# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2142 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-12-13 _audit_update_record ? #======================================================================= # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'J.Chem.Soc.,Dalton' _publ_requested_category ? _publ_section_title ; Trimethylpalladium(IV) and platinum(IV) complexes containing phosphine donor ligands, including studies of 1,5,9,triethyl-1,5,9- triphosphacyclodecane and X-ray structural studies of [PdMe3(2,2'-bipy)(PMe2Ph)][O3SCF3](2,2'-bipy = 2,2'-bipyridine) and the palladium(II) complex [PdMe(phen)PMe2Ph)][O3SCF3](phen=1,10-phenanthroline) ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Bayler, Angela' . ; School of Chemistry, University of Tasmania, Hobart, Tasmania, 7001 Australia. ; 'Canty, Allan J.' . ; School of Chemistry, University of Tasmania, Hobart, Tasmania, 7001 Australia. ; 'Edwards, Peter G.' . ; Department of Chemistry, University of Wales, P.O. Box 912, Cardiff CF1 3TB U.K. ; 'Skelton, Brian W.' . ; Department of Chemistry University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Department of Chemistry University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_pdabgn # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H22 F3 N2 O3 P1 Pd1 S1' _chemical_formula_moiety ? _chemical_formula_weight 564.86 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.6042(9) _cell_length_b 11.5323(10) _cell_length_c 20.241(2) _cell_angle_alpha 90.00000 _cell_angle_beta 98.6520(10) _cell_angle_gamma 90.00000 _cell_volume 2216.4(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7834 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.053 _exptl_crystal_description prism _exptl_crystal_size_max .25 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .13 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .714 _exptl_absorpt_correction_T_max .831 _diffrn_reflns_number 21967 _reflns_number_total 5635 _reflns_Friedel_coverage 0 _reflns_number_gt 4590 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.08 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .0274 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .03 _refine_ls_wR_factor_ref .035 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_number_reflns 4590 _refine_ls_number_parameters 368 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .038 _refine_diff_density_min -.625 _refine_diff_density_max .99 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _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 80 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 12 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 4 -1.177 1.007 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 4 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd .216740(17) .605925(14) .087647(9) .02232(9) Uani ? ? 1.00000 ? ? C0 .3820(3) .6248(2) .03535(15) .0344(14) Uani ? ? 1.00000 ? ? P .30251(6) .76617(5) .14123(3) .0252(3) Uani ? ? 1.00000 ? ? C11 .2316(2) .7943(2) .21788(12) .0262(11) Uani ? ? 1.00000 ? ? C12 .2518(3) .7108(2) .26880(14) .0348(13) Uani ? ? 1.00000 ? ? C13 .1911(3) .7242(2) .32598(14) .0383(14) Uani ? ? 1.00000 ? ? C14 .1103(3) .8214(3) .33418(14) .0367(14) Uani ? ? 1.00000 ? ? C15 .0933(3) .9050(2) .28560(14) .0338(13) Uani ? ? 1.00000 ? ? C16 .1525(3) .8920(2) .22732(13) .0288(12) Uani ? ? 1.00000 ? ? C21 .2708(3) .8975(2) .09241(15) .0323(13) Uani ? ? 1.00000 ? ? C22 .4909(3) .7663(3) .17173(17) .0363(14) Uani ? ? 1.00000 ? ? N1a .03181(19) .56489(17) .13024(9) .0233(9) Uani ? ? 1.00000 ? ? C2a -.0134(2) .4538(2) .11961(11) .0246(11) Uani ? ? 1.00000 ? ? C3a -.1226(3) .4098(2) .14940(13) .0322(13) Uani ? ? 1.00000 ? ? C4a -.1927(3) .4818(3) .18850(13) .0365(14) Uani ? ? 1.00000 ? ? C5a -.1537(3) .5968(2) .19526(13) .0310(12) Uani ? ? 1.00000 ? ? C6a -.0410(2) .6345(2) .16616(12) .0266(11) Uani ? ? 1.00000 ? ? N1b .1585(2) .44139(17) .04454(9) .0240(9) Uani ? ? 1.00000 ? ? C2b .0581(2) .38529(19) .07268(11) .0236(10) Uani ? ? 