 0.4369(5) 0.3041(6) -0.1464(7) 0.086(2) 1.0 . Uani d ? C19' 0.4277(4) 0.2360(6) -0.1464(6) 0.073(2) 1.0 . Uani d ? C20' 0.4144(3) 0.2066(4) -0.0721(5) 0.054(1) 1.0 . Uani d ? C21' 0.4045(5) 0.1354(4) -0.0705(6) 0.061(3) 1.0 . Uani d ? N2' 0.4289(4) 0.1123(3) 0.0130(4) 0.053(3) 1.0 . Uani d ? C22' 0.3195(7) 0.1225(6) -0.0900(8) 0.084(4) 1.0 . Uani d ? C23' 0.4027(7) 0.0472(5) 0.0277(7) 0.070(3) 1.0 . Uani d ? C24' 0.5120(6) 0.1141(6) 0.0183(8) 0.072(4) 1.0 . Uani d ? CL1 0.5000(0) 0.0000(0) 0.2496(2) 0.047(1) 1.0 . Uani d ? P2 0.4954(3) 0.0075(2) 0.7481(2) 0.036(2) 0.5 . Uani d ? F21 0.5225(5) 0.0039(4) 0.8423(3) 0.075(2) 0.5 . Uani d ? F22 0.4878(4) -0.0669(3) 0.7458(4) 0.051(2) 0.5 . Uani d ? F23 0.5807(4) 0.0020(3) 0.7179(5) 0.082(4) 0.5 . Uani d ? F24 0.4683(5) 0.0110(3) 0.6539(3) 0.086(3) 0.5 . Uani d ? F25 0.5031(4) 0.0818(3) 0.7503(4) 0.052(2) 0.5 . Uani d ? F26 0.4101(4) 0.0130(3) 0.7782(5) 0.080(4) 0.5 . Uani d ? P3 0.1396(9) -0.0276(8) 0.3168(12) 0.433(9) 0.5 . Uani d ? F31 0.2099(9) -0.0539(9) 0.3675(14) 0.185(6) 0.5 . Uani d ? F32 0.0881(11) -0.0819(10) 0.3539(23) 0.719(21) 0.5 . Uani d ? F33 0.1612(18) -0.0714(17) 0.2404(14) 1.258(27) 0.5 . Uani d ? F34 0.0693(16) -0.0012(16) 0.2662(21) 1.717(52) 0.5 . Uani d ? F35 0.1911(17) 0.0268(13) 0.2798(22) 1.094(47) 0.5 . Uani d ? F36 0.1180(13) 0.0163(10) 0.3933(19) 0.732(29) 0.5 . Uani d ? P3' 0.1313(6) -0.0399(5) 0.3553(13) 0.292(7) 0.5 . Uani d ? F31' 0.1731(15) -0.1044(10) 0.3746(32) 0.582(21) 0.5 . Uani d ? F32' 0.0579(12) -0.0650(11) 0.4017(28) 0.817(40) 0.5 . Uani d ? F33' 0.1008(23) -0.0681(25) 0.2701(20) 1.252(21) 0.5 . Uani d ? F34' 0.0895(15) 0.0245(12) 0.3361(34) 1.036(45) 0.5 . Uani d ? F35' 0.2047(12) -0.0149(11) 0.3090(23) 0.361(12) 0.5 . Uani d ? F36' 0.1618(23) -0.0118(23) 0.4406(17) 0.809(21) 0.5 . Uani d ? O1 -0.2327(8) 0.9375(6) 0.1098(11) 0.177(6) 1.0 . Uani d ? C25 -0.1638(10) 0.9309(6) 0.1013(11) 0.252(10) 1.0 . Uani d ? C26 -0.1267(14) 0.9791(12) 0.0632(26) 0.370(22) 1.0 . Uani d ? C27 -0.1341(14) 0.8762(13) 0.1311(31) 0.485(27) 1.0 . Uani d ? O2 0.4196(12) 0.5289(10) 0.1387(17) 0.167(23) 0.5 . Uani d ? C28 0.4813(13) 0.5045(7) 0.1541(11) 0.117(18) 0.5 . Uani d ? C29 0.4944(20) 0.4476(10) 0.1177(22) 0.204(31) 0.5 . Uani d ? C30 0.5280(18) 0.5376(13) 0.2053(20) 0.162(23) 0.5 . Uani d ? H1C1 0.6021 0.3189 0.2176 0.058 1.0 . Uani c ? H2C1 0.5741 0.3249 0.3145 0.058 1.0 . Uani c ? H1C2 0.5002 0.2314 0.2954 0.053 1.0 . Uani c ? H2C2 0.5237 0.2321 0.1967 0.053 1.0 . Uani c ? H1C1' 0.4608 0.3311 0.1825 0.058 1.0 . Uani c ? H2C1' 0.4328 0.3252 0.2794 0.058 1.0 . Uani c ? H1N1 0.6017 0.0784 0.2820 0.053 1.0 . Uani c ? H2N1 0.6897 0.0715 0.3128 0.060 1.0 . Uani c ? H1C4 0.6887 0.0458 0.1505 0.086 1.0 . Uani c ? H1C5 0.7298 0.0891 0.0248 0.105 1.0 . Uani c ? H1C6 0.7422 0.2016 0.0115 0.098 1.0 . Uani c ? H1C7 0.7120 0.2695 0.1284 0.080 1.0 . Uani c ? H1N1' 0.4150 0.0918 0.2123 0.053 1.0 . Uani c ? H2N1' 0.3271 0.0864 0.1808 0.060 1.0 . Uani c ? H1C4' 0.3242 0.0610 0.3425 0.086 1.0 . Uani c ? H1C5' 0.2833 0.1054 0.4676 0.105 1.0 . Uani c ? H1C6' 0.2757 0.2182 0.4811 0.098 1.0 . Uani c ? H1C7' 0.3104 0.2853 0.3650 0.080 1.0 . Uani c ? H1C10 0.8070 0.2102 0.3510 0.094 1.0 . Uani c ? H1C11 0.9206 0.2692 0.3800 0.150 1.0 . Uani c ? H1C12 0.9196 0.3801 0.3660 0.165 1.0 . Uani c ? H1C13 0.8089 