Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1201 data_global _audit_creation_method Xtal3.6 _audit_creation_date 01-03-22 _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_Cambridge 186 _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 #---------------------- loop_ _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; loop_ _publ_author_name 'Atkinson, Ian M.' 'Chartres, Jy D.' 'Groth, Andrew M.' 'Lindoy, L.' 'Lowe, Mark P.' 'Meehan, George V.' 'White, A.H.' _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 ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; _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_llsyd _database_code_CSD 165073 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C19 H32 F12 N2 P2 Pd1 S2' _chemical_formula_moiety ? _chemical_formula_weight 748.95 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc 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 8.712(3) _cell_length_b 9.094(2) _cell_length_c 34.48(2) _cell_angle_alpha 90.00000 _cell_angle_beta 92.00(4) _cell_angle_gamma 90.00000 _cell_volume 2730(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 23.5 _cell_measurement_theta_max 24 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.046 _exptl_crystal_description block _exptl_crystal_size_max .75 _exptl_crystal_size_mid .65 _exptl_crystal_size_min .65 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .53 _exptl_absorpt_correction_T_max .57 _diffrn_reflns_number 8410 _reflns_number_total 7957 _reflns_Friedel_coverage ? _reflns_number_gt 6948 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 29.99 _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 -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .044 _refine_ls_wR_factor_ref .052 _refine_ls_goodness_of_fit_ref 1.33 _refine_ls_number_reflns 6948 _refine_ls_number_parameters 362 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .054 _refine_diff_density_min -.818 _refine_diff_density_max 1.32 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 12186(536) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _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 76 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 128 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 48 .013977 .01001 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 0 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .090027 .094971 '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 8 .109985 .124023 '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 .64081(2) .63942(2) .374490(10) .03134(12) Uani ? ? 1.00000 ? ? N10 .5456(3) .5374(3) .32412(7) .0379(13) Uani ? ? 1.00000 ? ? C10 .5306(4) .3732(3) .33055(10) .0442(17) Uani ? ? 1.00000 ? ? C1 .4129(4) .3298(3) .35937(10) .0406(16) Uani ? ? 1.00000 ? ? C2 .4392(4) .3514(4) .39872(10) .0470(18) Uani ? ? 1.00000 ? ? C3 .3286(5) .3111(4) .42510(12) .059(2) Uani ? ? 1.00000 ? ? C4 .1943(4) .2485(5) .41239(13) .066(3) Uani ? ? 1.00000 ? ? C5 .1680(4) .2247(5) .37374(14) .069(3) Uani ? ? 1.00000 ? ? C6 .2757(4) .2651(4) .34672(11) .054(2) Uani ? ? 1.00000 ? ? C11 .3851(4) .5910(4) .31323(11) .051(2) Uani ? ? 1.00000 ? ? C12 .3670(5) .7503(4) .30157(11) .061(2) Uani ? ? 1.00000 ? ? C13 .3998(5) .8638(4) .33191(13) .063(2) Uani ? ? 1.00000 ? ? S14 .42578(9) .78708(9) .38041(3) .0429(4) Uani ? ? 