1.00000 ? ? C3b .0226(3) .2710(2) .05666(14) .0319(12) Uani ? ? 1.00000 ? ? C4b .0910(3) .2124(2) .01100(14) .0351(13) Uani ? ? 1.00000 ? ? C5b .1936(3) .2690(2) -.01716(13) .0341(13) Uani ? ? 1.00000 ? ? C6b .2250(3) .3834(2) .00083(12) .0304(12) Uani ? ? 1.00000 ? ? S -.16587(6) 1.01069(5) .13966(3) .0252(3) Uani ? ? 1.00000 ? ? O1 -.12453(18) 1.09871(14) .18964(9) .0329(9) Uani ? ? 1.00000 ? ? O2 -.0882(2) 1.01271(16) .08409(9) .0390(10) Uani ? ? 1.00000 ? ? O3 -.19094(19) .89730(14) .16508(9) .0328(9) Uani ? ? 1.00000 ? ? C -.3416(3) 1.0568(2) .10262(13) .0345(13) Uani ? ? 1.00000 ? ? F1 -.33963(19) 1.16219(15) .07514(9) .0542(10) Uani ? ? 1.00000 ? ? F2 -.42952(15) 1.06071(15) .14753(8) .0446(9) Uani ? ? 1.00000 ? ? F3 -.39694(17) .98384(16) .05419(8) .0511(9) Uani ? ? 1.00000 ? ? H0a .342(3) .608(2) -.0097(17) .047(9) Uiso ? ? 1.00000 ? ? H0b .444(3) .565(3) .0533(14) .037(8) Uiso ? ? 1.00000 ? ? H0c .434(3) .701(2) .0348(13) .033(7) Uiso ? ? 1.00000 ? ? H12 .301(3) .650(2) .2636(14) .034(7) Uiso ? ? 1.00000 ? ? H13 .211(4) .672(3) .3612(18) .070(11) Uiso ? ? 1.00000 ? ? H14 .069(3) .825(2) .3714(13) .033(7) Uiso ? ? 1.00000 ? ? H15 .039(3) .967(2) .2893(14) .043(8) Uiso ? ? 1.00000 ? ? H16 .131(3) .949(2) .1908(13) .032(7) Uiso ? ? 1.00000 ? ? H21a .309(3) .892(2) .0562(17) .049(10) Uiso ? ? 1.00000 ? ? H21b .312(3) .965(3) .1157(15) .048(9) Uiso ? ? 1.00000 ? ? H21c .178(3) .913(2) .0810(14) .037(8) Uiso ? ? 1.00000 ? ? H22a .538(3) .755(2) .1409(15) .038(8) Uiso ? ? 1.00000 ? ? H22b .521(3) .701(3) .2022(16) .056(9) Uiso ? ? 1.00000 ? ? H22c .517(3) .841(3) .1919(15) .050(9) Uiso ? ? 1.00000 ? ? H3a -.151(3) .339(3) .1405(14) .035(8) Uiso ? ? 1.00000 ? ? H4a -.259(3) .453(2) .2119(13) .033(7) Uiso ? ? 1.00000 ? ? H5a -.197(3) .644(3) .2189(15) .042(8) Uiso ? ? 1.00000 ? ? H6a -.015(2) .710(2) .1689(12) .023(6) Uiso ? ? 1.00000 ? ? H3b -.049(3) .237(2) .0757(13) .030(7) Uiso ? ? 1.00000 ? ? H4b .068(3) .134(2) .0003(13) .033(7) Uiso ? ? 1.00000 ? ? H5b .240(3) .231(2) -.0480(15) .043(8) Uiso ? ? 1.00000 ? ? H6b .297(3) .425(2) -.0175(13) .030(7) Uiso ? ? 1.00000 ? ? 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 .02240(9) .02023(10) .02530(10) -.00101(7) .00675(7) -.00079(7) C0 .0350(14) .0323(15) .0398(16) -.0038(12) .0180(12) -.0001(12) P .0245(3) .0214(3) .0298(3) -.0021(2) .0037(2) .0010(2) C11 .0260(11) .0229(12) .0285(12) -.0058(9) -.0002(9) -.0018(9) C12 .0400(14) .0265(14) .0365(15) .0008(11) .0009(12) .0020(11) C13 .0465(15) .0370(16) .0290(14) -.0076(13) -.0018(12) .0057(12) C14 .0397(14) .0452(17) .0258(13) -.0120(12) .0063(11) -.0079(12) C15 .0323(13) .0335(15) .0356(15) -.0015(11) .0046(11) -.0083(12) C16 .0294(12) .0245(12) .0310(13) -.0018(10) -.0001(10) .0001(10) C21 .0367(14) .0267(13) .0339(15) -.0041(12) .0067(12) .0037(11) C22 .0259(12) .0364(16) .0467(18) -.0021(11) .0051(12) .0016(14) N1a .0217(9) .0234(10) .0248(10) -.0003(8) .0036(8) -.0009(8) C2a .0255(11) .0243(12) .0237(12) -.0012(9) .0023(9) .0001(9) C3a .0344(13) .0303(14) .0326(14) -.0073(11) .0075(11) -.0013(11) C4a .0348(14) .0458(16) .0321(14) -.0077(12) .0150(11) .0012(12) C5a .0253(11) .0418(15) .0273(13) .0005(11) .0085(10) -.0069(11) C6a .0264(12) .0279(13) .0256(12) -.0010(10) .0044(9) -.0054(10) N1b .0271(9) .0230(10) .0220(10) .0007(8) .0044(8) -.0011(8) C2b .0243(11) .0223(12) .0237(11) .0001(9) .0015(9) .0004(9) C3b .0326(13) .0253(13) .0373(15) -.0034(10) .0040(11) -.0038(11) C4b .0401(14) .0257(13) .0370(15) .0018(11) -.0024(12) -.0083(11) C5b .0400(14) .0328(14) .0290(14) .0090(11) .0035(11) -.0095(11) C6b .0349(13) .0324(14) .0244(12) .0016(11) .0056(10) -.0026(10) S .0264(3) .0233(3) .0268(3) -.0024(2) .0070(2) -.0034(2) O1 .0344(9) .0311(10) .0334(10) -.0058(7) .0054(8) -.0104(7) O2 .0439(11) .0377(11) .0404(11) -.0059(8) .0231(9) -.0083(8) O3 .0346(9) .0233(9) .0402(10) -.0019(7) .0046(8) .0041(7) C .0353(13) .0351(14) .0324(14) -.0012(12) .0029(11) .0049(11) F1 .0573(10) .0414(10) .0618(12) .0085(9) .0024(9) .0213(9) F2 .0305(8) .0549(10) .0503(10) .0052(7) .0120(7) .0021(8) F3 .0461(9) .0626(11) .0389(9) -.0071(8) -.0117(8) -.0092(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Pd C0 . . 