0.4343 0.3238 0.172 1.0 . Uani c ? H1C14 0.6950 0.3757 0.2946 0.108 1.0 . Uani c ? H1C10' 0.2097 0.2380 0.1643 0.094 1.0 . Uani c ? H1C11' 0.1032 0.3073 0.1432 0.153 1.0 . Uani c ? H1C12' 0.1219 0.4176 0.1461 0.176 1.0 . Uani c ? H1C13' 0.2434 0.4613 0.1695 0.182 1.0 . Uani c ? H1C14' 0.3502 0.3925 0.1907 0.111 1.0 . Uani c ? H1C16 0.6053 0.3168 0.4355 0.065 1.0 . Uani c ? H1C17 0.5782 0.3703 0.5626 0.100 1.0 . Uani c ? H1C18 0.5677 0.3160 0.6903 0.109 1.0 . Uani c ? H1C19 0.5852 0.2002 0.6924 0.088 1.0 . Uani c ? H1C21 0.5838 0.1035 0.6097 0.082 1.0 . Uani c ? H1C22 0.7149 0.1270 0.6391 0.104 1.0 . Uani c ? H2C22 0.7106 0.0638 0.5810 0.105 1.0 . Uani c ? H3C22 0.7327 0.1316 0.5391 0.078 1.0 . Uani c ? H1C23 0.6779 0.0339 0.4693 0.082 1.0 . Uani c ? H2C23 0.6010 0.0062 0.5130 0.090 1.0 . Uani c ? H3C23 0.6029 0.0193 0.4124 0.073 1.0 . Uani c ? H1C24 0.4911 0.1419 0.4896 0.078 1.0 . Uani c ? H2C24 0.4933 0.0828 0.4244 0.080 1.0 . Uani c ? H3C24 0.4913 0.0697 0.5249 0.090 1.0 . Uani c ? H1C16' 0.4151 0.3301 0.0560 0.065 1.0 . Uani c ? H1C17' 0.4383 0.3827 -0.0727 0.099 1.0 . Uani c ? H1C18' 0.4467 0.3273 -0.1998 0.108 1.0 . Uani c ? H1C19' 0.4309 0.2113 -0.1996 0.088 1.0 . Uani c ? H1C21' 0.4370 0.1159 -0.1147 0.081 1.0 . Uani c ? H1C22' 0.3070 0.1391 -0.1468 0.105 1.0 . Uani c ? H2C22' 0.3099 0.0760 -0.0884 0.106 1.0 . Uani c ? H3C22' 0.2871 0.1439 -0.0474 0.078 1.0 . Uani c ? H1C23' 0.3460 0.0457 0.0242 0.081 1.0 . Uani c ? H2C23' 0.4249 0.0187 -0.0156 0.089 1.0 . Uani c ? H3C23' 0.4193 0.0331 0.0844 0.073 1.0 . Uani c ? H1C24' 0.5301 0.1581 0.0084 0.078 1.0 . Uani c ? H2C24' 0.5284 0.0998 0.0750 0.081 1.0 . Uani c ? H3C24' 0.5341 0.0854 -0.0250 0.091 1.0 . Uani c ? 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 PD1 0.0359(3) 0.0409(2) 0.0345(3) -0.0106(2) -0.0004(2) 0.0032(2) PD1' 0.0359(3) 0.0409(2) 0.0345(3) 0.0106(2) -0.0004(2) -0.0032(2) P1 0.044(1) 0.048(1) 0.041(1) -0.015(1) -0.003(1) 0.007(1) C1 0.069(5) 0.035(4) 0.070(6) -0.002(4) -0.024(5) 0.002(4) C2 0.049(6) 0.035(5) 0.076(8) 0.000 -0.024(6) 0.000 C1' 0.069(5) 0.035(4) 0.070(6) 0.002(4) -0.024(5) -0.002(4) P1' 0.044(1) 0.048(1) 0.041(1) 0.015(1) -0.003(1) -0.007(1) N1 0.042(3) 0.052(4) 0.046(2) -0.001(2) -0.002(2) -0.004(2) C3 0.038(3) 0.068(4) 0.042(2) -0.004(2) -0.001(1) -0.008(2) C4 0.064(4) 0.093(4) 0.053(2) -0.002(3) 0.008(2) -0.021(2) C5 0.067(4) 0.131(6) 0.049(2) -0.009(3) 0.012(2) -0.022(2) C6 0.058(3) 0.137(6) 0.042(2) -0.022(3) 0.007(2) -0.001(2) C7 0.054(3) 0.101(4) 0.043(2) -0.023(3) 0.001(2) 0.010(2) C8 0.035(3) 0.071(3) 0.039(2) -0.012(2) -0.003(1) 0.003(2) N1' 0.042(3) 0.052(4) 0.046(2) 0.000(2) -0.002(2) 0.004(2) C3' 0.038(3) 0.069(4) 0.042(2) 0.003(2) -0.001(1) 0.007(2) C4' 0.063(4) 0.094(4) 0.053(2) 0.001(3) 0.009(2) 0.021(2) C5' 0.066(4) 0.132(6) 0.049(2) 0.009(3) 0.012(2) 0.021(2) C6' 0.059(3) 0.137(6) 0.042(2) 0.023(3) 0.007(2) 0.000(2) C7' 0.055(3) 0.101(4) 0.044(2) 0.023(3) 0.001(2) -0.011(2) C8' 0.035(3) 0.071(3) 0.039(2) 0.012(2) -0.003(1) -0.003(2) C9 0.056(1) 0.075(1) 0.042(1) -0.032(1) -0.001(1) 0.003(1) C10 0.045(1) 0.128(3) 0.061(2) -0.017(1) -0.005(1) -0.022(2) C11 0.051(1) 0.217(6) 0.066(3) -0.048(2) 0.005(1) -0.046(4) C12 0.108(3) 0.220(6) 0.049(3) -0.119(4) 0.015(2) -0.024(4) C13 0.169(5) 0.135(3) 0.066(4) -0.119(4) -0.012(4) 0.011(3) C14 0.123(3) 