# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1666 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-07-21 _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 'Effendy' _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 ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Effendy' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, 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 ; 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_cp9 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C63 H53 Ag1 N3 O3 P3' _chemical_formula_moiety ? _chemical_formula_weight 1100.93 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 15.805(4) _cell_length_b 13.353(3) _cell_length_c 13.251(2) _cell_angle_alpha 83.32(2) _cell_angle_beta 83.92(2) _cell_angle_gamma 87.91(2) _cell_volume 2761.1(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.324 _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 13.9 _cell_measurement_theta_max 17.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .5 _exptl_crystal_description prism _exptl_crystal_size_max .42 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .12 _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 .85 _exptl_absorpt_correction_T_max .94 _diffrn_reflns_number 13097 _reflns_number_total 9673 _reflns_Friedel_coverage ? _reflns_number_gt 6504 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .046 _refine_ls_goodness_of_fit_ref 1.550 _refine_ls_number_reflns 6504 _refine_ls_number_parameters 676 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .088 _refine_diff_density_min -.37 _refine_diff_density_max .53 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1945(440) _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 ? 0 126 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 106 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 2 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 6 .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 6 .09 .095 '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 Ag .25097(2) .22020(3) .26094(3) .0425(3) Uani ? ? 1.00000 ? ? N1a .1115(3) .2739(3) .2261(3) .060(3) Uani ? ? 1.00000 ? ? C2a .0399(3) .2932(4) .2810(4) .056(4) Uani ? ? 1.00000 ? ? N3a -.0263(2) .3051(3) .2254(3) .057(3) Uani ? ? 1.00000 ? ? C4a .0047(3) .2928(4) .1267(4) .060(4) Uani ? ? 1.00000 ? ? C5a .0887(3) .2720(5) .1298(4) .068(5) Uani ? ? 1.00000 ? ? C41 -.0487(3) .3028(5) .0401(4) .077(5) Uani ? ? 1.00000 ? ? C42 -.1310(3) .3224(5) .0499(4) .088(5) Uani ? ? 1.00000 ? ? C43a -.1764(6) .3357(8) -.0410(7) .110(9) Uani ? ? .75000 ? ? C44a -.1427(5) .3093(6) -.1249(6) .076(7) Uani ? ? .75000 ? ? C45a -.0616(5) .2678(8) -.1309(6) .108(8) Uani ? ? .75000 ? ? C46a -.0146(5) .2589(8) -.0496(6) .093(8) Uani ? ? .75000 ? ? C43b -.1772(8) .3301(13) -.0241(13) .040(5) Uiso ? ? .25000 ? ? C44b -.1424(12) .3819(17) -.1282(17) .075(7) Uiso ? ? .25000 ? ? C45b -.0654(18) .411(2) -.127(2) .102(9) Uiso ? ? .25000 ? ? C46b -.0032(15) .378(2) -.045(2) .133(12) Uiso ? ? .25000 ? ? P1 .26735(8) .21232(10) .44890(9) .0406(9) Uani ? ? 1.00000 ? ? C111 .1916(3) .2867(3) .5239(3) .046(3) Uani ? ? 1.00000 ? ? C112 .1549(3) .3724(4) .4739(4) .066(4) Uani ? ? 1.00000 ? ? C113 .1034(4) .4375(5) .5298(5) .089(6) Uani ? ? 1.00000 ? ? C114 .0878(4) .4161(5) .6334(5) .094(6) Uani ? ? 1.00000 ? ? C115 .1222(4) .3305(5) .6823(4) .082(5) Uani ? ? 1.00000 ? ? C116 .1750(3) .2664(4) .6278(4) .060(4) Uani ? ? 1.00000 ? ? C121 .2659(3) .0884(3) .5223(3) .042(3) Uani ? ? 1.00000 ? ? C122 .1999(3) .0245(4) .5180(4) .055(4) Uani ? ? 1.00000 ? ? C123 .1977(4) -.0706(4) .5709(4) .068(5) Uani ? ? 1.00000 ? ? C124 .2616(4) -.1038(4) .6289(4) .077(5) Uani ? ? 1.00000 ? ? C125 .3270(4) -.0422(4) .6344(5) .085(5) Uani ? ? 1.00000 ? ? C126 .3299(3) .0538(4) .5827(4) .062(4) Uani ? ? 1.00000 ? ? C131 .3698(3) .2612(3) .4693(3) .045(3) Uani ? ? 1.00000 ? ? C132 .4424(3) .2271(4) .4130(4) .055(4) Uani ? ? 1.00000 ? ? C133 .5211(3) .2644(5) .4227(4) .072(5) Uani ? ? 1.00000 ? ? C134 .5293(4) .3365(5) .4857(4) .081(5) Uani ? ? 1.00000 ? ? C135 .4580(4) .3719(5) .5413(4) .076(5) Uani ? ? 1.00000 ? ? C136 .3785(3) .3346(4) .5323(4) .060(4) Uani ? ? 1.00000 ? ? P2 .35310(8) .34370(9) .15310(9) .0414(9) Uani ? ? 1.00000 ? ? C211 .3538(3) .4707(3) .1910(3) .042(3) Uani ? ? 1.00000 ? ? C212 .3300(3) .4827(4) .2925(4) .057(4) Uani ? ? 1.00000 ? ? C213 .3314(4) .5776(4) .3266(4) .073(5) Uani ? ? 1.00000 ? ? C214 .3548(3) .6601(4) .2589(4) .067(5) Uani ? ? 1.00000 ? ? C215 .3767(3) .6486(4) .1578(4) .062(4) Uani ? ? 1.00000 ? ? C216 .3763(3) .5545(4) .1244(4) .051(4) Uani ? ? 1.00000 ? ? C221 .3371(3) .3700(3) .0180(3) .044(3) Uani ? ? 1.00000 ? ? C222 .2587(3) .4098(4) -.0065(4) .058(4) Uani ? ? 1.00000 ? ? C223 .2425(4) .4323(4) -.1075(4) .070(5) Uani ? ? 1.00000 ? ? C224 .3037(4) .4156(4) -.1848(4) .073(5) Uani ? ? 1.00000 ? ? C225 .3806(4) .3745(4) -.1613(4) .066(4) Uani ? ? 1.00000 ? ? C226 .3977(3) .3529(4) -.0611(3) .051(4) Uani ? ? 1.00000 ? ? C231 .4641(3) .3016(3) .1493(3) .042(3) Uani ? ? 1.00000 ? ? C232 .4839(3) .2007(4) .1374(4) .053(4) Uani ? ? 1.00000 ? ? C233 .5664(3) .1637(4) .1328(4) .062(4) Uani ? ? 1.00000 ? ? C234 .6312(3) .2264(4) .1428(4) .068(4) Uani ? ? 1.00000 ? ? C235 .6139(3) .3263(4) .1562(4) .067(4) Uani ? ? 1.00000 ? ? C236 .5306(3) .3626(4) .1597(4) .055(4) Uani ? ? 1.00000 ? ? P3 .24707(8) .04726(10) .19719(10) .0446(9) Uani ? ? 1.00000 ? ? C311 .2277(3) .0439(3) .0647(4) .049(4) Uani ? ? 1.00000 ? ? C312 .2601(3) .1190(4) -.0086(4) .060(4) Uani ? ? 1.00000 ? ? C313 .2458(4) .1215(4) -.1098(4) .078(5) Uani ? ? 1.00000 ? ? C314 .1985(5) .0482(5) -.1390(4) .092(6) Uani ? ? 1.00000 ? ? C315 .1668(5) -.0265(5) -.0693(5) .111(7) Uani ? ? 1.00000 ? ? C316 .1817(4) -.0300(4) .0323(4) .084(5) Uani ? ? 1.00000 ? ? C321 .1659(3) -.0344(4) .2674(3) .048(4) Uani ? ? 1.00000 ? ? C322 .0848(3) .0059(5) .2818(5) .078(5) Uani ? ? 1.00000 ? ? C323 .0199(4) -.0501(5) .3363(6) .105(7) Uani ? ? 1.00000 ? ? C324 .0367(4) -.1460(6) .3801(5) .103(6) Uani ? ? 1.00000 ? ? C325 .1158(4) -.1861(5) .3670(5) .089(6) Uani ? ? 1.00000 ? ? C326 .1814(3) -.1311(4) .3108(4) .066(4) Uani ? ? 1.00000 ? ? C331 .3466(3) -.0241(3) .2092(3) .045(3) Uani ? ? 1.00000 ? ? C332 .3760(3) -.0386(4) .3048(4) .055(4) Uani ? ? 1.00000 ? ? C333 .4538(3) -.0868(4) .3193(4) .067(5) Uani ? ? 1.00000 ? ? C334 .5041(3) -.1176(4) .2368(5) .073(5) Uani ? ? 1.00000 ? ? C335 .4756(3) -.1033(4) .1423(4) .068(5) Uani ? ? 1.00000 ? ? C336 .3979(3) -.0567(4) .1274(4) .055(4) Uani ? ? 1.00000 ? ? N -.2036(3) .3673(4) .3777(3) .080(4) Uani ? ? 1.00000 ? ? O1 -.1952(3) .3656(4) .2846(3) .098(4) Uani ? ? 1.00000 ? ? O2 -.2680(3) .4051(5) .4186(4) .155(6) Uani ? ? 1.00000 ? ? O3 -.1439(3) .3342(3) .4241(3) .118(5) Uani ? ? 1.00000 ? ? H2a .03570 .29813 .35277 .07050 Uiso ? ? 1.00000 ? ? H3a -.08431 .31907 .24963 .07170 Uiso ? ? 1.00000 ? ? H5a .12697 .25769 .07239 .08500 Uiso ? ? 1.00000 ? ? H42 -.16041 .32848 .11547 .11110 Uiso ? ? 1.00000 ? ? H43a -.23265 .36350 -.03692 .13990 Uiso ? ? .75000 ? ? H44a -.17316 .31840 -.18368 .09770 Uiso ? ? .75000 ? ? H45a -.03782 .24444 -.19309 .13910 Uiso ? ? .75000 ? ? H46a .03938 .22468 -.05252 .11920 Uiso ? ? .75000 ? ? H43b -.23312 .30496 -.01430 .05180 Uiso ? ? .25000 ? ? H44b -.17314 .39155 -.18637 .09500 Uiso ? ? .25000 ? ? H45b -.04372 .45857 -.18203 .12830 Uiso ? ? .25000 ? ? H46b .05431 .39713 -.04793 .16850 Uiso ? ? .25000 ? ? H112 .16509 .38638 .40127 .08230 Uiso ? ? 1.00000 ? ? H113 .07925 .49666 .49589 .11170 Uiso ? ? 1.00000 ? ? H114 .05321 .46057 .67167 .12010 Uiso ? ? 1.00000 ? ? H115 .10961 .31481 .75409 .10270 Uiso ? ? 1.00000 ? ? H116 .19996 .20797 .66262 .07490 Uiso ? ? 1.00000 ? ? H122 .15478 .04674 .47753 .06810 Uiso ? ? 1.00000 ? ? H123 .15157 -.11342 .56707 .08440 Uiso ? ? 1.00000 ? ? H124 .26029 -.16959 .66527 .09430 Uiso ? ? 1.00000 ? ? H125 .37165 -.06570 .67457 .10560 Uiso ? ? 1.00000 ? ? H126 .37591 .09645 .58850 .07750 Uiso ? ? 1.00000 ? ? H132 .43769 .17765 .36750 .06830 Uiso ? ? 1.00000 ? ? H133 .57041 .23932 .38493 .08810 Uiso ? ? 1.00000 ? ? H134 .58371 .36219 .49112 .10090 Uiso ? ? 1.00000 ? ? H135 .46332 .42162 .58604 .09640 Uiso ? ? 1.00000 ? ? H136 .32928 .36030 .57004 .07580 Uiso ? ? 1.00000 ? ? H212 .31259 .42565 .33929 .07110 Uiso ? ? 1.00000 ? ? H213 .31600 .58500 .39688 .09290 Uiso ? ? 1.00000 ? ? H214 .35590 .72483 .28195 .08510 Uiso ? ? 1.00000 ? ? H215 .39213 .70584 .11037 .07770 Uiso ? ? 1.00000 ? ? H216 .39175 .54739 .05387 .06280 Uiso ? ? 1.00000 ? ? H222 .21538 .42172 .04685 .07250 Uiso ? ? 1.00000 ? ? H223 .18831 .45949 -.12315 .08980 Uiso ? ? 1.00000 ? ? H224 .29294 .43229 -.25412 .09220 Uiso ? ? 1.00000 ? ? H225 .42280 .36047 -.21491 .08150 Uiso ? ? 1.00000 ? ? H226 .45236 .32574 -.04632 .06420 Uiso ? ? 1.00000 ? ? H232 .43907 .15627 .13227 .06710 Uiso ? ? 1.00000 ? ? H233 .57846 .09490 .12282 .07600 Uiso ? ? 1.00000 ? ? H234 .68837 .20087 .14040 .08250 Uiso ? ? 1.00000 ? ? H235 .65888 .36982 .16289 .08260 Uiso ? ? 1.00000 ? ? H236 .51884 .43151 .16967 .06830 Uiso ? ? 1.00000 ? ? H312 .29300 .17034 .01127 .07540 Uiso ? ? 1.00000 ? ? H313 .26846 .17385 -.15889 .09710 Uiso ? ? 1.00000 ? ? H314 .18797 .04981 -.20845 .11530 Uiso ? ? 1.00000 ? ? H315 .13391 -.07700 -.09006 .14370 Uiso ? ? 1.00000 ? ? H316 .16004 -.08392 .08014 .10600 Uiso ? ? 1.00000 ? ? H322 .07321 .07330 .25410 .09610 Uiso ? ? 1.00000 ? ? H323 -.03629 -.02263 .34302 .13120 Uiso ? ? 1.00000 ? ? H324 -.00716 -.18373 .41978 .12780 Uiso ? ? 1.00000 ? ? H325 .12698 -.25295 .39642 .11050 Uiso ? ? 1.00000 ? ? H326 .23722 -.16043 .30225 .08160 Uiso ? ? 1.00000 ? ? H332 .34227 -.01492 .36162 .06920 Uiso ? ? 1.00000 ? ? H333 .47220 -.09856 .38602 .08540 Uiso ? ? 1.00000 ? ? H334 .55832 -.14870 .24576 .09140 Uiso ? ? 1.00000 ? ? H335 .51011 -.12570 .08548 .08520 Uiso ? ? 1.00000 ? ? H336 .37927 -.04686 .06061 .06790 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 Ag .0432(2) .0449(2) .0402(2) .00109(16) -.00777(16) -.00557(16) N1a .049(3) .075(3) .055(3) .014(2) -.010(2) -.008(2) C2a .057(3) .067(4) .045(3) .010(3) -.012(3) -.008(3) N3a .044(3) .075(3) .053(3) .008(2) -.007(2) -.009(2) C4a .041(3) .090(4) .048(3) .003(3) -.000(2) -.008(3) C5a .047(3) .099(5) .058(4) .003(3) -.002(3) -.017(3) C41 .046(3) .135(6) .050(4) -.009(4) -.006(3) -.011(4) C42 .053(4) .144(6) .068(4) .029(4) -.012(3) -.016(4) C43a .086(7) .167(10) .083(7) .043(7) -.050(5) -.020(6) C44a .071(6) .101(7) .063(5) -.016(5) -.030(4) -.010(5) C45a .072(6) .213(11) .045(5) -.033(7) -.001(4) -.039(6) C46a .048(5) .169(9) .069(6) -.007(5) -.003(4) -.041(6) P1 .0417(8) .0471(8) .0329(7) -.0017(6) -.0034(6) -.0047(6) C111 .041(3) .047(3) .051(3) -.001(2) -.004(2) -.013(2) C112 .057(4) .070(4) .071(4) .011(3) -.009(3) -.012(3) C113 .079(5) .075(5) .115(6) .028(4) -.011(4) -.025(4) C114 .073(5) .100(5) .114(6) .012(4) .008(4) -.054(4) C115 .071(4) .112(5) .066(4) -.016(4) .017(3) -.037(4) C116 .057(4) .070(4) .053(3) -.000(3) .006(3) -.017(3) C121 .046(3) .046(3) .034(3) .001(2) -.001(2) -.005(2) C122 .057(3) .061(4) .046(3) -.007(3) -.005(3) -.004(3) C123 .084(4) .058(4) .061(4) -.019(3) -.003(3) -.006(3) C124 .112(5) .054(4) .062(4) .001(3) -.010(4) .008(3) C125 .106(5) .066(4) .082(5) .006(4) -.036(4) .021(3) C126 .065(4) .058(4) .063(4) -.003(3) -.021(3) .004(3) C131 .048(3) .052(3) .033(3) -.004(2) -.006(2) .003(2) C132 .050(3) .071(4) .042(3) .004(3) -.004(2) -.004(3) C133 .046(3) .103(5) .063(4) .003(3) -.000(3) .006(3) C134 .062(4) .115(5) .066(4) -.031(4) -.012(3) .007(4) C135 .072(4) .096(5) .065(4) -.036(4) -.012(3) -.018(3) C136 .056(3) .078(4) .049(3) -.013(3) -.003(3) -.011(3) P2 .0482(8) .0382(7) .0376(7) -.0025(6) -.0036(6) -.0033(6) C211 .042(3) .040(3) .045(3) .002(2) -.004(2) -.005(2) C212 .082(4) .049(3) .040(3) -.007(3) -.003(3) -.002(2) C213 .094(5) .076(4) .053(4) .004(4) -.009(3) -.029(3) C214 .066(4) .044(3) .095(5) .003(3) -.016(3) -.021(3) C215 .065(4) .045(3) .077(4) .001(3) -.004(3) -.008(3) C216 .053(3) .047(3) .050(3) -.001(3) .002(3) -.001(2) C221 .054(3) .038(3) .039(3) -.005(2) -.006(2) -.004(2) C222 .056(3) .064(4) .053(3) .003(3) -.008(3) -.010(3) C223 .076(4) .079(4) .061(4) .012(3) -.028(3) -.013(3) C224 .109(5) .071(4) .042(3) -.005(4) -.016(3) -.009(3) C225 .091(4) .063(4) .043(3) .006(3) .004(3) -.010(3) C226 .064(4) .049(3) .041(3) .002(3) -.006(3) -.004(2) C231 .051(3) .039(3) .033(3) -.003(2) -.001(2) .002(2) C232 .055(3) .051(3) .054(3) -.003(3) -.006(3) -.008(3) C233 .067(4) .054(3) .060(4) .011(3) .001(3) -.004(3) C234 .053(4) .084(4) .061(4) .019(3) -.001(3) .006(3) C235 .055(4) .066(4) .077(4) -.006(3) -.012(3) .004(3) C236 .055(3) .045(3) .065(4) -.002(3) -.005(3) -.005(3) P3 .0474(8) .0427(8) .0441(8) -.0008(6) -.0024(6) -.0087(6) C311 .054(3) .041(3) .052(3) -.002(2) -.003(3) -.006(2) C312 .068(4) .058(4) .055(3) -.010(3) -.002(3) -.010(3) C313 .106(5) .074(4) .053(4) -.020(4) -.006(3) .003(3) C314 .136(6) .093(5) .049(4) -.009(4) -.018(4) -.006(3) C315 .189(8) .093(5) .061(4) -.061(5) -.038(5) -.009(4) C316 .130(6) .064(4) .060(4) -.043(4) -.018(4) .002(3) C321 .043(3) .057(3) .047(3) -.009(2) -.007(2) -.010(3) C322 .060(4) .076(4) .095(5) -.013(3) .008(3) -.005(4) C323 .059(4) .117(6) .140(7) -.016(4) .007(4) -.030(5) C324 .090(5) .136(6) .080(5) -.061(5) .013(4) -.006(4) C325 .104(5) .086(5) .077(4) -.047(4) -.019(4) .018(4) C326 .068(4) .059(4) .069(4) -.015(3) -.006(3) .002(3) C331 .049(3) .037(3) .049(3) -.005(2) .000(2) -.008(2) C332 .048(3) .059(3) .059(3) .006(3) -.004(3) -.017(3) C333 .058(4) .074(4) .073(4) .005(3) -.015(3) -.018(3) C334 .057(4) .065(4) .099(5) .009(3) -.013(3) -.016(3) C335 .060(4) .057(4) .087(4) .007(3) .011(3) -.025(3) C336 .061(4) .047(3) .055(3) .006(3) -.001(3) -.012(3) N .095(4) .093(4) .049(3) -.021(3) .002(3) -.009(3) O1 .074(3) .155(4) .066(3) .031(3) -.005(2) -.023(3) O2 .090(4) .258(7) .120(4) -.016(4) .047(3) -.084(5) O3 .177(5) .099(4) .083(3) .020(3) -.052(3) .003(3) # 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 Ag N1a . . 2.369(4) ? Ag P1 . . 2.5209(13) ? Ag P2 . . 2.5543(13) ? Ag P3 . . 2.5545(15) ? N1a C2a . . 1.313(6) ? N1a C5a . . 1.364(7) ? C2a N3a . . 1.337(7) ? C2a H2a . . .956(5) ? N3a C4a . . 1.374(6) ? N3a H3a . . .958(4) ? C4a C5a . . 1.351(7) ? C4a C41 . . 1.485(7) ? C5a H5a . . .954(5) ? C41 C42 . . 1.313(7) ? C41 C46a . . 1.432(10) ? C41 C46b . . 1.56(3) ? C42 C43a . . 1.457(11) ? C42 C43b . . 1.276(17) ? C42 H42 . . .952(6) ? C43a C44a . . 1.263(12) ? C43a C43b . . .227(19) ? C43a C44b . . 1.32(2) ? C43a H43a . . .949(9) ? C43a H43b . . 1.011(9) ? C44a C45a . . 1.376(11) ? C44a C43b . . 1.442(18) ? C44a C44b . . .97(2) ? C44a C45b . . 1.85(3) ? C44a H44a . . .953(8) ? C44a H44b . . 1.392(8) ? C45a C46a . . 1.363(11) ? C45a C44b . . 1.95(2) ? C45a C45b . . 1.91(3) ? C45a H45a . . .950(8) ? C46a C46b . . 1.61(3) ? C46a H46a . . .952(8) ? C43b C44b . . 1.53(3) ? C43b H43a . . .990(13) ? C43b H43b . . .947(13) ? C44b C45b . . 1.29(3) ? C44b H44a . . 1.32(2) ? C44b H44b . . .95(2) ? C45b C46b . . 1.56(4) ? C45b H45b . . .95(3) ? C46b H46b . . .95(2) ? P1 C111 . . 1.816(5) ? P1 C121 . . 1.819(4) ? P1 C131 . . 1.825(5) ? C111 C112 . . 1.393(7) ? C111 C116 . . 1.371(7) ? C112 C113 . . 1.392(8) ? C112 H112 . . .956(5) ? C113 C114 . . 1.368(9) ? C113 H113 . . .951(6) ? C114 C115 . . 1.370(9) ? C114 H114 . . .946(7) ? C115 C116 . . 1.384(8) ? C115 H115 . . .952(6) ? C116 H116 . . .953(5) ? C121 C122 . . 1.382(7) ? C121 C126 . . 1.389(7) ? C122 C123 . . 1.377(7) ? C122 H122 . . .955(5) ? C123 C124 . . 1.363(8) ? C123 H123 . . .952(6) ? C124 C125 . . 1.358(9) ? C124 H124 . . .951(5) ? C125 C126 . . 1.382(7) ? C125 H125 . . .950(6) ? C126 H126 . . .954(5) ? C131 C132 . . 1.393(6) ? C131 C136 . . 1.380(7) ? C132 C133 . . 1.381(8) ? C132 H132 . . .954(5) ? C133 C134 . . 1.364(9) ? C133 H133 . . .952(5) ? C134 C135 . . 1.379(8) ? C134 H134 . . .950(6) ? C135 C136 . . 1.390(8) ? C135 H135 . . .952(6) ? C136 H136 . . .954(5) ? P2 C211 . . 1.825(5) ? P2 C221 . . 1.826(5) ? P2 C231 . . 1.820(5) ? C211 C212 . . 1.382(7) ? C211 C216 . . 1.375(6) ? C212 C213 . . 1.396(8) ? C212 H212 . . .954(5) ? C213 C214 . . 1.373(7) ? C213 H213 . . .952(5) ? C214 C215 . . 1.372(8) ? C214 H214 . . .951(5) ? C215 C216 . . 1.381(7) ? C215 H215 . . .953(5) ? C216 H216 . . .955(5) ? C221 C222 . . 1.386(7) ? C221 C226 . . 1.378(6) ? C222 C223 . . 1.386(7) ? C222 H222 . . .954(5) ? C223 C224 . . 1.364(8) ? C223 H223 . . .952(6) ? C224 C225 . . 1.367(8) ? C224 H224 . . .951(5) ? C225 C226 . . 1.378(7) ? C225 H225 . . .952(5) ? C226 H226 . . .955(5) ? C231 C232 . . 1.395(7) ? C231 C236 . . 1.380(7) ? C232 C233 . . 1.375(7) ? C232 H232 . . .954(5) ? C233 C234 . . 1.373(8) ? C233 H233 . . .952(5) ? C234 C235 . . 1.380(8) ? C234 H234 . . .953(5) ? C235 C236 . . 1.384(7) ? C235 H235 . . .952(6) ? C236 H236 . . .954(5) ? P3 C311 . . 1.820(5) ? P3 C321 . . 1.820(5) ? P3 C331 . . 1.821(5) ? C311 C312 . . 1.384(6) ? C311 C316 . . 1.380(8) ? C312 C313 . . 1.379(8) ? C312 H312 . . .953(6) ? C313 C314 . . 1.366(9) ? C313 H313 . . .951(5) ? C314 C315 . . 1.351(9) ? C314 H314 . . .951(6) ? C315 C316 . . 1.386(9) ? C315 H315 . . .948(8) ? C316 H316 . . .951(5) ? C321 C322 . . 1.375(7) ? C321 C326 . . 1.376(7) ? C322 C323 . . 1.381(8) ? C322 H322 . . .951(6) ? C323 C324 . . 1.372(10) ? C323 H323 . . .947(6) ? C324 C325 . . 1.345(9) ? C324 H324 . . .947(6) ? C325 C326 . . 1.391(8) ? C325 H325 . . .949(6) ? C326 H326 . . .953(5) ? C331 C332 . . 1.385(7) ? C331 C336 . . 1.385(7) ? C332 C333 . . 1.388(7) ? C332 H332 . . .954(5) ? C333 C334 . . 1.376(8) ? C333 H333 . . .954(6) ? C334 C335 . . 1.366(8) ? C334 H334 . . .951(5) ? C335 C336 . . 1.379(7) ? C335 H335 . . .953(5) ? C336 H336 . . .955(5) ? N O1 . . 1.231(6) ? N O2 . . 1.222(7) ? N O3 . . 1.222(7) ? H43a H43b . . .80397(16) ? H44a H44b . . .9733(2) ? 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 N1a Ag P1 . . . 111.24(10) ? N1a Ag P2 . . . 106.90(10) ? N1a Ag P3 . . . 96.56(11) ? P1 Ag P2 . . . 112.11(5) ? P1 Ag P3 . . . 113.78(4) ? P2 Ag P3 . . . 114.96(4) ? Ag N1a C2a . . . 135.6(3) ? Ag N1a C5a . . . 119.0(3) ? C2a N1a C5a . . . 104.4(4) ? N1a C2a N3a . . . 112.4(4) ? N1a C2a H2a . . . 123.7(5) ? N3a C2a H2a . . . 123.9(5) ? C2a N3a C4a . . . 106.8(4) ? C2a N3a H3a . . . 126.8(4) ? C4a N3a H3a . . . 126.4(4) ? N3a C4a C5a . . . 105.2(4) ? N3a C4a C41 . . . 123.7(4) ? C5a C4a C41 . . . 131.0(5) ? N1a C5a C4a . . . 