1.00000 ? ? C15 .5053(4) .9487(4) .40445(12) .057(2) Uani ? ? 1.00000 ? ? C16 .5475(5) .9190(5) .44626(11) .060(2) Uani ? ? 1.00000 ? ? C17 .6180(5) .7668(5) .45512(10) .056(2) Uani ? ? 1.00000 ? ? C21 .6433(4) .5639(4) .28980(10) .052(2) Uani ? ? 1.00000 ? ? C22 .7978(5) .4891(4) .28993(10) .058(2) Uani ? ? 1.00000 ? ? C23 .9169(4) .5440(4) .31997(11) .054(2) Uani ? ? 1.00000 ? ? S24 .86319(9) .50192(9) .36914(3) .0444(4) Uani ? ? 1.00000 ? ? C25 1.0106(4) .5994(4) .39728(11) .053(2) Uani ? ? 1.00000 ? ? C26 .9882(4) .7656(5) .39844(11) .056(2) Uani ? ? 1.00000 ? ? C27 .8683(4) .8185(4) .42533(11) .052(2) Uani ? ? 1.00000 ? ? N20 .7335(3) .7178(3) .42674(8) .0423(14) Uani ? ? 1.00000 ? ? P1 .83792(11) .01194(11) .29295(3) .0503(5) Uani ? ? 1.00000 ? ? F11 .7708(3) -.1041(3) .32292(8) .0882(19) Uani ? ? 1.00000 ? ? F12 .8976(3) .1215(3) .26222(10) .106(2) Uani ? ? 1.00000 ? ? F13 1.0056(3) -.0442(3) .30362(8) .089(2) Uani ? ? 1.00000 ? ? F14 .8472(4) .1272(3) .32666(10) .109(2) Uani ? ? 1.00000 ? ? F15 .6672(3) .0688(3) .28302(7) .0791(16) Uani ? ? 1.00000 ? ? F16 .8178(4) -.1078(3) .26011(9) .112(2) Uani ? ? 1.00000 ? ? P2 .79892(11) .29427(12) .48627(3) .0538(5) Uani ? ? 1.00000 ? ? F21 .6221(3) .2616(3) .48033(7) .0827(18) Uani ? ? 1.00000 ? ? F22 .9765(3) .3225(4) .49197(11) .116(3) Uani ? ? 1.00000 ? ? F23 .8210(4) .2107(5) .44545(11) .125(3) Uani ? ? .867(2) ? ? F24 .7818(5) .4400(4) .46364(14) .139(3) Uani ? ? .867(2) ? ? F25 .7744(4) .3591(5) .52685(10) .118(3) Uani ? ? .867(2) ? ? F26 .8182(5) .1354(4) .50567(14) .122(3) Uani ? ? .867(2) ? ? F23' .8211(18) .3324(18) .4438(5) .059(4) Uiso ? ? .133(2) ? ? F24' .740(3) .458(3) .4990(7) .102(7) Uiso ? ? .133(2) ? ? F25' .7874(19) .225(2) .5269(5) .065(4) Uiso ? ? .133(2) ? ? F26' .868(2) .1581(19) .4755(5) .065(4) Uiso ? ? .133(2) ? ? H10a .62867 .33457 .33931 .05600 Uiso ? ? 1.00000 ? ? H10b .50395 .32724 .30614 .05600 Uiso ? ? 1.00000 ? ? H2 .53487 .39257 .40804 .05800 Uiso ? ? 1.00000 ? ? H3 .34791 .33027 .45240 .07400 Uiso ? ? 1.00000 ? ? H4 .11866 .21933 .43075 .08000 Uiso ? ? 1.00000 ? ? H5 .07216 .18243 .36487 .08500 Uiso ? ? 1.00000 ? ? H6 .25564 .24665 .31897 .07000 Uiso ? ? 1.00000 ? ? H11a .32178 .57534 .33567 .06200 Uiso ? ? 1.00000 ? ? H11b .34399 .53089 .29279 .06200 Uiso ? ? 1.00000 ? ? H12a .26358 .76610 .29193 .07600 Uiso ? ? 1.00000 ? ? H12b .43476 .76848 .28098 .07600 Uiso ? ? 1.00000 ? ? H13a .31559 .93206 .33222 .07600 Uiso ? ? 1.00000 ? ? H13b .49018 .91617 .32580 .07600 Uiso ? ? 1.00000 ? ? H15a .43212 1.02870 .40322 .07100 Uiso ? ? 1.00000 ? ? H15b .59563 .98224 .39165 .07100 Uiso ? ? 1.00000 ? ? H16a .45729 .92813 .46096 .07400 Uiso ? ? 1.00000 ? ? H16b .62088 .99032 .45540 .07400 Uiso ? ? 1.00000 ? ? H17a .53435 .69941 .45566 .06900 Uiso ? ? 1.00000 ? ? H17b .66472 .77248 .48067 .06900 Uiso ? ? 1.00000 ? ? H21a .66215 .66839 .28799 .06400 Uiso ? ? 1.00000 ? ? H21b .58619 .53492 .26690 .06400 Uiso ? ? 1.00000 ? ? H22a .83825 .49900 .26451 .07000 Uiso ? ? 1.00000 ? ? H22b .78029 .38672 .29455 .07000 Uiso ? ? 1.00000 ? ? H23a .92936 .64785 .31715 .06900 Uiso ? ? 1.00000 ? ? H23b 1.01499 .49862 .31514 .06900 Uiso ? ? 1.00000 ? ? H25a 1.10850 .57746 .38735 .06700 Uiso ? ? 1.00000 ? ? H25b 1.00955 .56586 .42377 .06700 Uiso ? ? 1.00000 ? ? H26a .95867 .79447 .37181 .07000 Uiso ? ? 