0.076(1) 0.063(2) -0.061(2) -0.018(2) 0.014(2) C9' 0.061(1) 0.072(1) 0.043(1) 0.035(1) -0.002(1) -0.005(1) C10' 0.047(1) 0.135(3) 0.055(2) 0.030(1) 0.001(1) 0.022(2) C11' 0.066(1) 0.222(6) 0.056(3) 0.076(3) 0.013(2) 0.040(4) C12' 0.142(4) 0.204(6) 0.052(3) 0.138(5) 0.008(3) 0.010(4) C13' 0.197(5) 0.113(2) 0.082(4) 0.114(4) -0.027(4) -0.018(3) C14' 0.133(3) 0.065(1) 0.074(3) 0.053(2) -0.026(3) -0.015(1) C15 0.041(2) 0.050(2) 0.045(2) -0.008(2) 0.003(2) -0.002(2) C16 0.064(3) 0.051(2) 0.064(2) -0.002(2) -0.001(2) -0.010(2) C17 0.089(4) 0.071(2) 0.079(3) 0.004(2) 0.003(3) -0.028(2) C18 0.092(4) 0.099(3) 0.067(2) -0.005(3) 0.013(2) -0.033(3) C19 0.077(3) 0.097(3) 0.047(2) -0.018(3) 0.013(2) -0.013(2) C20 0.053(2) 0.068(2) 0.041(2) -0.015(2) 0.006(2) -0.001(2) C21 0.082(5) 0.058(3) 0.042(4) -0.025(3) -0.010(3) 0.013(2) N2 0.058(5) 0.054(3) 0.045(3) -0.023(3) -0.006(2) 0.007(2) C22 0.102(5) 0.074(4) 0.075(5) -0.005(3) -0.048(4) 0.017(3) C23 0.094(6) 0.052(3) 0.066(5) -0.020(3) -0.004(4) 0.007(2) C24 0.058(5) 0.080(4) 0.076(5) -0.039(3) 0.004(3) -0.010(3) C15' 0.041(2) 0.050(2) 0.045(2) 0.008(2) 0.003(2) 0.002(2) C16' 0.064(3) 0.051(2) 0.063(2) 0.002(2) -0.001(2) 0.010(2) C17' 0.089(4) 0.071(2) 0.078(3) -0.003(2) 0.003(3) 0.028(2) C18' 0.092(4) 0.099(3) 0.066(2) 0.006(3) 0.012(2) 0.033(2) C19' 0.077(3) 0.096(3) 0.046(2) 0.019(3) 0.012(2) 0.013(2) C20' 0.053(2) 0.068(2) 0.041(2) 0.015(2) 0.006(2) 0.001(2) C21' 0.082(5) 0.058(3) 0.042(4) 0.025(3) -0.010(3) -0.013(2) N2' 0.058(5) 0.054(3) 0.046(3) 0.024(3) -0.005(2) -0.007(2) C22' 0.103(5) 0.074(4) 0.075(5) 0.005(3) -0.048(4) -0.017(3) C23' 0.094(6) 0.052(3) 0.065(5) 0.021(3) -0.003(4) -0.007(2) C24' 0.056(6) 0.081(4) 0.078(5) 0.038(3) 0.002(3) 0.010(3) CL1 0.043(2) 0.051(2) 0.048(2) 0.000 0.000 0.000 P2 0.042(4) 0.025(2) 0.040(2) 0.002(1) 0.000 0.000 F21 0.127(7) 0.047(3) 0.050(2) -0.017(4) -0.029(2) 0.007(1) F22 0.068(5) 0.025(2) 0.061(3) 0.000(1) 0.001(1) -0.002(1) F23 0.056(4) 0.051(3) 0.139(7) 0.001(1) 0.038(4) -0.009(2) F24 0.153(8) 0.053(4) 0.051(2) -0.023(5) -0.035(2) 0.009(2) F25 0.068(5) 0.025(2) 0.062(3) 0.000(1) -0.001(1) 0.001(1) F26 0.048(4) 0.050(3) 0.143(7) 0.003(1) 0.026(3) -0.006(1) P3 0.168(6) 0.495(17) 0.637(21) 0.065(9) -0.016(10) 0.044(19) F31 0.130(5) 0.142(7) 0.284(13) -0.010(5) 0.075(7) -0.083(9) F32 0.144(6) 0.261(15) 1.753(85) -0.117(9) 0.269(15) -0.414(28) F33 0.723(33) 2.427(84) 0.624(22) -0.036(58) -0.216(26) -0.830(35) F34 0.579(29) 2.644(99) 1.928(91) 0.513(52) -0.419(41) 0.838(94) F35 0.583(31) 0.886(29) 1.814(59) 0.378(28) 0.552(36) 1.009(43) F36 0.309(14) 0.146(11) 1.741(80) -0.069(9) 0.578(31) -0.359(25) P3' 0.106(5) 0.116(6) 0.654(21) -0.021(4) 0.116(8) -0.116(10) F31' 0.268(12) 0.114(8) 1.363(43) 0.035(6) 0.452(21) 0.115(14) F32' 0.301(12) 0.153(16) 1.997(97) -0.034(13) 0.659(34) -0.095(36) F33' 0.423(17) 2.077(76) 1.257(57) -0.059(38) -0.408(31) -0.804(59) F34' 0.271(12) 0.481(23) 2.356(99) 0.236(17) 0.382(27) 0.522(42) F35' 0.226(9) 0.288(10) 0.568(16) 0.069(8) 0.179(11) 0.147(13) F36' 0.605(27) 1.118(44) 0.704(24) -0.100(37) 0.370(25) -0.678(33) O1 0.109(8) 0.164(8) 0.257(13) -0.001(7) 0.042(10) 0.044(11) C25 0.113(8) 0.167(9) 0.478(27) 0.000(7) 0.070(11) 0.054(14) C26 0.182(13) 0.182(15) 0.748(62) 0.003(12) 0.226(25) 0.074(27) C27 0.129(10) 0.242(22) 1.082(97) 0.022(13) 