111.1(4) ? N1a C5a H5a . . . 124.5(5) ? C4a C5a H5a . . . 124.4(5) ? C4a C41 C42 . . . 123.7(5) ? C4a C41 C46a . . . 116.6(5) ? C4a C41 C46b . . . 106.6(11) ? C42 C41 C46a . . . 116.9(6) ? C42 C41 C46b . . . 110.5(10) ? C46a C41 C46b . . . 65.3(12) ? C41 C42 C43a . . . 119.1(6) ? C41 C42 C43b . . . 123.9(8) ? C41 C42 H42 . . . 120.4(6) ? C43a C42 C43b . . . 5.8(7) ? C43a C42 H42 . . . 120.5(6) ? C43b C42 H42 . . . 115.6(8) ? C42 C43a C44a . . . 121.0(8) ? C42 C43a C43b . . . 34(4) ? C42 C43a C44b . . . 121.8(12) ? C42 C43a H43a . . . 119.5(8) ? C42 C43a H43b . . . 101.8(7) ? C44a C43a C43b . . . 139(5) ? C44a C43a C44b . . . 43.9(11) ? C44a C43a H43a . . . 119.5(9) ? C44a C43a H43b . . . 116.0(10) ? C43b C43a C44b . . . 156(5) ? C43b C43a H43a . . . 94(4) ? C43b C43a H43b . . . 67(4) ? C44b C43a H43a . . . 102.0(11) ? C44b C43a H43b . . . 136.3(13) ? H43a C43a H43b . . . 48.3(4) ? C43a C44a C45a . . . 119.7(8) ? C43a C44a C43b . . . 5.9(7) ? C43a C44a C44b . . . 70.9(14) ? C43a C44a C45b . . . 87.6(11) ? C43a C44a H44a . . . 120.1(8) ? C43a C44a H44b . . . 96.2(7) ? C45a C44a C43b . . . 115.0(8) ? C45a C44a C44b . . . 111.9(14) ? C45a C44a C45b . . . 71.0(10) ? C45a C44a H44a . . . 120.2(7) ? C45a C44a H44b . . . 127.4(6) ? C43b C44a C44b . . . 75.8(15) ? C43b C44a C45b . . . 89.3(11) ? C43b C44a H44a . . . 124.6(9) ? C43b C44a H44b . . . 102.2(8) ? C44b C44a C45b . . . 41.1(15) ? C44b C44a H44a . . . 87.1(15) ? C44b C44a H44b . . . 42.8(14) ? C45b C44a H44a . . . 111.2(10) ? C45b C44a H44b . . . 73.9(9) ? H44a C44a H44b . . . 44.3(3) ? C44a C45a C46a . . . 121.6(8) ? C44a C45a C44b . . . 27.3(7) ? C44a C45a C45b . . . 66.2(10) ? C44a C45a H45a . . . 119.2(8) ? C46a C45a C44b . . . 112.0(10) ? C46a C45a C45b . . . 88.5(11) ? C46a C45a H45a . . . 119.2(8) ? C44b C45a C45b . . . 39.0(11) ? C44b C45a H45a . . . 122.0(9) ? C45b C45a H45a . . . 116.3(11) ? C41 C46a C45a . . . 118.1(7) ? C41 C46a C46b . . . 61.1(11) ? C41 C46a H46a . . . 121.0(7) ? C45a C46a C46b . . . 97.1(12) ? C45a C46a H46a . . . 120.9(8) ? C46b C46a H46a . . . 110.3(11) ? C42 C43b C43a . . . 140(4) ? C42 C43b C44a . . . 121.2(10) ? C42 C43b C44b . . . 119.5(12) ? C42 C43b H43a . . . 134.7(16) ? C42 C43b H43b . . . 120.4(15) ? C43a C43b C44a . . . 35(4) ? C43a C43b C44b . . . 20(4) ? C43a C43b H43a . . . 73(4) ? C43a C43b H43b . . . 100(4) ? C44a C43b C44b . . . 37.8(10) ? C44a C43b H43a . . . 102.4(13) ? C44a C43b H43b . . . 106.1(15) ? C44b C43b H43a . . . 87.0(13) ? C44b C43b H43b . . . 120.1(16) ? H43a C43b H43b . . . 49.0(6) ? C43a C44b C44a . . . 65.2(14) ? C43a C44b C45a . . . 86.2(12) ? C43a C44b C43b . . . 3.5(7) ? C43a C44b C45b . . . 115(2) ? C43a C44b H44a . . . 93.9(15) ? C43a C44b H44b . . . 121.1(19) ? C44a C44b C45a . . . 40.8(10) ? C44a C44b C43b . . . 66.4(14) ? C44a C44b C45b . . . 109(2) ? C44a C44b H44a . . . 46.1(11) ? C44a C44b H44b . . . 93(2) ? C45a C44b C43b . . . 85.3(12) ? C45a C44b C45b . . . 68.8(15) ? C45a C44b H44a . . . 73.8(11) ? C45a C44b H44b . . . 113.0(18) ? C43b C44b C45b . . . 111(2) ? C43b C44b H44a . . . 96.8(15) ? C43b C44b H44b . . . 124.5(18) ? C45b C44b H44a . . . 130(2) ? C45b C44b H44b . . . 124(2) ? H44a C44b H44b . . . 47.4(11) ? C44a C45b C45a . . . 42.8(7) ? C44a C45b C44b . . . 29.4(12) ? C44a C45b C46b . . . 108.4(18) ? C44a C45b H45b . . . 130(2) ? C45a C45b C44b . . . 72.2(17) ? C45a C45b C46b . . . 79.6(16) ? C45a C45b H45b . . . 125(2) ? C44b C45b C46b . . . 127(2) ? C44b C45b H45b . . . 117(3) ? C46b C45b H45b . . . 115(3) ? C41 C46b C46a . . . 53.7(10) ? C41 C46b C45b . . . 109.0(18) ? C41 C46b H46b . . . 125(2) ? C46a C46b C45b . . . 94(2) ? C46a C46b H46b . . . 114(2) ? C45b C46b H46b . . . 126(3) ? Ag P1 C111 . . . 116.77(16) ? Ag P1 C121 . . . 117.33(16) ? Ag P1 C131 . . . 110.93(14) ? C111 P1 C121 . . . 103.7(2) ? C111 P1 C131 . . . 103.1(2) ? C121 P1 C131 . . . 103.3(2) ? P1 C111 C112 . . . 117.8(4) ? P1 C111 C116 . . . 122.6(4) ? C112 C111 C116 . . . 119.4(5) ? C111 C112 C113 . . . 119.9(5) ? C111 C112 H112 . . . 120.0(5) ? C113 C112 H112 . . . 120.1(5) ? C112 C113 C114 . . . 119.9(6) ? C112 C113 H113 . . . 120.0(6) ? C114 C113 H113 . . . 120.1(6) ? C113 C114 C115 . . . 120.2(6) ? C113 C114 H114 . . . 120.0(6) ? C115 C114 H114 . . . 119.8(6) ? C114 C115 C116 . . . 120.5(5) ? C114 C115 H115 . . . 119.9(6) ? C116 C115 H115 . . . 119.6(6) ? C111 C116 C115 . . . 120.1(5) ? C111 C116 H116 . . . 119.9(5) ? C115 C116 H116 . . . 120.0(5) ? P1 C121 C122 . . . 119.9(3) ? P1 C121 C126 . . . 122.4(4) ? C122 C121 C126 . . . 117.7(4) ? C121 C122 C123 . . . 121.4(5) ? C121 C122 H122 . . . 119.3(5) ? C123 C122 H122 . . . 119.3(5) ? C122 C123 C124 . . . 120.2(5) ? C122 C123 H123 . . . 120.1(5) ? C124 C123 H123 . . . 119.8(5) ? C123 C124 C125 . . . 119.5(5) ? C123 C124 H124 . . . 120.3(6) ? C125 C124 H124 . . . 120.2(6) ? C124 C125 C126 . . . 121.2(6) ? C124 C125 H125 . . . 119.3(5) ? C126 C125 H125 . . . 119.5(6) ? C121 C126 C125 . . . 120.1(5) ? C121 C126 H126 . . . 120.0(5) ? C125 C126 H126 . . . 120.0(5) ? P1 C131 C132 . . . 118.0(4) ? P1 C131 C136 . . . 123.5(4) ? C132 C131 C136 . . . 118.3(5) ? C131 C132 C133 . . . 120.4(5) ? C131 C132 H132 . . . 119.8(5) ? C133 C132 H132 . . . 119.8(5) ? C132 C133 C134 . . . 120.9(5) ? C132 C133 H133 . . . 119.5(6) ? C134 C133 H133 . . . 119.5(6) ? C133 C134 C135 . . . 119.5(5) ? C133 C134 H134 . . . 120.2(6) ? C135 C134 H134 . . . 120.3(6) ? C134 C135 C136 . . . 120.0(6) ? C134 C135 H135 . . . 120.0(6) ? C136 C135 H135 . . . 120.0(5) ? C131 C136 C135 . . . 120.8(5) ? C131 C136 H136 . . . 119.5(5) ? C135 C136 H136 . . . 119.6(6) ? Ag P2 C211 . . . 116.72(14) ? Ag P2 C221 . . . 116.27(16) ? Ag P2 C231 . . . 113.56(14) ? C211 P2 C221 . . . 101.6(2) ? C211 P2 C231 . . . 103.9(2) ? C221 P2 C231 . . . 102.9(2) ? P2 C211 C212 . . . 117.8(3) ? P2 C211 C216 . . . 123.6(4) ? C212 C211 C216 . . . 118.6(4) ? C211 C212 C213 . . . 120.4(4) ? C211 C212 H212 . . . 119.7(5) ? C213 C212 H212 . . . 119.9(5) ? C212 C213 C214 . . . 119.9(5) ? C212 C213 H213 . . . 119.9(5) ? C214 C213 H213 . . . 120.1(6) ? C213 C214 C215 . . . 119.6(5) ? C213 C214 H214 . . . 120.2(6) ? C215 C214 H214 . . . 120.2(5) ? C214 C215 C216 . . . 120.3(4) ? C214 C215 H215 . . . 119.9(5) ? C216 C215 H215 . . . 119.8(5) ? C211 C216 C215 . . . 121.0(4) ? C211 C216 H216 . . . 119.4(5) ? C215 C216 H216 . . . 119.6(4) ? P2 C221 C222 . . . 117.8(3) ? P2 C221 C226 . . . 124.3(4) ? C222 C221 C226 . . . 117.8(4) ? C221 C222 C223 . . . 120.8(5) ? C221 C222 H222 . . . 119.5(5) ? C223 C222 H222 . . . 119.7(5) ? C222 C223 C224 . . . 120.5(5) ? C222 C223 H223 . . . 119.8(5) ? C224 C223 H223 . . . 119.7(5) ? C223 C224 C225 . . . 119.1(5) ? C223 C224 H224 . . . 120.5(6) ? C225 C224 H224 . . . 120.5(5) ? C224 C225 C226 . . . 120.9(5) ? C224 C225 H225 . . . 119.4(5) ? C226 C225 H225 . . . 119.6(5) ? C221 C226 C225 . . . 120.8(5) ? C221 C226 H226 . . . 119.5(5) ? C225 C226 H226 . . . 119.6(5) ? P2 C231 C232 . . . 118.4(4) ? P2 C231 C236 . . . 124.3(4) ? C232 C231 C236 . . . 117.3(4) ? C231 C232 C233 . . . 121.8(5) ? C231 C232 H232 . . . 119.1(5) ? C233 C232 H232 . . . 119.1(5) ? C232 C233 C234 . . . 119.5(5) ? C232 C233 H233 . . . 120.2(5) ? C234 C233 H233 . . . 120.2(5) ? C233 C234 C235 . . . 120.3(5) ? C233 C234 H234 . . . 119.9(6) ? C235 C234 H234 . . . 119.8(6) ? C234 C235 C236 . . . 119.4(5) ? C234 C235 H235 . . . 120.2(5) ? C236 C235 H235 . . . 120.4(5) ? C231 C236 C235 . . . 121.7(5) ? C231 C236 H236 . . . 119.2(5) ? C235 C236 H236 . . . 119.1(5) ? Ag P3 C311 . . . 117.50(15) ? Ag P3 C321 . . . 113.95(16) ? Ag P3 C331 . . . 112.09(16) ? C311 P3 C321 . . . 103.1(2) ? C311 P3 C331 . . . 104.2(2) ? C321 P3 C331 . . . 104.7(2) ? P3 C311 C312 . . . 119.2(4) ? P3 C311 C316 . . . 123.5(4) ? C312 C311 C316 . . . 117.3(5) ? C311 C312 C313 . . . 121.7(5) ? C311 C312 H312 . . . 119.2(5) ? C313 C312 H312 . . . 119.1(5) ? C312 C313 C314 . . . 119.5(5) ? C312 C313 H313 . . . 120.3(6) ? C314 C313 H313 . . . 120.2(6) ? C313 C314 C315 . . . 120.2(6) ? C313 C314 H314 . . . 120.0(6) ? C315 C314 H314 . . . 119.9(7) ? C314 C315 C316 . . . 120.6(7) ? C314 C315 H315 . . . 119.7(6) ? C316 C315 H315 . . . 119.8(6) ? C311 C316 C315 . . . 120.8(5) ? C311 C316 H316 . . . 119.6(6) ? C315 C316 H316 . . . 119.6(6) ? P3 C321 C322 . . . 117.2(4) ? P3 C321 C326 . . . 124.3(4) ? C322 C321 C326 . . . 118.3(5) ? C321 C322 C323 . . . 121.0(5) ? C321 C322 H322 . . . 119.6(5) ? C323 C322 H322 . . . 119.5(6) ? C322 C323 C324 . . . 119.9(6) ? C322 C323 H323 . . . 120.1(7) ? C324 C323 H323 . . . 120.0(6) ? C323 C324 C325 . . . 119.8(6) ? C323 C324 H324 . . . 120.2(6) ? C325 C324 H324 . . . 120.0(7) ? C324 C325 C326 . . . 120.8(6) ? C324 C325 H325 . . . 119.5(6) ? C326 C325 H325 . . . 119.7(6) ? C321 C326 C325 . . . 120.2(5) ? C321 C326 H326 . . . 119.9(5) ? C325 C326 H326 . . . 119.9(5) ? P3 C331 C332 . . . 117.5(3) ? P3 C331 C336 . . . 124.0(4) ? C332 C331 C336 . . . 118.3(4) ? C331 C332 C333 . . . 121.2(5) ? C331 C332 H332 . . . 119.4(5) ? C333 C332 H332 . . . 119.4(5) ? C332 C333 C334 . . . 119.5(5) ? C332 C333 H333 . . . 120.2(5) ? C334 C333 H333 . . . 120.2(5) ? C333 C334 C335 . . . 119.5(5) ? C333 C334 H334 . . . 120.1(6) ? C335 C334 H334 . . . 120.4(6) ? C334 C335 C336 . . . 121.3(5) ? C334 C335 H335 . . . 119.4(5) ? C336 C335 H335 . . . 119.3(5) ? C331 C336 C335 . . . 120.1(5) ? C331 C336 H336 . . . 119.9(5) ? C335 C336 H336 . . . 120.0(5) ? O1 N O2 . . . 119.8(5) ? O1 N O3 . . . 116.8(5) ? O2 N O3 . . . 123.4(5) ? C43a H43a C43b . . . 13.2(11) ? C43a H43a H43b . . . 69.9(6) ? C43b H43a H43b . . . 62.7(9) ? C44a H44a C44b . . . 46.9(11) ? C44a H44a H44b . . . 92.6(5) ? C44b H44a H44b . . . 45.7(9) ? C43a H43b C43b . . . 12.8(11) ? C43a H43b H43a . . . 61.8(6) ? C43b H43b H43a . . . 68.3(9) ? C44a H44b C44b . . . 43.8(15) ? C44a H44b H44a . . . 43.1(3) ? C44b H44b H44a . . . 86.9(14) ? 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 Ag C2a 3.433(5) . . ? Ag C5a 3.257(5) . . ? Ag C111 3.712(5) . . ? Ag C112 3.820(6) . . ? Ag C121 3.725(4) . . ? Ag C122 4.072(5) . . ? Ag C131 3.602(5) . . ? Ag C132 3.818(5) . . ? Ag C211 3.748(4) . . ? Ag C212 3.846(5) . . ? Ag C221 3.740(4) . . ? Ag C222 4.102(5) . . ? Ag C231 3.682(4) . . ? Ag C232 3.881(5) . . ? Ag C311 3.759(5) . . ? Ag C312 3.951(5) . . ? Ag C321 3.689(5) . . ? Ag C322 3.921(6) . . ? Ag C331 3.652(5) . . ? Ag C332 3.933(5) . . ? Ag H2a 3.6468(8) . . ? Ag H5a 3.3179(6) . . ? Ag H112 3.2295(6) . . ? Ag H132 3.4058(8) . . ? Ag H212 3.2595(7) . . ? Ag H232 3.3991(7) . . ? Ag H312 3.4416(6) . . ? Ag H322 3.4995(7) . . ? Ag H332 3.5808(7) . . ? N1a N3a 2.203(6) . . ? N1a C4a 2.239(7) . . ? N1a H2a 2.008(4) . . ? N1a H5a 2.060(4) . . ? N1a H322 2.742(4) . . ? C2a C4a 2.177(7) . . ? C2a C5a 2.116(7) . . ? C2a O3 3.360(7) . . ? C2a H3a 2.058(5) . . ? N3a C5a 2.165(6) . . ? N3a C41 2.522(7) . . ? N3a C42 2.977(7) . . ? N3a O1 2.817(5) . . ? N3a O3 3.111(6) . . ? N3a H2a 2.031(4) . . ? N3a H42 2.686(4) . . ? C4a C42 2.469(8) . . ? C4a C46a 2.482(10) . . ? C4a C46b 2.44(3) . . ? C4a H3a 2.090(5) . . ? C4a H5a 2.047(5) . . ? C4a H42 2.651(5) . . ? C4a H46a 2.638(5) . . ? C4a H46b 2.618(5) . . ? C5a C41 2.582(7) . . ? C5a C46a 3.048(10) . . ? C5a C46b 3.05(3) . . ? C5a H46a 2.763(6) . . ? C5a H46b 2.815(5) . . ? C41 C43a 2.390(11) . . ? C41 C44a 2.761(10) . . ? C41 C45a 2.397(10) . . ? C41 C43b 2.286(15) . . ? C41 C44b 2.88(2) . . ? C41 C45b 2.53(3) . . ? C41 H3a 2.806(5) . . ? C41 H5a 2.885(5) . . ? C41 H42 1.974(5) . . ? C41 H46a 2.088(5) . . ? C41 H46b 2.236(5) . . ? C42 C44a 2.369(10) . . ? C42 C45a 2.696(10) . . ? C42 C46a 2.339(10) . . ? C42 C44b 2.42(2) . . ? C42 C45b 2.63(3) . . ? C42 C46b 2.36(2) . . ? C42 O1 3.277(7) . . ? C42 H3a 2.817(6) . . ? C42 H43a 2.094(6) . . ? C42 H43b 1.936(6) . . ? C43a C45a 2.283(12) . . ? C43a C46a 2.717(12) . . ? C43a C45b 2.20(3) . . ? C43a C46b 2.81(3) . . ? C43a H42 2.107(9) . . ? C43a H44a 1.926(9) . . ? C43a H44b 1.979(9) . . ? C44a C46a 2.391(11) . . ? C44a C46b 2.77(3) . . ? C44a H43a 1.917(7) . . ? C44a H45a 2.018(8) . . ? C44a H43b 1.933(7) . . ? C44a H45b 2.573(8) . . ? C45a C43b 2.378(17) . . ? C45a C46b 2.24(3) . . ? C45a H44a 2.030(8) . . ? C45a H46a 2.025(8) . . ? C45a H44b 2.482(9) . . ? C45a H45b 2.577(11) . . ? C46a C43b 2.709(15) . . ? C46a C44b 2.77(2) . . ? C46a C45b 2.32(3) . . ? C46a H5a 2.894(8) . . ? C46a H45a 2.006(8) . . ? C46a H46b 2.181(10) . . ? C43b C45b 2.33(3) . . ? C43b C46b 2.82(3) . . ? C43b H42 1.894(17) . . ? C43b H44a 2.132(17) . . ? C43b H44b 2.206(16) . . ? C44b C46b 2.56(3) . . ? C44b H43a 1.77(2) . . ? C44b H45a 2.59(2) . . ? C44b H43b 2.16(2) . . ? C44b H45b 1.92(2) . . ? C45b H43a 2.85(3) . . ? C45b H44a 2.37(3) . . ? C45b H45a 2.49(3) . . ? C45b H44b 1.98(3) . . ? C45b H46b 2.25(3) . . ? C46b H46a 2.14(3) . . ? C46b H45b 2.14(3) . . ? P1 C112 2.756(5) . . ? P1 C116 2.804(5) . . ? P1 C122 2.778(5) . . ? P1 C126 2.819(5) . . ? P1 C132 2.767(5) . . ? P1 C136 2.831(6) . . ? P1 H112 2.8308(14) . . ? P1 H116 2.9130(12) . . ? P1 H122 2.8542(14) . . ? P1 H126 2.9279(13) . . ? P1 H132 2.8348(14) . . ? P1 H136 2.9413(14) . . ? C111 C113 2.410(8) . . ? C111 C114 2.767(8) . . ? C111 C115 2.388(7) . . ? C111 C121 2.858(6) . . ? C111 C131 2.851(6) . . ? C111 C136 3.061(7) . . ? C111 H112 2.046(4) . . ? C111 H116 2.023(4) . . ? C111 H136 2.579(5) . . ? C112 C114 2.389(9) . . ? C112 C115 2.751(8) . . ? C112 C116 2.387(7) . . ? C112 H2a 2.874(6) . . ? C112 H113 2.040(5) . . ? C113 C115 2.374(9) . . ? C113 C116 2.760(8) . . ? C113 O3 3.277(8) . '2 566' ? C113 H112 2.046(7) . . ? C113 H114 2.015(7) . . ? C114 C116 2.391(8) . . ? C114 H113 2.021(6) . . ? C114 H115 2.021(6) . . ? C115 H114 2.015(6) . . ? C115 H116 2.035(6) . . ? C116 C121 3.125(7) . . ? C116 H115 2.030(5) . . ? C116 H136 2.777(5) . . ? C121 C123 2.406(7) . . ? C121 C124 2.781(7) . . ? C121 C125 2.400(7) . . ? C121 C131 2.858(6) . . ? C121 H116 2.692(4) . . ? C121 H122 2.028(5) . . ? C121 H126 2.040(5) . . ? C121 H332 2.813(4) . . ? C122 C124 2.375(7) . . ? C122 C125 2.724(8) . . ? C122 C126 2.371(8) . . ? C122 H123 2.029(5) . . ? C123 C125 2.351(9) . . ? C123 C126 2.745(8) . . ? C123 H122 2.024(5) . . ? C123 H124 2.018(5) . . ? C124 C126 2.387(8) . . ? C124 H123 2.013(6) . . ? C124 H125 2.003(6) . . ? C125 H124 2.012(6) . . ? C125 H126 2.034(6) . . ? C126 C131 3.046(7) . . ? C126 H125 2.026(5) . . ? C131 C133 2.407(7) . . ? C131 C134 2.787(8) . . ? C131 C135 2.409(8) . . ? C131 H126 2.560(4) . . ? C131 H132 2.042(4) . . ? C131 H136 2.028(5) . . ? C131 H212 2.813(4) . . ? C132 C134 2.388(8) . . ? C132 C135 2.753(8) . . ? C132 C136 2.381(7) . . ? C132 H126 2.868(5) . . ? C132 H133 2.027(5) . . ? C133 C135 2.369(8) . . ? C133 C136 2.746(7) . . ? C133 H132 2.032(6) . . ? C133 H134 2.017(6) . . ? C134 C136 2.398(7) . . ? C134 O2 3.364(7) . '1 655' ? C134 H133 2.011(6) . . ? C134 H135 2.030(6) . . ? C135 H134 2.031(6) . . ? C135 H136 2.038(6) . . ? C136 H135 2.040(6) . . ? P2 C212 2.755(5) . . ? P2 C216 2.828(5) . . ? P2 C222 2.760(5) . . ? P2 C226 2.841(5) . . ? P2 C232 2.771(5) . . ? P2 C236 2.837(5) . . ? P2 H212 2.8172(13) . . ? P2 H216 2.9358(13) . . ? P2 H222 2.8192(13) . . ? P2 H226 2.9569(12) . . ? P2 H232 2.8319(13) . . ? P2 H236 2.9480(14) . . ? C211 C213 2.412(7) . . ? C211 C214 2.782(7) . . ? C211 C215 2.398(7) . . ? C211 C221 2.829(7) . . ? C211 C222 3.346(7) . . ? C211 C231 2.871(6) . . ? C211 C236 3.108(6) . . ? C211 H212 2.032(4) . . ? C211 H216 2.023(4) . . ? C211 H236 2.633(4) . . ? C212 C214 2.398(7) . . ? C212 C215 2.749(7) . . ? C212 C216 2.372(6) . . ? C212 H213 2.045(5) . . ? C213 C215 2.373(7) . . ? C213 C216 2.749(7) . . ? C213 H212 2.046(6) . . ? C213 H214 2.025(6) . . ? C214 C216 2.388(8) . . ? C214 H213 2.026(5) . . ? C214 H215 2.024(5) . . ? C215 H214 2.025(5) . . ? C215 H216 2.030(5) . . ? C216 C221 3.089(7) . . ? C216 H43a 2.789(5) . '2 565' ? C216 H215 2.030(5) . . ? C216 H236 2.814(5) . . ? C221 C223 2.410(7) . . ? C221 C224 2.788(7) . . ? C221 C225 2.397(7) . . ? C221 C231 2.851(6) . . ? C221 H216 2.661(5) . . ? C221 H222 2.032(4) . . ? C221 H226 2.026(4) . . ? C221 H312 2.794(5) . . ? C222 C224 2.387(7) . . ? C222 C225 2.731(7) . . ? C222 C226 2.367(7) . . ? C222 H223 2.034(5) . . ? C223 C225 2.354(8) . . ? C223 C226 2.738(8) . . ? C223 H222 2.034(5) . . ? C223 H224 2.020(5) . . ? C224 C226 2.389(8) . . ? C224 H223 2.013(6) . . ? C224 H225 2.014(6) . . ? C225 H224 2.022(6) . . ? C225 H226 2.028(5) . . ? C226 C231 3.077(7) . . ? C226 H225 2.026(5) . . ? C231 C233 2.419(7) . . ? C231 C234 2.786(7) . . ? C231 C235 2.414(7) . . ? C231 H226 2.600(4) . . ? C231 H232 2.037(5) . . ? C231 H236 2.024(5) . . ? C232 C234 2.374(7) . . ? C232 C235 2.747(8) . . ? C232 C236 2.369(7) . . ? C232 H226 2.865(5) . . ? C232 H233 2.028(5) . . ? C233 C235 2.388(8) . . ? C233 C236 2.751(7) . . ? C233 H232 2.019(5) . . ? C233 H234 2.024(5) . . ? C234 C236 2.386(7) . . ? C234 H233 2.027(6) . . ? C234 H235 2.033(6) . . ? C235 H234 2.030(5) . . ? C235 H236 2.027(5) . . ? C236 H235 2.039(5) . . ? P3 C312 2.772(5) . . ? P3 C316 2.826(7) . . ? P3 C322 2.737(6) . . ? P3 C326 2.833(5) . . ? P3 C332 2.751(5) . . ? P3 C336 2.838(5) . . ? P3 H312 2.8397(13) . . ? P3 H316 2.9370(15) . . ? P3 H322 2.7915(14) . . ? P3 H326 2.9565(14) . . ? P3 H332 2.8077(14) . . ? P3 H336 2.9593(13) . . ? C311 C313 2.413(7) . . ? C311 C314 2.779(8) . . ? C311 C315 2.405(9) . . ? C311 C321 2.850(6) . . ? C311 C331 2.873(7) . . ? C311 C336 3.111(7) . . ? C311 H312 2.028(4) . . ? C311 H316 2.026(5) . . ? C311 H336 2.643(5) . . ? C312 C314 2.371(9) . . ? C312 C315 2.724(9) . . ? C312 C316 2.360(8) . . ? C312 H313 2.032(5) . . ? C313 C315 2.354(9) . . ? C313 C316 2.742(8) . . ? C313 H312 2.022(6) . . ? C313 H314 2.016(6) . . ? C314 C316 2.377(8) . . ? C314 H313 2.019(7) . . ? C314 H315 1.998(7) . . ? C315 H314 2.002(6) . . ? C315 H316 2.032(6) . . ? C316 C321 3.092(7) . . ? C316 H315 2.031(6) . . ? C321 C323 2.398(8) . . ? C321 C324 2.772(8) . . ? C321 C325 2.398(7) . . ? C321 C331 2.882(6) . . ? C321 H316 2.653(5) . . ? C321 H322 2.021(5) . . ? C321 H326 2.027(5) . . ? C322 C324 2.382(9) . . ? C322 C325 2.727(8) . . ? C322 C326 2.362(8) . . ? C322 H323 2.029(5) . . ? C323 C325 2.350(9) . . ? C323 C326 2.739(8) . . ? C323 H322 2.025(7) . . ? C323 H324 2.021(7) . . ? C324 C326 2.379(8) . . ? C324 H323 2.020(7) . . ? C324 H325 1.992(7) . . ? C325 O3 3.270(7) . '2 556' ? C325 H324 1.995(6) . . ? C325 H326 2.041(6) . . ? C326 C331 3.122(7) . . ? C326 C332 