1.00000 ? ? H26b 1.08480 .81018 .40443 .07000 Uiso ? ? 1.00000 ? ? H27a .83078 .91341 .41735 .06800 Uiso ? ? 1.00000 ? ? H27b .91284 .82753 .45097 .06800 Uiso ? ? 1.00000 ? ? H20 .77794 .63053 .43520 .05300 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 .03179(12) .02928(12) .03302(12) .00224(9) .00202(8) -.00056(9) N10 .0456(14) .0340(13) .0340(13) .0006(11) -.0005(11) -.0007(10) C10 .0530(19) .0345(16) .0452(18) .0014(14) .0033(14) -.0063(14) C1 .0429(16) .0305(15) .0483(18) .0024(12) -.0013(14) -.0038(13) C2 .0469(18) .0436(18) .050(2) -.0047(15) -.0037(15) .0019(15) C3 .066(2) .052(2) .060(2) .0041(19) .0117(19) .0037(19) C4 .048(2) .060(2) .091(3) .0039(19) .022(2) .006(2) C5 .0366(18) .060(3) .110(4) -.0044(17) -.006(2) .004(2) C6 .054(2) .046(2) .063(2) -.0012(17) -.0100(17) -.0049(17) C11 .054(2) .0438(18) .054(2) .0031(16) -.0161(16) -.0055(16) C12 .072(3) .050(2) .059(2) .013(2) -.011(2) .0051(18) C13 .072(3) .046(2) .070(3) .0145(19) -.008(2) .0090(19) S14 .0352(4) .0403(4) .0535(5) .0037(3) .0075(3) -.0050(4) C15 .061(2) .0352(18) .076(3) .0031(16) .008(2) -.0113(18) C16 .068(2) .055(2) .059(2) -.002(2) .0153(19) -.025(2) C17 .070(2) .062(2) .0366(17) -.003(2) .0123(16) -.0070(17) C21 .065(2) .054(2) .0390(18) -.0059(18) .0029(16) .0010(16) C22 .074(3) .058(2) .045(2) -.004(2) .0230(18) -.0058(17) C23 .051(2) .059(2) .054(2) .0065(17) .0183(16) .0045(18) S24 .0410(4) .0423(4) .0502(5) .0108(3) .0058(3) .0043(4) C25 .0351(16) .061(2) .064(2) .0066(16) -.0029(15) .0073(19) C26 .0381(17) .062(2) .066(2) -.0075(17) -.0072(16) .006(2) C27 .0457(18) .051(2) .060(2) -.0067(16) -.0089(16) -.0062(17) N20 .0460(15) .0404(15) .0405(14) -.0005(12) .0009(11) -.0008(12) P1 .0549(5) .0477(5) .0485(5) .0085(4) .0019(4) .0056(4) F11 .0847(18) .090(2) .091(2) .0072(15) .0120(15) .0419(16) F12 .089(2) .101(2) .129(3) .0109(17) .0328(18) .062(2) F13 .0604(15) .106(2) .102(2) .0282(15) .0064(14) .0226(17) F14 .103(2) .112(2) .110(2) .0263(18) -.0354(18) -.055(2) F15 .0629(14) .107(2) .0671(15) .0211(15) -.0035(12) .0183(15) F16 .171(3) .082(2) .082(2) .020(2) -.013(2) -.0277(16) P2 .0493(5) .0567(6) .0553(6) -.0075(5) -.0001(4) .0084(5) F21 .0536(13) .118(2) .0767(17) -.0109(15) -.0013(12) .0018(16) F22 .0580(16) .149(3) .138(3) -.0335(18) -.0047(17) .015(2) F23 .119(3) .154(4) .105(3) -.026(3) .038(2) -.064(3) F24 .154(4) .076(2) .182(4) -.029(2) -.040(3) .081(3) F25 .120(3) .161(4) .074(2) -.009(3) -.006(2) -.055(2) F26 .121(3) .069(2) .173(4) -.002(2) -.021(3) .043(2) # 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 N10 . . 2.113(3) ? Pd S14 . . 2.3197(10) ? Pd S24 . . 2.3186(10) ? Pd N20 . . 2.075(3) ? N10 C10 . . 1.516(4) ? N10 C11 . . 1.516(4) ? N10 C21 . . 1.501(4) ? C10 C1 . . 1.505(5) ? C10 H10a . . .963(3) ? C10 H10b . . .961(3) ? C1 C2 . . 1.382(5) ? C1 C6 . . 1.389(5) ? C2 C3 . . 1.397(5) ? C2 H2 . . .959(3) ? C3 C4 . . 1.360(6) ? C3 H3 . . .966(4) ? C4 C5 . . 1.362(7) ? C4 H4 . . .967(4) ? C5 C6 . . 1.395(6) ? C5 H5 . . .959(4) ? C6 H6 . . .981(4) ? C11 C12 . . 1.510(5) ? C11 H11a . . .976(4) ? C11 H11b . . .952(4) ? C12 C13 . . 1.490(6) ? C12 H12a . . .960(4) ? C12 H12b . . .954(4) ? C13 S14 . . 1.819(5) ? C13 H13a . . .962(4) ? C13 H13b . . .950(4) ? S14 C15 . . 1.813(4) ? C15 C16 . . 1.500(6) ? C15 H15a . . .967(4) ? C15 H15b . . .965(4) ? C16 C17 . . 