0.028(27) 0.232(39) O2 0.157(36) 0.077(15) 0.268(30) -0.049(20) 0.031(20) -0.010(18) C28 0.180(28) 0.029(12) 0.141(24) -0.035(16) 0.051(23) -0.002(13) C29 0.280(37) 0.036(14) 0.296(49) -0.060(17) 0.156(38) -0.040(16) C30 0.250(30) 0.068(15) 0.167(33) -0.064(18) -0.028(25) 0.046(18) H1C1 0.069 0.035 0.070 -0.002 -0.024 0.002 H2C1 0.069 0.035 0.070 -0.002 -0.024 0.002 H1C2 0.049 0.035 0.076 0.000 -0.024 0.000 H2C2 0.049 0.035 0.076 0.000 -0.024 0.000 H1C1' 0.069 0.035 0.070 0.002 -0.024 -0.002 H2C1' 0.069 0.035 0.070 0.002 -0.024 -0.002 H1N1 0.056 0.053 0.050 -0.013 -0.001 -0.009 H2N1 0.059 0.060 0.060 0.015 0.002 -0.001 H1C4 0.098 0.090 0.071 0.004 0.016 -0.032 H1C5 0.094 0.161 0.059 -0.008 0.021 -0.038 H1C6 0.075 0.173 0.044 -0.033 0.011 0.006 H1C7 0.081 0.104 0.055 -0.033 0.003 0.022 H1N1' 0.056 0.053 0.050 0.012 -0.001 0.009 H2N1' 0.058 0.062 0.060 -0.015 0.001 0.001 H1C4' 0.096 0.091 0.071 -0.006 0.016 0.031 H1C5' 0.092 0.163 0.059 0.007 0.022 0.037 H1C6' 0.076 0.174 0.044 0.033 0.011 -0.007 H1C7' 0.082 0.104 0.056 0.032 0.003 -0.023 H1C10 0.061 0.126 0.097 0.017 -0.030 -0.030 H1C11 0.047 0.298 0.106 -0.021 -0.009 -0.085 H1C12 0.137 0.305 0.054 -0.169 0.024 -0.040 H1C13 0.274 0.138 0.105 -0.159 -0.042 0.026 H1C14 0.169 0.054 0.101 -0.043 -0.049 0.019 H1C10' 0.049 0.143 0.088 -0.006 -0.018 0.039 H1C11' 0.053 0.319 0.086 0.063 0.011 0.084 H1C12' 0.188 0.281 0.058 0.198 0.014 0.018 H1C13' 0.307 0.106 0.135 0.137 -0.066 -0.029 H1C14' 0.168 0.049 0.116 0.024 -0.056 -0.010 H1C16 0.078 0.044 0.073 -0.001 -0.007 -0.004 H1C17 0.122 0.073 0.105 0.013 -0.003 -0.038 H1C18 0.120 0.127 0.079 -0.004 0.018 -0.051 H1C19 0.100 0.122 0.044 -0.029 0.016 -0.010 H1C21 0.130 0.069 0.046 -0.044 0.004 0.011 H1C22 0.142 0.093 0.078 -0.012 -0.068 0.021 H2C22 0.137 0.077 0.102 0.008 -0.061 0.022 H3C22 0.064 0.079 0.091 -0.002 -0.039 0.004 H1C23 0.095 0.057 0.093 -0.001 -0.014 0.005 H2C23 0.142 0.054 0.073 -0.029 -0.002 0.013 H3C23 0.096 0.057 0.068 -0.030 0.005 -0.002 H1C24 0.046 0.090 0.098 -0.029 0.000 -0.016 H2C24 0.061 0.093 0.087 -0.042 -0.009 -0.015 H3C24 0.092 0.090 0.088 -0.060 0.028 -0.017 H1C16' 0.078 0.044 0.073 0.001 -0.007 0.004 H1C17' 0.121 0.073 0.104 -0.011 -0.003 0.038 H1C18' 0.120 0.127 0.077 0.005 0.018 0.049 H1C19' 0.100 0.121 0.043 0.030 0.015 0.009 H1C21' 0.129 0.069 0.046 0.044 0.004 -0.011 H1C22' 0.144 0.093 0.077 0.012 -0.068 -0.021 H2C22' 0.139 0.077 0.102 -0.008 -0.061 -0.022 H3C22' 0.065 0.079 0.091 0.002 -0.040 -0.005 H1C23' 0.096 0.056 0.091 0.002 -0.014 -0.006 H2C23' 0.141 0.054 0.072 0.032 0.001 -0.012 H3C23' 0.096 0.058 0.067 0.031 0.006 0.003 H1C24' 0.045 0.091 0.099 0.027 -0.002 0.016 H2C24' 0.060 0.095 0.089 0.040 -0.013 0.015 H3C24' 0.087 0.093 0.092 0.060 0.027 0.019 #--------------------------------------------------------------------------- #-- _refine_special_details ; The structure was solved by direct methods and most of the remaining non-hydrogen atoms were located in Fourier maps. Pseudo-symmetry was soon recognized. This structure can be thought of as a displacive modulation of a parent structure in space group I222 with the same unit cell axes. The reference Pd2(C47H56N4P2)2+ dication has a pseudo 2 fold axis parallel to b approximately described by -x,y,1/2-z. If this were an exact symmetry operation P21212 would become I222 with a 222 