3.346(7) . . ? C326 H325 2.035(5) . . ? C331 C333 2.416(7) . . ? C331 C334 2.784(7) . . ? C331 C335 2.395(7) . . ? C331 H232 2.890(4) . . ? C331 H326 2.660(4) . . ? C331 H332 2.031(5) . . ? C331 H336 2.037(5) . . ? C332 C334 2.388(7) . . ? C332 C335 2.734(7) . . ? C332 C336 2.378(7) . . ? C332 H326 2.784(5) . . ? C332 H333 2.042(5) . . ? C333 C335 2.369(8) . . ? C333 C336 2.761(8) . . ? C333 H332 2.033(5) . . ? C333 H334 2.027(5) . . ? C334 C336 2.393(8) . . ? C334 H333 2.031(6) . . ? C334 H335 2.013(6) . . ? C335 H334 2.022(6) . . ? C335 H336 2.033(6) . . ? C336 H335 2.024(5) . . ? N H3a 2.518(5) . . ? O1 O2 2.122(6) . . ? O1 O3 2.088(6) . . ? O1 H3a 1.867(4) . . ? O1 H42 2.355(4) . . ? O1 H124 2.828(5) . '2 556' ? O2 O3 2.152(7) . . ? O2 H134 2.498(5) . '1 455' ? O2 H213 2.499(5) . '2 566' ? O3 H3a 2.430(4) . . ? O3 H113 2.868(5) . '2 566' ? O3 H325 2.534(4) . '2 556' ? H3a H42 2.2389(3) . . ? H5a H46a 2.3558(3) . . ? H42 H43b 2.2241(3) . . ? H43a H44a 2.2074(3) . . ? H43a H44b 2.0989(3) . . ? H44a H45a 2.3204(5) . . ? H44a H43b 2.3315(3) . . ? H45a H46a 2.3177(3) . . ? H46a H46b 2.3318(5) . . ? H44b H45b 2.2713(5) . . ? H45b H114 2.3383(3) . '1 554' ? H46b H223 2.3792(5) . . ? H112 H113 2.3462(3) . . ? H113 H114 2.3189(3) . . ? H114 H115 2.3153(4) . . ? H115 H116 2.3304(3) . . ? H122 H123 2.3214(4) . . ? H123 H124 2.3154(4) . . ? H124 H125 2.3024(4) . . ? H125 H126 2.3266(4) . . ? H132 H133 2.3247(5) . . ? H133 H134 2.3110(3) . . ? H134 H135 2.3340(4) . . ? H135 H136 2.3378(5) . . ? H212 H213 2.3468(5) . . ? H213 H214 2.3290(3) . . ? H214 H215 2.3258(3) . . ? H214 H326 2.3911(4) . '1 565' ? H215 H216 2.3254(5) . . ? H222 H223 2.3315(3) . . ? H223 H224 2.3181(3) . . ? H224 H225 2.3170(5) . . ? H225 H226 2.3213(3) . . ? H232 H233 2.3183(5) . . ? H233 H234 2.3272(4) . . ? H234 H235 2.3336(5) . . ? H235 H236 2.3297(5) . . ? H312 H313 2.3229(3) . . ? H313 H314 2.3188(3) . . ? H314 H315 2.2939(3) . . ? H315 H316 2.3263(3) . . ? H322 H323 2.3244(4) . . ? H323 H324 2.3221(4) . . ? H324 H325 2.2868(5) . . ? H325 H326 2.3360(4) . . ? H332 H333 2.3363(5) . . ? H333 H334 2.3329(3) . . ? H334 H335 2.3151(3) . . ? H335 H336 2.3234(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 [(Ph3P)3Ag(C9H8N2)](NO3) _exptl_crystal_F_000 1136 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 8 8 6 11 0 0 0 9 0 0 0 10 -8 -8 -6 -11 0 0 0 -9 0 0 0 -10 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min -15 _reflns_limit_l_max 15 _reflns_number_observed 6504 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression Zachariasen _refine_ls_matrix_type 'block diagonal' _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .076 _refine_ls_wR_factor_all .051 _refine_ls_goodness_of_fit_all 1.395 _refine_ls_shift/su_mean .003 #========================================================================== # 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 data_cp11 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C42 H38 Ag1 N5 O3 P2' _chemical_formula_moiety ? _chemical_formula_weight 830.61 _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 12.947(7) _cell_length_b 15.034(2) _cell_length_c 20.551(2) _cell_angle_alpha 90.00000 _cell_angle_beta 99.43(3) _cell_angle_gamma 90.00000 _cell_volume 3946(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.398 _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 14.0 _cell_measurement_theta_max 15.3 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .64 _exptl_crystal_description prism _exptl_crystal_size_max .31 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .18 _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 .88 _exptl_absorpt_correction_T_max .90 _diffrn_reflns_number 5482 _reflns_number_total 5482 _reflns_Friedel_coverage ? _reflns_number_gt 2281 _reflns_threshold_expression 'I > 2.50 sig(I )' _diffrn_reflns_theta_max 23 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .069 _refine_ls_wR_factor_ref .068 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_number_reflns 2281 _refine_ls_number_parameters 476 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .013 _refine_diff_density_min -.59 _refine_diff_density_max .95 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _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 ? 0 168 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 152 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 4 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 20 .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 8 .09 .095 '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 Ag .72386(9) .56551(9) .27090(6) .0528(7) Uani ? ? 1.00000 ? ? N1a .6121(12) .6368(12) .1918(8) .075(12) Uani ? ? 1.00000 ? ? C2a .5354(18) .6088(13) .1481(10) .081(14) Uani ? ? 1.00000 ? ? N3a .4619(15) .6641(19) .1259(9) .110(16) Uani ? ? 1.00000 ? ? C4a .496(3) .743(2) .1582(15) .13(3) Uani ? ? 1.00000 ? ? C5a .584(2) .7236(18) .1964(10) .11(2) Uani ? ? 1.00000 ? ? N1b .7221(10) .4332(13) .2111(8) .076(10) Uani ? ? 1.00000 ? ? C2b .7120(15) .3460(16) .2230(11) .087(15) Uani ? ? 1.00000 ? ? N3b .6955(16) .3022(15) .1613(16) .16(2) Uani ? ? 1.00000 ? ? C4b .7019(16) .3689(17) .1167(11) .076(15) Uani ? ? 1.00000 ? ? C5b .7155(14) .4384(16) .1482(11) .089(15) Uani ? ? 1.00000 ? ? P1 .9029(3) .6199(3) .28740(19) .051(3) Uani ? ? 1.00000 ? ? C111 .9234(12) .7255(10) .3307(7) .049(10) Uani ? ? 1.00000 ? ? C112 .8462(13) .7539(11) .3645(9) .071(12) Uani ? ? 1.00000 ? ? C113 .8582(16) .8314(14) .3997(9) .085(14) Uani ? ? 1.00000 ? ? C114 .9422(17) .8820(12) .4023(10) .080(14) Uani ? ? 1.00000 ? ? C115 1.0224(17) .8551(13) .3715(11) .101(16) Uani ? ? 1.00000 ? ? C116 1.0125(15) .7763(14) .3363(10) .086(15) Uani ? ? 1.00000 ? ? C121 .9635(15) .6315(10) .2128(9) .057(11) Uani ? ? 1.00000 ? ? C122 .8970(16) .6398(11) .1529(10) .078(13) Uani ? ? 1.00000 ? ? C123 .936(2) .6442(13) .0945(9) .088(15) Uani ? ? 1.00000 ? ? C124 1.040(2) .6411(13) .0967(11) .089(17) Uani ? ? 1.00000 ? ? C125 1.1083(17) .6307(13) .1540(13) .091(16) Uani ? ? 1.00000 ? ? C126 1.0705(14) .6254(11) .2149(8) .068(12) Uani ? ? 1.00000 ? ? C131 .9835(12) .5397(10) .3342(8) .049(11) Uani ? ? 1.00000 ? ? C132 .9896(13) .4533(13) .3086(8) .067(12) Uani ? ? 1.00000 ? ? C133 1.0389(16) .3869(13) .3448(11) .081(15) Uani ? ? 1.00000 ? ? C134 1.0826(14) .4009(14) .4090(12) .078(14) Uani ? ? 1.00000 ? ? C135 1.0778(15) .4842(16) .4368(9) .072(14) Uani ? ? 1.00000 ? ? C136 1.0296(14) .5529(11) .3991(10) .066(12) Uani ? ? 1.00000 ? ? P2 .6205(3) .5384(3) .3591(2) .051(3) Uani ? ? 1.00000 ? ? C211 .6712(11) .4493(9) .4097(6) .042(9) Uani ? ? 1.00000 ? ? C212 .7686(13) .4146(11) .4079(8) .059(11) Uani ? ? 1.00000 ? ? C213 .8101(15) .3467(12) .4462(10) .083(14) Uani ? ? 1.00000 ? ? C214 .7545(16) .3080(11) .4900(9) .075(13) Uani ? ? 1.00000 ? ? C215 .6570(15) .3352(13) .4921(9) .071(13) Uani ? ? 1.00000 ? ? C216 .6154(13) .4053(11) .4540(9) .063(12) Uani ? ? 1.00000 ? ? C221 .4865(12) .5117(10) .3284(8) .053(10) Uani ? ? 1.00000 ? ? C222 .4613(12) .4716(12) .2705(9) .066(12) Uani ? ? 1.00000 ? ? C223 .3635(15) .4480(14) .2410(8) .082(13) Uani ? ? 1.00000 ? ? C224 .2816(14) .4667(14) .2755(13) .094(16) Uani ? ? 1.00000 ? ? C225 .3032(15) .5045(15) .3366(11) .088(15) Uani ? ? 1.00000 ? ? C226 .4029(14) .5266(12) .3633(8) .070(12) Uani ? ? 1.00000 ? ? C231 .6139(12) .6278(12) .4142(8) .054(11) Uani ? ? 1.00000 ? ? C232 .5727(14) .7084(14) .3884(9) .072(13) Uani ? ? 1.00000 ? ? C233 .5746(16) .7842(13) .4274(12) .086(15) Uani ? ? 1.00000 ? ? C234 .6121(16) .7782(17) .4920(14) .089(17) Uani ? ? 1.00000 ? ? C235 .6512(18) .701(2) .5205(10) .102(18) Uani ? ? 1.00000 ? ? C236 .6517(13) .6281(13) .4807(11) .076(13) Uani ? ? 1.00000 ? ? N .710(2) .4655(18) -.0289(13) .13(2) Uani ? ? 1.00000 ? ? O1 .6855(16) .3887(12) -.0200(8) .149(14) Uani ? ? 1.00000 ? ? O2 .6740(18) .4975(13) -.0801(11) .189(19) Uani ? ? 1.00000 ? ? O3 .763(2) .5060(15) .0120(11) .21(2) Uani ? ? 1.00000 ? ? H2a .53317 .54883 .13262 .09660 Uiso ? ? 1.00000 ? ? H3a .40013 .65350 .09514 .13460 Uiso ? ? 1.00000 ? ? H4a .46150 .79811 .15331 .16930 Uiso ? ? 1.00000 ? ? H5a .62409 .76590 .22422 .13110 Uiso ? ? 1.00000 ? ? H2b .71541 .31867 .26486 .11030 Uiso ? ? 1.00000 ? ? H3b .68313 .24122 .15224 .20000 Uiso ? ? 1.00000 ? ? H4b .69687 .36285 .07014 .09280 Uiso ? ? 1.00000 ? ? H5b .72085 .49395 .12669 .11120 Uiso ? ? 1.00000 ? ? H112 .78402 .71932 .36340 .09290 Uiso ? ? 1.00000 ? ? H113 .80401 .84939 .42308 .11000 Uiso ? ? 1.00000 ? ? H114 .94642 .93702 .42559 .10250 Uiso ? ? 1.00000 ? ? H115 1.08410 .88984 .37416 .12900 Uiso ? ? 1.00000 ? ? H116 1.06891 .75673 .31529 .11080 Uiso ? ? 1.00000 ? ? H122 .82312 .64243 .15214 .10090 Uiso ? ? 1.00000 ? ? H123 .88950 .64971 .05354 .11140 Uiso ? ? 1.00000 ? ? H124 1.06745 .64625 .05644 .11620 Uiso ? ? 1.00000 ? ? H125 1.18109 .62660 .15296 .12220 Uiso ? ? 1.00000 ? ? H126 1.11726 .61810 .25564 .08990 Uiso ? ? 1.00000 ? ? H132 .95801 .44152 .26416 .08510 Uiso ? ? 1.00000 ? ? H133 1.04330 .32962 .32571 .10100 Uiso ? ? 1.00000 ? ? H134 1.11658 .35338 .43478 .09690 Uiso ? ? 1.00000 ? ? H135 1.10780 .49415 .48197 .09130 Uiso ? ? 1.00000 ? ? H136 1.02823 .61087 .41820 .08410 Uiso ? ? 1.00000 ? ? H212 .80912 .43968 .37761 .07460 Uiso ? ? 1.00000 ? ? H213 .87857 .32560 .44314 .10650 Uiso ? ? 1.00000 ? ? H214 .78539 .26191 .51871 .09350 Uiso ? ? 1.00000 ? ? H215 .61631 .30544 .52008 .09000 Uiso ? ? 1.00000 ? ? H216 .54625 .42506 .45743 .07990 Uiso ? ? 1.00000 ? ? H222 .51742 .45796 .24729 .08190 Uiso ? ? 1.00000 ? ? H223 .35146 .41984 .19889 .10070 Uiso ? ? 1.00000 ? ? H224 .21141 .45340 .25652 .11370 Uiso ? ? 1.00000 ? ? H225 .24757 .51554 .36055 .11100 Uiso ? ? 1.00000 ? ? H226 .41687 .55212 .40637 .09030 Uiso ? ? 1.00000 ? ? H232 .54205 .71167 .34286 .09230 Uiso ? ? 1.00000 ? ? H233 .54991 .83956 .40832 .11190 Uiso ? ? 1.00000 ? ? H234 .61090 .82950 .51885 .11480 Uiso ? ? 1.00000 ? ? H235 .67726 .69768 .56634 .12930 Uiso ? ? 1.00000 ? ? H236 .68014 .57387 .50017 .09540 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 Ag .0545(8) .0585(8) .0501(7) -.0049(9) .0220(6) -.0031(9) N1a .068(12) .088(14) .071(12) -.005(11) .015(10) -.006(10) C2a .067(14) .094(17) .071(14) .011(13) -.016(11) .040(13) N3a .083(14) .17(2) .072(14) .017(16) -.006(11) .033(14) C4a .18(3) .15(3) .08(2) .08(3) .03(2) .03(2) C5a .17(3) .09(2) .059(15) .01(2) .014(16) .018(14) N1b .068(9) .092(13) .073(11) -.014(11) .030(8) -.017(12) C2b .089(16) .059(15) .121(19) -.009(13) .043(14) -.011(14) N3b .118(17) .11(2) .25(3) -.018(15) .021(19) -.10(2) C4b .079(15) .060(16) .084(16) -.002(13) -.004(12) -.013(14) C5b .075(13) .104(18) .094(17) -.010(14) .029(12) -.068(16) P1 .053(3) .057(3) .045(3) -.005(3) .020(2) .001(2) C111 .052(11) .048(11) .052(11) -.011(9) .025(9) -.005(9) C112 .079(14) .039(11) .110(15) -.006(10) .054(12) -.021(11) C113 .091(15) .079(15) .095(15) -.016(13) .047(13) -.045(12) C114 .090(16) .051(13) .108(16) .001(12) .045(14) .004(11) C115 .108(19) .059(15) .14(2) -.057(13) .045(16) -.039(14) C116 .073(15) .095(17) .103(17) -.009(13) .049(13) -.012(13) C121 .095(15) .025(10) .060(12) .004(10) .040(12) .019(9) C122 .108(16) .055(13) .081(14) -.018(12) .048(14) .001(12) C123 .114(19) .088(16) .068(14) -.026(15) .033(14) -.015(12) C124 .15(3) .063(14) .071(15) -.017(16) .055(17) .005(12) C125 .095(18) .065(14) .14(2) .007(13) .084(17) -.000(15) C126 .072(14) .070(13) .074(13) .009(11) .045(11) .003(10) C131 .051(10) .038(13) .063(12) -.013(8) .028(9) -.005(9) C132 .073(13) .060(14) .070(12) -.004(11) .021(10) .009(11) C133 .087(17) .060(14) .096(17) .007(12) .017(13) .025(13) C134 .058(13) .075(16) .101(17) .005(11) .018(13) .048(14) C135 .082(15) .067(15) .074(14) -.011(13) .029(11) -.013(13) C136 .079(13) .035(11) .090(14) -.004(11) .032(11) .009(13) P2 .049(3) .058(3) .049(3) -.002(2) .021(2) -.003(2) C211 .058(10) .033(10) .040(8) -.008(9) .022(8) -.003(8) C212 .065(12) .052(13) .065(11) .010(10) .026(9) .017(10) C213 .105(16) .050(12) .104(16) .014(12) .049(14) .023(12) C214 .085(15) .060(13) .081(14) -.031(12) .015(12) .020(10) C215 .053(13) .091(16) .075(13) -.004(12) .032(11) .019(12) C216 .066(12) .056(13) .072(13) .006(10) .027(10) .008(10) C221 .062(12) .060(11) .041(10) -.002(9) .016(9) .006(9) C222 .037(11) .105(17) .059(12) .004(10) .012(9) -.002(11) C223 .071(13) .114(17) .059(11) .003(15) .001(10) .002(12) C224 .040(12) .10(2) .13(2) -.006(11) -.004(14) .006(15) C225 .046(13) .123(18) .100(17) .009(13) .023(13) .023(15) C226 .053(12) .094(15) .072(12) -.009(11) .035(11) -.001(10) C231 .054(11) .063(13) .049(11) -.020(10) .018(9) -.020(10) C232 .082(14) .057(13) .085(14) .022(12) .038(11) -.002(12) C233 .098(17) .056(14) .118(18) .002(12) .058(16) -.007(14) C234 .060(15) .10(2) .12(2) -.023(14) .052(16) -.051(18) C235 .103(19) .13(2) .082(17) -.003(17) .035(14) -.010(17) C236 .065(13) .076(15) .091(16) -.008(11) .021(12) -.024(13) N .13(2) .11(2) .12(2) -.033(17) -.014(16) .035(18) O1 .22(2) .081(12) .128(14) -.032(14) -.036(12) .019(12) O2 .24(2) .145(17) .16(2) -.029(16) -.018(17) .046(15) O3 .27(3) .17(2) .16(2) -.078(19) -.027(19) .004(16) # 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 Ag N1a . . 2.261(15) ? Ag N1b . . 2.336(18) ? Ag P1 . . 2.428(4) ? Ag P2 . . 2.458(5) ? N1a C2a . . 1.30(3) ? N1a C5a . . 1.36(3) ? C2a N3a . . 1.29(3) ? C2a H2a . . .95(2) ? N3a C4a . . 1.39(4) ? N3a H3a . . .948(18) ? C4a C5a . . 1.31(4) ? C4a H4a . . .94(3) ? C5a H5a . . .95(3) ? N1b C2b . . 1.34(3) ? N1b C5b . . 1.28(3) ? C2b N3b . . 1.41(4) ? C2b H2b . . .95(2) ? N3b C4b . . 1.37(4) ? N3b H3b . . .94(2) ? C4b C5b . . 1.23(3) ? C4b H4b . . .95(2) ? C5b H5b . . .95(2) ? P1 C111 . . 1.819(16) ? P1 C121 . . 1.84(2) ? P1 C131 . . 1.772(15) ? C111 C112 . . 1.37(2) ? C111 C116 . . 1.37(3) ? C112 C113 . . 1.37(3) ? C112 H112 . . .956(17) ? C113 C114 . . 1.32(3) ? C113 H113 . . .95(2) ? C114 C115 . . 1.36(3) ? C114 H114 . . .953(18) ? C115 C116 . . 1.38(3) ? C115 H115 . . .95(2) ? C116 H116 . . .95(2) ? C121 C122 . . 1.39(3) ? C121 C126 . . 1.38(3) ? C122 C123 . . 1.38(3) ? C122 H122 . . .95(2) ? C123 C124 . . 1.35(4) ? C123 H123 . . .95(2) ? C124 C125 . . 1.36(3) ? C124 H124 . . .95(3) ? C125 C126 . . 1.42(3) ? C125 H125 . . .95(2) ? C126 H126 . . .956(16) ? C131 C132 . . 1.41(2) ? C131 C136 . . 1.38(2) ? C132 C133 . . 1.34(3) ? C132 H132 . . .955(16) ? C133 C134 . . 1.36(3) ? C133 H133 . . .95(2) ? C134 C135 . . 1.38(3) ? C134 H134 . . .95(2) ? C135 C136 . . 1.38(3) ? C135 H135 . . .957(17) ? C136 H136 . . .956(18) ? P2 C211 . . 1.755(14) ? P2 C221 . . 1.793(16) ? P2 C231 . . 1.769(18) ? C211 C212 . . 1.37(2) ? C211 C216 . . 1.42(2) ? C212 C213 . . 1.35(2) ? C212 H212 . . .954(17) ? C213 C214 . . 1.37(3) ? C213 H213 . . .95(2) ? C214 C215 . . 1.33(3) ? C214 H214 . . .954(17) ? C215 C216 . . 1.37(2) ? C215 H215 . . .95(2) ? C216 H216 . . .957(17) ? C221 C222 . . 1.32(2) ? C221 C226 . . 1.41(3) ? C222 C223 . . 1.36(2) ? C222 H222 . . .954(18) ? C223 C224 . . 1.40(3) ? C223 H223 . . .953(17) ? C224 C225 . . 1.36(3) ? C224 H224 . . .950(18) ? C225 C226 . . 1.36(3) ? C225 H225 . . .95(2) ? C226 H226 . . .955(16) ? C231 C232 . . 1.39(3) ? C231 C236 . . 1.37(3) ? C232 C233 . . 1.39(3) ? C232 H232 . . .956(17) ? C233 C234 . . 1.34(4) ? C233 H233 . . .95(2) ? C234 C235 . . 1.36(4) ? C234 H234 . . .95(3) ? C235 C236 . . 1.37(3) ? C235 H235 . . .95(2) ? C236 H236 . . .955(19) ? N O1 . . 1.22(3) ? N O2 . . 1.18(3) ? N O3 . . 1.17(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 N1a Ag N1b . . . 94.4(6) ? N1a Ag P1 . . . 115.1(4) ? N1a Ag P2 . . . 104.3(4) ? N1b Ag P1 . . . 106.7(3) ? N1b Ag P2 . . . 106.7(4) ? P1 Ag P2 . . . 125.12(14) ? Ag N1a C2a . . . 132.2(15) ? Ag N1a C5a . . . 123.3(13) ? C2a N1a C5a . . . 100.3(17) ? N1a C2a N3a . . . 118(2) ? N1a C2a H2a . . . 121(2) ? N3a C2a H2a . . . 121(2) ? C2a N3a C4a . . . 103(2) ? C2a N3a H3a . . . 128(3) ? C4a N3a H3a . . . 129(3) ? N3a C4a C5a . . . 106(3) ? N3a C4a H4a . . . 127(3) ? C5a C4a H4a . . . 127(3) ? N1a C5a C4a . . . 112(2) ? N1a C5a H5a . . . 124(3) ? C4a C5a H5a . . . 123(3) ? Ag N1b C2b . . . 136.8(14) ? Ag N1b C5b . . . 118.1(15) ? C2b N1b C5b . . . 104.4(19) ? N1b C2b N3b . . . 107(2) ? N1b C2b H2b . . . 127(2) ? N3b C2b H2b . . . 126(2) ? C2b N3b C4b . . . 104(2) ? C2b N3b H3b . . . 129(3) ? C4b N3b H3b . . . 127(3) ? N3b C4b C5b . . . 107(2) ? N3b C4b H4b . . . 127(3) ? C5b C4b H4b . . . 126(3) ? N1b C5b C4b . . . 117(2) ? N1b C5b H5b . . . 122(2) ? C4b C5b H5b . . . 121(2) ? Ag P1 C111 . . . 115.0(6) ? Ag P1 C121 . . . 116.3(6) ? Ag P1 C131 . . . 108.1(5) ? C111 P1 C121 . . . 106.1(7) ? C111 P1 C131 . . . 107.6(7) ? C121 P1 C131 . . . 102.9(8) ? P1 C111 C112 . . . 117.3(12) ? P1 C111 C116 . . . 125.4(14) ? C112 C111 C116 . . . 117.2(15) ? C111 C112 C113 . . . 120.2(16) ? C111 C112 H112 . . . 119.9(16) ? C113 C112 H112 . . . 119.9(19) ? C112 C113 C114 . . . 122(2) ? C112 C113 H113 . . . 119(2) ? C114 C113 H113 . . . 119(2) ? C113 C114 C115 . . . 119.7(18) ? C113 C114 H114 . . . 120(2) ? C115 C114 H114 . . . 120(2) ? C114 C115 C116 . . . 119(2) ? C114 C115 H115 . . . 121(2) ? C116 C115 H115 . . . 120(2) ? C111 C116 C115 . . . 122(2) ? C111 C116 H116 . . . 119(2) ? C115 C116 H116 . . . 119(2) ? P1 C121 C122 . . . 117.3(16) ? P1 C121 C126 . . . 122.0(13) ? C122 C121 C126 . . . 120.5(18) ? C121 C122 C123 . . . 121(2) ? C121 C122 H122 . . . 120(2) ? C123 C122 H122 . . . 119(2) ? C122 C123 C124 . . . 118.4(19) ? C122 C123 H123 . . . 121(2) ? C124 C123 H123 . . . 121(2) ? C123 C124 C125 . . . 122(2) ? C123 C124 H124 . . . 119(2) ? C125 C124 H124 . . . 119(3) ? C124 C125 C126 . . . 120(2) ? C124 C125 H125 . . . 119(3) ? C126 C125 H125 . . . 120(2) ? C121 C126 C125 . . . 117.3(16) ? C121 C126 H126 . . . 121.5(18) ? C125 C126 H126 . . . 121.2(19) ? P1 C131 C132 . . . 119.3(12) ? P1 C131 C136 . . . 123.3(12) ? C132 C131 C136 . . . 116.8(14) ? C131 C132 C133 . . . 122.0(16) ? C131 C132 H132 . . . 119.2(17) ? C133 C132 H132 . . . 118.8(19) ? C132 C133 C134 . . . 120.3(19) ? C132 C133 H133 . . . 120(2) ? C134 C133 H133 . . . 120(2) ? C133 C134 C135 . . . 120.0(19) ? C133 C134 H134 . . . 120(2) ? C135 C134 H134 . . . 120(2) ? C134 C135 C136 . . . 119.6(17) ? C134 C135 H135 . . . 120(2) ? C136 C135 H135 . . . 120(2) ? C131 C136 C135 . . . 121.2(16) ? C131 C136 H136 . . . 119.5(16) ? C135 C136 H136 . . . 119.3(18) ? Ag P2 C211 . . . 111.6(5) ? Ag P2 C221 . . . 112.9(6) ? Ag P2 C231 . . . 