1.540(6) ? C16 H16a . . .954(4) ? C16 H16b . . .956(4) ? C17 N20 . . 1.496(5) ? C17 H17a . . .953(4) ? C17 H17b . . .959(4) ? C21 C22 . . 1.508(6) ? C21 H21a . . .967(4) ? C21 H21b . . .956(4) ? C22 C23 . . 1.524(5) ? C22 H22a . . .960(4) ? C22 H22b . . .958(4) ? C23 S24 . . 1.815(4) ? C23 H23a . . .956(4) ? C23 H23b . . .969(4) ? S24 C25 . . 1.813(4) ? C25 C26 . . 1.525(6) ? C25 H25a . . .952(3) ? C25 H25b . . .963(4) ? C26 C27 . . 1.500(5) ? C26 H26a . . .981(4) ? C26 H26b . . .950(3) ? C27 N20 . . 1.491(4) ? C27 H27a . . .960(4) ? C27 H27b . . .957(4) ? N20 H20 . . .926(3) ? P1 F11 . . 1.602(3) ? P1 F12 . . 1.557(3) ? P1 F13 . . 1.578(3) ? P1 F14 . . 1.565(4) ? P1 F15 . . 1.600(3) ? P1 F16 . . 1.576(3) ? P2 F21 . . 1.575(3) ? P2 F22 . . 1.574(3) ? P2 F23 . . 1.617(4) ? P2 F24 . . 1.542(4) ? P2 F25 . . 1.540(4) ? P2 F26 . . 1.599(4) ? P2 F23' . . 1.524(16) ? P2 F24' . . 1.64(2) ? P2 F25' . . 1.542(17) ? P2 F26' . . 1.429(17) ? F23 F23' . . 1.109(17) ? F23 F26' . . 1.199(18) ? F24 F23' . . 1.249(17) ? F24 F24' . . 1.30(2) ? F25 F24' . . 1.34(2) ? F25 F25' . . 1.226(18) ? F26 F25' . . 1.133(18) ? F26 F26' . . 1.158(18) ? 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 N10 Pd S14 . . . 91.79(8) ? N10 Pd S24 . . . 90.18(8) ? N10 Pd N20 . . . 173.92(10) ? S14 Pd S24 . . . 177.19(4) ? S14 Pd N20 . . . 90.90(8) ? S24 Pd N20 . . . 87.33(8) ? Pd N10 C10 . . . 110.22(18) ? Pd N10 C11 . . . 113.3(2) ? Pd N10 C21 . . . 111.1(2) ? C10 N10 C11 . . . 105.7(2) ? C10 N10 C21 . . . 109.1(3) ? C11 N10 C21 . . . 107.3(2) ? N10 C10 C1 . . . 114.8(3) ? N10 C10 H10a . . . 109.0(3) ? N10 C10 H10b . . . 108.6(3) ? C1 C10 H10a . . . 108.4(3) ? C1 C10 H10b . . . 108.4(3) ? H10a C10 H10b . . . 107.5(3) ? C10 C1 C2 . . . 121.2(3) ? C10 C1 C6 . . . 120.2(3) ? C2 C1 C6 . . . 118.7(3) ? C1 C2 C3 . . . 120.5(3) ? C1 C2 H2 . . . 119.8(3) ? C3 C2 H2 . . . 119.7(3) ? C2 C3 C4 . . . 120.3(4) ? C2 C3 H3 . . . 119.1(4) ? C4 C3 H3 . . . 120.5(4) ? C3 C4 C5 . . . 119.7(4) ? C3 C4 H4 . . . 120.2(4) ? C5 C4 H4 . . . 120.1(4) ? C4 C5 C6 . . . 121.2(4) ? C4 C5 H5 . . . 119.4(4) ? C6 C5 H5 . . . 119.4(4) ? C1 C6 C5 . . . 119.6(4) ? C1 C6 H6 . . . 120.1(4) ? C5 C6 H6 . . . 120.3(4) ? N10 C11 C12 . . . 117.5(3) ? N10 C11 H11a . . . 107.4(3) ? N10 C11 H11b . . . 108.6(3) ? C12 C11 H11a . . . 107.1(3) ? C12 C11 H11b . . . 108.7(3) ? H11a C11 H11b . . . 107.1(3) ? C11 C12 C13 . . . 117.5(3) ? C11 C12 H12a . . . 108.9(4) ? C11 C12 H12b . . . 107.6(4) ? C13 C12 H12a . . . 107.1(4) ? C13 C12 H12b . . . 107.1(4) ? H12a C12 H12b . . . 108.3(4) ? C12 C13 S14 . . . 113.2(3) ? C12 C13 H13a . . . 109.1(4) ? C12 C13 H13b . . . 109.4(4) ? S14 C13 H13a . . . 107.9(3) ? S14 C13 H13b . . . 108.6(3) ? H13a C13 H13b . . . 108.5(4) ? Pd S14 C13 . . . 102.48(14) ? Pd S14 C15 . . . 102.27(12) ? C13 S14 C15 . . . 98.20(18) ? S14 C15 C16 . . . 111.7(3) ? S14 C15 H15a . . . 110.4(3) ? S14 C15 H15b . . . 110.6(3) ? C16 C15 H15a . . . 108.5(4) ? C16 C15 H15b . . . 108.7(3) ? H15a C15 H15b . . . 106.8(3) ? C15 C16 C17 . . . 115.8(3) ? C15 C16 H16a . . . 108.4(3) ? C15 C16 H16b . . . 109.5(4) ? C17 C16 H16a . . . 107.6(3) ? C17 C16 H16b . . . 106.7(3) ? H16a C16 H16b . . . 108.6(4) ? C16 C17 N20 . . . 114.2(3) ? C16 C17 H17a . . . 106.4(3) ? C16 C17 H17b . . . 106.7(3) ? N20 C17 H17a . . . 