2.048(3) ? Pd P . . 2.2363(6) ? Pd N1a . . 2.141(2) ? Pd N1b . . 2.128(2) ? C0 H0a . . .95(3) ? C0 H0b . . .95(3) ? C0 H0c . . 1.01(3) ? P C11 . . 1.815(3) ? P C21 . . 1.809(3) ? P C22 . . 1.822(3) ? C11 C12 . . 1.402(4) ? C11 C16 . . 1.388(3) ? C12 C13 . . 1.380(4) ? C12 H12 . . .87(3) ? C13 C14 . . 1.388(4) ? C13 H13 . . .93(4) ? C14 C15 . . 1.369(4) ? C14 H14 . . .90(3) ? C15 C16 . . 1.393(4) ? C15 H15 . . .90(3) ? C16 H16 . . .99(3) ? C21 H21a . . .87(4) ? C21 H21b . . .96(3) ? C21 H21c . . .90(3) ? C22 H22a . . .84(3) ? C22 H22b . . .99(3) ? C22 H22c . . .97(3) ? N1a C2a . . 1.359(3) ? N1a C6a . . 1.347(3) ? C2a C3a . . 1.383(4) ? C2a C2b . . 1.481(3) ? C3a C4a . . 1.389(4) ? C3a H3a . . .87(3) ? C4a C5a . . 1.379(4) ? C4a H4a . . .91(3) ? C5a C6a . . 1.378(4) ? C5a H5a . . .87(3) ? C6a H6a . . .91(2) ? N1b C2b . . 1.356(3) ? N1b C6b . . 1.344(3) ? C2b C3b . . 1.388(3) ? C3b C4b . . 1.387(4) ? C3b H3b . . .93(3) ? C4b C5b . . 1.375(4) ? C4b H4b . . .95(3) ? C5b C6b . . 1.390(4) ? C5b H5b . . .93(3) ? C6b H6b . . .96(3) ? S O1 . . 1.4460(18) ? S O2 . . 1.440(2) ? S O3 . . 1.4387(17) ? S C . . 1.820(3) ? C F1 . . 1.338(3) ? C F2 . . 1.331(3) ? C F3 . . 1.340(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C0 Pd P . . . 84.57(8) ? C0 Pd N1a . . . 170.51(10) ? C0 Pd N1b . . . 93.39(10) ? P Pd N1a . . . 104.76(5) ? P Pd N1b . . . 172.17(5) ? N1a Pd N1b . . . 77.60(8) ? Pd C0 H0a . . . 104(2) ? Pd C0 H0b . . . 102.2(18) ? Pd C0 H0c . . . 121.3(16) ? H0a C0 H0b . . . 111(2) ? H0a C0 H0c . . . 107(2) ? H0b C0 H0c . . . 111(2) ? Pd P C11 . . . 113.83(8) ? Pd P C21 . . . 114.04(9) ? Pd P C22 . . . 116.08(11) ? C11 P C21 . . . 105.28(13) ? C11 P C22 . . . 101.03(13) ? C21 P C22 . . . 105.16(14) ? P C11 C12 . . . 118.54(19) ? P C11 C16 . . . 123.10(19) ? C12 C11 C16 . . . 118.3(2) ? C11 C12 C13 . . . 120.7(3) ? C11 C12 H12 . . . 119.3(19) ? C13 C12 H12 . . . 120(2) ? C12 C13 C14 . . . 120.3(3) ? C12 C13 H13 . . . 121(2) ? C14 C13 H13 . . . 119(2) ? C13 C14 C15 . . . 119.4(3) ? C13 C14 H14 . . . 117.5(17) ? C15 C14 H14 . . . 123.0(17) ? C14 C15 C16 . . . 120.8(3) ? C14 C15 H15 . . . 121(2) ? C16 C15 H15 . . . 118.4(19) ? C11 C16 C15 . . . 120.4(2) ? C11 C16 H16 . . . 119.6(16) ? C15 C16 H16 . . . 119.8(16) ? P C21 H21a . . . 110.3(19) ? P C21 H21b . . . 112.6(18) ? P C21 H21c . . . 112.9(18) ? H21a C21 H21b . . . 106(3) ? H21a C21 H21c . . . 109(3) ? H21b C21 H21c . . . 106(2) ? P C22 H22a . . . 111.7(19) ? P C22 H22b . . . 113.4(18) ? P C22 H22c . . . 109.0(18) ? H22a C22 H22b . . . 101(3) ? H22a C22 H22c . . . 109(3) ? H22b C22 H22c . . . 112(3) ? Pd N1a C2a . . . 114.14(15) ? Pd N1a C6a . . . 127.98(16) ? C2a N1a C6a . . . 117.9(2) ? N1a C2a C3a . . . 121.4(2) ? N1a C2a C2b . . . 115.9(2) ? C3a C2a C2b . . . 122.6(2) ? C2a C3a C4a . . . 119.6(2) ? C2a C3a H3a . . . 119(2) ? C4a C3a H3a . . . 120.8(19) ? C3a C4a C5a . . . 118.9(3) ? C3a C4a H4a . . . 120.7(17) ? C5a C4a H4a . . . 120.3(17) ? C4a C5a C6a . . . 118.7(3) ? C4a C5a H5a . . . 120(2) ? C6a C5a H5a . . . 121(2) ? N1a C6a C5a . . . 123.2(2) ? N1a C6a H6a . . . 116.4(16) ? C5a C6a H6a . . . 120.4(16) ? Pd N1b C2b . . . 114.39(15) ? Pd N1b C6b . . . 126.29(16) ? C2b N1b C6b . . . 118.5(2) ? C2a C2b N1b . . . 116.3(2) ? C2a C2b C3b . . . 122.4(2) ? N1b C2b C3b . . . 121.4(2) ? C2b C3b C4b . . . 119.6(2) ? C2b C3b H3b . . . 118.5(16) ? C4b C3b H3b . . . 121.9(16) ? C3b C4b C5b . . . 119.0(2) ? C3b C4b H4b . . . 119.7(17) ? C5b C4b H4b . . . 121.2(17) ? C4b C5b C6b . . . 118.9(3) ? C4b C5b H5b . . . 120.3(18) ? C6b C5b H5b . . . 120.8(18) ? N1b C6b C5b . . . 122.6(2) ? N1b C6b H6b . . . 116.8(16) ? C5b C6b H6b . . . 120.6(16) ? O1 S O2 . . . 114.53(11) ? O1 S O3 . . . 115.53(11) ? O1 S C . . . 102.89(11) ? O2 S O3 . . . 