115.8(6) ? C211 P2 C221 . . . 106.5(7) ? C211 P2 C231 . . . 104.7(7) ? C221 P2 C231 . . . 104.5(8) ? P2 C211 C212 . . . 122.0(12) ? P2 C211 C216 . . . 123.9(12) ? C212 C211 C216 . . . 114.1(13) ? C211 C212 C213 . . . 123.5(17) ? C211 C212 H212 . . . 118.3(15) ? C213 C212 H212 . . . 118.2(17) ? C212 C213 C214 . . . 120.3(18) ? C212 C213 H213 . . . 120(2) ? C214 C213 H213 . . . 119.7(18) ? C213 C214 C215 . . . 119.4(17) ? C213 C214 H214 . . . 120(2) ? C215 C214 H214 . . . 120(2) ? C214 C215 C216 . . . 120.3(18) ? C214 C215 H215 . . . 119.6(18) ? C216 C215 H215 . . . 120.1(18) ? C211 C216 C215 . . . 122.2(16) ? C211 C216 H216 . . . 118.9(15) ? C215 C216 H216 . . . 118.9(18) ? P2 C221 C222 . . . 120.0(13) ? P2 C221 C226 . . . 124.3(12) ? C222 C221 C226 . . . 115.6(14) ? C221 C222 C223 . . . 126.4(17) ? C221 C222 H222 . . . 116.8(15) ? C223 C222 H222 . . . 116.8(17) ? C222 C223 C224 . . . 116.8(17) ? C222 C223 H223 . . . 121(2) ? C224 C223 H223 . . . 122(2) ? C223 C224 C225 . . . 119.5(17) ? C223 C224 H224 . . . 120(2) ? C225 C224 H224 . . . 120(2) ? C224 C225 C226 . . . 121(2) ? C224 C225 H225 . . . 119.4(19) ? C226 C225 H225 . . . 120(2) ? C221 C226 C225 . . . 120.9(17) ? C221 C226 H226 . . . 119.4(16) ? C225 C226 H226 . . . 120(2) ? P2 C231 C232 . . . 118.2(13) ? P2 C231 C236 . . . 126.3(14) ? C232 C231 C236 . . . 115.4(16) ? C231 C232 C233 . . . 121.6(17) ? C231 C232 H232 . . . 119.3(19) ? C233 C232 H232 . . . 119(2) ? C232 C233 C234 . . . 119(2) ? C232 C233 H233 . . . 120(2) ? C234 C233 H233 . . . 120(2) ? C233 C234 C235 . . . 122(2) ? C233 C234 H234 . . . 119(2) ? C235 C234 H234 . . . 119(3) ? C234 C235 C236 . . . 118(2) ? C234 C235 H235 . . . 121(3) ? C236 C235 H235 . . . 121(3) ? C231 C236 C235 . . . 124.1(19) ? C231 C236 H236 . . . 118(2) ? C235 C236 H236 . . . 118(2) ? O1 N O2 . . . 116(2) ? O1 N O3 . . . 122(3) ? O2 N O3 . . . 122(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 Ag C2a 3.28(2) . . ? Ag C5a 3.22(3) . . ? Ag C2b 3.44(2) . . ? Ag C5b 3.15(2) . . ? Ag C111 3.596(15) . . ? Ag C112 3.638(16) . . ? Ag C121 3.64(2) . . ? Ag C122 3.73(2) . . ? Ag C131 3.421(14) . . ? Ag C132 3.796(17) . . ? Ag C211 3.506(14) . . ? Ag C212 3.588(16) . . ? Ag C221 3.562(17) . . ? Ag C222 3.680(17) . . ? Ag C231 3.600(18) . . ? Ag C232 3.98(2) . . ? Ag H2a 3.4547(14) . . ? Ag H5a 3.3554(14) . . ? Ag H5b 3.1471(13) . . ? Ag H112 3.0137(13) . . ? Ag H122 3.1581(14) . . ? Ag H132 3.5807(19) . . ? Ag H212 2.9687(13) . . ? Ag H222 3.0933(17) . . ? N1a N3a 2.22(2) . . ? N1a C4a 2.22(4) . . ? N1a N1b 3.37(3) . . ? N1a C5b 3.45(3) . . ? N1a P2 3.729(17) . . ? N1a H2a 1.966(16) . . ? N1a H5a 2.049(18) . . ? N1a H122 2.978(16) . . ? C2a C4a 2.09(4) . . ? C2a C5a 2.04(3) . . ? C2a O2 3.26(3) . '3 665' ? C2a H3a 2.02(2) . . ? N3a C5a 2.16(3) . . ? N3a N 3.36(3) . '3 665' ? N3a O1 2.77(2) . '3 665' ? N3a O2 3.06(3) . '3 665' ? N3a H2a 1.96(3) . . ? N3a H4a 2.09(3) . . ? C4a H3a 2.12(3) . . ? C4a H5a 2.00(3) . . ? C5a H4a 2.03(3) . . ? N1b N3b 2.22(3) . . ? N1b C4b 2.14(3) . . ? N1b H2b 2.055(18) . . ? N1b H5b 1.959(17) . . ? N1b H222 2.892(14) . . ? C2b C4b 2.19(3) . . ? C2b C5b 2.08(3) . . ? C2b H3b 2.13(2) . . ? N3b C5b 2.09(3) . . ? N3b H2b 2.12(3) . . ? N3b H4b 2.09(3) . . ? C4b N 3.34(4) . . ? C4b O1 2.80(3) . . ? C4b O3 3.17(3) . . ? C4b H3b 2.08(2) . . ? C4b H5b 1.90(2) . . ? C4b H115 2.76(2) . '2 745' ? C5b O1 3.50(3) . . ? C5b O3 3.13(3) . . ? C5b H2a 2.86(2) . . ? C5b H4b 1.95(2) . . ? C5b H115 2.81(2) . '2 745' ? P1 C112 2.737(18) . . ? P1 C116 2.84(2) . . ? P1 C122 2.77(2) . . ? P1 C126 2.83(2) . . ? P1 C132 2.750(19) . . ? P1 C136 2.783(18) . . ? P1 H112 2.798(4) . . ? P1 H116 2.963(4) . . ? P1 H122 2.823(4) . . ? P1 H126 2.954(5) . . ? P1 H132 2.835(4) . . ? P1 H136 2.907(4) . . ? C111 C113 2.38(3) . . ? C111 C114 2.76(2) . . ? C111 C115 2.41(3) . . ? C111 C121 2.92(2) . . ? C111 C131 2.90(2) . . ? C111 C136 3.16(2) . . ? C111 H112 2.028(17) . . ? C111 H116 2.017(16) . . ? C111 H136 2.692(14) . . ? C112 C114 2.35(2) . . ? C112 C115 2.73(3) . . ? C112 C116 2.34(3) . . ? C112 H113 2.006(18) . . ? C113 C115 2.32(3) . . ? C113 C116 2.69(3) . . ? C113 H112 2.02(2) . . ? C113 H114 1.98(2) . . ? C114 C116 2.37(3) . . ? C114 H113 1.97(2) . . ? C114 H115 2.02(2) . . ? C115 H114 2.02(2) . . ? C115 H116 2.03(2) . . ? C116 C121 3.32(3) . . ? C116 H115 2.04(2) . . ? C121 C123 2.41(3) . . ? C121 C124 2.74(3) . . ? C121 C125 2.39(3) . . ? C121 C131 2.82(2) . . ? C121 C132 3.31(2) . . ? C121 H122 2.036(18) . . ? C121 H126 2.050(19) . . ? C122 C124 2.34(4) . . ? C122 C125 2.74(3) . . ? C122 C126 2.40(3) . . ? C122 H123 2.03(2) . . ? C123 C125 2.38(3) . . ? C123 C126 2.80(3) . . ? C123 O3 3.31(3) . . ? C123 H122 2.02(2) . . ? C123 H124 1.99(3) . . ? C124 C126 2.41(3) . . ? C124 H123 2.01(3) . . ? C124 H125 2.00(3) . . ? C125 H124 2.00(3) . . ? C125 H126 2.08(3) . . ? C126 C131 3.14(3) . . ? C126 H116 2.858(17) . . ? C126 H125 2.07(2) . . ? C131 C133 2.41(2) . . ? C131 C134 2.78(3) . . ? C131 C135 2.41(2) . . ? C131 H126 2.813(17) . . ? C131 H132 2.050(16) . . ? C131 H136 2.033(16) . . ? C132 C134 2.35(3) . . ? C132 C135 2.73(2) . . ? C132 C136 2.38(3) . . ? C132 H133 1.996(18) . . ? C133 C135 2.38(3) . . ? C133 C136 2.75(3) . . ? C133 H132 1.99(2) . . ? C133 H134 2.02(2) . . ? C134 C136 2.38(3) . . ? C134 H133 2.01(2) . . ? C134 H135 2.04(2) . . ? C135 H134 2.03(2) . . ? C135 H136 2.03(2) . . ? C136 H135 2.034(18) . . ? P2 C212 2.741(17) . . ? P2 C216 2.803(17) . . ? P2 C222 2.710(16) . . ? P2 C226 2.839(19) . . ? P2 C232 2.72(2) . . ? P2 C236 2.81(2) . . ? P2 H212 2.829(4) . . ? P2 H216 2.923(4) . . ? P2 H222 2.743(4) . . ? P2 H226 2.962(5) . . ? P2 H232 2.797(4) . . ? P2 H236 2.924(4) . . ? C211 C213 2.39(2) . . ? C211 C214 2.80(2) . . ? C211 C215 2.44(2) . . ? C211 C221 2.84(2) . . ? C211 C231 2.79(2) . . ? C211 C236 3.09(2) . . ? C211 H212 2.008(15) . . ? C211 H216 2.057(15) . . ? C211 H236 2.628(14) . . ? C212 C214 2.36(2) . . ? C212 C215 2.71(3) . . ? C212 C216 2.34(2) . . ? C212 H135 2.895(15) . '3 766' ? C212 H213 2.000(16) . . ? C213 C215 2.34(3) . . ? C213 C216 2.70(3) . . ? C213 H212 1.983(19) . . ? C213 H214 2.03(2) . . ? C214 C216 2.34(2) . . ? C214 O1 3.09(2) . 4 ? C214 H213 2.02(2) . . ? C214 H215 1.99(2) . . ? C215 O1 3.40(3) . 4 ? C215 H214 1.995(19) . . ? C215 H216 2.013(19) . . ? C216 C221 3.26(2) . . ? C216 H4a 2.781(16) . '2 645' ? C216 H215 2.022(17) . . ? C216 H236 2.787(16) . . ? C221 C223 2.40(2) . . ? C221 C224 2.78(2) . . ? C221 C225 2.41(3) . . ? C221 C231 2.82(2) . . ? C221 C232 3.33(2) . . ? C221 H222 1.951(16) . . ? C221 H226 2.056(17) . . ? C222 C224 2.35(2) . . ? C222 C225 2.68(3) . . ? C222 C226 2.32(3) . . ? C222 H223 2.027(16) . . ? C223 C225 2.39(3) . . ? C223 C226 2.75(2) . . ? C223 O2 3.37(3) . '3 665' ? C223 H5a 2.83(2) . '2 645' ? C223 H222 1.98(2) . . ? C223 H224 2.05(2) . . ? C224 C226 2.37(3) . . ? C224 H223 2.06(3) . . ? C224 H225 2.01(3) . . ? C225 H224 2.02(2) . . ? C225 H226 2.01(2) . . ? C226 C231 3.15(2) . . ? C226 H216 2.889(16) . . ? C226 H225 2.009(18) . . ? C231 C233 2.43(3) . . ? C231 C234 2.77(3) . . ? C231 C235 2.42(3) . . ? C231 H226 2.773(16) . . ? C231 H232 2.039(16) . . ? C231 H236 2.004(16) . . ? C232 C234 2.35(3) . . ? C232 C235 2.74(3) . . ? C232 C236 2.34(3) . . ? C232 H112 2.87(2) . . ? C232 H233 2.04(2) . . ? C233 C235 2.36(3) . . ? C233 C236 2.71(3) . . ? C233 H232 2.03(2) . . ? C233 H234 1.98(2) . . ? C234 C236 2.33(3) . . ? C234 H233 2.00(3) . . ? C234 H235 2.02(3) . . ? C235 H234 2.00(3) . . ? C235 H236 2.00(3) . . ? C236 H235 2.03(2) . . ? N H3a 2.54(3) . '3 665' ? N H4b 2.58(3) . . ? O1 O2 2.04(3) . . ? O1 O3 2.08(3) . . ? O1 H3a 1.859(17) . '3 665' ? O1 H4b 1.875(17) . . ? O1 H214 2.663(18) . '4 554' ? O2 O3 2.05(3) . . ? O2 H2a 2.81(2) . '3 665' ? O2 H3a 2.46(2) . '3 665' ? O2 H113 2.85(2) . '4 564' ? O2 H223 2.71(2) . '3 665' ? O2 H233 2.92(2) . '4 564' ? O3 H4b 2.67(2) . . ? O3 H5b 2.51(2) . . ? O3 H113 2.94(2) . '4 564' ? O3 H123 2.76(2) . . ? H2a H3a 2.3668(6) . . ? H4b H5b 2.2833(2) . . ? H112 H113 2.3002(2) . . ? H113 H114 2.2598(8) . . ? H114 H115 2.3270(8) . . ? H115 H116 2.3300(2) . . ? H122 H123 2.3296(3) . . ? H123 H124 2.2955(12) . . ? H124 H125 2.2870(4) . . ? H125 H126 2.3924(3) . . ? H132 H133 2.2786(3) . . ? H133 H134 2.3141(2) . . ? H134 H135 2.3385(3) . . ? H135 H136 2.3271(3) . . ? H212 H213 2.2731(2) . . ? H213 H214 2.3234(4) . . ? H214 H215 2.2894(11) . . ? H215 H216 2.3091(2) . . ? H222 H223 2.2879(10) . . ? H223 H224 2.3767(8) . . ? H224 H225 2.3097(2) . . ? H225 H226 2.3059(10) . . ? H232 H233 2.3392(2) . . ? H233 H234 2.2844(2) . . ? H234 H235 2.3116(3) . . ? H235 H236 2.3091(2) . . ? _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 [(Ph3P)2Ag(C3H4N2)2](NO3) _exptl_crystal_F_000 1704 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 7 9 4 -7 9 -4 -7 -9 -4 7 -9 4 7 -9 4 -7 -9 -4 -7 9 -4 7 9 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed 2281 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression none _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .164 _refine_ls_wR_factor_all .104 _refine_ls_goodness_of_fit_all 1.056 _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-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_clpt1 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C44 H42 Ag N5 O3 P2' _chemical_formula_moiety ? _chemical_formula_weight 858.67 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.888(2) _cell_length_b 9.895(3) _cell_length_c 19.241(4) _cell_angle_alpha 90.00000 _cell_angle_beta 92.090(10) _cell_angle_gamma 90.00000 _cell_volume 4164.5(16) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.37 _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 20.4 _cell_measurement_theta_max 21.0 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .61 _exptl_crystal_description prism _exptl_crystal_size_max .68 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .40 _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 ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.83 _diffrn_reflns_number 7421 _reflns_number_total 5932 _reflns_Friedel_coverage ? _reflns_number_gt 4981 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 29.98 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .041 _refine_ls_wR_factor_ref .043 _refine_ls_goodness_of_fit_ref 1.75 _refine_ls_number_reflns 4981 _refine_ls_number_parameters 266 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .058 _refine_diff_density_min -.73 _refine_diff_density_max .70 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 11010(647) _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 Ag ? 0 4 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' C ? 0 176 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 168 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 20 .004028 .002991 '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' 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 Ag .50000 .06950(2) .25000 .04405(14) Uani ? ? 1.00000 ? ? N1a .43910(9) .2344(2) .19360(10) .0552(11) Uani ? ? 1.00000 ? ? C2a .40162(12) .2221(3) .13883(13) .0629(15) Uani ? ? 1.00000 ? ? C21a .40537(17) .1180(4) .08399(17) .105(3) Uani ? ? 1.00000 ? ? N3a .35649(11) .3135(3) .14118(12) .0787(16) Uani ? ? 1.00000 ? ? C4a .36496(15) .3865(3) .20074(17) .079(2) Uani ? ? 1.00000 ? ? C5a .41628(13) .3392(3) .23187(14) .0645(16) Uani ? ? 1.00000 ? ? P1 .41896(3) -.04392(6) .31442(3) .0416(3) Uani ? ? 1.00000 ? ? C111 .44066(11) -.2063(2) .35342(11) .0460(12) Uani ? ? 1.00000 ? ? C112 .49949(12) -.2513(3) .34475(12) .0585(14) Uani ? ? 1.00000 ? ? C113 .51811(14) -.3764(3) .37106(15) .0744(18) Uani ? ? 1.00000 ? ? C114 .47841(17) -.4546(3) .40609(15) .080(2) Uani ? ? 1.00000 ? ? C115 .42014(16) -.4099(3) .41618(17) .083(2) Uani ? ? 1.00000 ? ? C116 .40106(13) -.2854(3) .38972(14) .0691(17) Uani ? ? 1.00000 ? ? C121 .38625(11) .0521(2) .38537(11) .0459(12) Uani ? ? 1.00000 ? ? C122 .42161(13) .1536(3) .41534(13) .0632(16) Uani ? ? 1.00000 ? ? C123 .40161(16) .2250(3) .47190(14) .0783(19) Uani ? ? 1.00000 ? ? C124 .34588(16) .1982(3) .49718(13) .080(2) Uani ? ? 1.00000 ? ? C125 .30936(14) .1000(3) .46772(15) .077(2) Uani ? ? 1.00000 ? ? C126 .32962(12) .0271(3) .41126(13) .0596(15) Uani ? ? 1.00000 ? ? C131 .35264(10) -.0832(2) .25790(11) .0455(11) Uani ? ? 1.00000 ? ? C132 .31522(12) .0231(3) .23511(13) .0577(14) Uani ? ? 1.00000 ? ? C133 .26687(13) .0010(3) .18811(14) .0688(17) Uani ? ? 1.00000 ? ? C134 .25554(13) -.1283(3) .16308(13) .0697(17) Uani ? ? 1.00000 ? ? C135 .29180(13) -.2328(3) .18439(13) .0668(16) Uani ? ? 1.00000 ? ? C136 .34084(12) -.2116(3) .23192(12) .0566(14) Uani ? ? 1.00000 ? ? N .75000 .25000 .50000 .225(6) Uani ? ? 1.00000 ? ? O1 .7510(2) .2475(6) .4359(2) .108(3) Uani ? ? .50000 ? ? O2 .7366(3) .2875(6) .5381(3) .149(5) Uani ? ? .50000 ? ? O3 .7970(2) .1264(7) .5154(3) .126(4) Uani ? ? .50000 ? ? H21a1 .36586 .08031 .07396 .12900 Uiso ? ? 1.00000 ? ? H21a2 .41950 .15743 .04185 .12900 Uiso ? ? 1.00000 ? ? H21a3 .43435 .04224 .09738 .12900 Uiso ? ? 1.00000 ? ? H3a .32380 .32419 .10615 .09600 Uiso ? ? 1.00000 ? ? H4a .33892 .45612 .21673 .09900 Uiso ? ? 1.00000 ? ? H5a .43455 .37379 .27431 .08900 Uiso ? ? 1.00000 ? ? H112 .52809 -.19695 .31976 .07500 Uiso ? ? 1.00000 ? ? H113 .55937 -.40673 .36326 .09000 Uiso ? ? 1.00000 ? ? H114 .49242 -.54033 .42313 .10200 Uiso ? ? 1.00000 ? ? H115 .39119 -.46693 .43993 .10700 Uiso ? ? 1.00000 ? ? H116 .35977 -.25271 .39804 .09000 Uiso ? ? 1.00000 ? ? H122 .46106 .17497 .39577 .07900 Uiso ? ? 1.00000 ? ? H123 .42686 .29479 .49347 .09600 Uiso ? ? 1.00000 ? ? H124 .33120 .24951 .53550 .09900 Uiso ? ? 1.00000 ? ? H125 .27036 .08121 .48706 .09600 Uiso ? ? 1.00000 ? ? H126 .30381 -.04344 .39012 .07600 Uiso ? ? 1.00000 ? ? H132 .32431 .11351 .25202 .07400 Uiso ? ? 1.00000 ? ? H133 .24066 .07342 .17238 .08900 Uiso ? ? 1.00000 ? ? H134 .22262 -.14528 .12990 .08600 Uiso ? ? 1.00000 ? ? H135 .28426 -.32081 .16559 .08200 Uiso ? ? 1.00000 ? ? H136 .36594 -.28696 .24797 .07200 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 Ag .04399(15) .04508(14) .04312(14) .00000 .00197(10) .00000 N1a .0584(13) .0535(11) .0529(11) .0073(10) -.0084(10) -.0001(9) C2a .0612(16) .0741(17) .0527(14) .0077(14) -.0076(12) .0052(13) C21a .097(3) .143(3) .072(2) .019(3) -.026(2) -.038(2) N3a .0634(15) .0916(18) .0800(15) .0202(14) -.0110(13) .0262(15) C4a .081(2) .0599(16) .098(2) .0158(16) .0112(18) .0031(16) C5a .0748(19) .0505(14) .0682(16) .0046(14) -.0001(15) -.0023(13) P1 .0428(3) .0408(3) .0415(3) -.0003(2) .0050(2) .0003(2) C111 .0543(13) .0427(11) .0409(11) .0032(11) -.0014(10) -.0003(9) C112 .0640(16) .0604(15) .0513(13) .0096(13) .0038(12) .0044(12) C113 .083(2) .0702(17) .0695(17) .0294(17) .0011(16) .0045(15) C114 .116(3) .0524(16) .0708(18) .0164(17) -.0131(19) .0076(13) C115 .096(2) .0645(18) .089(2) -.0039(17) .0074(19) .0300(16) C116 .0682(18) .0621(16) .0776(18) .0035(14) .0109(15) .0199(15) C121 .0532(13) .0452(12) .0396(11) .0047(10) .0054(10) .0016(9) C122 .0786(19) .0581(15) .0538(14) -.0077(14) .0123(14) -.0077(12) C123 .116(3) .0656(17) .0541(15) -.0084(18) .0124(17) -.0132(14) C124 .121(3) .0722(18) .0493(14) .025(2) .0182(17) -.0053(14) C125 .074(2) .099(2) .0608(16) .0229(18) .0253(15) .0097(16) C126 .0539(15) .0718(16) .0536(14) .0043(13) .0086(12) -.0017(13) C131 .0467(12) .0505(12) .0395(11) -.0046(10) .0044(9) .0024(9) C132 .0568(15) .0584(14) .0578(14) .0036(13) -.0010(12) .0019(12) C133 .0584(16) .084(2) .0631(16) .0100(16) -.0083(14) .0066(15) C134 .0598(16) .099(2) .0492(14) -.0108(16) -.0059(13) -.0048(15) C135 .0683(18) .0714(17) .0604(15) -.0168(15) -.0023(14) -.0103(13) C136 .0609(16) .0539(14) .0549(13) -.0067(13) .0002(12) -.0011(11) N .177(5) .400(10) .095(3) -.230(7) -.040(3) .040(5) O1 .070(3) .173(5) .079(3) -.023(3) -.017(2) -.005(3) O2 .100(4) .147(5) .204(7) .004(4) .046(4) -.007(5) O3 .087(4) .180(5) .111(4) -.029(4) -.028(3) -.017(4) # 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 Ag N1a . . 2.348(2) ? Ag P1 . . 2.4704(7) ? Ag N1a . '2 655' 2.348(2) ? Ag P1 . '2 655' 2.4704(7) ? N1a C2a . . 1.317(3) ? N1a C5a . . 1.376(3) ? C2a C21a . . 1.479(5) ? C2a N3a . . 1.342(4) ? C21a H21a1 . . .955(4) ? C21a H21a2 . . .961(4) ? C21a H21a3 . . 1.009(4) ? N3a C4a . . 1.362(4) ? N3a H3a . . .971(2) ? C4a C5a . . 1.338(4) ? C4a H4a . . .952(3) ? C5a H5a . . .959(3) ? P1 C111 . . 1.828(2) ? P1 C121 . . 1.830(2) ? P1 C131 . . 1.824(2) ? C111 C112 . . 1.379(4) ? C111 C116 . . 1.377(4) ? C112 C113 . . 1.392(4) ? C112 H112 . . .967(3) ? C113 C114 . . 1.361(4) ? C113 H113 . . .969(3) ? C114 C115 . . 1.371(5) ? C114 H114 . . .956(3) ? C115 C116 . . 1.391(4) ? C115 H115 . . .975(3) ? C116 H116 . . .978(3) ? C121 C122 . . 1.381(3) ? C121 C126 . . 1.375(4) ? C122 C123 . . 1.382(4) ? C122 H122 . . .978(3) ? C123 C124 . . 1.356(5) ? C123 H123 . . .969(3) ? C124 C125 . . 1.368(4) ? C124 H124 . . .960(3) ? C125 C126 . . 1.390(4) ? C125 H125 . . .962(3) ? C126 H126 . . .977(3) ? C131 C132 . . 1.394(3) ? C131 C136 . . 1.386(3) ? C132 C133 . . 1.384(4) ? C132 H132 . . .970(3) ? C133 C134 . . 1.386(4) ? C133 H133 . . .960(3) ? C134 C135 . . 1.358(4) ? C134 H134 . . .960(3) ? C135 C136 . . 1.400(4) ? C135 H135 . . .955(3) ? C136 H136 . . .970(2) ? N O1 . . 1.235(4) ? N O2 . . .881(6) ? N O3 . . 1.619(6) ? N O1 . '7 656' 1.235(4) ? N O2 . '7 656' .881(6) ? N O3 . '7 656' 1.619(6) ? O1 O2 . '7 656' .659(8) ? O1 O3 . '7 656' 1.901(8) ? O2 O2 . '7 656' 1.761(9) ? O2 O3 . '7 656' 1.507(8) ? 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 N1a Ag P1 . . . 98.15(5) ? N1a Ag N1a . . '2 655' 91.94(7) ? N1a Ag P1 . . '2 655' 119.33(5) ? P1 Ag N1a . . '2 655' 119.33(5) ? P1 Ag P1 . . '2 655' 125.96(3) ? N1a Ag P1 '2 655' . '2 655' 98.15(5) ? Ag N1a C2a . . . 129.20(17) ? Ag N1a C5a . . . 119.17(16) ? C2a N1a C5a . . . 105.7(2) ? N1a C2a C21a . . . 125.9(3) ? N1a C2a N3a . . . 110.4(2) ? C21a C2a N3a . . . 123.6(3) ? C2a C21a H21a1 . . . 110.0(3) ? C2a C21a H21a2 . . . 110.3(4) ? C2a C21a H21a3 . . . 112.7(3) ? H21a1 C21a H21a2 . . . 107.8(3) ? H21a1 C21a H21a3 . . . 108.5(4) ? H21a2 C21a H21a3 . . . 107.4(3) ? C2a N3a C4a . . . 108.0(2) ? C2a N3a H3a . . . 125.1(2) ? C4a N3a H3a . . . 127.0(3) ? N3a C4a C5a . . . 106.1(3) ? N3a C4a H4a . . . 126.2(3) ? C5a C4a H4a . . . 127.7(3) ? N1a C5a C4a . . . 109.8(2) ? N1a C5a H5a . . . 125.2(3) ? C4a C5a H5a . . . 125.0(3) ? Ag P1 C111 . . . 115.12(8) ? Ag P1 C121 . . . 116.49(8) ? Ag P1 C131 . . . 