110.7(3) ? N20 C17 H17b . . . 110.1(3) ? H17a C17 H17b . . . 108.5(4) ? N10 C21 C22 . . . 117.1(3) ? N10 C21 H21a . . . 108.1(3) ? N10 C21 H21b . . . 108.3(3) ? C22 C21 H21a . . . 106.9(3) ? C22 C21 H21b . . . 108.5(3) ? H21a C21 H21b . . . 107.6(4) ? C21 C22 C23 . . . 116.1(3) ? C21 C22 H22a . . . 108.1(3) ? C21 C22 H22b . . . 107.0(4) ? C23 C22 H22a . . . 109.0(4) ? C23 C22 H22b . . . 108.3(3) ? H22a C22 H22b . . . 108.0(4) ? C22 C23 S24 . . . 112.0(3) ? C22 C23 H23a . . . 109.4(3) ? C22 C23 H23b . . . 109.1(3) ? S24 C23 H23a . . . 109.7(3) ? S24 C23 H23b . . . 109.2(3) ? H23a C23 H23b . . . 107.4(4) ? Pd S24 C23 . . . 101.75(12) ? Pd S24 C25 . . . 105.78(12) ? C23 S24 C25 . . . 101.31(17) ? S24 C25 C26 . . . 114.2(2) ? S24 C25 H25a . . . 109.4(3) ? S24 C25 H25b . . . 108.9(3) ? C26 C25 H25a . . . 109.5(3) ? C26 C25 H25b . . . 106.5(3) ? H25a C25 H25b . . . 108.2(3) ? C25 C26 C27 . . . 115.2(3) ? C25 C26 H26a . . . 105.7(3) ? C25 C26 H26b . . . 108.4(3) ? C27 C26 H26a . . . 109.1(3) ? C27 C26 H26b . . . 111.1(4) ? H26a C26 H26b . . . 106.9(4) ? C26 C27 N20 . . . 112.9(3) ? C26 C27 H27a . . . 110.4(3) ? C26 C27 H27b . . . 109.3(3) ? N20 C27 H27a . . . 107.5(3) ? N20 C27 H27b . . . 108.5(3) ? H27a C27 H27b . . . 108.1(4) ? Pd N20 C17 . . . 114.8(2) ? Pd N20 C27 . . . 117.8(2) ? Pd N20 H20 . . . 97.2(2) ? C17 N20 C27 . . . 112.8(3) ? C17 N20 H20 . . . 109.4(3) ? C27 N20 H20 . . . 102.4(2) ? F11 P1 F12 . . . 177.13(17) ? F11 P1 F13 . . . 89.55(15) ? F11 P1 F14 . . . 88.43(17) ? F11 P1 F15 . . . 89.63(14) ? F11 P1 F16 . . . 88.55(17) ? F12 P1 F13 . . . 92.14(16) ? F12 P1 F14 . . . 93.85(18) ? F12 P1 F15 . . . 88.70(15) ? F12 P1 F16 . . . 89.10(18) ? F13 P1 F14 . . . 91.14(17) ? F13 P1 F15 . . . 178.87(15) ? F13 P1 F16 . . . 91.31(18) ? F14 P1 F15 . . . 88.05(16) ? F14 P1 F16 . . . 176.1(2) ? F15 P1 F16 . . . 89.45(17) ? F21 P2 F22 . . . 178.48(19) ? F21 P2 F23 . . . 86.77(17) ? F21 P2 F24 . . . 91.1(2) ? F21 P2 F25 . . . 91.39(18) ? F21 P2 F26 . . . 88.41(19) ? F21 P2 F23' . . . 94.3(6) ? F21 P2 F24' . . . 83.7(8) ? F21 P2 F25' . . . 86.9(6) ? F21 P2 F26' . . . 102.6(7) ? F22 P2 F23 . . . 92.2(2) ? F22 P2 F24 . . . 90.0(2) ? F22 P2 F25 . . . 89.5(2) ? F22 P2 F26 . . . 90.4(2) ? F22 P2 F23' . . . 85.7(6) ? F22 P2 F24' . . . 97.8(8) ? F22 P2 F25' . . . 92.8(6) ? F22 P2 F26' . . . 75.8(7) ? F23 P2 F24 . . . 88.6(2) ? F23 P2 F25 . . . 174.4(2) ? F23 P2 F26 . . . 85.7(2) ? F23 P2 F23' . . . 41.2(6) ? F23 P2 F24' . . . 135.0(8) ? F23 P2 F25' . . . 127.7(7) ? F23 P2 F26' . . . 45.8(7) ? F24 P2 F25 . . . 96.7(2) ? F24 P2 F26 . . . 174.3(2) ? F24 P2 F23' . . . 48.1(6) ? F24 P2 F24' . . . 47.9(9) ? F24 P2 F25' . . . 143.4(7) ? F24 P2 F26' . . . 130.3(7) ? F25 P2 F26 . . . 89.0(2) ? F25 P2 F23' . . . 144.3(6) ? F25 P2 F24' . . . 49.8(8) ? F25 P2 F25' . . . 46.9(7) ? F25 P2 F26' . . . 129.8(7) ? F26 P2 F23' . . . 126.4(6) ? F26 P2 F24' . . . 137.6(9) ? F26 P2 F25' . . . 42.2(7) ? F26 P2 F26' . . . 44.5(7) ? F23' P2 F24' . . . 95.9(10) ? F23' P2 F25' . . . 168.5(9) ? F23' P2 F26' . . . 83.1(9) ? F24' P2 F25' . . . 95.6(11) ? F24' P2 F26' . . . 173.6(10) ? F25' P2 F26' . . . 85.5(10) ? P2 F23 F23' . . . 64.9(9) ? P2 F23 F26' . . . 58.8(8) ? F23' F23 F26' . . . 116.2(12) ? P2 F24 F23' . . . 65.2(8) ? P2 F24 F24' . . . 70.0(11) ? F23' F24 F24' . . . 135.0(13) ? P2 F25 F24' . . . 