115.36(11) ? O2 S C . . . 103.33(12) ? O3 S C . . . 102.60(12) ? S C F1 . . . 111.50(18) ? S C F2 . . . 111.89(17) ? S C F3 . . . 111.06(18) ? F1 C F2 . . . 107.6(2) ? F1 C F3 . . . 107.2(2) ? F2 C F3 . . . 107.4(2) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? # Special items requested by author for inclusion in paper #----------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #----------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #----------------------------------------------------------------------- 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 Pd C11 3.402(2) . . ? Pd C21 3.401(3) . . ? Pd C22 3.450(3) . . ? Pd C2a 2.968(2) . . ? Pd C6a 3.154(3) . . ? Pd N1b 4.1886(18) . '3 565' ? Pd C2b 2.958(2) . . ? Pd C6b 3.118(3) . . ? Pd H0a 2.46(4) . . ? Pd H0b 2.43(3) . . ? Pd H0c 2.71(3) . . ? Pd H6a 3.19(3) . . ? Pd H6b 3.16(3) . . ? C0 P 2.886(3) . . ? C0 N1b 3.039(3) . . ? C0 F1 3.306(3) . '3 575' ? C0 H6b 2.62(3) . . ? P C12 2.773(3) . . ? P C16 2.824(3) . . ? P N1a 3.467(2) . . ? P C6a 3.735(3) . . ? P N1b 4.354(2) . . ? P F1 4.523(2) . '3 575' ? P F2 4.2520(18) . '1 655' ? P F3 4.389(2) . '1 655' ? P H0a 3.62(3) . . ? P H0b 3.34(3) . . ? P H0c 2.76(3) . . ? P H12 2.82(3) . . ? P H16 2.94(3) . . ? P H21a 2.26(3) . . ? P H21b 2.35(3) . . ? P H21c 2.32(3) . . ? P H22a 2.27(3) . . ? P H22b 2.39(3) . . ? P H22c 2.32(3) . . ? P H6a 3.25(2) . . ? C11 C13 2.418(4) . . ? C11 C14 2.797(4) . . ? C11 C15 2.413(4) . . ? C11 C21 2.880(4) . . ? C11 C22 2.807(4) . . ? C11 N1a 3.578(3) . . ? C11 H12 1.98(3) . . ? C11 H16 2.07(3) . . ? C11 H6a 2.61(2) . . ? C12 C14 2.401(4) . . ? C12 C15 2.757(4) . . ? C12 C16 2.396(4) . . ? C12 N1a 3.658(3) . . ? C12 H13 2.02(4) . . ? C13 C15 2.381(4) . . ? C13 C16 2.766(4) . . ? C13 F2 3.250(3) . '2 445' ? C13 H12 1.96(3) . . ? C13 H14 1.97(3) . . ? C14 C16 2.402(4) . . ? C14 N1b 3.351(3) . 2 ? C14 F2 3.519(3) . '2 445' ? C14 H13 2.01(4) . . ? C14 H15 1.98(3) . . ? C15 S 3.767(3) . . ? C15 H14 2.01(3) . . ? C15 H16 2.07(3) . . ? C16 S 3.569(2) . . ? C16 H15 1.98(3) . . ? C21 C22 2.883(4) . . ? C21 F1 3.618(4) . '3 575' ? C21 F2 3.479(3) . '1 655' ? C21 F3 3.538(4) . '1 655' ? C21 F3 3.637(4) . '3 575' ? C21 H16 2.63(3) . . ? C22 F2 3.530(4) . '1 655' ? N1a C3a 2.392(3) . . ? N1a C4a 2.779(3) . . ? N1a C5a 2.397(3) . . ? N1a N1b 3.731(3) . '3 565' ? N1a N1b 2.675(3) . . ? N1a C2b 2.408(3) . . ? N1a C5b 3.479(3) . '3 565' ? N1a C6b 3.392(3) . '3 565' ? N1a H3a 3.17(3) . . ? N1a H5a 3.18(3) . . ? N1a H6a 1.93(3) . . ? C2a C4a 2.395(4) . . ? C2a C5a 2.739(4) . . ? C2a C6a 2.318(4) . . ? C2a N1b 3.613(3) . '3 565' ? C2a N1b 2.410(3) . . ? C2a C3b 2.514(4) . . ? C2a H3a 1.96(3) . . ? C2a H3b 2.66(3) . . ? C3a C5a 2.384(4) . . ? C3a C6a 2.713(4) . . ? C3a C2b 2.513(4) . . ? C3a C3b 2.970(4) . . ? C3a H4a 2.01(3) . . ? C3a H3b 2.65(3) . . ? C4a C6a 2.372(4) . . ? C4a S 3.934(3) . '2 445' ? C4a F2 3.471(3) . '2 445' ? C4a H3a 1.98(3) . . ? C4a H5a 1.97(3) . . ? C5a F2 3.189(3) . '2 445' ? C5a H4a 2.00(3) . . ? C5a H6a 2.00(3) . . ? C6a H5a 1.97(3) . . ? N1b N1b 3.563(3) . '3 565' ? N1b C2b 3.531(3) . '3 565' ? N1b C3b 2.392(3) . . ? N1b C4b 2.780(3) . . ? N1b C5b 2.398(3) . . ? N1b H0a 2.93(3) . . ? N1b H0b 3.07(3) . . ? N1b H14 3.19(2) . '2 545' ? N1b H3b 3.21(3) . . ? N1b H5b 3.23(3) . . ? N1b H6b 1.97(3) . . ? C2b C4b 2.399(4) . . ? C2b C5b 2.740(4) . . ? C2b C6b 2.321(4) . . ? C2b H3a 2.65(3) . . ? C2b H3b 2.00(3) . . ? C3b C5b 2.380(4) . . ? C3b C6b 2.720(4) . . ? C3b H3a 2.67(3) . . ? C3b H4b 2.03(3) . . ? C4b C6b 2.381(4) . . ? C4b H3b 2.04(3) . . ? C4b H5b 2.01(3) . . ? C5b F3 3.650(3) . '3 565' ? C5b H4b 2.03(3) . . ? C5b H6b 2.05(3) . . ? C6b H5b 2.03(3) . . ? S F1 2.6243(18) . . ? S F2 2.6251(16) . . ? S F3 2.6188(16) . . ? S H15 3.39(3) . . ? S H16 2.97(2) . . ? S H4a 3.26(3) . '2 455' ? S H5a 3.66(3) . '2 455' ? S H3b 3.19(3) . '1 565' ? S H4b 3.54(3) . '3 565' ? S H5b 3.37(3) . '3 565' ? O1 O2 2.428(3) . . ? O1 O3 2.440(2) . . ? O1 C 2.565(3) . . ? O1 F1 2.955(2) . . ? O1 F2 2.958(2) . . ? O1 F3 3.736(2) . . ? O1 H22b 2.55(3) . 