111.60(7) ? C111 P1 C121 . . . 104.63(10) ? C111 P1 C131 . . . 104.27(10) ? C121 P1 C131 . . . 103.35(11) ? P1 C111 C112 . . . 117.66(18) ? P1 C111 C116 . . . 123.3(2) ? C112 C111 C116 . . . 119.1(2) ? C111 C112 C113 . . . 120.4(2) ? C111 C112 H112 . . . 120.3(2) ? C113 C112 H112 . . . 119.3(3) ? C112 C113 C114 . . . 120.1(3) ? C112 C113 H113 . . . 118.8(3) ? C114 C113 H113 . . . 121.1(3) ? C113 C114 C115 . . . 120.1(3) ? C113 C114 H114 . . . 118.2(3) ? C115 C114 H114 . . . 121.8(3) ? C114 C115 C116 . . . 120.2(3) ? C114 C115 H115 . . . 120.2(3) ? C116 C115 H115 . . . 119.5(3) ? C111 C116 C115 . . . 120.2(3) ? C111 C116 H116 . . . 119.8(3) ? C115 C116 H116 . . . 119.9(3) ? P1 C121 C122 . . . 117.41(19) ? P1 C121 C126 . . . 124.01(18) ? C122 C121 C126 . . . 118.6(2) ? C121 C122 C123 . . . 120.8(3) ? C121 C122 H122 . . . 119.1(2) ? C123 C122 H122 . . . 120.1(3) ? C122 C123 C124 . . . 119.8(3) ? C122 C123 H123 . . . 120.7(3) ? C124 C123 H123 . . . 119.5(3) ? C123 C124 C125 . . . 120.7(3) ? C123 C124 H124 . . . 120.2(3) ? C125 C124 H124 . . . 119.1(3) ? C124 C125 C126 . . . 119.6(3) ? C124 C125 H125 . . . 119.4(3) ? C126 C125 H125 . . . 121.0(3) ? C121 C126 C125 . . . 120.5(2) ? C121 C126 H126 . . . 119.5(2) ? C125 C126 H126 . . . 120.0(3) ? P1 C131 C132 . . . 118.17(17) ? P1 C131 C136 . . . 122.99(17) ? C132 C131 C136 . . . 118.6(2) ? C131 C132 C133 . . . 120.8(2) ? C131 C132 H132 . . . 118.7(2) ? C133 C132 H132 . . . 120.5(3) ? C132 C133 C134 . . . 119.7(3) ? C132 C133 H133 . . . 121.4(3) ? C134 C133 H133 . . . 118.8(3) ? C133 C134 C135 . . . 120.2(3) ? C133 C134 H134 . . . 120.9(3) ? C135 C134 H134 . . . 118.9(3) ? C134 C135 C136 . . . 120.6(3) ? C134 C135 H135 . . . 119.3(3) ? C136 C135 H135 . . . 120.1(3) ? C131 C136 C135 . . . 120.1(2) ? C131 C136 H136 . . . 119.6(2) ? C135 C136 H136 . . . 120.3(2) ? O1 N O2 . . . 149.1(5) ? O1 N O3 . . . 97.7(3) ? O1 N O1 . . '7 656' 180.0000 ? O1 N O2 . . '7 656' 30.9(5) ? O1 N O3 . . '7 656' 82.3(3) ? O2 N O3 . . . 113.2(4) ? O2 N O1 . . '7 656' 30.9(5) ? O2 N O2 . . '7 656' 180.0000 ? O2 N O3 . . '7 656' 66.8(4) ? O3 N O1 . . '7 656' 82.3(3) ? O3 N O2 . . '7 656' 66.8(4) ? O3 N O3 . . '7 656' 180.0000 ? O1 N O2 '7 656' . '7 656' 149.1(5) ? O1 N O3 '7 656' . '7 656' 97.7(3) ? O2 N O3 '7 656' . '7 656' 113.2(4) ? N O1 O2 . . '7 656' 43.3(6) ? N O1 O3 . . '7 656' 57.6(3) ? O2 O1 O3 '7 656' . '7 656' 100.9(7) ? N O2 O1 . . '7 656' 105.7(9) ? N O2 O2 . . '7 656' .0(3) ? N O2 O3 . . '7 656' 80.8(5) ? O1 O2 O2 '7 656' . '7 656' 105.7(8) ? O1 O2 O3 '7 656' . '7 656' 173.2(9) ? O2 O2 O3 '7 656' . '7 656' 80.8(4) ? N O3 O1 . . '7 656' 40.1(2) ? N O3 O2 . . '7 656' 32.5(3) ? O1 O3 O2 '7 656' . '7 656' 72.5(4) ? 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 Ag C2a 3.340(3) . '2 655' ? Ag C2a 3.340(3) . . ? Ag C5a 3.249(3) . '2 655' ? Ag C5a 3.249(3) . . ? Ag C111 3.644(2) . . ? Ag C111 3.644(2) . '2 655' ? Ag C112 3.661(3) . '2 655' ? Ag C112 3.661(3) . . ? Ag C121 3.672(2) . . ? Ag C121 3.672(2) . '2 655' ? Ag C131 3.570(2) . '2 655' ? Ag C131 3.570(2) . . ? Ag H112 3.0118(7) . . ? Ag H112 3.0118(7) . '2 655' ? Ag H122 3.1395(5) . '2 655' ? Ag H122 3.1395(5) . . ? N1a C21a 2.491(4) . . ? N1a N3a 2.183(3) . . ? N1a C4a 2.222(4) . . ? N1a H5a 2.082(2) . . ? C2a C4a 2.187(4) . . ? C2a C5a 2.147(4) . . ? C2a H21a1 2.017(3) . . ? C2a H21a2 2.024(3) . . ? C2a H21a3 2.087(3) . . ? C2a H3a 2.059(3) . . ? C21a N3a 2.487(5) . . ? N3a C5a 2.158(4) . . ? N3a O1 2.812(5) . '2 655' ? N3a O3 2.770(6) . '8 454' ? N3a H4a 2.072(2) . . ? C4a H3a 2.094(3) . . ? C4a H5a 2.045(3) . . ? C5a H4a 2.063(3) . . ? P1 C112 2.754(3) . . ? P1 C116 2.829(3) . . ? P1 C122 2.754(3) . . ? P1 C126 2.838(3) . . ? P1 C132 2.770(3) . . ? P1 C136 2.828(3) . . ? C111 C113 2.404(4) . . ? C111 C114 2.773(4) . . ? C111 C115 2.400(4) . . ? C111 C121 2.895(3) . . ? C111 C131 2.883(3) . . ? C111 H112 2.045(2) . . ? C111 H116 2.048(2) . . ? C112 C114 2.386(4) . . ? C112 C115 2.746(4) . . ? C112 C116 2.375(4) . . ? C112 H113 2.043(3) . . ? C113 C115 2.366(5) . . ? C113 C116 2.752(4) . . ? C113 H112 2.047(3) . . ? C113 H114 1.998(3) . . ? C114 C116 2.394(4) . . ? C114 H113 2.037(4) . . ? C114 H115 2.043(4) . . ? C115 H114 2.043(3) . . ? C115 H116 2.062(3) . . ? C116 H115 2.055(3) . . ? C121 C123 2.402(4) . . ? C121 C124 2.764(4) . . ? C121 C125 2.401(4) . . ? C121 C131 2.867(3) . . ? C121 H122 2.044(2) . . ? C121 H126 2.042(2) . . ? C122 C124 2.369(4) . . ? C122 C125 2.741(4) . . ? C122 C126 2.370(4) . . ? C122 H123 2.053(3) . . ? C123 C125 2.367(5) . . ? C123 C126 2.747(4) . . ? C123 H122 2.055(3) . . ? C123 H124 2.017(3) . . ? C124 C126 2.384(4) . . ? C124 H123 2.017(3) . . ? C124 H125 2.021(3) . . ? C125 H124 2.018(3) . . ? C125 H126 2.061(3) . . ? C126 H125 2.058(3) . . ? C131 C133 2.416(4) . . ? C131 C134 2.786(3) . . ? C131 C135 2.414(3) . . ? C131 H132 2.045(2) . . ? C131 H136 2.047(2) . . ? C132 C134 2.396(4) . . ? C132 C135 2.755(4) . . ? C132 C136 2.391(4) . . ? C132 H133 2.055(3) . . ? C133 C135 2.379(4) . . ? C133 C136 2.767(4) . . ? C133 H132 2.054(3) . . ? C133 H134 2.051(3) . . ? C134 C136 2.396(4) . . ? C134 H133 2.031(3) . . ? C134 H135 2.006(3) . . ? C135 H134 2.007(3) . . ? C135 H136 2.067(3) . . ? C136 H135 2.053(2) . . ? O1 O1 2.470(6) . '7 656' ? O1 O2 2.041(8) . . ? O1 O3 2.163(7) . . ? O1 H3a 1.953(5) . '2 655' ? O2 O3 2.126(8) . . ? O3 H3a 1.886(5) . 8 ? H21a1 H21a2 1.54771(15) . . ? H21a1 H21a3 1.59469(13) . . ? H21a2 H21a3 1.5878(3) . . ? _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 [(Ph3P)2Ag(C4H6N2)2](NO3) _exptl_crystal_F_000 1768 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 12 6 10 12 -6 10 -12 -6 -10 -12 6 -10 14 6 -10 14 -6 -10 -14 -6 10 -14 6 10 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _reflns_number_observed 4981 _reflns_d_resolution_high .711 _reflns_d_resolution_low 10.937 _diffrn_reflns_av_sigmaI/netI .037 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression Zachariasen _refine_ls_matrix_type 'block diagonal' _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .051 _refine_ls_wR_factor_all .044 _refine_ls_goodness_of_fit_all 1.658 _refine_ls_shift/su_mean .004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_cp7 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C40 H36 Ag1 N3 O3 P2' _chemical_formula_moiety ? _chemical_formula_weight 776.56 _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 13.6840(10) _cell_length_b 12.965(2) _cell_length_c 23.464(3) _cell_angle_alpha 90.00000 _cell_angle_beta 116.461(8) _cell_angle_gamma 90.00000 _cell_volume 3726.7(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.384 _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 14.6 _cell_measurement_theta_max 14.7 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .667 _exptl_crystal_description prism _exptl_crystal_size_max .52 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .04 _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 .78 _exptl_absorpt_correction_T_max .97 _diffrn_reflns_number 6309 _reflns_number_total 6309 _reflns_Friedel_coverage 0 _reflns_number_gt 2695 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .052 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.47 _refine_ls_number_reflns 2695 _refine_ls_number_parameters 443 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .009 _refine_diff_density_min -.42 _refine_diff_density_max .546 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 3509(572) _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 ? 0 160 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 144 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 4 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .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 8 .09 .095 '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 Ag .22243(6) .79750(6) .37528(3) .0538(4) Uani ? ? 1.00000 ? ? N1a .0402(7) .7688(7) .3079(4) .068(6) Uani ? ? 1.00000 ? ? C2a -.0020(9) .7026(10) .2610(5) .069(7) Uani ? ? 1.00000 ? ? C21a .0554(9) .6245(10) .2393(6) .111(9) Uani ? ? 1.00000 ? ? N3a -.1093(7) .7111(9) .2329(5) .102(7) Uani ? ? 1.00000 ? ? C4a -.1373(9) .7850(12) .2634(7) .136(11) Uani ? ? 1.00000 ? ? C5a -.0426(10) .8202(9) .3096(6) .085(8) Uani ? ? 1.00000 ? ? P1 .3381(2) .8052(2) .32042(11) .0504(15) Uani ? ? 1.00000 ? ? C111 .3422(7) .6779(8) .2876(5) .055(6) Uani ? ? 1.00000 ? ? C112 .3708(9) .5969(10) .3293(6) .075(8) Uani ? ? 1.00000 ? ? C113 .3725(10) .4957(11) .3094(7) .091(9) Uani ? ? 1.00000 ? ? C114 .3437(12) .4793(10) .2456(9) .099(11) Uani ? ? 1.00000 ? ? C115 .3145(11) .5588(13) .2050(6) .098(10) Uani ? ? 1.00000 ? ? C116 .3098(9) .6595(9) .2235(6) .077(8) Uani ? ? 1.00000 ? ? C121 .2933(9) .8948(7) .2529(4) .052(6) Uani ? ? 1.00000 ? ? C122 .1845(9) .9219(11) .2223(6) .102(9) Uani ? ? 1.00000 ? ? C123 .1491(11) .9912(14) .1723(7) .151(13) Uani ? ? 1.00000 ? ? C124 .2196(14) 1.0332(11) .1533(6) .111(10) Uani ? ? 1.00000 ? ? C125 .3292(11) 1.0086(10) .1836(6) .089(9) Uani ? ? 1.00000 ? ? C126 .3651(8) .9397(9) .2335(5) .070(7) Uani ? ? 1.00000 ? ? C131 .4822(8) .8342(7) .3661(4) .049(6) Uani ? ? 1.00000 ? ? C132 .5080(9) .9171(8) .4080(5) .064(7) Uani ? ? 1.00000 ? ? C133 .6154(11) .9449(9) .4450(5) .080(8) Uani ? ? 1.00000 ? ? C134 .6985(9) .8951(10) .4390(5) .079(8) Uani ? ? 1.00000 ? ? C135 .6727(9) .8180(10) .3960(6) .079(8) Uani ? ? 1.00000 ? ? C136 .5650(9) .7864(8) .3591(4) .063(6) Uani ? ? 1.00000 ? ? P2 .2562(2) .7125(2) .47619(11) .0494(15) Uani ? ? 1.00000 ? ? C211 .3826(7) .7472(7) .5462(4) .047(5) Uani ? ? 1.00000 ? ? C212 .4661(9) .7848(9) .5352(5) .068(7) Uani ? ? 1.00000 ? ? C213 .5621(9) .8152(10) .5852(6) .086(8) Uani ? ? 1.00000 ? ? C214 .5745(9) .8134(10) .6463(6) .084(8) Uani ? ? 1.00000 ? ? C215 .4910(9) .7764(11) .6573(5) .093(8) Uani ? ? 1.00000 ? ? C216 .3948(8) .7433(9) .6079(5) .073(7) Uani ? ? 1.00000 ? ? C221 .1490(7) .7282(7) .5026(4) .046(6) Uani ? ? 1.00000 ? ? C222 .1242(10) .8248(8) .5135(6) .087(8) Uani ? ? 1.00000 ? ? C223 .0423(11) .8423(10) .5329(6) .098(9) Uani ? ? 1.00000 ? ? C224 -.0127(11) .7628(12) .5402(6) .091(10) Uani ? ? 1.00000 ? ? C225 .0082(12) .6686(12) .5276(8) .130(13) Uani ? ? 1.00000 ? ? C226 .0920(11) .6485(10) .5098(6) .105(10) Uani ? ? 1.00000 ? ? C231 .2672(9) .5742(8) .4693(5) .056(6) Uani ? ? 1.00000 ? ? C232 .1905(10) .5262(10) .4143(5) .077(8) Uani ? ? 1.00000 ? ? C233 .1918(12) .4214(12) .4051(7) .103(11) Uani ? ? 1.00000 ? ? C234 .2682(14) .3635(11) .4518(9) .109(12) Uani ? ? 1.00000 ? ? C235 .3458(12) .4101(13) .5041(8) .135(12) Uani ? ? 1.00000 ? ? C236 .3432(11) .5143(10) .5142(6) .097(9) Uani ? ? 1.00000 ? ? N .1830(8) 1.0376(9) .3926(5) .063(6) Uani ? ? 1.00000 ? ? O1 .1599(11) .9717(8) .4167(5) .193(10) Uani ? ? 1.00000 ? ? O2 .2192(8) 1.0150(8) .3556(5) .141(8) Uani ? ? 1.00000 ? ? O3 .1719(6) 1.1302(7) .3993(4) .090(5) Uani ? ? 1.00000 ? ? H21a1 .06241 .64796 .20337 .15760 Uiso ? ? 1.00000 ? ? H21a2 .01374 .56109 .22838 .15760 Uiso ? ? 1.00000 ? ? H21a3 .12564 .60954 .27297 .15760 Uiso ? ? 1.00000 ? ? H2 -.15889 .67190 .19734 .12120 Uiso ? ? 1.00000 ? ? H3 -.20867 .80761 .25437 .15440 Uiso ? ? 1.00000 ? ? H4 -.03588 .87495 .33885 .10040 Uiso ? ? 1.00000 ? ? H112 .38941 .60871 .37309 .09510 Uiso ? ? 1.00000 ? ? H113 .39276 .43920 .33872 .11340 Uiso ? ? 1.00000 ? ? H114 .34419 .41129 .23040 .13680 Uiso ? ? 1.00000 ? ? H115 .29503 .54455 .16109 .13570 Uiso ? ? 1.00000 ? ? H116 .28790 .71427 .19327 .10750 Uiso ? ? 1.00000 ? ? H122 .13414 .89410 .23604 .12550 Uiso ? ? 1.00000 ? ? H123 .07482 1.01123 .15095 .17570 Uiso ? ? 1.00000 ? ? H124 .19450 1.07939 .11854 .13730 Uiso ? ? 1.00000 ? ? H125 .37939 1.03812 .16977 .10950 Uiso ? ? 1.00000 ? ? H126 .44134 .92314 .25517 .08700 Uiso ? ? 1.00000 ? ? H132 .45069 .95415 .41114 .07990 Uiso ? ? 1.00000 ? ? H133 .63090 1.00020 .47544 .09290 Uiso ? ? 1.00000 ? ? H134 .77265 .91569 .46484 .09430 Uiso ? ? 1.00000 ? ? H135 .73090 .78505 .39129 .09600 Uiso ? ? 1.00000 ? ? H136 .54962 .73139 .32874 .07820 Uiso ? ? 1.00000 ? ? H212 .45679 .79040 .49224 .08530 Uiso ? ? 1.00000 ? ? H213 .62061 .83786 .57629 .10850 Uiso ? ? 1.00000 ? ? H214 .63989 .83724 .68093 .09740 Uiso ? ? 1.00000 ? ? H215 .49861 .77487 .69950 .10600 Uiso ? ? 1.00000 ? ? H216 .33770 .71704 .61616 .09170 Uiso ? ? 1.00000 ? ? H222 .16301 .88138 .50734 .12160 Uiso ? ? 1.00000 ? ? H223 .02622 .91057 .54121 .13960 Uiso ? ? 1.00000 ? ? H224 -.06888 .77373 .55381 .12600 Uiso ? ? 1.00000 ? ? H225 -.03481 .61315 .53077 .18760 Uiso ? ? 1.00000 ? ? H226 .10791 .57867 .50291 .15380 Uiso ? ? 1.00000 ? ? H232 .13512 .56785 .38198 .09250 Uiso ? ? 1.00000 ? ? H233 .13897 .38922 .36754 .13450 Uiso ? ? 1.00000 ? ? H234 .26952 .29081 .44839 .13960 Uiso ? ? 1.00000 ? ? H235 .40516 .36862 .53482 .15030 Uiso ? ? 1.00000 ? ? H236 .39509 .54475 .55357 .11190 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 Ag .0516(5) .0666(6) .0467(4) -.0032(6) .0250(4) -.0032(5) N1a .054(6) .083(8) .057(6) -.006(6) .015(5) -.022(5) C2a .049(7) .084(9) .071(8) -.004(8) .024(6) -.016(8) C21a .063(8) .149(13) .112(10) .015(8) .031(8) -.057(10) N3a .049(6) .119(9) .111(8) .001(7) .014(6) -.046(8) C4a .053(8) .145(14) .171(14) .009(9) .015(9) -.103(12) C5a .062(8) .076(10) .107(10) -.004(7) .029(8) -.040(8) P1 .0520(16) .0556(19) .0468(16) -.0024(17) .0251(13) .0015(17) C111 .042(6) .055(9) .070(8) .001(6) .027(6) -.012(7) C112 .071(9) .060(9) .095(10) .003(7) .038(8) -.006(8) C113 .084(10) .081(11) .110(12) -.005(8) .044(9) .017(10) C114 .104(12) .066(11) .162(17) -.003(9) .091(13) -.020(11) C115 .124(12) .107(13) .092(11) -.027(11) .073(10) -.046(10) C116 .098(10) .082(10) .070(8) -.025(8) .054(8) -.026(7) C121 .072(8) .048(7) .039(6) -.002(6) .028(6) .001(5) C122 .050(8) .155(14) .093(10) .014(9) .024(7) .043(10) C123 .093(12) .23(2) .105(12) .049(12) .025(10) .101(13) C124 .136(14) .117(13) .076(10) .007(12) .044(10) .040(9) C125 .092(10) .100(11) .079(10) -.001(9) .040(8) .019(8) C126 .061(8) .090(10) .059(8) -.007(7) .027(7) .020(7) C131 .057(7) .049(7) .042(6) -.010(6) .023(5) -.008(5) C132 .060(8) .063(8) .068(8) .002(6) .028(6) .007(7) C133 .089(10) .084(10) .058(8) -.016(9) .025(8) -.013(7) C134 .059(9) .086(11) .071(9) -.025(8) .011(7) .015(8) C135 .062(8) .085(11) .085(9) .003(7) .029(7) -.005(8) C136 .064(7) .059(8) .063(7) -.006(7) .024(6) -.001(6) P2 .0531(16) .0531(19) .0485(16) -.0015(16) .0284(13) -.0001(16) C211 .045(6) .045(6) .054(6) -.002(5) .026(5) -.004(5) C212 .066(7) .080(9) .063(7) -.014(7) .034(6) -.005(7) C213 .068(8) .105(11) .089(9) -.015(8) .038(8) -.026(9) C214 .050(7) .083(10) .095(10) .012(7) .010(7) -.027(9) C215 .054(7) .156(14) .050(7) .004(9) .004(6) -.023(8) C216 .061(7) .114(10) .052(7) -.005(7) .032(6) .002(7) C221 .046(6) .045(8) .050(6) -.001(5) .022(5) .008(5) C222 .113(10) .035(8) .151(12) .015(7) .094(10) .020(7) C223 .116(11) .083(10) .138(12) .046(9) .096(10) .032(9) C224 .097(11) .108(13) .105(10) .010(10) .078(9) .013(9) C225 .139(14) .116(14) .212(18) -.040(11) .147(14) -.032(12) C226 .132(12) .075(10) .170(13) -.005(9) .124(11) -.003(9) C231 .056(7) .068(8) .055(7) -.007(7) .035(6) -.011(7) C232 .089(9) .069(10) .065(8) -.011(8) .028(7) -.010(7) C233 .130(14) .074(12) .127(14) -.038(10) .077(12) -.044(10) C234 .111(14) .056(11) .18(2) -.003(10) .087(13) -.011(11) C235 .111(13) .079(13) .174(17) .015(10) .025(12) -.001(12) C236 .118(12) .054(9) .094(11) .012(9) .023(9) -.015(8) N .063(7) .058(8) .050(7) -.012(6) .009(5) -.011(6) O1 .323(17) .125(10) .095(8) -.111(11) .061(9) .009(7) O2 .110(8) .143(10) .168(11) .005(7) .061(8) -.060(8) O3 .093(6) .067(6) .084(6) .017(5) .017(5) -.011(5) # 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 Ag N1a . . 2.312(7) ? Ag P1 . . 2.447(3) ? Ag P2 . . 2.461(3) ? Ag O1 . . 2.742(13) ? Ag O2 . . 2.854(11) ? N1a C2a . . 1.309(14) ? N1a C5a . . 1.330(17) ? C2a C21a . . 1.50(2) ? C2a N3a . . 1.319(14) ? C21a H21a1 . . .941(14) ? C21a H21a2 . . .968(13) ? C21a H21a3 . . .953(10) ? N3a C4a . . 1.35(2) ? N3a H2 . . .954(9) ? C4a C5a . . 1.346(15) ? C4a H3 . . .948(14) ? C5a H4 . . .963(13) ? P1 C111 . . 1.832(11) ? P1 C121 . . 1.836(10) ? P1 C131 . . 1.816(9) ? C111 C112 . . 1.369(17) ? C111 C116 . . 1.386(17) ? C112 C113 . . 1.40(2) ? C112 H112 . . .953(13) ? C113 C114 . . 1.38(3) ? C113 H113 . . .957(14) ? C114 C115 . . 1.34(2) ? C114 H114 . . .952(15) ? C115 C116 . . 1.39(2) ? C115 H115 . . .961(14) ? C116 H116 . . .954(12) ? C121 C122 . . 1.379(15) ? C121 C126 . . 1.382(18) ? C122 C123 . . 1.38(2) ? C122 H122 . . .953(15) ? C123 C124 . . 1.34(3) ? C123 H123 . . .948(14) ? C124 C125 . . 1.38(2) ? C124 H124 . . .945(14) ? C125 C126 . . 1.378(17) ? C125 H125 . . .960(17) ? C126 H126 . . .959(10) ? C131 C132 . . 1.391(14) ? C131 C136 . . 1.365(17) ? C132 C133 . . 1.382(16) ? C132 H132 . . .950(13) ? C133 C134 . . 1.37(2) ? C133 H133 . . .967(12) ? C134 C135 . . 1.350(18) ? C134 H134 . . .960(10) ? C135 C136 . . 1.397(14) ? C135 H135 . . .953(14) ? C136 H136 . . .962(10) ? P2 C211 . . 1.833(8) ? P2 C221 . . 1.841(12) ? P2 C231 . . 1.812(11) ? C211 C212 . . 1.369(17) ? C211 C216 . . 1.383(16) ? C212 C213 . . 1.373(13) ? C212 H212 . . .960(11) ? C213 C214 . . 1.37(2) ? C213 H213 . . .958(15) ? C214 C215 . . 1.37(2) ? C214 H214 . . .953(10) ? C215 C216 . . 1.378(13) ? C215 H215 . . .948(12) ? C216 H216 . . .949(13) ? C221 C222 . . 1.351(15) ? C221 C226 . . 1.350(18) ? C222 C223 . . 1.40(2) ? C222 H222 . . .954(13) ? C223 C224 . . 1.33(2) ? C223 H223 . . .953(13) ? C224 C225 . . 1.32(2) ? C224 H224 . . .966(17) ? C225 C226 . . 1.41(3) ? C225 H225 . . .953(17) ? C226 H226 . . .961(13) ? C231 C232 . . 1.396(14) ? C231 C236 . . 1.348(15) ? C232 C233 . . 1.38(2) ? C232 H232 . . .963(11) ? C233 C234 . . 1.36(2) ? C233 H233 . . .952(13) ? C234 C235 . . 1.36(2) ? C234 H234 . . .946(14) ? C235 C236 . . 1.38(2) ? C235 H235 . . .973(14) ? C236 H236 . . .964(11) ? N O1 . . 1.144(18) ? N O2 . . 1.211(19) ? N O3 . . 1.229(14) ? 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 N1a Ag P1 . . . 113.6(3) ? N1a Ag P2 . . . 105.6(3) ? N1a Ag O1 . . . 87.9(3) ? N1a Ag O2 . . . 96.6(3) ? P1 Ag P2 . . . 129.49(9) ? P1 Ag O1 . . . 122.0(3) ? P1 Ag O2 . . . 80.9(3) ? P2 Ag O1 . . . 89.0(3) ? P2 Ag O2 . . . 125.5(3) ? O1 Ag O2 . . . 42.2(4) ? Ag N1a C2a . . . 128.1(8) ? Ag N1a C5a . . . 124.9(7) ? C2a N1a C5a . . . 107.0(9) ? N1a C2a C21a . . . 128.7(9) ? N1a C2a N3a . . . 109.9(12) ? C21a C2a N3a . . . 121.4(10) ? C2a C21a H21a1 . . . 