69.0(10) ? P2 F25 F25' . . . 66.6(8) ? F24' F25 F25' . . . 133.3(13) ? P2 F26 F25' . . . 66.2(9) ? P2 F26 F26' . . . 60.0(9) ? F25' F26 F26' . . . 123.7(13) ? P2 F23' F23 . . . 73.9(9) ? P2 F23' F24 . . . 66.7(8) ? F23 F23' F24 . . . 138.8(15) ? P2 F24' F24 . . . 62.1(10) ? P2 F24' F25 . . . 61.2(10) ? F24 F24' F25 . . . 121.7(18) ? P2 F25' F25 . . . 66.5(8) ? P2 F25' F26 . . . 71.6(9) ? F25 F25' F26 . . . 137.7(16) ? P2 F26' F23 . . . 75.4(9) ? P2 F26' F26 . . . 75.5(10) ? F23 F26' F26 . . . 136.3(16) ? 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 C10 2.996(3) . . ? Pd C1 3.474(3) . . ? Pd C2 3.278(3) . . ? Pd C11 3.048(4) . . ? Pd C12 3.551(4) . . ? Pd C13 3.242(4) . . ? Pd C15 3.233(4) . . ? Pd C17 3.025(4) . . ? Pd C21 3.001(4) . . ? Pd C22 3.538(4) . . ? Pd C23 3.223(4) . . ? Pd C25 3.309(3) . . ? Pd C26 3.314(4) . . ? Pd C27 3.068(4) . . ? Pd F11 3.166(3) . '1 565' ? Pd F24 3.740(5) . . ? Pd F23' 3.963(16) . . ? Pd H10a 3.0264(7) . . ? Pd H2 2.7026(6) . . ? Pd H11a 3.0978(9) . . ? Pd H17a 3.0285(16) . . ? Pd H21a 3.0063(18) . . ? Pd H20 2.3751(11) . . ? N10 C1 2.545(4) . . ? N10 C12 2.586(5) . . ? N10 C22 2.567(5) . . ? N10 H10a 2.043(2) . . ? N10 H10b 2.038(2) . . ? N10 H11a 2.033(3) . . ? N10 H11b 2.030(3) . . ? N10 H21a 2.023(3) . . ? N10 H21b 2.017(3) . . ? C10 C2 2.516(5) . . ? C10 C6 2.509(5) . . ? C10 C11 2.416(5) . . ? C10 C21 2.458(5) . . ? C10 C22 2.953(5) . . ? C10 F14 3.557(5) . . ? C10 F15 3.450(4) . . ? C10 H11b 2.499(3) . . ? C1 C3 2.413(6) . . ? C1 C4 2.785(5) . . ? C1 C5 2.405(5) . . ? C1 C11 2.865(5) . . ? C1 H10a 2.026(3) . . ? C1 H10b 2.025(4) . . ? C1 H2 2.036(3) . . ? C1 H6 2.063(3) . . ? C1 H11a 2.498(3) . . ? C2 C4 2.391(5) . . ? C2 C5 2.740(5) . . ? C2 C6 2.383(5) . . ? C2 F21 3.288(4) . . ? C2 F23' 3.627(16) . . ? C2 H3 2.049(4) . . ? C3 C5 2.353(6) . . ? C3 C6 2.758(6) . . ? C3 F21 3.167(5) . . ? C3 F25 3.557(6) . '3 666' ? C3 F24' 3.42(2) . '3 666' ? C3 H2 2.049(4) . . ? C3 H4 2.026(4) . . ? C4 C6 2.401(6) . . ? C4 F22 3.457(6) . '1 455' ? C4 F23 3.501(6) . '1 455' ? C4 F23' 3.546(17) . '1 455' ? C4 H3 2.029(4) . . ? C4 H5 2.014(4) . . ? C5 F14 3.304(5) . '1 455' ? C5 H4 2.027(5) . . ? C5 H6 2.071(5) . . ? C6 H5 2.044(4) . . ? C11 C13 2.565(5) . . ? C11 S14 2.935(4) . . ? C11 C21 2.429(5) . . ? C11 F12 3.530(5) . '2 655' ? C11 F15 3.340(5) . '2 655' ? C11 F16 3.532(5) . '2 655' ? C11 H12a 2.035(4) . . ? C11 H12b 2.015(4) . . ? C11 H21b 2.465(4) . . ? C12 S14 2.769(4) . . ? C12 C21 2.984(6) . . ? C12 F12 3.342(5) . '2 655' ? C12 F13 3.665(5) . '1 465' ? C12 F15 3.355(5) . '2 655' ? C12 H11a 2.025(4) . . ? C12 H11b 2.027(4) . . ? C12 H13a 2.021(4) . . ? C12 H13b 2.016(4) . . ? C13 C15 2.745(6) . . ? C13 F11 3.271(5) . '1 565' ? C13 F13 3.635(5) . '1 465' ? C13 F15 3.467(5) . '1 565' ? C13 H12a 1.996(4) . . ? C13 H12b 1.991(4) . . ? S14 C16 2.748(4) . . ? S14 C17 3.029(4) . . ? S14 F25' 3.754(17) . '3 666' ? S14 H13a 2.3042(12) . . ? S14 H13b 2.3048(13) . . ? S14 H15a 2.3338(10) . . ? S14 H15b 2.3344(9) . . ? C15 C17 2.575(5) . . ? C15 N20 2.974(5) . . ? C15 H16a 2.016(4) . . ? C15 H16b 2.030(4) . . ? C16 N20 2.550(5) . . ? C16 F21 3.398(5) . '3 666' ? C16 F21 3.385(5) . '1 565' ? C16 F23 3.566(6) . '1 565' ? C16 F26 3.646(6) . '1 565' ? C16 F25' 3.357(17) . '3 666' ? C16 F26' 3.650(18) . '1 565' ? C16 H15a 