2 ? O1 H5a 2.75(3) . '2 455' ? O2 O3 2.433(3) . . ? O2 C 2.568(3) . . ? O2 F1 2.950(3) . . ? O2 F2 3.737(3) . . ? O2 F3 2.954(2) . . ? O2 H3b 2.62(3) . '1 565' ? O2 H4b 2.80(3) . '1 565' ? O2 H4b 2.43(3) . '3 565' ? O3 C 2.554(3) . . ? O3 F1 3.729(2) . . ? O3 F2 2.947(2) . . ? O3 F3 2.935(2) . . ? O3 H4a 2.68(3) . '2 455' ? O3 H6a 2.74(2) . . ? O3 H5b 2.78(3) . '3 565' ? F1 F2 2.155(3) . . ? F1 F3 3.755(2) . '3 475' ? F1 F3 2.155(2) . . ? F1 H0a 2.96(3) . '3 575' ? F1 H0c 2.77(3) . '3 575' ? F1 H14 3.21(3) . '2 455' ? F1 H21a 2.79(3) . '3 575' ? F1 H3a 2.91(3) . '1 565' ? F1 H3b 2.92(3) . '1 565' ? F2 F3 2.152(2) . . ? F2 F3 4.203(2) . '3 475' ? F2 H13 2.97(3) . '2 455' ? F2 H14 3.33(3) . '2 455' ? F2 H21b 2.71(3) . '1 455' ? F2 H22c 2.76(3) . '1 455' ? F2 H5a 2.95(3) . '2 455' ? F3 F3 2.750(2) . '3 475' ? F3 H21a 2.88(3) . '3 575' ? F3 H21a 3.02(3) . '1 455' ? F3 H21b 3.23(3) . '1 455' ? F3 H22a 3.28(3) . '1 455' ? F3 H5b 2.92(3) . '3 565' ? H0a H0b 1.57(4) . . ? H0a H0c 1.58(4) . . ? H0a H6b 2.16(4) . . ? H0b H0c 1.61(4) . . ? H0c H22a 2.31(4) . . ? H12 H13 2.29(5) . . ? H13 H14 2.26(4) . . ? H14 H15 2.32(4) . . ? H15 H16 2.31(4) . . ? H16 H21c 2.37(4) . . ? H21a H21b 1.46(5) . . ? H21a H21c 1.44(5) . . ? H21b H21c 1.49(4) . . ? H22a H22b 1.42(5) . . ? H22a H22c 1.47(4) . . ? H22b H22c 1.62(5) . . ? H3a H4a 2.31(4) . . ? H3a H3b 2.11(4) . . ? H4a H5a 2.28(4) . . ? H5a H6a 2.28(4) . . ? H3b H4b 2.35(4) . . ? H4b H5b 2.34(4) . . ? H5b H6b 2.35(4) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1136 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -27 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 9.985 _diffrn_reflns_av_sigmaI/netI .045 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .041 _refine_ls_wR_factor_all .037 _refine_ls_goodness_of_fit_all 1.099 _refine_ls_shift/su_mean .001 #======================================================================= # Structure Factor lists should be submitted as separate files #======================================================================= #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end- #===END data_ajcph # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C24 H28 F3 N2 O3 P1 Pd1 S1' _chemical_formula_moiety ? _chemical_formula_weight 618.95 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/m_1 _symmetry_space_group_name_Hall -p_2yb loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-z -x,-y,-z +x,1/2-y,+z _cell_length_a 8.3640(10) _cell_length_b 11.493(2) _cell_length_c 13.860(2) _cell_angle_alpha 90.00000 _cell_angle_beta 105.812(2) _cell_angle_gamma 90.00000 _cell_volume 1281.9(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4856 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .918 _exptl_crystal_description plate _exptl_crystal_size_max .2 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .78 _exptl_absorpt_correction_T_max .89 _diffrn_reflns_number 12745 _reflns_number_total 3424 _reflns_Friedel_coverage 0 _reflns_number_gt 2905 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.3 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .034 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref 1.279 _refine_ls_number_reflns 2905 _refine_ls_number_parameters 172 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .03 _refine_diff_density_min -.611 _refine_diff_density_max .988 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _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 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 56 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 6 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 6 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 2 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 2 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 2 -1.177 1.007 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd .37790(3) .25000 .08143(2) .02203(14) Uani ? ? 