site at 0,0,1/4. In this I222 description, the Cl ion and one PF6 ion would be on separate 222 sites. Atoms of the cation have been labelled so that pseudo 2 fold related atoms are described as N1 and N1' , C1 and C1', etc. The Chloride ion links separate dications via Cl1...H-N1 hydrogen bonding. The second PF6 ion is on a general position which would have half occupancy for an I222 description but selects between -x,y,1/2-z related sites when the structure is ordered in P21212, the alternative site being occupied by an acetone molecule. The second H attached to N1 is Hydrogen bonded to a F of this PF6 ion at a general position while that on N1' is Hydrogen bonded to the O of the acetone. Both these entities are highly librating in holes in the structure. An additional acetone is found disordered about a 2 fold axis of P21212. Because of the pseudo symmetry and large mean square displacements of some atoms, the structure was refined using the program RAELS964, to allow sensible constraints and restraints. The I222 parent structure symmetry was used as a guide to choosing the parameter constraints and restraints. This allowed just 260 independent variables to adequately refine the structure down to R(F) = 0.060 for the 7442 reflections out of 8883 with I > 3\s(I). Octants for hkl and h-kl were both included and the absolute configuration verified. The alternative hand refined to R(F) = 0.075. The assignment of the absolute configuration is consistent with the known chirality of the (C10H14N) ligand. Data was segmented according to whether h+k+l was even or odd (see Table) and allowance was made for stacking faults by letting these subsets have different scale constants. This was found to be unnecessary and the final refinement has all intensities on a single scale. The atom positions for the cation were described with Pd1, Pd1', C1, C1', C2, N2, N2', C22, C22', C23, C23', C24, C24' as independent atoms and the remaining atoms as parts of groups, with refinable local coordinates defined relative to local orthonormal axial systems. Groups [N1, C3 - C8], [P1, C9 - C14] and [C15 - C21] were constrained to be planar and have the same local coordinates as their primed counterparts. Pseudo symmetry related bond lengths not already constrained were restrained to have their bond length differences approach zero. The PF6 ions were constrained to have exact octahedral local geometry with a common refinable bondlength (1.583(4) \%A), The acetone molecules were constrained to have an identical refinable local geometry of mm2 symmetry. The first PF6 group at approximately 1/2,0,3/4 was made to be 1:1 disordered by allowing it to be in a general position disordered by the local 2 fold axis. The other PF6 group was also made to be 1:1 disordered to better allow a description of its rather diffuse scattering density. The second acetone was also disordered about a 2-fold axis. The Cl ion was refined as an isolated atom. Atoms Pd1, Pd1', C1, C1', C2 and Cl1 were refined as anisotropic atoms with the allowed parameters constrained assuming the pseudo I222 symmetry holds exactly for these parameters. The remaining cation atoms were refined using 8 rigid body thermal parameterisations constrained to retain the pseudo symmetry relationship between primed and unprimed