2.026(4) . . ? C16 H15b 2.027(4) . . ? C16 H17a 2.027(4) . . ? C16 H17b 2.035(4) . . ? C17 C27 2.487(5) . . ? C17 F21 3.118(5) . '3 666' ? C17 F24 3.306(6) . . ? C17 F24' 3.35(2) . . ? C17 F25' 3.608(17) . '3 666' ? C17 H16a 2.043(4) . . ? C17 H16b 2.033(4) . . ? C17 H20 2.004(4) . . ? C21 C23 2.573(5) . . ? C21 F11 3.401(5) . '1 565' ? C21 F15 3.626(4) . '2 655' ? C21 F16 3.519(5) . '1 565' ? C21 H22a 2.024(4) . . ? C21 H22b 2.008(4) . . ? C22 S24 2.773(4) . . ? C22 F12 3.473(5) . '2 755' ? C22 F12 3.592(5) . . ? C22 F14 3.547(5) . . ? C22 H21a 2.013(4) . . ? C22 H21b 2.025(4) . . ? C22 H23a 2.050(4) . . ? C22 H23b 2.057(4) . . ? C23 C25 2.806(5) . . ? C23 F11 3.446(5) . '1 565' ? C23 F12 3.385(5) . '2 755' ? C23 H22a 2.050(4) . . ? C23 H22b 2.039(4) . . ? S24 C26 2.807(4) . . ? S24 N20 3.039(3) . . ? S24 F14 3.710(3) . . ? S24 F23 3.761(4) . . ? S24 F24 3.406(5) . . ? S24 F23' 3.033(16) . . ? S24 H23a 2.3193(13) . . ? S24 H23b 2.3213(13) . . ? S24 H25a 2.3108(10) . . ? S24 H25b 2.3118(13) . . ? C25 C27 2.555(5) . . ? C25 N20 2.862(4) . . ? C25 F24 3.410(6) . . ? C25 F25 3.187(5) . '3 766' ? C25 F23' 3.372(17) . . ? C25 F25' 3.489(17) . '3 766' ? C25 H26a 2.024(4) . . ? C25 H26b 2.036(4) . . ? C25 H20 2.466(4) . . ? C26 N20 2.493(4) . . ? C26 F11 3.380(5) . '1 565' ? C26 F25 3.439(5) . '3 766' ? C26 F25' 3.180(17) . '3 766' ? C26 H25a 2.050(4) . . ? C26 H25b 2.022(4) . . ? C26 H27a 2.043(4) . . ? C26 H27b 2.028(4) . . ? C27 F22 3.367(5) . '3 766' ? C27 F23 3.659(6) . '1 565' ? C27 F26 3.583(6) . '3 766' ? C27 F25' 3.395(17) . '3 766' ? C27 F26' 3.541(18) . '1 565' ? C27 H26a 2.043(4) . . ? C27 H26b 2.044(4) . . ? C27 H20 1.917(4) . . ? N20 F24 2.854(5) . . ? N20 F23' 3.631(16) . . ? N20 F24' 3.43(2) . . ? N20 H17a 2.038(3) . . ? N20 H17b 2.035(3) . . ? N20 H27a 2.001(3) . . ? N20 H27b 2.011(3) . . ? F11 F12 3.157(4) . . ? F11 F13 2.240(4) . . ? F11 F14 2.208(4) . . ? F11 F15 2.257(4) . . ? F11 F16 2.218(4) . . ? F11 H13b 2.457(3) . '1 545' ? F11 H15b 2.969(3) . '1 545' ? F11 H21a 2.559(3) . '1 545' ? F11 H23a 2.656(3) . '1 545' ? F11 H26a 2.486(3) . '1 545' ? F12 F13 2.258(4) . . ? F12 F13 3.905(4) . '2 755' ? F12 F14 2.280(5) . . ? F12 F15 2.207(4) . . ? F12 F16 2.198(4) . . ? F12 F16 3.597(5) . '2 755' ? F12 H11b 2.903(3) . '2 645' ? F12 H12a 2.647(3) . '2 645' ? F12 H22a 2.745(3) . '2 745' ? F12 H22b 2.861(3) . . ? F12 H23b 3.014(4) . '2 745' ? F13 F14 2.245(4) . . ? F13 F15 3.178(4) . . ? F13 F16 2.256(4) . . ? F13 H5 2.993(3) . '1 655' ? F13 H12a 2.873(3) . '1 645' ? F13 H13a 2.851(3) . '1 645' ? F13 H22a 2.783(3) . '2 745' ? F13 H23a 2.920(3) . '1 545' ? F13 H26a 2.813(3) . '1 545' ? F14 F15 2.200(4) . . ? F14 F16 3.139(5) . . ? F14 F23 4.180(6) . . ? F14 H10a 2.726(3) . . ? F14 H5 2.377(3) . '1 655' ? F14 H22b 2.663(3) . . ? F15 F16 2.235(4) . . ? F15 H10a 3.125(3) . . ? F15 H10b 2.874(3) . . ? F15 H11b 2.635(3) . '2 645' ? F15 H12b 2.970(3) . '2 645' ? F15 H13b 2.577(3) . '1 545' ? F15 H21b 2.769(2) . '2 645' ? F15 H22b 3.076(3) . . ? F16 H6 3.078(3) . '2 645' ? F16 H11b 2.593(3) . '2 645' ? F16 H21a 2.646(3) . '1 545' ? F16 H23a 3.101(3) . '1 545' ? F21 F22 3.148(4) . . ? F21 F23 2.193(5) . . ? F21 F24 2.225(5) . . ? F21 F25 2.229(4) . . ? F21 F26 2.213(5) . . ? F21 F23' 2.272(16) . . ? F21 F24' 4.14(2) . '3 666' ? F21 F24' 2.15(2) . . ? F21 F25' 