111.3(12) ? C2a C21a H21a2 . . . 109.1(12) ? C2a C21a H21a3 . . . 110.1(11) ? H21a1 C21a H21a2 . . . 108.7(12) ? H21a1 C21a H21a3 . . . 109.9(13) ? H21a2 C21a H21a3 . . . 107.7(12) ? C2a N3a C4a . . . 108.1(10) ? C2a N3a H2 . . . 126.3(12) ? C4a N3a H2 . . . 125.6(10) ? N3a C4a C5a . . . 105.5(12) ? N3a C4a H3 . . . 127.5(12) ? C5a C4a H3 . . . 127.0(16) ? N1a C5a C4a . . . 109.5(12) ? N1a C5a H4 . . . 125.4(10) ? C4a C5a H4 . . . 125.1(14) ? Ag P1 C111 . . . 109.4(4) ? Ag P1 C121 . . . 115.8(4) ? Ag P1 C131 . . . 119.0(4) ? C111 P1 C121 . . . 105.6(5) ? C111 P1 C131 . . . 101.9(4) ? C121 P1 C131 . . . 103.6(5) ? P1 C111 C112 . . . 116.3(9) ? P1 C111 C116 . . . 123.8(8) ? C112 C111 C116 . . . 119.7(11) ? C111 C112 C113 . . . 121.6(12) ? C111 C112 H112 . . . 120.1(13) ? C113 C112 H112 . . . 118.3(13) ? C112 C113 C114 . . . 117.8(13) ? C112 C113 H113 . . . 121.4(15) ? C114 C113 H113 . . . 120.7(14) ? C113 C114 C115 . . . 120.1(14) ? C113 C114 H114 . . . 120.1(16) ? C115 C114 H114 . . . 119.8(19) ? C114 C115 C116 . . . 122.9(14) ? C114 C115 H115 . . . 117.9(16) ? C116 C115 H115 . . . 119.2(14) ? C111 C116 C115 . . . 117.7(11) ? C111 C116 H116 . . . 121.5(12) ? C115 C116 H116 . . . 120.8(13) ? P1 C121 C122 . . . 118.5(10) ? P1 C121 C126 . . . 122.5(7) ? C122 C121 C126 . . . 118.9(10) ? C121 C122 C123 . . . 119.7(14) ? C121 C122 H122 . . . 120.2(12) ? C123 C122 H122 . . . 120.0(12) ? C122 C123 C124 . . . 120.8(13) ? C122 C123 H123 . . . 120.9(18) ? C124 C123 H123 . . . 118.2(16) ? C123 C124 C125 . . . 120.8(13) ? C123 C124 H124 . . . 120.3(16) ? C125 C124 H124 . . . 118.9(19) ? C124 C125 C126 . . . 118.7(15) ? C124 C125 H125 . . . 120.7(13) ? C126 C125 H125 . . . 120.5(12) ? C121 C126 C125 . . . 121.1(10) ? C121 C126 H126 . . . 119.7(11) ? C125 C126 H126 . . . 119.2(13) ? P1 C131 C132 . . . 116.3(8) ? P1 C131 C136 . . . 125.2(7) ? C132 C131 C136 . . . 118.3(9) ? C131 C132 C133 . . . 120.6(12) ? C131 C132 H132 . . . 119.2(9) ? C133 C132 H132 . . . 120.2(11) ? C132 C133 C134 . . . 120.8(11) ? C132 C133 H133 . . . 118.7(15) ? C134 C133 H133 . . . 120.6(12) ? C133 C134 C135 . . . 118.3(10) ? C133 C134 H134 . . . 119.7(13) ? C135 C134 H134 . . . 122.0(14) ? C134 C135 C136 . . . 122.2(12) ? C134 C135 H135 . . . 117.7(11) ? C136 C135 H135 . . . 120.1(12) ? C131 C136 C135 . . . 119.6(10) ? C131 C136 H136 . . . 120.4(10) ? C135 C136 H136 . . . 120.0(12) ? Ag P2 C211 . . . 116.7(4) ? Ag P2 C221 . . . 116.0(3) ? Ag P2 C231 . . . 110.1(4) ? C211 P2 C221 . . . 104.3(5) ? C211 P2 C231 . . . 103.9(4) ? C221 P2 C231 . . . 104.5(5) ? P2 C211 C212 . . . 116.9(8) ? P2 C211 C216 . . . 123.7(8) ? C212 C211 C216 . . . 119.3(8) ? C211 C212 C213 . . . 120.2(11) ? C211 C212 H212 . . . 119.5(9) ? C213 C212 H212 . . . 120.3(13) ? C212 C213 C214 . . . 121.0(13) ? C212 C213 H213 . . . 118.5(13) ? C214 C213 H213 . . . 120.5(10) ? C213 C214 C215 . . . 118.8(9) ? C213 C214 H214 . . . 121.2(14) ? C215 C214 H214 . . . 120.0(14) ? C214 C215 C216 . . . 121.0(11) ? C214 C215 H215 . . . 119.5(10) ? C216 C215 H215 . . . 119.5(14) ? C211 C216 C215 . . . 119.6(12) ? C211 C216 H216 . . . 120.1(9) ? C215 C216 H216 . . . 120.3(12) ? P2 C221 C222 . . . 118.1(9) ? P2 C221 C226 . . . 123.3(9) ? C222 C221 C226 . . . 118.6(13) ? C221 C222 C223 . . . 121.0(12) ? C221 C222 H222 . . . 118.7(15) ? C223 C222 H222 . . . 120.2(12) ? C222 C223 C224 . . . 119.7(13) ? C222 C223 H223 . . . 120.5(14) ? C224 C223 H223 . . . 119.8(17) ? C223 C224 C225 . . . 119.8(17) ? C223 C224 H224 . . . 120.5(16) ? C225 C224 H224 . . . 119.7(17) ? C224 C225 C226 . . . 121.7(16) ? C224 C225 H225 . . . 119(2) ? C226 C225 H225 . . . 119.7(15) ? C221 C226 C225 . . . 119.1(12) ? C221 C226 H226 . . . 120.9(16) ? C225 C226 H226 . . . 120.0(15) ? P2 C231 C232 . . . 117.8(8) ? P2 C231 C236 . . . 124.5(8) ? C232 C231 C236 . . . 117.8(11) ? C231 C232 C233 . . . 121.9(10) ? C231 C232 H232 . . . 118.8(12) ? C233 C232 H232 . . . 119.4(11) ? C232 C233 C234 . . . 118.7(12) ? C232 C233 H233 . . . 121.3(13) ? C234 C233 H233 . . . 120.0(15) ? C233 C234 C235 . . . 119.7(14) ? C233 C234 H234 . . . 121.3(15) ? C235 C234 H234 . . . 118.9(15) ? C234 C235 C236 . . . 121.6(13) ? C234 C235 H235 . . . 118.9(16) ? C236 C235 H235 . . . 119.5(14) ? C231 C236 C235 . . . 120.1(11) ? C231 C236 H236 . . . 119.7(12) ? C235 C236 H236 . . . 120.2(12) ? O1 N O2 . . . 117.7(13) ? O1 N O3 . . . 126.1(14) ? O2 N O3 . . . 116.2(12) ? Ag O1 N . . . 104.0(11) ? Ag O2 N . . . 96.0(8) ? 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 ? ? ? ? ? ? _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 [(Ph3P)2Ag(C4H6N2)(NO3)] _exptl_crystal_F_000 1592 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 6 -9 7 -6 -9 -7 -6 9 -7 6 9 4 4 9 4 -4 9 -4 -4 -9 -4 4 -9 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -27 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 12.25 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_reduction_process 'perpendicular monochr Lp' _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .128 _refine_ls_wR_factor_all .066 _refine_ls_goodness_of_fit_all 1.248 _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-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_cp12 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C32 H33 Ag1 F3 N6 O2 P1' _chemical_formula_moiety ? _chemical_formula_weight 729.49 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 14.516(5) _cell_length_b 14.219(5) _cell_length_c 10.022(4) _cell_angle_alpha 89.71(3) _cell_angle_beta 71.83(3) _cell_angle_gamma 62.54(3) _cell_volume 1720.2(13) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.408 _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 13.3 _cell_measurement_theta_max 17.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .69 _exptl_crystal_description prism _exptl_crystal_size_max .38 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .20 _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 ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .83 _exptl_absorpt_correction_T_max .90 _diffrn_reflns_number 6141 _reflns_number_total 6076 _reflns_Friedel_coverage ? _reflns_number_gt 3537 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_ref 0.043 _refine_ls_goodness_of_fit_ref 1.668 _refine_ls_number_reflns 3537 _refine_ls_number_parameters 539 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall #<< use NfA code _refine_ls_shift/su_max 0.325 _refine_diff_density_min -.61 _refine_diff_density_max .53 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 850(85) _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 _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 64 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 66 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 2 -1.085 1.101 '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 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .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' 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 Ag .79675(4) .84510(4) .87609(5) .0575(6) Uani ? ? 1.00000 ? ? N1a .7152(5) .7435(5) .8427(6) .075(9) Uani ? ? 1.00000 ? ? C2a .7453(7) .6567(6) .7639(8) .071(10) Uani ? ? 1.00000 ? ? C21a .8548(10) .5930(11) .6460(16) .111(17) Uani ? ? 1.00000 ? ? N3a .6691(7) .6264(6) .7937(8) .082(10) Uani ? ? 1.00000 ? ? C4a .5797(8) .7026(8) .9044(11) .094(13) Uani ? ? 1.00000 ? ? C5a .6070(7) .7712(7) .9359(9) .082(11) Uani ? ? 1.00000 ? ? N1b .6727(4) .9947(4) .8106(5) .060(7) Uani ? ? 1.00000 ? ? C2b .6772(5) 1.0837(6) .7925(7) .059(8) Uani ? ? 1.00000 ? ? C21b .7475(11) 1.1155(11) .8370(17) .097(17) Uani ? ? 1.00000 ? ? N3b .6114(6) 1.1420(5) .7218(7) .073(9) Uani ? ? 1.00000 ? ? C4b .5612(7) 1.0885(7) .6955(8) .075(11) Uani ? ? 1.00000 ? ? C5b .5986(6) .9995(6) .7496(8) .068(10) Uani ? ? 1.00000 ? ? N1c .9429(5) .8023(5) .6621(6) .072(8) Uani ? ? 1.00000 ? ? C2c 1.0456(7) .7261(7) .6191(9) .078(11) Uani ? ? 1.00000 ? ? C21c 1.0975(13) .6395(12) .6909(15) .127(19) Uani ? ? 1.00000 ? ? N3c 1.0975(7) .7372(9) .4929(10) .125(14) Uani ? ? 1.00000 ? ? C4c 1.0293(9) .8222(11) .4499(12) .147(17) Uani ? ? 1.00000 ? ? C5c .9317(8) .8623(9) .5555(10) .100(13) Uani ? ? 1.00000 ? ? P1 .82399(14) .84736(13) 1.09763(17) .053(2) Uani ? ? 1.00000 ? ? C111 .7649(5) .7795(5) 1.2235(6) .050(7) Uani ? ? 1.00000 ? ? C112 .7618(6) .6948(6) 1.1703(9) .069(10) Uani ? ? 1.00000 ? ? C113 .7185(7) .6390(7) 1.2608(11) .087(13) Uani ? ? 1.00000 ? ? C114 .6787(7) .6707(8) 1.4028(11) .092(14) Uani ? ? 1.00000 ? ? C115 .6798(7) .7565(7) 1.4581(9) .087(12) Uani ? ? 1.00000 ? ? C116 .7235(6) .8108(6) 1.3682(7) .068(10) Uani ? ? 1.00000 ? ? C121 .7689(5) .9780(5) 1.1982(6) .053(8) Uani ? ? 1.00000 ? ? C122 .6664(7) 1.0574(6) 1.2023(8) .071(10) Uani ? ? 1.00000 ? ? C123 .6162(9) 1.1583(7) 1.2794(9) .088(12) Uani ? ? 1.00000 ? ? C124 .6699(11) 1.1797(8) 1.3559(10) .101(15) Uani ? ? 1.00000 ? ? C125 .7702(10) 1.1046(8) 1.3516(9) .092(14) Uani ? ? 1.00000 ? ? C126 .8207(7) 1.0029(7) 1.2747(8) .075(11) Uani ? ? 1.00000 ? ? C131 .9684(5) .7812(6) 1.0804(7) .059(8) Uani ? ? 1.00000 ? ? C132 1.0349(8) .8176(9) .9977(9) .093(14) Uani ? ? 1.00000 ? ? C133 1.1463(10) .7692(12) .9743(11) .118(19) Uani ? ? 1.00000 ? ? C134 1.1906(9) .6802(12) 1.0337(14) .125(18) Uani ? ? 1.00000 ? ? C135 1.1289(9) .6420(10) 1.1156(14) .132(17) Uani ? ? 1.00000 ? ? C136 1.0165(7) .6930(7) 1.1382(11) .101(13) Uani ? ? 1.00000 ? ? O1 .3185(4) .5494(4) 1.3448(6) .110(8) Uani ? ? 1.00000 ? ? O2 .3524(5) .6820(4) 1.3559(6) .110(8) Uani ? ? 1.00000 ? ? C1 .3776(7) .5903(6) 1.3252(7) .066(10) Uani ? ? 1.00000 ? ? C2 .5015(12) .5038(13) 1.2752(18) .17(3) Uani ? ? 1.00000 ? ? F1 .5284(5) .4193(5) 1.2235(12) .245(13) Uani ? ? 1.00000 ? ? F2 .5598(7) .5141(10) 1.3172(16) .32(2) Uani ? ? 1.00000 ? ? F3 .5359(9) .5412(10) 1.1515(12) .329(18) Uani ? ? 1.00000 ? ? H21a1 .892(9) .559(8) .712(11) .19(6) Uiso ? ? 1.00000 ? ? H21b1 .820(6) 1.055(6) .814(8) .11(3) Uiso ? ? 1.00000 ? ? H21c1 1.053(6) .644(6) .784(8) .10(3) Uiso ? ? 1.00000 ? ? H21a2 .870(6) .636(6) .613(8) .08(3) Uiso ? ? 1.00000 ? ? H21a3 .852(7) .532(7) .602(9) .14(4) Uiso ? ? 1.00000 ? ? H3a .690(6) .565(6) .740(8) .11(3) Uiso ? ? 1.00000 ? ? H4a .516(6) .687(5) .958(7) .10(3) Uiso ? ? 1.00000 ? ? H5a .563(5) .843(5) 1.009(7) .11(3) Uiso ? ? 1.00000 ? ? H21b2 .721(9) 1.146(10) .923(11) .19(7) Uiso ? ? 1.00000 ? ? H21b3 .745(8) 1.176(8) .824(10) .15(4) Uiso ? ? 1.00000 ? ? H3b .602(5) 1.201(5) .708(6) .06(2) Uiso ? ? 1.00000 ? ? H4b .511(5) 1.123(4) .650(6) .06(2) Uiso ? ? 1.00000 ? ? H5b .579(4) .942(4) .752(6) .064(19) Uiso ? ? 1.00000 ? ? H21c2 1.142(7) .647(7) .735(10) .13(4) Uiso ? ? 1.00000 ? ? H21c3 1.118(10) .580(9) .654(13) .21(7) Uiso ? ? 1.00000 ? ? H3c 1.154(5) .698(5) .451(7) .06(2) Uiso ? ? 1.00000 ? ? H4c 1.053(12) .851(12) .354(16) .33(8) Uiso ? ? 1.00000 ? ? H5c .880(6) .927(6) .571(8) .10(3) Uiso ? ? 1.00000 ? ? H112 .788(5) .672(4) 1.077(6) .06(2) Uiso ? ? 1.00000 ? ? H113 .720(4) .580(4) 1.215(6) .056(18) Uiso ? ? 1.00000 ? ? H114 .655(6) .630(6) 1.460(8) .11(3) Uiso ? ? 1.00000 ? ? H115 .655(6) .770(5) 1.566(8) .11(3) Uiso ? ? 1.00000 ? ? H116 .730(5) .872(4) 1.409(6) .07(2) Uiso ? ? 1.00000 ? ? H122 .629(5) 1.041(5) 1.160(6) .07(2) Uiso ? ? 1.00000 ? ? H123 .545(6) 1.215(6) 1.288(8) .11(3) Uiso ? ? 1.00000 ? ? H124 .637(6) 1.242(5) 1.400(7) .09(3) Uiso ? ? 1.00000 ? ? H125 .808(5) 1.114(5) 1.404(7) .09(3) Uiso ? ? 1.00000 ? ? H126 .892(4) .951(4) 1.266(5) .045(18) Uiso ? ? 1.00000 ? ? H132 1.001(7) .877(6) .959(8) .12(4) Uiso ? ? 1.00000 ? ? H133 1.192(7) .798(6) .916(9) .13(3) Uiso ? ? 1.00000 ? ? H134 1.257(6) .658(6) 1.023(7) .09(3) Uiso ? ? 1.00000 ? ? H135 1.160(8) .571(8) 1.136(10) .17(4) Uiso ? ? 1.00000 ? ? H136 .984(6) .658(6) 1.186(7) .09(3) 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 Ag .0654(4) .0587(3) .0518(3) -.0328(3) -.0203(3) .0106(2) N1a .102(5) .069(4) .074(4) -.054(4) -.037(4) .012(3) C2a .081(6) .060(5) .083(6) -.036(5) -.040(5) .017(4) C21a .093(8) .090(9) .120(10) -.033(8) -.017(7) -.016(8) N3a .096(6) .061(5) .108(6) -.045(5) -.049(5) .014(4) C4a .086(7) .091(7) .110(7) -.053(6) -.024(6) .005(6) C5a .076(6) .084(6) .078(6) -.045(5) -.006(5) -.009(5) N1b .059(4) .049(3) .069(4) -.026(3) -.021(3) .013(3) C2b .057(4) .060(5) .059(4) -.029(4) -.017(4) .008(4) C21b .106(9) .091(8) .131(11) -.071(8) -.052(8) .026(7) N3b .086(5) .046(4) .083(5) -.029(4) -.028(4) .020(4) C4b .072(6) .066(6) .087(6) -.026(5) -.040(5) .020(5) C5b .067(5) .061(5) .084(5) -.033(4) -.034(4) .015(4) N1c .057(4) .080(4) .057(4) -.020(4) -.012(3) .002(3) C2c .067(6) .083(6) .066(5) -.021(5) -.021(5) -.008(5) C21c .127(10) .113(10) .092(9) -.010(8) -.053(9) -.001(8) N3c .054(6) .172(10) .085(7) -.024(6) .008(5) .004(6) C4c .072(8) .192(12) .103(9) -.027(8) .001(7) .050(8) C5c .078(7) .102(8) .073(6) -.018(6) -.008(5) .027(6) P1 .0555(11) .0566(11) .0522(10) -.0306(9) -.0195(9) .0114(8) C111 .052(4) .052(4) .054(4) -.029(3) -.021(3) .018(3) C112 .087(6) .068(5) .069(6) -.047(5) -.035(5) .025(5) C113 .116(7) .074(6) .100(7) -.060(6) -.054(6) .027(5) C114 .102(7) .103(7) .101(8) -.069(6) -.041(6) .053(7) C115 .100(7) .099(7) .072(6) -.062(6) -.023(5) .033(5) C116 .089(6) .072(5) .056(5) -.049(5) -.024(4) .018(4) C121 .058(4) .057(4) .046(4) -.031(4) -.017(3) .014(3) C122 .064(6) .072(6) .069(5) -.035(5) -.010(4) .004(4) C123 .093(7) .063(6) .071(6) -.026(6) -.001(5) -.000(5) C124 .152(11) .061(7) .064(6) -.045(7) -.017(7) .004(5) C125 .142(9) .076(7) .079(6) -.057(7) -.061(6) .015(5) C126 .089(6) .065(6) .083(6) -.035(5) -.048(5) .013(4) C131 .056(4) .073(5) .057(4) -.040(4) -.018(4) .006(4) C132 .068(6) .147(9) .083(6) -.067(7) -.023(5) .029(6) C133 .092(9) .179(12) .096(8) -.089(10) -.012(6) .010(8) C134 .052(7) .159(12) .130(10) -.035(8) -.015(7) -.028(8) C135 .069(8) .106(9) .201(12) -.029(7) -.044(8) .048(8) C136 .053(6) .087(7) .153(9) -.028(5) -.032(6) .049(6) O1 .077(4) .096(4) .137(5) -.053(3) .006(3) -.039(3) O2 .142(5) .053(3) .124(5) -.049(4) -.029(4) .004(3) C1 .069(6) .053(5) .066(5) -.027(4) -.014(4) .002(4) C2 .148(13) .196(15) .200(14) -.154(13) .027(11) -.052(11) F1 .086(4) .079(4) .498(15) -.021(4) -.041(6) -.068(7) F2 .122(7) .273(11) .56(2) -.090(7) -.129(10) -.048(13) F3 .146(8) .277(12) .268(11) .045(7) .062(8) .100(10) # 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 Ag N1a . . 2.330(9) ? Ag N1b . . 2.321(5) ? Ag N1c . . 2.336(5) ? Ag P1 . . 2.376(2) ? N1a C2a . . 1.279(11) ? N1a C5a . . 1.419(11) ? C2a C21a . . 1.501(13) ? C2a N3a . . 1.315(15) ? C21a H21a1 . . .97(12) ? C21a H21a2 . . .78(9) ? C21a H21a3 . . 1.00(11) ? N3a C4a . . 1.381(10) ? N3a H3a . . .90(9) ? C4a C5a . . 1.283(18) ? C4a H4a . . 1.03(9) ? C5a H5a . . 1.05(7) ? N1b C2b . . 1.307(11) ? N1b C5b . . 1.370(12) ? C2b C21b . . 1.47(2) ? C2b N3b . . 1.337(10) ? C21b H21b1 . . .96(7) ? C21b H21b2 . . .85(11) ? C21b H21b3 . . .86(12) ? N3b C4b . . 1.346(15) ? N3b H3b . . .81(7) ? C4b C5b . . 1.317(11) ? C4b H4b . . .92(7) ? C5b H5b . . .98(7) ? N1c C2c . . 1.302(9) ? N1c C5c . . 1.366(12) ? C2c C21c . . 1.441(18) ? C2c N3c . . 1.306(13) ? C21c H21c1 . . .94(8) ? C21c H21c2 . . .94(12) ? C21c H21c3 . . .81(13) ? N3c C4c . . 1.335(16) ? N3c H3c . . .72(5) ? C4c C5c . . 1.334(13) ? C4c H4c . . 1.06(16) ? C5c H5c . . .85(6) ? P1 C111 . . 1.826(7) ? P1 C121 . . 1.803(7) ? P1 C131 . . 1.807(7) ? C111 C112 . . 1.345(13) ? C111 C116 . . 1.371(9) ? C112 C113 . . 1.395(14) ? C112 H112 . . .89(5) ? C113 C114 . . 1.347(15) ? C113 H113 . . .95(7) ? C114 C115 . . 1.351(17) ? C114 H114 . . .92(9) ? C115 C116 . . 1.378(14) ? C115 H115 . . 1.01(7) ? C116 H116 . . 1.01(7) ? C121 C122 . . 1.380(10) ? C121 C126 . . 1.375(15) ? C122 C123 . . 1.372(12) ? C122 H122 . . .90(8) ? C123 C124 . . 1.37(2) ? C123 H123 . . .95(7) ? C124 C125 . . 1.338(16) ? C124 H124 . . .83(7) ? C125 C126 . . 1.380(13) ? C125 H125 . . .91(9) ? C126 H126 . . .92(5) ? C131 C132 . . 1.359(15) ? C131 C136 . . 1.354(12) ? C132 C133 . . 1.372(17) ? C132 H132 . . .91(8) ? C133 C134 . . 1.36(2) ? C133 H133 . . .97(10) ? C134 C135 . . 1.33(2) ? C134 H134 . . .83(8) ? C135 C136 . . 1.385(15) ? C135 H135 . . .95(10) ? C136 H136 . . .88(9) ? O1 C1 . . 1.211(13) ? O2 C1 . . 1.193(10) ? C1 C2 . . 1.550(15) ? C2 F1 . . 1.15(2) ? C2 F2 . . 1.12(3) ? C2 F3 . . 1.39(2) ? F1 F2 . . 1.937(19) ? F1 F3 . . 1.911(16) ? F2 F3 . . 1.80(2) ? 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 N1a Ag N1b . . . 92.7(2) ? N1a Ag N1c . . . 105.0(2) ? N1a Ag P1 . . . 115.86(17) ? N1b Ag N1c . . . 93.93(19) ? N1b Ag P1 . . . 123.49(14) ? N1c Ag P1 . . . 120.6(2) ? Ag N1a C2a . . . 136.6(6) ? Ag N1a C5a . . . 119.4(6) ? C2a N1a C5a . . . 103.7(8) ? N1a C2a C21a . . . 125.6(11) ? N1a C2a N3a . . . 113.4(7) ? C21a C2a N3a . . . 121.0(10) ? C2a C21a H21a1 . . . 93(5) ? C2a C21a H21a2 . . . 105(4) ? C2a C21a H21a3 . . . 106(5) ? H21a1 C21a H21a2 . . . 113(12) ? H21a1 C21a H21a3 . . . 101(10) ? H21a2 C21a H21a3 . . . 132(8) ? C2a N3a C4a . . . 106.1(9) ? C2a N3a H3a . . . 114(6) ? C4a N3a H3a . . . 140(6) ? N3a C4a C5a . . . 107.1(10) ? N3a C4a H4a . . . 119(4) ? C5a C4a H4a . . . 132(4) ? N1a C5a C4a . . . 109.7(7) ? N1a C5a H5a . . . 118(5) ? C4a C5a H5a . . . 132(5) ? Ag N1b C2b . . . 126.2(5) ? Ag N1b C5b . . . 127.4(5) ? C2b N1b C5b . . . 104.7(6) ? N1b C2b C21b . . . 125.8(8) ? N1b C2b N3b . . . 110.7(8) ? C21b C2b N3b . . . 123.5(9) ? C2b C21b H21b1 . . . 110(6) ? C2b C21b H21b2 . . . 116(11) ? C2b C21b H21b3 . . . 121(8) ? H21b1 C21b H21b2 . . . 112(10) ? H21b1 C21b H21b3 . . . 115(9) ? H21b2 C21b H21b3 . . . 80(12) ? C2b N3b C4b . . . 107.8(7) ? C2b N3b H3b . . . 122(5) ? C4b N3b H3b . . . 130(5) ? N3b C4b C5b . . . 106.1(9) ? N3b C4b H4b . . . 115(5) ? C5b C4b H4b . . . 139(5) ? N1b C5b C4b . . . 110.8(9) ? N1b C5b H5b . . . 120(4) ? C4b C5b H5b . . . 129(4) ? Ag N1c C2c . . . 131.1(6) ? Ag N1c C5c . . . 122.3(5) ? C2c N1c C5c . . . 106.6(6) ? N1c C2c C21c . . . 128.0(9) ? N1c C2c N3c . . . 108.7(8) ? C21c C2c N3c . . . 123.2(8) ? C2c C21c H21c1 . . . 115(4) ? C2c C21c H21c2 . . . 116(6) ? C2c C21c H21c3 . . . 116(10) ? H21c1 C21c H21c2 . . . 84(9) ? H21c1 C21c H21c3 . . . 103(11) ? H21c2 C21c H21c3 . . . 117(12) ? C2c N3c C4c . . . 110.8(8) ? C2c N3c H3c . . . 122(6) ? C4c N3c H3c . . . 127(6) ? N3c C4c C5c . . . 104.8(11) ? N3c C4c H4c . . . 125(7) ? C5c C4c H4c . . . 130(7) ? N1c C5c C4c . . . 109.0(9) ? N1c C5c H5c . . . 122(5) ? C4c C5c H5c . . . 124(5) ? Ag P1 C111 . . . 114.4(3) ? Ag P1 C121 . . . 