1.00000 ? ? C10a .2627(4) .3725(3) -.0210(2) .0515(18) Uani ? ? 1.00000 ? ? C10c .5658(5) .25000 .0091(3) .0321(18) Uani ? ? 1.00000 ? ? N11 .5280(3) .13163(19) .19447(16) .0265(10) Uani ? ? 1.00000 ? ? C12 .6473(3) .1877(3) .26582(18) .0304(12) Uani ? ? 1.00000 ? ? C13 .7696(4) .1276(4) .3390(2) .0520(19) Uani ? ? 1.00000 ? ? C14 .7622(6) .0047(5) .3362(3) .077(3) Uani ? ? 1.00000 ? ? C15 .6429(6) -.0490(3) .2665(3) .071(3) Uani ? ? 1.00000 ? ? C16 .5245(4) .0161(3) .1963(3) .0431(16) Uani ? ? 1.00000 ? ? C17 .8928(4) .1912(5) .4104(2) .082(3) Uani ? ? 1.00000 ? ? P1 .15247(11) .25000 .16016(7) .0219(4) Uani ? ? 1.00000 ? ? C111 .0124(4) .1274(3) .1314(2) .0403(15) Uani ? ? 1.00000 ? ? C121 .2363(5) .25000 .2955(3) .047(2) Uani ? ? 1.00000 ? ? C122 .2739(5) .1442(5) .3463(3) .081(3) Uani ? ? 1.00000 ? ? C123 .3535(6) .1470(9) .4494(3) .147(5) Uani ? ? 1.00000 ? ? C124 .3919(9) .25000 .5003(5) .199(11) Uani ? ? 1.00000 ? ? S1 .21977(12) -.25000 .20169(7) .0379(5) Uani ? ? 1.00000 ? ? O11 .1637(3) -.3544(2) .14873(19) .0567(13) Uani ? ? 1.00000 ? ? O13 .3911(4) -.25000 .2562(3) .103(3) Uani ? ? 1.00000 ? ? C0 .1172(6) -.25000 .3026(4) .054(3) Uani ? ? 1.00000 ? ? F1 .1592(4) -.3434(3) .36067(18) .1008(19) Uani ? ? 1.00000 ? ? F2 -.0464(4) -.25000 .2682(3) .069(2) Uani ? ? 1.00000 ? ? H10aA .15407 .34559 -.05193 .07700 Uiso ? ? 1.00000 ? ? H10aB .25564 .44223 .01604 .07700 Uiso ? ? 1.00000 ? ? H10aC .32621 .38856 -.06711 .07700 Uiso ? ? 1.00000 ? ? H10cA .63471 .18251 .02665 .05100 Uiso ? ? 1.00000 ? ? H10cB .51948 .25000 -.06166 .05100 Uiso ? ? 1.00000 ? ? H14 .84353 -.04012 .38392 .09600 Uiso ? ? 1.00000 ? ? H15 .63527 -.13313 .26427 .08900 Uiso ? ? 1.00000 ? ? H16 .43631 -.02342 .14638 .05800 Uiso ? ? 1.00000 ? ? H17 .97730 .15043 .45916 .10300 Uiso ? ? 1.00000 ? ? H111A -.03622 .12225 .06053 .06300 Uiso ? ? 1.00000 ? ? H111B -.07447 .13593 .16336 .06300 Uiso ? ? 1.00000 ? ? H111C .07080 .05688 .15381 .06300 Uiso ? ? 1.00000 ? ? H122 .24429 .07009 .30986 .10800 Uiso ? ? 1.00000 ? ? H123 .37797 .07307 .48606 .18300 Uiso ? ? 1.00000 ? ? H124 .44923 .25000 .56847 .25200 Uiso ? ? 1.00000 ? ? 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 .01710(14) .02963(16) .01891(14) .00000 .00415(9) .00000 C10a .0366(17) .078(3) .0415(17) .0165(17) .0135(13) .0350(18) C10c .0258(19) .048(2) .0248(18) .00000 .0103(15) .00000 N11 .0270(11) .0284(11) .0276(11) .0060(9) .0134(9) .0053(9) C12 .0206(12) .0523(17) .0212(12) .0077(11) .0106(9) .0061(11) C13 .0365(16) .097(3) .0261(15) .0319(18) .0144(12) .0172(17) C14 .089(3) .107(4) .044(2) .072(3) .030(2) .039(2) C15 .111(4) .052(2) .070(3) .050(2) .059(3) .032(2) C16 .057(2) .0311(15) .0522(18) .0127(14) .0330(16) .0076(14) C17 .0294(16) .188(6) .0247(14) .028(2) .0032(12) .014(2) P1 .0182(4) .0255(5) .0224(4) .00000 .0064(3) .00000 C111 .0333(15) .0368(16) .0543(18) -.0101(13) .0178(13) -.0009(14) C121 .0192(18) .101(4) .023(2) .00000 .0087(15) .00000 C122 .049(2) .161(5) .043(2) .053(3) .0298(16) .047(3) C123 .060(3) .339(11) .052(3) .090(5) .032(3) .086(5) C124 .031(3) .54(3) .026(3) .00000 .004(3) .00000 S1 .0254(5) .0594(7) .0278(5) .00000 .0052(4) .00000 O11 .0696(17) .0438(14) .0630(15) .0045(12) .0288(13) -.0059(12) O13 .0244(18) .240(6) .042(2) .00000 .0030(15) .00000 C0 .046(3) .072(4) .046(3) .00000 .019(2) .00000 F1 .120(2) .134(2) .0634(15) .042(2) .0498(15) .0513(16) F2 .0475(17) .086(2) .086(2) .00000 .0386(17) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Pd C10a . . 2.045(3) ? Pd C10c . . 2.082(4) ? Pd N11 . . 2.193(2) ? Pd P1 . . 2.4222(11) ? Pd C10a . 4 2.045(3) ? Pd N11 . 4 2.193(2) ? C10a H10aA . . .945(3) ? C10a H10aB . . .962(4) ? C10a H10aC . . .953(4) ? C10c H10cA . . .957(2) ? C10c H10cB . . .951(4) ? C10c H10cA . 4 .957(2) ? N11 C12 . . 1.361(3) ? N11 C16 . . 1.328(4) ? C12 C13 . . 1.410(4) ? C12 C12 . 4 1.433(4) ? C13 C14 . . 1.413(7) ? C13 C17 . . 1.421(5) ? C14 C15 . . 1.336(6) ? C14 H14 . . .959(4) ? C15 C16 . . 