2.144(17) . . ? F21 F26' 2.347(17) . . ? F21 H2 2.842(3) . . ? F21 H3 2.620(2) . . ? F21 H16a 2.766(3) . '3 666' ? F21 H16b 2.613(3) . '1 545' ? F21 H17a 2.658(3) . '3 666' ? F21 H17b 2.895(2) . '3 666' ? F22 F22 3.299(5) . '3 766' ? F22 F23 2.300(5) . . ? F22 F24 3.350(5) . '3 766' ? F22 F24 2.204(5) . . ? F22 F25 3.690(5) . '3 766' ? F22 F25 2.192(5) . . ? F22 F26 2.251(5) . . ? F22 F23' 2.108(16) . . ? F22 F23' 4.194(16) . '3 766' ? F22 F24' 3.18(2) . '3 766' ? F22 F24' 2.42(2) . . ? F22 F25' 2.256(17) . . ? F22 F26' 1.849(17) . . ? F22 H4 2.656(4) . '1 655' ? F22 H25b 3.076(4) . '3 766' ? F22 H27b 2.555(4) . '3 766' ? F23 F24 2.208(6) . . ? F23 F25 3.153(6) . . ? F23 F26 2.187(6) . . ? F23 F24' 3.01(2) . . ? F23 F25' 2.836(17) . . ? F23 H4 2.661(4) . '1 655' ? F23 H16b 2.686(4) . '1 545' ? F23 H27a 2.874(5) . '1 545' ? F24 F25 4.279(6) . '3 766' ? F24 F25 2.303(6) . . ? F24 F26 3.137(5) . . ? F24 F25' 2.928(18) . . ? F24 F26' 2.697(18) . . ? F24 H2 2.864(5) . . ? F24 H25b 2.707(4) . . ? F24 H20 1.991(4) . . ? F25 F26 2.200(5) . . ? F25 F23' 2.917(17) . . ? F25 F26' 2.689(18) . . ? F25 H3 3.111(4) . '3 666' ? F25 H17a 2.828(4) . '3 666' ? F25 H25a 3.149(4) . '3 766' ? F25 H25b 2.585(4) . '3 766' ? F25 H26b 3.047(4) . '3 766' ? F26 F26 4.041(6) . '3 756' ? F26 F23' 2.787(17) . . ? F26 F24' 3.02(2) . . ? F26 F26' 3.862(18) . '3 756' ? F26 H16a 2.759(4) . '3 666' ? F26 H16b 2.737(4) . '1 545' ? F26 H27b 2.756(4) . '3 766' ? F23' F24' 2.35(3) . . ? F23' F25' 3.05(2) . . ? F23' F26' 1.96(2) . . ? F23' H2 2.797(16) . . ? F23' H4 2.839(16) . '1 655' ? F23' H25b 2.785(16) . . ? F23' H20 2.752(16) . . ? F24' F24' 4.25(3) . '3 666' ? F24' F25' 2.36(3) . . ? F24' F26' 3.06(3) . . ? F24' H3 2.68(2) . '3 666' ? F24' H17b 3.00(2) . . ? F24' H20 2.73(2) . . ? F25' F26' 2.02(2) . . ? F25' H16a 2.592(17) . '3 666' ? F25' H17a 2.968(17) . '3 666' ? F25' H25b 3.072(17) . '3 766' ? F25' H26b 2.602(17) . '3 766' ? F25' H27b 2.738(16) . '3 766' ? F26' F26' 4.02(2) . '3 756' ? F26' H4 2.777(18) . '1 655' ? F26' H16b 2.706(17) . '1 545' ? F26' H27a 3.005(17) . '1 545' ? F26' H27b 3.152(17) . '1 545' ? F26' H27b 3.125(17) . '3 766' ? H10a H10b 1.5512(5) . . ? H11a H11b 1.5514(8) . . ? H12a H12b 1.5512(5) . . ? H13a H13b 1.5514(5) . . ? H15a H15b 1.5513(5) . . ? H16a H16b 1.5514(5) . . ? H17a H17b 1.5514(4) . . ? H21a H21b 1.5513(3) . . ? H22a H22b 1.5514(4) . . ? H23a H23b 1.5513(3) . . ? H25a H25b 1.5514(6) . . ? H26a H26b 1.5513(5) . . ? H27a H27b 1.5514(5) . . ? _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 1504 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 6 21 6 -6 21 -6 -6 -21 -6 6 -21 5 6 -25 -5 -6 25 -5 6 25 5 -6 -26 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 12 _reflns_limit_l_min -48 _reflns_limit_l_max 48 _reflns_number_observed 7043 _reflns_d_resolution_high .711 _reflns_d_resolution_low 8.793 _diffrn_reflns_av_sigmaI/netI .027 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_matrix_type atom_block _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .05 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all 1.207 _refine_ls_shift/su_mean .005 #========================================================================== # 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-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end