116.3(2) ? Ag P1 C131 . . . 113.2(2) ? C111 P1 C121 . . . 103.9(3) ? C111 P1 C131 . . . 104.1(3) ? C121 P1 C131 . . . 103.5(4) ? P1 C111 C112 . . . 117.8(5) ? P1 C111 C116 . . . 123.4(7) ? C112 C111 C116 . . . 118.8(7) ? C111 C112 C113 . . . 120.6(8) ? C111 C112 H112 . . . 121(5) ? C113 C112 H112 . . . 118(5) ? C112 C113 C114 . . . 119.7(11) ? C112 C113 H113 . . . 115(3) ? C114 C113 H113 . . . 125(4) ? C113 C114 C115 . . . 120.6(11) ? C113 C114 H114 . . . 118(5) ? C115 C114 H114 . . . 121(5) ? C114 C115 C116 . . . 119.5(9) ? C114 C115 H115 . . . 115(5) ? C116 C115 H115 . . . 125(5) ? C111 C116 C115 . . . 120.8(9) ? C111 C116 H116 . . . 119(3) ? C115 C116 H116 . . . 120(3) ? P1 C121 C122 . . . 118.0(7) ? P1 C121 C126 . . . 124.3(5) ? C122 C121 C126 . . . 117.7(7) ? C121 C122 C123 . . . 122.2(10) ? C121 C122 H122 . . . 119(3) ? C123 C122 H122 . . . 119(3) ? C122 C123 C124 . . . 118.4(9) ? C122 C123 H123 . . . 126(6) ? C124 C123 H123 . . . 116(6) ? C123 C124 C125 . . . 120.5(10) ? C123 C124 H124 . . . 115(6) ? C125 C124 H124 . . . 124(6) ? C124 C125 C126 . . . 121.2(13) ? C124 C125 H125 . . . 124(4) ? C126 C125 H125 . . . 115(4) ? C121 C126 C125 . . . 119.9(9) ? C121 C126 H126 . . . 117(4) ? C125 C126 H126 . . . 123(4) ? P1 C131 C132 . . . 118.5(6) ? P1 C131 C136 . . . 124.1(7) ? C132 C131 C136 . . . 117.3(8) ? C131 C132 C133 . . . 122.2(11) ? C131 C132 H132 . . . 116(6) ? C133 C132 H132 . . . 121(6) ? C132 C133 C134 . . . 118.0(14) ? C132 C133 H133 . . . 121(5) ? C134 C133 H133 . . . 121(5) ? C133 C134 C135 . . . 121.9(12) ? C133 C134 H134 . . . 114(6) ? C135 C134 H134 . . . 124(6) ? C134 C135 C136 . . . 118.8(12) ? C134 C135 H135 . . . 122(6) ? C136 C135 H135 . . . 117(7) ? C131 C136 C135 . . . 121.8(11) ? C131 C136 H136 . . . 126(5) ? C135 C136 H136 . . . 112(5) ? O1 C1 O2 . . . 128.9(7) ? O1 C1 C2 . . . 111.2(10) ? O2 C1 C2 . . . 119.2(12) ? C1 C2 F1 . . . 119.6(17) ? C1 C2 F2 . . . 120.3(14) ? C1 C2 F3 . . . 96.9(11) ? F1 C2 F2 . . . 117.6(14) ? F1 C2 F3 . . . 97.6(13) ? F2 C2 F3 . . . 91.5(16) ? C2 F1 F2 . . . 30.8(10) ? C2 F1 F3 . . . 46.0(10) ? F2 F1 F3 . . . 55.9(6) ? C2 F2 F1 . . . 31.6(9) ? C2 F2 F3 . . . 50.2(12) ? F1 F2 F3 . . . 61.3(8) ? C2 F3 F1 . . . 36.4(9) ? C2 F3 F2 . . . 38.3(10) ? F1 F3 F2 . . . 62.8(7) ? 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 Ag C2a 3.376(11) . . ? Ag C21a 3.868(16) . . ? Ag C5a 3.269(12) . . ? Ag C2b 3.267(7) . . ? Ag C21b 3.616(16) . . ? Ag C5b 3.335(8) . . ? Ag C2c 3.339(7) . . ? Ag C21c 3.778(13) . . ? Ag C5c 3.276(10) . . ? Ag C111 3.545(7) . . ? Ag C112 3.677(9) . . ? Ag C121 3.563(7) . . ? Ag C122 3.789(8) . . ? Ag C131 3.507(8) . . ? Ag C132 3.869(13) . . ? Ag H21b1 3.20(9) . . ? Ag H21c1 3.31(6) . . ? Ag H21a2 3.51(8) . . ? Ag H5a 3.25(8) . . ? Ag H5b 3.44(7) . . ? Ag H5c 3.34(8) . . ? Ag H112 3.19(6) . . ? Ag H122 3.36(5) . . ? Ag H132 3.54(11) . . ? N1a C21a 2.475(13) . . ? N1a N3a 2.168(14) . . ? N1a C4a 2.210(16) . . ? N1a N1b 3.364(9) . . ? N1a P1 3.988(9) . . ? N1a H21a1 2.63(8) . . ? N1a H21a2 2.52(6) . . ? N1a H5a 2.13(5) . . ? N1a H112 2.86(6) . . ? C2a C4a 2.154(13) . . ? C2a C5a 2.123(9) . . ? C2a H21a1 1.82(10) . . ? C2a H21a2 1.86(8) . . ? C2a H21a3 2.03(7) . . ? C2a H3a 1.87(11) . . ? C2a H115 2.81(8) . '1 554' ? C21a N3a 2.452(16) . . ? C21a H3a 2.50(10) . . ? N3a C5a 2.144(12) . . ? N3a O1 2.770(12) . '2 667' ? N3a F1 3.272(14) . '2 667' ? N3a H21a1 2.75(12) . . ? N3a H21a3 2.47(7) . . ? N3a H4a 2.09(6) . . ? C4a F1 3.300(17) . '2 667' ? C4a F3 3.479(17) . . ? C4a H3a 2.15(7) . . ? C4a H5a 2.14(9) . . ? C5a H4a 2.12(10) . . ? N1b C21b 2.47(2) . . ? N1b N3b 2.175(8) . . ? N1b C4b 2.211(11) . . ? N1b P1 4.138(6) . . ? N1b H21b1 2.66(11) . . ? N1b H21b2 2.88(16) . . ? N1b H5b 2.05(8) . . ? C2b C4b 2.168(14) . . ? C2b C5b 2.119(14) . . ? C2b O2 3.538(10) . '2 677' ? C2b H21b1 2.01(10) . . ? C2b H21b2 1.99(16) . . ? C2b H21b3 2.05(14) . . ? C2b H3b 1.89(6) . . ? C21b N3b 2.47(2) . . ? C21b O2 3.460(16) . '2 677' ? C21b H3b 2.63(7) . . ? N3b C5b 2.128(13) . . ? N3b O2 2.843(11) . '2 677' ? N3b H21b3 2.68(13) . . ? N3b H4b 1.93(8) . . ? C4b H5a 2.84(6) . '2 677' ? C4b H3b 1.97(8) . . ? C4b H5b 2.08(6) . . ? C5b H5a 2.83(6) . '2 677' ? C5b H4b 2.10(6) . . ? N1c C21c 2.467(16) . . ? N1c N3c 2.120(9) . . ? N1c C4c 2.198(14) . . ? N1c P1 4.093(6) . . ? N1c H21c1 2.64(8) . . ? N1c H3c 2.80(5) . . ? N1c H5c 1.95(7) . . ? C2c C4c 2.174(16) . . ? C2c C5c 2.140(13) . . ? C2c H21c1 2.02(8) . . ? C2c H21c2 2.04(10) . . ? C2c H21c3 1.94(11) . . ? C2c H3c 1.80(6) . . ? C21c N3c 2.42(2) . . ? C21c H3c 2.55(7) . . ? N3c C5c 2.114(12) . . ? N3c O1 2.966(9) . '1 654' ? N3c O2 3.219(12) . '1 654' ? N3c H21c2 2.86(10) . . ? N3c H21c3 2.71(13) . . ? N3c H4c 2.13(16) . . ? C4c H3c 1.85(6) . . ? C4c H5c 1.94(6) . . ? C5c H3c 2.81(5) . . ? C5c H4c 2.17(14) . . ? P1 C112 2.726(10) . . ? P1 C113 4.046(11) . . ? P1 C115 4.103(10) . . ? P1 C116 2.823(8) . . ? P1 C122 2.737(7) . . ? P1 C123 4.039(8) . . ? P1 C125 4.085(12) . . ? P1 C126 2.817(11) . . ? P1 C132 2.730(12) . . ? P1 C133 4.033(15) . . ? P1 C135 4.089(12) . . ? P1 C136 2.799(9) . . ? P1 H112 2.79(7) . . ? P1 H116 2.94(5) . . ? P1 H122 2.78(5) . . ? P1 H126 2.89(7) . . ? P1 H132 2.74(10) . . ? P1 H136 2.99(7) . . ? C111 C113 2.379(14) . . ? C111 C114 2.746(14) . . ? C111 C115 2.391(11) . . ? C111 C121 2.858(11) . . ? C111 C131 2.864(10) . . ? C111 C136 3.083(12) . . ? C111 H112 1.96(7) . . ? C111 H116 2.06(6) . . ? C111 H136 2.73(7) . . ? C112 C114 2.371(14) . . ? C112 C115 2.725(12) . . ? C112 C116 2.338(12) . . ? C112 H113 1.99(7) . . ? C113 C115 2.343(15) . . ? C113 C116 2.715(15) . . ? C113 F2 3.425(19) . . ? C113 H112 1.98(6) . . ? C113 H114 1.95(7) . . ? C114 C116 2.358(16) . . ? C114 H113 2.04(6) . . ? C114 H115 2.01(8) . . ? C115 H114 1.99(10) . . ? C115 H116 2.08(7) . . ? C116 C121 3.113(11) . . ? C116 H115 2.13(7) . . ? C121 C123 2.409(9) . . ? C121 C124 2.760(12) . . ? C121 C125 2.385(15) . . ? C121 C131 2.835(7) . . ? C121 C132 3.352(10) . . ? C121 H116 2.66(6) . . ? C121 H122 1.97(7) . . ? C121 H126 1.98(7) . . ? C122 C124 2.356(17) . . ? C122 C125 2.704(18) . . ? C122 C126 2.357(15) . . ? C122 H123 2.08(6) . . ? C123 C125 2.352(19) . . ? C123 C126 2.750(13) . . ? C123 F1 3.431(12) . '1 565' ? C123 H122 1.97(7) . . ? C123 H124 1.88(9) . . ? C124 C126 2.368(11) . . ? C124 F1 3.575(13) . '1 565' ? C124 H123 1.98(10) . . ? C124 H125 2.00(8) . . ? C125 H124 1.93(6) . . ? C125 H126 2.03(4) . . ? C126 C131 3.091(10) . . ? C126 C132 3.384(10) . . ? C126 H116 2.86(7) . . ? C126 H125 1.95(8) . . ? C131 C133 2.391(17) . . ? C131 C134 2.736(14) . . ? C131 C135 2.392(13) . . ? C131 H126 2.61(5) . . ? C131 H132 1.94(9) . . ? C131 H136 2.00(8) . . ? C132 C134 2.342(16) . . ? C132 C135 2.707(17) . . ? C132 C136 2.317(17) . . ? C132 H126 2.84(4) . . ? C132 H133 2.05(10) . . ? C133 C135 2.35(2) . . ? C133 C136 2.71(2) . . ? C133 H132 2.00(8) . . ? C133 H134 1.86(7) . . ? C134 C136 2.333(17) . . ? C134 H133 2.04(9) . . ? C134 H135 1.99(12) . . ? C135 H134 1.92(9) . . ? C135 H136 1.90(9) . . ? C136 H135 2.00(9) . . ? O1 O2 2.169(10) . . ? O1 C2 2.286(18) . . ? O1 F1 2.588(7) . . ? O1 F2 3.220(14) . . ? O1 F3 3.095(14) . . ? O1 H21a3 3.09(11) . '2 667' ? O1 H3a 1.91(10) . '2 667' ? O1 H3c 2.26(5) . '1 456' ? O2 C2 2.372(14) . . ? O2 F1 3.373(7) . . ? O2 F2 2.750(10) . . ? O2 F3 2.649(10) . . ? O2 H21b3 2.87(10) . '2 677' ? O2 H3b 2.08(7) . '2 677' ? O2 H3c 2.64(8) . '1 456' ? C1 F1 2.338(8) . . ? C1 F2 2.324(14) . . ? C1 F3 2.199(12) . . ? C1 H3c 2.72(6) . '1 456' ? F1 H3a 2.98(10) . '2 667' ? F1 H4a 2.77(9) . '2 667' ? F1 H123 2.88(9) . '1 545' ? F1 H134 3.01(6) . '2 767' ? F2 H113 2.80(7) . . ? F3 H4a 2.81(7) . . ? F3 H134 3.00(6) . '2 767' ? H21a1 H21a2 1.47(14) . . ? H21a1 H21a3 1.52(18) . . ? H21b1 H21b2 1.50(11) . . ? H21b1 H21b3 1.54(12) . . ? H21c1 H21c2 1.25(14) . . ? H21c1 H21c3 1.37(13) . . ? H21a2 H21a3 1.63(15) . . ? H21a3 H3a 2.15(12) . . ? H21b2 H21b3 1.10(16) . . ? H3b H4b 2.27(12) . . ? H21c2 H21c3 1.5(2) . . ? H3c H4c 2.40(16) . . ? H112 H113 2.22(9) . . ? H113 H114 2.32(9) . . ? H114 H115 2.27(13) . . ? H122 H123 2.36(10) . . ? H123 H124 2.14(14) . . ? H124 H125 2.32(9) . . ? H125 H126 2.26(8) . . ? H132 H133 2.35(13) . . ? H133 H134 2.20(11) . . ? H134 H135 2.31(15) . . ? H135 H136 2.15(12) . . ? _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 [(Ph3P)Ag(C4H6N2)3](CF3CO2) _exptl_crystal_F_000 744 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 7 4 8 0 0 0 10 0 0 0 8 -8 0 0 0 -10 0 0 0 -8 -7 -7 -4 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min -14 _reflns_limit_k_max 16 _reflns_limit_l_min -11 _reflns_limit_l_max 11 _reflns_number_observed 3537 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression Zachariasen _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .087 _refine_ls_wR_factor_all .050 _refine_ls_goodness_of_fit_all 1.416 _refine_ls_shift/su_mean .013 #========================================================================== # 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 data_cp8 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C46 H48 Ag2 N4 O6 P2 S2' _chemical_formula_moiety ? _chemical_formula_weight 1094.73 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_2/c _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 29.421(3) _cell_length_b 9.2700(10) _cell_length_c 19.122(2) _cell_angle_alpha 90.00000 _cell_angle_beta 117.8880(10) _cell_angle_gamma 90.00000 _cell_volume 4609.5(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7497 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.062 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .08 _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 0.774 _exptl_absorpt_correction_T_max 0.928 _diffrn_reflns_number 26676 _reflns_number_total 5800 _reflns_Friedel_coverage 0 _reflns_number_gt 5209 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.11 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .023 _refine_ls_wR_factor_ref .032 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_number_reflns 5209 _refine_ls_number_parameters 377 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .031 _refine_diff_density_min -.354 _refine_diff_density_max .664 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1027(207) _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 ? 0 184 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 192 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 8 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 8 .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 Ag .326929(5) .150466(14) .467356(8) .02454(7) Uani ? ? 1.00000 ? ? N1a .28515(6) -.04324(16) .40482(8) .0229(6) Uani ? ? 1.00000 ? ? C2a .29352(7) -.1233(2) .35469(10) .0251(7) Uani ? ? 1.00000 ? ? N3a .26806(6) -.24921(16) .34001(9) .0244(6) Uani ? ? 1.00000 ? ? C31a .26775(10) -.3617(2) .28611(14) .0364(10) Uani ? ? 1.00000 ? ? C4a .24152(7) -.2503(2) .38331(10) .0247(7) Uani ? ? 1.00000 ? ? C5a .25243(7) -.1232(2) .42302(10) .0229(7) Uani ? ? 1.00000 ? ? P1 .396495(16) .30474(5) .48973(3) .02040(17) Uani ? ? 1.00000 ? ? C111 .39522(6) .35042(18) .39624(10) .0212(7) Uani ? ? 1.00000 ? ? C112 .38023(7) .2435(2) .33783(11) .0261(7) Uani ? ? 1.00000 ? ? C113 .38128(7) .2690(2) .26719(11) .0293(8) Uani ? ? 1.00000 ? ? C114 .39582(7) .4036(2) .25272(11) .0292(8) Uani ? ? 1.00000 ? ? C115 .40964(7) .5116(2) .30934(11) .0283(8) Uani ? ? 1.00000 ? ? C116 .40986(7) .4848(2) .38118(10) .0251(7) Uani ? ? 1.00000 ? ? C121 .40494(6) .47972(18) .53840(10) .0203(7) Uani ? ? 1.00000 ? ? C122 .36153(7) .5668(2) .51681(10) .0235(7) Uani ? ? 1.00000 ? ? C123 .36693(7) .7056(2) .54747(11) .0269(8) Uani ? ? 1.00000 ? ? C124 .41539(8) .7584(2) .59976(11) .0290(8) Uani ? ? 1.00000 ? ? C125 .45827(8) .6714(2) .62241(12) .0299(8) Uani ? ? 1.00000 ? ? C126 .45326(7) .5327(2) .59196(11) .0260(7) Uani ? ? 1.00000 ? ? C131 .45879(7) .21671(19) .54624(10) .0232(7) Uani ? ? 1.00000 ? ? C132 .46931(9) .1535(2) .61849(13) .0368(10) Uani ? ? 1.00000 ? ? C133 .51729(9) .0933(3) .66588(13) .0441(11) Uani ? ? 1.00000 ? ? C134 .55479(8) .0932(2) .64150(13) .0358(9) Uani ? ? 1.00000 ? ? C135 .54408(8) .1505(2) .56866(13) .0314(8) Uani ? ? 1.00000 ? ? C136 .49622(7) .2133(2) .52118(11) .0265(8) Uani ? ? 1.00000 ? ? S .301191(16) .13707(4) .62707(2) .02050(17) Uani ? ? 1.00000 ? ? O1 .32119(6) .05106(15) .58339(8) .0359(7) Uani ? ? 1.00000 ? ? O2 .24524(6) .14522(16) .58636(10) .0417(7) Uani ? ? 1.00000 ? ? O3 .32196(5) .08980(16) .70846(7) .0314(6) Uani ? ? 1.00000 ? ? C0 .32342(8) .3140(2) .62822(12) .0289(8) Uani ? ? 1.00000 ? ? H2a .3137(8) -.099(2) .3310(13) .027(5) Uiso ? ? 1.00000 ? ? H31a1 .2993(13) -.365(3) .2861(18) .056(9) Uiso ? ? 1.00000 ? ? H31a2 .2446(15) -.339(4) .236(2) .087(13) Uiso ? ? 1.00000 ? ? H31a3 .2603(13) -.452(4) .301(2) .078(10) Uiso ? ? 1.00000 ? ? H4a .2229(10) -.336(3) .3861(15) .038(7) Uiso ? ? 1.00000 ? ? H5a .2417(8) -.087(2) .4568(13) .027(5) Uiso ? ? 1.00000 ? ? H112 .3684(9) .155(2) .3439(14) .032(6) Uiso ? ? 1.00000 ? ? H113 .3717(9) .197(3) .2280(14) .036(6) Uiso ? ? 1.00000 ? ? H114 .3957(9) .422(3) .2044(14) .033(6) Uiso ? ? 1.00000 ? ? H115 .4203(9) .611(3) .2987(14) .038(6) Uiso ? ? 1.00000 ? ? H116 .4204(8) .558(2) .4191(12) .024(5) Uiso ? ? 1.00000 ? ? H122 .3295(6) .5404(19) .4775(9) .003(4) Uiso ? ? 1.00000 ? ? H123 .3396(9) .764(3) .5368(13) .031(6) Uiso ? ? 1.00000 ? ? H124 .4178(9) .852(2) .6188(14) .031(6) Uiso ? ? 1.00000 ? ? H125 .4915(10) .706(3) .6587(14) .037(6) Uiso ? ? 1.00000 ? ? H126 .4828(8) .473(2) .6099(13) .027(5) Uiso ? ? 1.00000 ? ? H132 .4432(10) .155(2) .6347(15) .038(7) Uiso ? ? 1.00000 ? ? H133 .5236(10) .046(3) .7171(16) .053(8) Uiso ? ? 1.00000 ? ? H134 .5865(10) .055(3) .6752(15) .042(7) Uiso ? ? 1.00000 ? ? H135 .5707(11) .152(3) .5508(16) .046(7) Uiso ? ? 1.00000 ? ? H136 .4895(8) .254(3) .4734(14) .031(6) Uiso ? ? 1.00000 ? ? H1a .3620(10) .309(3) .6513(14) .035(6) Uiso ? ? 1.00000 ? ? H1b .3131(10) .373(3) .6559(16) .044(7) Uiso ? ? 1.00000 ? ? H1c .3095(11) .352(3) .5739(18) .054(8) 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 Ag .02566(8) .02268(8) .02873(8) -.00820(5) .01562(6) -.00411(5) N1a .0258(7) .0217(7) .0207(7) -.0042(6) .0105(6) .0001(5) C2a .0291(9) .0247(9) .0222(8) -.0043(7) .0125(7) .0007(6) N3a .0283(8) .0222(7) .0214(7) -.0039(6) .0104(6) -.0024(5) C31a .0492(13) .0287(10) .0372(11) -.0079(9) .0250(11) -.0107(8) C4a .0221(8) .0238(8) .0262(8) -.0042(7) .0095(7) .0012(6) C5a .0223(8) .0226(8) .0237(8) -.0017(6) .0107(7) .0013(6) P1 .0183(2) .0200(2) .0236(2) -.00244(16) .01033(16) .00006(16) C111 .0170(7) .0229(8) .0222(8) -.0001(6) .0080(6) .0004(6) C112 .0256(9) .0223(9) .0291(9) -.0017(7) .0115(7) -.0021(7) C113 .0288(9) .0297(10) .0243(9) .0036(7) .0081(7) -.0039(7) C114 .0293(9) .0341(10) .0222(8) .0064(8) .0104(7) .0037(7) C115 .0297(9) .0278(9) .0270(9) .0001(7) .0129(7) .0042(7) C116 .0244(8) .0254(9) .0231(8) -.0041(7) .0090(7) -.0018(7) C121 .0210(8) .0197(8) .0220(8) -.0021(6) .0116(6) .0002(6) C122 .0198(8) .0249(9) .0232(8) -.0012(6) .0080(7) .0028(6) C123 .0296(9) .0239(9) .0291(9) .0039(7) .0152(7) .0041(7) C124 .0377(10) .0223(9) .0306(9) -.0037(7) .0188(8) -.0027(7) C125 .0247(9) .0331(10) .0300(9) -.0080(7) .0112(8) -.0082(7) C126 .0199(8) .0288(9) .0293(9) -.0008(7) .0114(7) -.0029(7) C131 .0230(8) .0189(8) .0265(8) -.0007(6) .0107(7) .0008(6) C132 .0392(11) .0406(12) .0371(11) .0113(9) .0234(10) .0127(8) C133 .0486(13) .0469(13) .0361(11) .0202(11) .0193(10) .0150(10) C134 .0304(10) .0285(10) .0380(11) .0079(8) .0072(8) -.0009(8) C135 .0237(9) .0277(10) .0424(11) .0021(7) .0150(8) -.0025(7) C136 .0246(9) .0251(9) .0299(9) -.0008(7) .0130(7) .0006(7) S .0213(2) .0196(2) .01876(19) -.00323(14) .00782(15) -.00079(14) O1 .0623(10) .0232(7) .0354(7) -.0042(6) .0337(7) -.0037(5) O2 .0215(7) .0324(8) .0539(10) -.0038(6) .0030(7) .0067(6) O3 .0365(7) .0361(8) .0215(6) .0002(6) .0136(6) .0030(5) C0 .0338(10) .0213(8) .0361(10) -.0060(7) .0202(9) -.0058(7) # 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 Ag N1a . . 2.1886(14) ? Ag P1 . . 2.3659(5) ? Ag O1 . . 2.4802(18) ? Ag O2 . '7 556' 2.6665(15) ? N1a C2a . . 1.324(3) ? N1a C5a . . 1.382(3) ? C2a N3a . . 1.343(2) ? C2a H2a . . .93(3) ? N3a C31a . . 1.463(3) ? N3a C4a . . 1.379(3) ? C31a H31a1 . . .93(4) ? C31a H31a2 . . .90(4) ? C31a H31a3 . . .94(4) ? C4a C5a . . 1.356(3) ? C4a H4a . . .98(3) ? C5a H5a . . .91(3) ? P1 C111 . . 1.820(2) ? P1 C121 . . 1.8284(18) ? P1 C131 . . 1.8275(17) ? C111 C112 . . 1.401(3) ? C111 C116 . . 1.392(3) ? C112 C113 . . 1.386(3) ? C112 H112 . . .92(3) ? C113 C114 . . 1.388(3) ? C113 H113 . . .94(3) ? C114 C115 . . 1.388(3) ? C114 H114 . . .94(3) ? C115 C116 . . 1.393(3) ? C115 H115 . . 1.02(3) ? C116 H116 . . .93(2) ? C121 C122 . . 1.400(3) ? C121 C126 . . 1.396(2) ? C122 C123 . . 1.392(3) ? C122 H122 . . .922(14) ? C123 C124 . . 1.392(3) ? C123 H123 . . .91(3) ? C124 C125 . . 1.384(3) ? C124 H124 . . .93(2) ? C125 C126 . . 1.391(3) ? C125 H125 . . .95(2) ? C126 H126 . . .95(2) ? C131 C132 . . 1.396(3) ? C131 C136 . . 1.392(3) ? C132 C133 . . 1.389(3) ? C132 H132 . . .95(3) ? C133 C134 . . 1.384(4) ? C133 H133 . . 1.01(3) ? C134 C135 . . 1.383(3) ? C134 H134 . . .92(2) ? C135 C136 . . 1.396(2) ? C135 H135 . . .99(4) ? C136 H136 . . .92(3) ? S O1 . . 1.463(2) ? S O3 . . 1.4486(14) ? S C0 . . 1.762(2) ? S O2 . . 1.4570(15) ? C0 H1a . . 1.01(3) ? C0 H1b . . .90(3) ? C0 H1c . . .99(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 N1a Ag P1 . . . 144.29(5) ? N1a Ag O1 . . . 85.87(6) ? N1a Ag O2 . . '7 556' 103.29(5) ? P1 Ag O1 . . . 118.55(4) ? P1 Ag O2 . . '7 556' 96.08(4) ? O1 Ag O2 . . '7 556' 103.50(6) ? Ag N1a C2a . . . 127.50(15) ? Ag N1a C5a . . . 125.58(13) ? C2a N1a C5a . . . 105.59(16) ? N1a C2a N3a . . . 111.4(2) ? N1a C2a H2a . . . 126.5(14) ? N3a C2a H2a . . . 122.1(14) ? C2a N3a C31a . . . 125.8(2) ? C2a N3a C4a . . . 107.34(17) ? C31a N3a C4a . . . 126.81(19) ? N3a C31a H31a1 . . . 110.5(18) ? N3a C31a H31a2 . . . 109(3) ? N3a C31a H31a3 . . . 110(3) ? H31a1 C31a H31a2 . . . 106(4) ? H31a1 C31a H31a3 . . . 110(3) ? H31a2 C31a H31a3 . . . 111(3) ? N3a C4a C5a . . . 106.11(18) ? N3a C4a H4a . . . 121.8(19) ? C5a C4a H4a . . . 131.7(19) ? N1a C5a C4a . . . 109.6(2) ? N1a C5a H5a . . . 119.7(15) ? C4a C5a H5a . . . 130.7(15) ? Ag P1 C111 . . . 110.14(5) ? Ag P1 C121 . . . 121.90(7) ? Ag P1 C131 . . . 112.37(6) ? C111 P1 C121 . . . 103.24(8) ? C111 P1 C131 . . . 