1.402(5) ? C15 H15 . . .968(4) ? C16 H16 . . .975(3) ? C17 H17 . . .957(3) ? C17 C17 . 4 1.352(7) ? P1 C111 . . 1.806(3) ? P1 C121 . . 1.814(4) ? P1 C111 . 4 1.806(3) ? C111 H111A . . .957(3) ? C111 H111B . . .953(4) ? C111 H111C . . .954(3) ? C121 C122 . . 1.398(5) ? C121 C122 . 4 1.398(5) ? C122 C123 . . 1.403(6) ? C122 H122 . . .987(5) ? C123 C124 . . 1.370(9) ? C123 H123 . . .983(9) ? C124 H124 . . .936(7) ? S1 O11 . . 1.418(2) ? S1 O13 . . 1.426(3) ? S1 C0 . . 1.828(6) ? S1 O11 . '4 545' 1.418(2) ? C0 F1 . . 1.330(4) ? C0 F2 . . 1.321(6) ? C0 F1 . '4 545' 1.330(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C10a Pd C10c . . . 86.58(12) ? C10a Pd N11 . . . 173.18(11) ? C10a Pd P1 . . . 92.03(10) ? C10a Pd C10a . . 4 87.02(14) ? C10a Pd N11 . . 4 97.97(11) ? C10c Pd N11 . . . 89.07(10) ? C10c Pd P1 . . . 178.09(11) ? C10c Pd C10a . . 4 86.58(12) ? C10c Pd N11 . . 4 89.07(10) ? N11 Pd P1 . . . 92.43(7) ? N11 Pd C10a . . 4 97.97(11) ? N11 Pd N11 . . 4 76.69(8) ? P1 Pd C10a . . 4 92.03(10) ? P1 Pd N11 . . 4 92.43(7) ? C10a Pd N11 4 . 4 173.18(11) ? Pd C10a H10aA . . . 107.6(3) ? Pd C10a H10aB . . . 106.7(2) ? Pd C10a H10aC . . . 110.8(3) ? H10aA C10a H10aB . . . 108.9(3) ? H10aA C10a H10aC . . . 113.7(3) ? H10aB C10a H10aC . . . 108.8(4) ? Pd C10c H10cA . . . 111.0(3) ? Pd C10c H10cB . . . 110.3(3) ? Pd C10c H10cA . . 4 111.0(3) ? H10cA C10c H10cB . . . 108.0(3) ? H10cA C10c H10cA . . 4 108.2(3) ? H10cB C10c H10cA . . 4 108.0(3) ? Pd N11 C12 . . . 112.92(17) ? Pd N11 C16 . . . 128.47(18) ? C12 N11 C16 . . . 118.4(2) ? N11 C12 C13 . . . 122.4(3) ? N11 C12 C12 . . 4 118.2(2) ? C13 C12 C12 . . 4 119.3(2) ? C12 C13 C14 . . . 116.9(3) ? C12 C13 C17 . . . 119.7(4) ? C14 C13 C17 . . . 123.5(3) ? C13 C14 C15 . . . 120.0(4) ? C13 C14 H14 . . . 120.0(4) ? C15 C14 H14 . . . 120.0(5) ? C14 C15 C16 . . . 120.2(4) ? C14 C15 H15 . . . 120.9(4) ? C16 C15 H15 . . . 118.9(4) ? N11 C16 C15 . . . 122.1(3) ? N11 C16 H16 . . . 118.0(3) ? C15 C16 H16 . . . 119.9(3) ? C13 C17 H17 . . . 119.7(5) ? C13 C17 C17 . . 4 121.0(3) ? H17 C17 C17 . . 4 119.3(4) ? Pd P1 C111 . . . 116.00(12) ? Pd P1 C121 . . . 109.68(14) ? Pd P1 C111 . . 4 116.00(12) ? C111 P1 C121 . . . 105.84(14) ? C111 P1 C111 . . 4 102.52(14) ? C121 P1 C111 . . 4 105.84(14) ? P1 C111 H111A . . . 110.1(3) ? P1 C111 H111B . . . 110.4(2) ? P1 C111 H111C . . . 110.3(2) ? H111A C111 H111B . . . 108.6(3) ? H111A C111 H111C . . . 108.6(3) ? H111B C111 H111C . . . 108.9(3) ? P1 C121 C122 . . . 119.5(2) ? P1 C121 C122 . . 4 119.5(2) ? C122 C121 C122 . . 4 120.9(4) ? C121 C122 C123 . . . 118.2(6) ? C121 C122 H122 . . . 120.1(3) ? C123 C122 H122 . . . 121.7(6) ? C122 C123 C124 . . . 121.6(7) ? C122 C123 H123 . . . 118.7(8) ? C124 C123 H123 . . . 119.7(5) ? C123 C124 H124 . . . 120.2(4) ? C123 C124 C123 . . 4 119.5(6) ? H124 C124 C123 . . 4 120.2(4) ? O11 S1 O13 . . . 114.62(12) ? O11 S1 C0 . . . 103.77(15) ? O11 S1 O11 . . '4 545' 115.62(15) ? O13 S1 C0 . . . 102.0(2) ? O13 S1 O11 . . '4 545' 114.62(12) ? C0 S1 O11 . . '4 545' 103.77(15) ? S1 C0 F1 . . . 111.2(3) ? S1 C0 F2 . . . 112.3(3) ? S1 C0 F1 . . '4 545' 111.2(3) ? F1 C0 F2 . . . 107.2(3) ? F1 C0 F1 . . '4 545' 107.5(4) ? F2 C0 F1 . . '4 545' 107.2(3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #----------------------------------------------------------------------- # Special items requested by author for inclusion in paper #----------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #----------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #----------------------------------------------------------------------- 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 Pd C12 2.997(2) . 4 ? Pd C12 2.997(2) . . ? Pd C16 3.193(3) . 4 ? Pd C16 3.193(3) . . ? Pd H10aA 2.4985(3) . 4 ? Pd H10aA 2.4985(3) . . ? Pd H10aB 2.4986(4) . 4 ? Pd H10aB 2.4986(4) . . ? Pd H10aC 2.5449(4) . 4 ? Pd H10aC 2.5449(4) . . ? Pd H10cA 2.5847(4) . . ? Pd H10cA 2.5847(4) . 4 ? Pd H10cB 2.5720(4) . . ? C10a C10a 2.816(6) . 4 ? C10a C10c 2.830(5) . . ? C10a N11 3.199(3) . 