atoms. [N1, C3 - C8], and [N2, C21 - C24] were refined using 15 parameter TLX models whereas [C15 - C21] and [P1, C9 - C14] were refined using 12 parameter TL models with centres of action constrained to lie on Pd1 and P1 respectively. The PF6 at 1/2,0,3/4 was refined using a 9 parameter TLX model constrained by the 2 fold symmetry of the site it was disordered about.5 the other disordered PF6 was refined as a 12 parameter TL model centred on a point midway between F31 anf F35' each of which appears to be involved in Hydrogen bonding. This anion has very large displacement parameters and this is consistent with its crystal environment. The acetone pseudo symmetrically related to the disordered PF6 was considered to be ordered and was refined using a TL model centred on O1 which is involved in Hydrogen bonding. The remaining acetone was refined using a TLX model. Errors quoted for the refinement are conditional on the appropriateness of the various constraints and restraints used. Refinement was on F and used 260 variables to fit the 7442 reflections (out of 8883 independent reflections) with I > 3\s(I). When refinement was terminated, shift/error ratios were less than 0.3 for parameters. Unweighted and weighted agreement factors for the final model are: R = \S ||Fo| - |Fc|| / \S |Fo| = 0.060 Rw = [\S w(|Fo| - |Fc|)2 / \S wFo2]1/2 = 0.093 The standard deviation of an observation of unit weight (goodness of fit indicator) is 1.46 for the reflections used and 0.91 (R = 0.55) for the remaining 1441 reflections with I < 3\s(I). The weighting scheme was based on counting statistics and included a factor (5%) to downweight the intense reflections: w = 1/(\s(F)2 + (0.05F)2). The maximum and minimum peaks on the final difference Fourier map corresponded to 1.0 and -0.8 e-/\%A3, respectively, with the largest features being close to the Pd atoms and within the disordered solvate. Neutral atom scattering factors were taken from the International Tables for Crystallography, Volume C. Anomalous dispersion effects were included in Fc; the values for \Df' and \Df" were also taken from Volume C, as were the values for the mass attenuation coefficients. Calculations were performed using crystallographic software packages teXsan and RAELS96. Appendix Refinement Statistics. Class** Number R(F) R(F2) wR Gof <|F2|>* 1 3947 0.057 0.110 0.092 1.520 1000 2 3495 0.066 0.115 0.093 1.406 294 1-2 7442 0.060 0.112 0.093 1.463 668 3 1441 0.547 0.856 0.381 0.908 17 1-3 8883 0.076 0.115 0.096 1.396 563 An uncorrelated 5% error in |F(h)| was included along with counting statistic error for evaluating weights w = 1/(\s(F)2 + (0.05F)2). Refinement was on F. * Scaled relative to 1000 for Class 1. ** 1 Reflections with h+k+l even and I(h) > 3\s(I(h)). ** 2 Reflections with h+k+l odd and I(h) > 3\s(I(h)). 3 Reflections with I(h) < 3\s(I(h)). ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0025|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7442 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.076 _refine_ls_R_factor_gt 0.060 _refine_ls_wR_factor_all 0.096 _refine_ls_wR_factor_ref 0.093 _refine_ls_goodness_of_fit_all 1.396 _refine_ls_goodness_of_fit_ref 1.463 _refine_ls_shift/su_max 0.3 _refine_ls_shift/su_mean 0.1 _refine_diff_density_min -0.8 _refine_diff_density_max 1.0 #--------------------------------------------------------------------------- #-- 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 PD1 P1 2.206(2) . . yes PD1 N1 2.159(6) . . yes PD1 C15 2.007(7) . . yes PD1 N2 2.144(6) . . yes PD1' P1' 2.207(2) . . yes PD1' N1' 2.159(6) . . yes PD1' C15' 2.006(8) . . yes PD1' N2' 2.144(6) . . yes P1 C1 1.818(8) . . yes P1 C8 1.806(8) . . yes P1 C9 1.821(7) . . yes C1 C2 1.510(11) . . yes C2 C1' 1.511(11) . . yes C1' P1' 1.820(8) . . yes P1' C8' 1.804(8) . . yes P1' C9' 1.821(7) . . yes N1 C3 1.435(10) . . yes C3 C4 1.382(11) . . yes C3 C8 1.427(11) . . yes C4 C5 1.349(15) . . yes C5 C6 1.402(16) . . yes C6 C7 1.412(14) . . yes C7 C8 1.399(11) . . yes N1' C3' 1.435(10) . . yes C3' C4' 1.382(11) . . yes C3' C8' 1.427(11) . . yes C4' C5' 1.349(15) . . yes C5' C6' 1.402(16) . . yes C6' C7' 1.412(14) . . yes C7' C8' 1.399(11) . . yes C9 C10 1.374(7) . . yes C9 C14 1.374(7) . . yes C10 C11 1.392(10) . . yes C11 C12 1.371(11) . . yes C12 C13 1.371(11) . . yes C13 C14 1.392(10) . . yes C9' C10' 1.374(7) . . yes C9' C14' 1.374(7) . . yes C10' C11' 1.392(10) . . yes C11' C12' 1.371(11) . . yes C12' C13' 1.371(11) . . yes C13' C14' 1.392(10) . . yes C15 C16 1.408(11) . . yes C15 C20 1.402(11) . . yes C16 C17 1.391(13) . . yes C17 C18 1.361(16) . . yes C18 C19 1.455(16) . . yes C19 C20 1.362(12) . . yes C20 C21 1.519(12) . . yes C21 N2 1.477(10) . . yes C21 C22 1.553(13) . . yes N2 C23 1.469(12) . . yes N2 C24 1.468(12) . . yes C15' C16' 1.408(11) . . yes C15' C20' 1.402(11) . . yes C16' C17' 1.391(13) . . yes C17' C18' 1.361(16) . . yes C18' C19' 1.455(16) . . yes C19' C20' 1.362(12) . . yes C20' C21' 1.519(12) . . yes C21' N2' 1.486(11) . . yes C21' C22' 1.555(13) . . yes N2' C23' 1.476(12) . . yes N2' C24' 1.468(12) . . yes P2 F21 1.583(4) . . yes O1 C25 1.229(17) . . yes C25 C26 1.358(15) . . yes C25 C27 1.358(15) . . yes O2 C28 1.229(17) . . yes C28 C29 1.358(15) . . yes C28 C30 1.358(15) . . yes N1 CL1 3.482(7) . . yes N1 F31 2.923(18) . 2_655 yes N1 F35' 3.165(22) . 2_655 yes N1' CL1 3.482(7) . . yes N1' O1 3.007(15) . 2_565 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 P1 PD1 N1 85.5(2) . . . yes P1 PD1 C15 97.2(2) . . . yes P1 PD1 N2 177.7(2) . . . yes N1 PD1 C15 176.8(3) . . . yes N1 PD1 N2 95.4(3) . . . yes C15 PD1 N2 82.0(3) . . . yes P1' PD1' N1' 85.2(2) . . . yes P1' PD1' C15' 97.4(2) . . . yes P1' PD1' N2' 174.0(2) . . . yes N1' PD1' C15' 176.5(3) . . . yes N1' PD1' N2' 95.9(3) . . . yes C15' PD1' N2' 81.9(3) . . . yes PD1 P1 C1 116.6(4) . . . yes PD1 P1 C8 102.9(3) . . . yes PD1 P1 C9 117.9(2) . . . yes C1 P1 C8 105.6(4) . . . yes C1 P1 C9 106.8(4) . . . yes C8 P1 C9 105.7(3) . . . yes P1 C1 C2 110.6(6) . . . yes C1 C2 C1' 113.5(9) . . . yes C2 C1' P1' 111.3(7) . . . yes PD1' P1' C1' 114.2(4) . . . yes PD1' P1' C8' 103.2(3) . . . yes PD1' P1' C9' 121.5(2) . . . yes C1' P1' C8' 104.5(4) . . . yes C1' P1' C9' 106.9(4) . . . yes C8' P1' C9' 104.7(3) . . . yes PD1 N1 C3 115.6(5) . . . yes N1 C3 C4 123.4(8) . . . yes N1 C3 C8 119.3(7) . . . yes C4 C3 C8 117.3(8) . . . yes C3 C4 C5 123.8(10) . . . yes C4 C5 C6 119.2(9) . . . yes C5 C6 C7 120.5(9) . . . yes C6 C7 C8 118.5(9) . . . yes P1 C8 C3 116.6(6) . . . yes P1 C8 C7 122.6(7) . . . yes C3 C8 C7 120.8(8) . . . yes PD1' N1' C3' 115.8(5) . . . yes N1' C3' C4' 123.4(8) . . . yes N1' C3' C8' 119.3(7) . . . yes C4' C3' C8' 117.3(8) . . . yes C3' C4' C5' 123.8(10) . . . yes C4' C5' C6' 119.2(9) . . . yes C5' C6' C7' 120.5(9) . . . yes C6' C7' C8' 118.5(9) . . . yes P1' C8' C3' 116.4(6) . . . yes P1' C8' C7' 122.9(7) . . . yes C3' C8' C7' 120.8(8) . . . yes P1 C9 C10 116.2(5) . . . yes P1 C9 C14 121.7(6) . . . yes C10 C9 C14 122.0(9) . . . yes C9 C10 C11 118.8(8) . . . yes C10 C11 C12 119.3(9) . . . yes C11 C12 C13 121.7(9) . . . yes C12 C13 C14 119.3(9) . . . yes C9 C14 C13 118.8(8) . . . yes P1' C9' C10' 116.2(5) . . . yes P1' C9' C14' 121.7(6) . . . yes C10' C9' C14' 122.0(9) . . . yes C9' C10' C11' 118.8(8) . . . yes C10' C11' C12' 119.3(9) . . . yes C11' C12' C13' 121.7(9) . . . yes C12' C13' C14' 119.3(9) . . . yes C9' C14' C13' 118.8(8) . . . yes PD1 C15 C16 128.8(6) . . . yes PD1 C15 C20 112.6(6) . . . yes C16 C15 C20 118.5(7) . . . yes C15 C16 C17 119.3(9) . . . yes C16 C17 C18 122.4(10) . . . yes C17 C18 C19 118.9(9) . . . yes C18 C19 C20 118.3(9) . . . yes C15 C20 C19 122.6(8) . . . yes C15 C20 C21 118.1(7) . . . yes C19 C20 C21 119.3(8) . . . yes C20 C21 N2 108.4(6) . . . yes C20 C21 C22 107.5(6) . . . yes N2 C21 C22 110.4(8) . . . yes PD1 N2 C21 106.9(5) . . . yes PD1 N2 C23 116.3(6) . . . yes PD1 N2 C24 106.1(6) . . . yes C21 N2 C23 112.3(7) . . . yes C21 N2 C24 106.5(8) . . . yes C23 N2 C24 108.1(8) . . . yes PD1' C15' C16' 129.2(6) . . . yes PD1' C15' C20' 112.3(6) . . . yes C16' C15' C20' 118.5(7) . . . yes C15' C16' C17' 119.3(9) . . . yes C16' C17' C18' 122.4(10) . . . yes C17' C18' C19' 118.9(9) . . . yes C18' C19' C20' 118.3(9) . . . yes C15' C20' C19' 122.6(8) . . . yes C15' C20' C21' 118.1(7) . . . yes C19' C20' C21' 119.3(8) . . . yes C20' C21' N2' 108.0(6) . . . yes C20' C21' C22' 106.4(6) . . . yes N2' C21' C22' 113.6(9) . . . yes PD1' N2' C21' 106.0(5) . . . yes PD1' N2' C23' 116.2(6) . . . yes PD1' N2' C24' 104.8(6) . . . yes C21' N2' C23' 111.2(7) . . . yes C21' N2' C24' 109.3(8) . . . yes C23' N2' C24' 109.1(8) . . . yes PD1 N1 CL1 114.9(2) . . . yes PD1 N1 F31 94.2(5) . . 2_655 yes PD1 N1 F35' 117.5(5) . . 2_655 yes C3 N1 CL1 107.9(3) . . . yes C3 N1 F31 103.1(5) . . 2_655 yes C3 N1 F35' 92.7(8) . . 2_655 yes CL1 N1 F31 120.5(4) . . 2_655 yes CL1 N1 F35' 105.6(4) . . 2_655 yes PD1' N1' CL1 119.5(2) . . . yes PD1' N1' O1 92.2(4) . . 2_565 yes C3' N1' CL1 107.4(3) . . . yes C3' N1' O1 108.9(4) . . 2_565 yes CL1 N1' O1 111.8(3) . . 2_565 yes N1 CL1 N1 156.9(2) . . 2_655 yes N1 CL1 N1' 96.7(2) . . . yes N1 CL1 N1' 88.5(2) . . 2_655 yes N1' CL1 N1' 154.1(2) . . 2_655 yes F21 P2 F22 90.0(0) . . . yes O1 C25 C26 116.1(10) . . . yes O1 C25 C27 116.1(10) . . . yes C26 C25 C27 127.9(20) . . . yes N1 F31 P3 125.1(11) 2_655 . . yes N1 F35' P3' 120.3(9) 2_655 . . yes N1' O1 F35 81.1(8) 2_565 . 2_565 yes N1' O1 C25 142.2(9) 2_565 . . yes F35 O1 C25 83.4(13) 2_565 . . yes O2 C28 C29 116.1(10) . . . yes O2 C28 C30 116.1(10) . . . yes C29 C28 C30 127.9(20) . . . 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 C19 C20 C21 N2 152.3(6) . . . . yes C19 C20 C21 C22 -88.4(7) . . . . yes C19' C20' C21' N2' 152.3(6) . . . . yes C19' C20' C21' C22' -85.4(7) . . . . yes C7 C8 P1 C1 58.6(4) . . . . yes C7 C8 P1 C9 -54.3(3) . . . . yes C7' C8' P1' C1' 62.8(4) . . . . yes C7' C8' P1' C9' -49.4(3) . . . . yes #===END