4 ? C10a P1 3.225(4) . . ? C10a H10aA 2.661(4) . 4 ? C10c N11 2.999(4) . . ? C10c N11 2.999(4) . 4 ? C10c S1 3.822(4) . '2 655' ? C10c H10aC 2.552(3) . . ? C10c H10aC 2.552(3) . 4 ? N11 N11 2.721(3) . 4 ? N11 C12 2.398(3) . 4 ? N11 C13 3.681(4) . 4 ? N11 C13 2.428(3) . . ? N11 C14 2.780(5) . . ? N11 C15 2.390(5) . . ? N11 P1 3.336(2) . . ? N11 C121 3.409(5) . . ? N11 C122 3.377(5) . . ? N11 H10aB 2.992(2) . 4 ? N11 H10cA 2.772(2) . . ? N11 H15 3.245(2) . . ? N11 H16 1.982(2) . . ? N11 H122 3.279(2) . . ? C12 C13 2.454(5) . 4 ? C12 C14 2.405(6) . . ? C12 C15 2.721(5) . . ? C12 C16 2.309(4) . . ? C12 C17 2.447(3) . . ? C12 C17 2.815(4) . 4 ? C13 C13 2.815(6) . 4 ? C13 C15 2.382(6) . . ? C13 C16 2.748(4) . . ? C13 C17 2.413(6) . 4 ? C13 H14 2.067(4) . . ? C13 H17 2.070(3) . . ? C14 C16 2.373(5) . . ? C14 C17 2.496(7) . . ? C14 F2 3.584(6) . '1 655' ? C14 H15 2.014(5) . . ? C14 H17 2.697(4) . . ? C15 F2 3.472(5) . '1 655' ? C15 H14 1.997(4) . . ? C15 H16 2.068(4) . . ? C16 P1 4.038(3) . . ? C16 H15 2.053(3) . . ? C17 F1 3.342(4) . '2 656' ? C17 H14 2.700(5) . . ? C17 H17 2.003(5) . 4 ? P1 C122 2.782(4) . 4 ? P1 C122 2.782(4) . . ? P1 H10aA 3.1417(10) . 4 ? P1 H10aA 3.1417(10) . . ? P1 H10aB 3.2489(8) . . ? P1 H10aB 3.2489(8) . 4 ? P1 H111A 2.3164(6) . 4 ? P1 H111A 2.3164(6) . . ? P1 H111B 2.3172(8) . 4 ? P1 H111B 2.3172(8) . . ? P1 H111C 2.3169(5) . . ? P1 H111C 2.3169(5) . 4 ? P1 H122 2.8813(7) . 4 ? P1 H122 2.8813(7) . . ? C111 C111 2.818(4) . 4 ? C111 C121 2.888(4) . . ? C121 C123 2.403(7) . 4 ? C121 C123 2.403(7) . . ? C121 C124 2.782(8) . . ? C121 H122 2.0766(5) . . ? C121 H122 2.0766(5) . 4 ? C122 C122 2.432(8) . 4 ? C122 C123 2.779(10) . 4 ? C122 C124 2.420(7) . . ? C122 F1 3.608(6) . '4 545' ? C122 H123 2.063(4) . . ? C123 C123 2.367(14) . 4 ? C123 H122 2.096(6) . . ? C123 H124 2.011(7) . . ? C124 H123 2.0432(8) . 4 ? C124 H123 2.0432(8) . . ? S1 F1 2.621(3) . '4 545' ? S1 F1 2.621(3) . . ? S1 F2 2.631(4) . . ? S1 H10aA 3.4286(9) . '2 545' ? S1 H10aA 3.4286(9) . 3 ? S1 H10cB 3.2908(12) . '2 645' ? S1 H15 3.6043(10) . . ? S1 H15 3.6043(10) . '4 545' ? S1 H16 3.3772(8) . '4 545' ? S1 H16 3.3772(8) . . ? S1 H124 3.6065(10) . '2 646' ? O11 O11 2.401(3) . '4 545' ? O11 O13 2.394(4) . . ? O11 C0 2.567(6) . . ? O11 F1 2.951(4) . . ? O11 F2 2.976(4) . . ? O11 H10aA 2.633(2) . 3 ? O11 H16 2.685(3) . '4 545' ? O11 H111C 2.460(2) . '4 545' ? O13 C0 2.542(7) . . ? O13 F1 2.923(5) . . ? O13 F1 2.923(5) . '4 545' ? O13 H15 2.421(3) . '4 545' ? O13 H15 2.421(3) . . ? O13 H124 2.434(3) . '2 646' ? F1 F1 2.146(5) . '4 545' ? F1 F2 2.133(4) . . ? F1 H14 3.055(3) . '4 445' ? F1 H17 3.016(3) . '2 646' ? F1 H122 2.840(3) . '4 545' ? F1 H124 3.330(3) . '2 646' ? F2 H10aA 3.087(3) . '2 545' ? F2 H10aA 3.087(3) . 3 ? F2 H14 3.169(3) . '4 445' ? F2 H14 3.169(3) . '1 455' ? F2 H15 2.970(3) . '4 445' ? F2 H15 2.970(3) . '1 455' ? H10aA H10aA 2.1972(4) . 4 ? H10aA H10aB 1.55134(18) . . ? H10aA H10aC 1.58940(17) . . ? H10aB H10aC 1.55812(15) . . ? H10aB H16 2.2204(2) . 4 ? H10aC H10cB 2.2557(3) . . ? H10cA H10cA 1.5513(3) . 4 ? H10cA H10cB 1.54460(14) . . ? H14 H15 2.3136(2) . . ? H15 H16 2.3552(2) . . ? H17 H17 2.2887(5) . 4 ? H111A H111B 1.5514(2) . . ? H111A H111C 1.55129(15) . . ? H111B H111C 1.55142(16) . . ? H111C H122 2.2575(3) . . ? H122 H123 2.3932(3) . . ? H123 H124 2.3289(4) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 628 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -18 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high .726 _reflns_d_resolution_low 13.3 _diffrn_reflns_av_sigmaI/netI .044 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .043 _refine_ls_wR_factor_all .043 _refine_ls_goodness_of_fit_all 1.22 _refine_ls_shift/su_mean .001 #======================================================================= # Structure Factor lists should be submitted as separate files #======================================================================= #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #===END