103.81(9) ? C121 P1 C131 . . . 103.61(7) ? P1 C111 C112 . . . 118.20(15) ? P1 C111 C116 . . . 123.04(14) ? C112 C111 C116 . . . 118.7(2) ? C111 C112 C113 . . . 120.93(19) ? C111 C112 H112 . . . 121.8(18) ? C113 C112 H112 . . . 117.2(17) ? C112 C113 C114 . . . 119.82(18) ? C112 C113 H113 . . . 121.2(18) ? C114 C113 H113 . . . 118.9(18) ? C113 C114 C115 . . . 119.8(2) ? C113 C114 H114 . . . 119.8(15) ? C115 C114 H114 . . . 120.3(15) ? C114 C115 C116 . . . 120.3(2) ? C114 C115 H115 . . . 119.8(16) ? C116 C115 H115 . . . 119.8(16) ? C111 C116 C115 . . . 120.29(17) ? C111 C116 H116 . . . 120.7(16) ? C115 C116 H116 . . . 119.0(16) ? P1 C121 C122 . . . 118.24(11) ? P1 C121 C126 . . . 122.33(14) ? C122 C121 C126 . . . 119.29(16) ? C121 C122 C123 . . . 119.99(15) ? C121 C122 H122 . . . 122.1(12) ? C123 C122 H122 . . . 117.4(11) ? C122 C123 C124 . . . 120.29(18) ? C122 C123 H123 . . . 122.7(14) ? C124 C123 H123 . . . 116.9(14) ? C123 C124 C125 . . . 119.80(18) ? C123 C124 H124 . . . 118.3(14) ? C125 C124 H124 . . . 121.9(14) ? C124 C125 C126 . . . 120.31(16) ? C124 C125 H125 . . . 120.3(16) ? C126 C125 H125 . . . 119.4(17) ? C121 C126 C125 . . . 120.30(17) ? C121 C126 H126 . . . 120.3(12) ? C125 C126 H126 . . . 119.4(12) ? P1 C131 C132 . . . 118.01(18) ? P1 C131 C136 . . . 122.89(14) ? C132 C131 C136 . . . 119.09(17) ? C131 C132 C133 . . . 120.1(3) ? C131 C132 H132 . . . 118.3(13) ? C133 C132 H132 . . . 121.5(14) ? C132 C133 C134 . . . 120.5(2) ? C132 C133 H133 . . . 118.5(18) ? C134 C133 H133 . . . 121.0(18) ? C133 C134 C135 . . . 119.8(2) ? C133 C134 H134 . . . 118(2) ? C135 C134 H134 . . . 122(2) ? C134 C135 C136 . . . 120.1(2) ? C134 C135 H135 . . . 120.6(14) ? C136 C135 H135 . . . 119.2(14) ? C131 C136 C135 . . . 120.4(2) ? C131 C136 H136 . . . 119.6(16) ? C135 C136 H136 . . . 120.0(16) ? O1 S O3 . . . 111.62(9) ? O1 S C0 . . . 105.57(12) ? O1 S O2 . . . 112.27(10) ? O3 S C0 . . . 107.49(9) ? O3 S O2 . . . 113.15(11) ? C0 S O2 . . . 106.17(9) ? Ag O1 S . . . 121.48(8) ? Ag O2 S . '7 556' '7 556' 137.71(9) ? S C0 H1a . . . 107.2(14) ? S C0 H1b . . . 110(2) ? S C0 H1c . . . 110.7(15) ? H1a C0 H1b . . . 113(2) ? H1a C0 H1c . . . 108(3) ? H1b C0 H1c . . . 108(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 Ag C2a 3.1731(18) . . ? Ag C5a 3.1971(18) . . ? Ag C111 3.446(2) . . ? Ag C112 3.602(2) . . ? Ag C121 3.6759(16) . . ? Ag C131 3.4969(18) . . ? Ag S 3.4755(6) . . ? Ag S 3.8705(5) . '7 556' ? Ag C0 3.474(3) . . ? Ag H2a 3.37(2) . . ? Ag H5a 3.27(2) . . ? Ag H112 3.12(3) . . ? Ag H1c 2.98(4) . . ? N1a N3a 2.203(2) . . ? N1a C4a 2.238(2) . . ? N1a O1 3.188(2) . . ? N1a H2a 2.02(3) . . ? N1a H5a 1.99(3) . . ? C2a C31a 2.499(3) . . ? C2a C4a 2.193(3) . . ? C2a C5a 2.156(3) . . ? C2a H31a1 2.64(3) . . ? N3a C5a 2.186(3) . . ? N3a H2a 2.00(3) . . ? N3a H31a1 1.99(4) . . ? N3a H31a2 1.95(4) . . ? N3a H31a3 1.99(4) . . ? N3a H4a 2.07(3) . . ? C31a C4a 2.541(4) . . ? C4a H31a3 2.66(4) . . ? C4a H5a 2.07(2) . . ? C5a H4a 2.14(2) . . ? C5a H123 2.68(2) . '1 545' ? P1 C112 2.773(2) . . ? P1 C116 2.831(2) . . ? P1 C122 2.779(2) . . ? P1 C126 2.8325(18) . . ? P1 C132 2.772(2) . . ? P1 C136 2.835(2) . . ? P1 O1 4.166(2) . . ? P1 O2 3.7476(17) . '7 556' ? P1 H112 2.87(3) . . ? P1 H116 2.95(2) . . ? P1 H122 2.878(18) . . ? P1 H126 2.95(2) . . ? P1 H132 2.82(2) . . ? P1 H136 2.93(3) . . ? P1 H1a 3.67(3) . . ? P1 H1c 3.63(4) . . ? C111 C113 2.425(3) . . ? C111 C114 2.797(3) . . ? C111 C115 2.415(3) . . ? C111 C121 2.860(3) . . ? C111 C131 2.871(2) . . ? C111 H112 2.04(2) . . ? C111 H116 2.03(2) . . ? C111 H136 2.61(2) . . ? C112 C114 2.400(3) . . ? C112 C115 2.768(3) . . ? C112 C116 2.403(3) . . ? C112 H113 2.04(3) . . ? C113 C115 2.403(3) . . ? C113 C116 2.783(3) . . ? C113 H112 1.98(3) . . ? C113 H114 2.02(3) . . ? C114 C116 2.413(3) . . ? C114 H113 2.02(3) . . ? C114 H115 2.09(3) . . ? C115 H114 2.03(3) . . ? C115 H116 2.02(2) . . ? C116 H115 2.10(3) . . ? C121 C123 2.417(3) . . ? C121 C124 2.794(3) . . ? C121 C125 2.417(2) . . ? C121 C131 2.873(3) . . ? C121 H116 2.63(3) . . ? C121 H122 2.045(16) . . ? C121 H126 2.05(2) . . ? C122 C124 2.415(2) . . ? C122 C125 2.783(2) . . ? C122 C126 2.413(2) . . ? C122 H123 2.03(3) . . ? C123 C125 2.402(3) . . ? C123 C126 2.778(3) . . ? C123 H122 1.992(16) . . ? C123 H124 2.01(2) . . ? C124 C126 2.407(3) . . ? C124 H123 1.98(2) . . ? C124 H125 2.04(2) . . ? C125 H124 2.04(2) . . ? C125 H126 2.03(2) . . ? C126 H125 2.03(2) . . ? C131 C133 2.413(3) . . ? C131 C134 2.792(3) . . ? C131 C135 2.419(3) . . ? C131 H126 2.61(2) . . ? C131 H132 2.03(3) . . ? C131 H136 2.01(3) . . ? C132 C134 2.407(4) . . ? C132 C135 2.776(4) . . ? C132 C136 2.403(4) . . ? C132 H133 2.07(2) . . ? C133 C135 2.394(4) . . ? C133 C136 2.770(3) . . ? C133 H132 2.05(3) . . ? C133 H134 1.99(3) . . ? C134 C136 2.407(3) . . ? C134 H133 2.09(4) . . ? C134 H135 2.07(4) . . ? C135 H134 2.03(2) . . ? C135 H136 2.02(2) . . ? C136 H135 2.07(3) . . ? S H4a 2.86(2) . '7 546' ? S H1a 2.28(3) . . ? S H1b 2.24(3) . . ? S H1c 2.30(3) . . ? O1 O2 2.424(3) . . ? O1 O3 2.408(2) . . ? O1 C0 2.575(2) . . ? O1 H4a 2.59(3) . '7 546' ? O1 H5a 2.769(19) . . ? O1 H1a 2.72(2) . . ? O1 H1c 2.81(3) . . ? O2 O3 2.4250(18) '7 556' '7 556' ? O2 C0 2.580(3) '7 556' '7 556' ? O2 H31a3 2.86(4) '7 556' '1 565' ? O2 H122 2.603(16) '7 556' . ? O2 H1b 2.78(3) '7 556' '7 556' ? O2 H1c 2.78(3) '7 556' '7 556' ? O2 H1c 2.71(3) '7 556' . ? O3 C0 2.596(3) . . ? O3 H2a 2.47(3) . 4 ? O3 H31a3 2.67(4) . '7 546' ? O3 H4a 2.88(2) . '7 546' ? O3 H134 2.59(2) . '2 656' ? O3 H1a 2.81(3) . . ? O3 H1b 2.78(3) . . ? H31a1 H31a2 1.46(5) . . ? H31a1 H31a3 1.53(6) . . ? H31a2 H31a3 1.52(5) . . ? H112 H113 2.30(4) . . ? H113 H114 2.31(4) . . ? H114 H115 2.37(4) . . ? H115 H116 2.35(4) . . ? H122 H123 2.31(3) . . ? H123 H124 2.25(3) . . ? H124 H125 2.36(4) . . ? H125 H126 2.32(3) . . ? H132 H133 2.37(3) . . ? H133 H133 2.27(5) . '2 656' ? H133 H134 2.34(5) . . ? H134 H135 2.38(4) . . ? H135 H136 2.34(3) . . ? H1a H1b 1.60(4) . . ? H1a H1c 1.61(3) . . ? H1b H1c 1.53(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 [(Ph3P)AgSO3CH3(C4H6N2)]2 _exptl_crystal_F_000 2224 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 39 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -25 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 12.968 _diffrn_reflns_av_sigmaI/netI .02 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .027 _refine_ls_wR_factor_all .034 _refine_ls_goodness_of_fit_all 1.057 _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-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_cp6 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C42 H38 Ag2 N6 O4 P2' _chemical_formula_moiety ? _chemical_formula_weight 968.49 _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 11.972(5) _cell_length_b 10.496(6) _cell_length_c 17.976(17) _cell_angle_alpha 90.00000 _cell_angle_beta 111.24(6) _cell_angle_gamma 90.00000 _cell_volume 2105(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 17.2 _cell_measurement_theta_max 23.9 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.054 _exptl_crystal_description prism _exptl_crystal_size_max 1.10 _exptl_crystal_size_mid .80 _exptl_crystal_size_min .60 _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 .41 _exptl_absorpt_correction_T_max .56 _diffrn_reflns_number 10291 _reflns_number_total 3700 _reflns_Friedel_coverage ? _reflns_number_gt 3105 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .058 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 14 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .037 _refine_ls_wR_factor_ref .054 _refine_ls_goodness_of_fit_ref 1.61 _refine_ls_number_reflns 3105 _refine_ls_number_parameters 263 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .032 _refine_diff_density_min -.78 _refine_diff_density_max .62 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 3687(710) _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 84 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 76 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 4 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .090027 .094971 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 8 .007996 .005981 '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 Ag .62971(4) .55176(4) .46069(5) .0749(3) Uani ? ? .911(2) ? ? Ag1' .6574(4) .5270(4) .5014(4) .0667(14) Uiso ? ? .089(2) ? ? N1a .6667(3) .3720(3) .40838(17) .0739(16) Uani ? ? 1.00000 ? ? C2a .6153(3) .3391(4) .3338(2) .079(2) Uani ? ? 1.00000 ? ? N3a .6618(3) .2327(3) .31825(17) .0797(17) Uani ? ? 1.00000 ? ? C4a .7490(4) .1949(4) .3865(2) .082(2) Uani ? ? 1.00000 ? ? C5a .7515(4) .2808(4) .4411(2) .081(2) Uani ? ? 1.00000 ? ? P1 .75971(6) .72426(7) .51863(5) .0566(4) Uani ? ? 1.00000 ? ? C111 .8985(3) .6832(3) .59964(19) .0669(16) Uani ? ? 1.00000 ? ? C112 .9471(5) .5645(4) .5963(3) .101(3) Uani ? ? 1.00000 ? ? C113 1.0533(5) .5259(7) .6556(4) .132(4) Uani ? ? 1.00000 ? ? C114 1.1077(4) .6033(8) .7167(4) .123(4) Uani ? ? 1.00000 ? ? C115 1.0624(4) .7230(6) .7216(2) .105(3) Uani ? ? 1.00000 ? ? C116 .9558(3) .7615(4) .6623(2) .080(2) Uani ? ? 1.00000 ? ? C121 .8070(3) .7964(3) .44278(17) .0565(14) Uani ? ? 1.00000 ? ? C122 .7224(3) .8064(4) .3657(2) .077(2) Uani ? ? 1.00000 ? ? C123 .7528(4) .8582(4) .3057(2) .087(2) Uani ? ? 1.00000 ? ? C124 .8659(4) .8979(4) .3191(2) .081(2) Uani ? ? 1.00000 ? ? C125 .9505(3) .8876(5) .3938(2) .088(2) Uani ? ? 1.00000 ? ? C126 .9214(3) .8380(4) .4557(2) .0756(18) Uani ? ? 1.00000 ? ? C131 .6961(2) .8540(3) .55734(16) .0539(13) Uani ? ? 1.00000 ? ? C132 .6302(3) .8237(4) .6034(2) .085(2) Uani ? ? 1.00000 ? ? C133 .5790(4) .9179(5) .6340(3) .103(3) Uani ? ? 1.00000 ? ? C134 .5893(3) 1.0427(4) .6167(2) .081(2) Uani ? ? 1.00000 ? ? C135 .6524(4) 1.0738(4) .5697(2) .079(2) Uani ? ? 1.00000 ? ? C136 .7050(3) .9810(3) .54038(19) .0679(17) Uani ? ? 1.00000 ? ? N .3695(4) .5942(4) .3595(2) .094(2) Uani ? ? 1.00000 ? ? O1 .4153(4) .5587(4) .4256(2) .131(3) Uani ? ? 1.00000 ? ? O2 .4447(3) .6162(3) .32758(17) .098(2) Uani ? ? .911(2) ? ? O2' .284(3) .613(3) .345(2) .090(9) Uiso ? ? .089(2) ? ? H2 .55338 .38909 .29338 .09400 Uiso ? ? 1.00000 ? ? H3 .63549 .18599 .26797 .09600 Uiso ? ? 1.00000 ? ? H4 .80216 .12324 .39473 .09700 Uiso ? ? 1.00000 ? ? H5 .80756 .28245 .49573 .09300 Uiso ? ? 1.00000 ? ? H112 .90650 .51122 .55371 .12600 Uiso ? ? 1.00000 ? ? H113 1.08213 .43978 .64868 .16000 Uiso ? ? 1.00000 ? ? H114 1.17867 .57155 .75456 .15300 Uiso ? ? 1.00000 ? ? H115 1.10919 .77500 .76519 .13000 Uiso ? ? 1.00000 ? ? H116 .92010 .84527 .66636 .09700 Uiso ? ? 1.00000 ? ? H122 .64217 .77247 .35356 .09000 Uiso ? ? 1.00000 ? ? H123 .69244 .86923 .25221 .11000 Uiso ? ? 1.00000 ? ? H124 .88598 .93523 .27808 .10100 Uiso ? ? 1.00000 ? ? H125 1.03141 .90956 .40223 .11000 Uiso ? ? 1.00000 ? ? H126 .98292 .83289 .50781 .08800 Uiso ? ? 1.00000 ? ? H132 .61823 .73591 .61425 .10300 Uiso ? ? 1.00000 ? ? H133 .53554 .89653 .66700 .11500 Uiso ? ? 1.00000 ? ? H134 .55461 1.10776 .63859 .09600 Uiso ? ? 1.00000 ? ? H135 .65638 1.16046 .55515 .09000 Uiso ? ? 1.00000 ? ? H136 .75074 1.00647 .50846 .07900 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 Ag .0816(3) .0558(2) .0873(5) -.01632(14) .0304(3) -.0073(2) N1a .0812(18) .0622(17) .0804(19) -.0033(14) .0318(15) -.0018(15) C2a .071(2) .077(2) .083(2) -.0030(18) .0224(18) -.001(2) N3a .081(2) .082(2) .081(2) -.0164(16) .0365(16) -.0207(16) C4a .093(2) .064(2) .091(3) .0002(19) .037(2) -.004(2) C5a .102(3) .063(2) .074(2) -.002(2) .0272(19) .0006(19) P1 .0524(4) .0509(4) .0627(5) -.0044(3) .0162(3) .0022(4) C111 .0572(16) .072(2) .0691(19) .0025(16) .0201(14) .0215(17) C112 .090(3) .087(3) .114(3) .022(2) .023(2) .019(2) C113 .094(4) .134(5) .155(5) .047(3) .029(4) .061(4) C114 .067(3) .178(6) .117(4) .019(3) .024(3) .075(4) C115 .069(2) .156(5) .076(2) -.015(3) .0109(18) .029(3) C116 .0646(19) .103(3) .0640(18) -.0082(19) .0128(15) .016(2) C121 .0556(16) .0506(16) .0620(16) .0004(13) .0196(13) -.0040(14) C122 .0648(19) .094(3) .0644(19) -.0066(18) .0143(15) -.0028(19) C123 .095(3) .106(3) .0558(18) -.000(2) .0220(17) .002(2) C124 .105(3) .075(2) .078(2) .009(2) .051(2) .004(2) C125 .073(2) .104(3) .094(3) -.016(2) .039(2) .006(2) C126 .0617(18) .086(2) .073(2) -.0135(17) .0176(15) .0048(19) C131 .0475(14) .0571(17) .0509(14) -.0058(12) .0103(11) .0037(13) C132 .087(2) .076(2) .105(3) -.002(2) .051(2) .010(2) C133 .106(3) .105(4) .131(4) -.009(3) .081(3) -.008(3) C134 .069(2) .089(3) .085(2) .0044(18) .0269(18) -.016(2) C135 .092(3) .064(2) .081(2) .0039(18) .030(2) -.0072(19) C136 .081(2) .061(2) .0670(18) -.0023(17) .0336(16) -.0017(16) N .090(3) .088(2) .094(3) -.004(2) .022(2) .004(2) O1 .111(3) .184(4) .096(2) -.016(2) .0356(19) .046(2) O2 .095(2) .109(3) .0813(18) .0008(19) .0207(16) .0203(17) # 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 Ag Ag' . . .733(6) ? Ag N1a . . 2.223(3) ? Ag P1 . . 2.3687(12) ? Ag O1 . . 2.412(4) ? Ag O2 . . 2.692(3) ? Ag O1 . '3 666' 2.571(5) ? Ag' N1a . . 2.365(7) ? Ag' P1 . . 2.369(4) ? Ag' O1 . . 2.739(6) ? Ag' O1 . '3 666' 2.028(8) ? N1a C2a . . 1.303(5) ? N1a C5a . . 1.364(5) ? C2a N3a . . 1.322(5) ? C2a H2 . . .981(3) ? N3a C4a . . 1.350(4) ? N3a H3 . . .975(3) ? C4a C5a . . 1.325(6) ? C4a H4 . . .962(4) ? C5a H5 . . .968(3) ? P1 C111 . . 1.821(3) ? P1 C121 . . 1.820(4) ? P1 C131 . . 1.817(3) ? C111 C112 . . 1.385(6) ? C111 C116 . . 1.363(5) ? C112 C113 . . 1.391(7) ? C112 H112 . . .930(5) ? C113 C114 . . 1.331(9) ? C113 H113 . . .991(7) ? C114 C115 . . 1.383(10) ? C114 H114 . . .937(5) ? C115 C116 . . 1.394(5) ? C115 H115 . . .952(5) ? C116 H116 . . .992(4) ? C121 C122 . . 1.393(4) ? C121 C126 . . 1.374(5) ? C122 C123 . . 1.368(6) ? C122 H122 . . .972(4) ? C123 C124 . . 1.353(7) ? C123 H123 . . .978(3) ? C124 C125 . . 1.361(5) ? C124 H124 . . .940(5) ? C125 C126 . . 1.383(6) ? C125 H125 . . .953(4) ? C126 H126 . . .961(3) ? C131 C132 . . 1.372(6) ? C131 C136 . . 1.381(5) ? C132 C133 . . 1.379(7) ? C132 H132 . . .963(4) ? C133 C134 . . 1.362(7) ? C133 H133 . . .947(6) ? C134 C135 . . 1.362(7) ? C134 H134 . . .955(5) ? C135 C136 . . 1.365(6) ? C135 H135 . . .952(4) ? C136 H136 . . .963(4) ? N O1 . . 1.175(5) ? N O2 . . 1.251(7) ? N O2' . . .98(4) ? O1 O2' . . 1.80(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 Ag' Ag N1a . . . 92.0(4) ? Ag' Ag P1 . . . 81.1(3) ? Ag' Ag O1 . . . 108.9(4) ? Ag' Ag O2 . . . 154.8(4) ? Ag' Ag O1 . . '3 666' 36.4(4) ? N1a Ag P1 . . . 129.41(9) ? N1a Ag O1 . . . 105.75(13) ? N1a Ag O2 . . . 93.61(11) ? N1a Ag O1 . . '3 666' 94.85(14) ? P1 Ag O1 . . . 124.00(11) ? P1 Ag O2 . . . 113.39(9) ? P1 Ag O1 . . '3 666' 106.79(11) ? O1 Ag O2 . . . 45.98(13) ? O1 Ag O1 . . '3 666' 73.24(13) ? O2 Ag O1 . . '3 666' 118.53(13) ? Ag Ag' N1a . . . 70.0(4) ? Ag Ag' P1 . . . 81.1(3) ? Ag Ag' O1 . . . 56.4(3) ? Ag Ag' O1 . . '3 666' 131.2(4) ? N1a Ag' P1 . . . 122.6(3) ? N1a Ag' O1 . . . 92.6(2) ? N1a Ag' O1 . . '3 666' 107.1(2) ? P1 Ag' O1 . . . 111.25(18) ? P1 Ag' O1 . . '3 666' 128.8(3) ? O1 Ag' O1 . . '3 666' 75.6(2) ? Ag N1a Ag' . . . 18.06(13) ? Ag N1a C2a . . . 124.6(2) ? Ag N1a C5a . . . 130.1(2) ? Ag' N1a C2a . . . 141.7(3) ? Ag' N1a C5a . . . 113.3(3) ? C2a N1a C5a . . . 105.0(3) ? N1a C2a N3a . . . 111.3(3) ? N1a C2a H2 . . . 124.6(4) ? N3a C2a H2 . . . 124.0(4) ? C2a N3a C4a . . . 107.6(3) ? C2a N3a H3 . . . 126.9(3) ? C4a N3a H3 . . . 125.4(4) ? N3a C4a C5a . . . 106.1(4) ? N3a C4a H4 . . . 128.3(4) ? C5a C4a H4 . . . 125.6(4) ? N1a C5a C4a . . . 110.1(3) ? N1a C5a H5 . . . 124.0(4) ? C4a C5a H5 . . . 125.8(4) ? Ag P1 Ag' . . . 17.81(15) ? Ag P1 C111 . . . 115.75(12) ? Ag P1 C121 . . . 108.76(11) ? Ag P1 C131 . . . 116.20(10) ? Ag' P1 C111 . . . 100.16(16) ? Ag' P1 C121 . . . 123.5(2) ? Ag' P1 C131 . . . 115.88(18) ? C111 P1 C121 . . . 104.84(16) ? C111 P1 C131 . . . 105.00(15) ? C121 P1 C131 . . . 105.22(15) ? P1 C111 C112 . . . 117.0(3) ? P1 C111 C116 . . . 124.0(3) ? C112 C111 C116 . . . 119.0(3) ? C111 C112 C113 . . . 120.7(5) ? C111 C112 H112 . . . 118.3(4) ? C113 C112 H112 . . . 121.0(5) ? C112 C113 C114 . . . 119.5(6) ? C112 C113 H113 . . . 115.7(6) ? C114 C113 H113 . . . 124.8(6) ? C113 C114 C115 . . . 121.4(5) ? C113 C114 H114 . . . 115.2(8) ? C115 C114 H114 . . . 123.3(6) ? C114 C115 C116 . . . 119.0(4) ? C114 C115 H115 . . . 116.5(4) ? C116 C115 H115 . . . 124.4(6) ? C111 C116 C115 . . . 120.3(4) ? C111 C116 H116 . . . 119.6(3) ? C115 C116 H116 . . . 120.1(4) ? P1 C121 C122 . . . 117.7(3) ? P1 C121 C126 . . . 124.5(2) ? C122 C121 C126 . . . 117.7(3) ? C121 C122 C123 . . . 120.6(3) ? C121 C122 H122 . . . 119.9(4) ? C123 C122 H122 . . . 119.5(3) ? C122 C123 C124 . . . 121.1(3) ? C122 C123 H123 . . . 120.6(4) ? C124 C123 H123 . . . 118.2(4) ? C123 C124 C125 . . . 119.3(4) ? C123 C124 H124 . . . 120.9(3) ? C125 C124 H124 . . . 119.8(4) ? C124 C125 C126 . . . 120.6(4) ? C124 C125 H125 . . . 119.2(5) ? C126 C125 H125 . . . 120.0(3) ? C121 C126 C125 . . . 120.6(3) ? C121 C126 H126 . . . 120.8(4) ? C125 C126 H126 . . . 118.5(4) ? P1 C131 C132 . . . 118.0(3) ? P1 C131 C136 . . . 124.2(3) ? C132 C131 C136 . . . 117.7(3) ? C131 C132 C133 . . . 120.7(4) ? C131 C132 H132 . . . 120.3(4) ? C133 C132 H132 . . . 119.0(5) ? C132 C133 C134 . . . 120.6(5) ? C132 C133 H133 . . . 120.3(5) ? C134 C133 H133 . . . 119.2(6) ? C133 C134 C135 . . . 119.3(5) ? C133 C134 H134 . . . 120.3(5) ? C135 C134 H134 . . . 120.4(4) ? C134 C135 C136 . . . 120.4(4) ? C134 C135 H135 . . . 119.5(5) ? C136 C135 H135 . . . 120.0(5) ? C131 C136 C135 . . . 121.4(4) ? C131 C136 H136 . . . 120.4(4) ? C135 C136 H136 . . . 118.2(4) ? O1 N O2 . . . 111.9(4) ? O1 N O2' . . . 113(2) ? O2 N O2' . . . 134(2) ? Ag O1 Ag' . . . 14.67(15) ? Ag O1 N . . . 109.7(4) ? Ag O1 O2' . . . 139.0(14) ? Ag O1 Ag . . '3 666' 106.76(13) ? Ag O1 Ag' . . '3 666' 118.9(2) ? Ag' O1 N . . . 124.3(4) ? Ag' O1 O2' . . . 153.6(14) ? Ag' O1 Ag . . '3 666' 92.20(18) ? Ag' O1 Ag' . . '3 666' 104.4(2) ? N O1 O2' . . . 30.0(14) ? N O1 Ag . . '3 666' 142.3(4) ? N O1 Ag' . . '3 666' 130.0(4) ? O2' O1 Ag . . '3 666' 114.2(14) ? O2' O1 Ag' . . '3 666' 102.0(14) ? Ag O1 Ag' '3 666' . '3 666' 12.39(12) ? Ag O2 N . . . 92.5(2) ? N O2' O1 . . . 36.8(12) ? 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 Ag Ag 4.0005(18) . '3 666' ? Ag Ag' 3.828(6) . '3 666' ? Ag C2a 3.152(5) . . ? Ag C5a 3.273(4) . . ? Ag C111 3.560(3) . . ? Ag C112 3.699(5) . . ? Ag C121 3.420(3) . . ? Ag C122 3.559(5) . . ? Ag C131 3.565(3) . . ? Ag C132 3.836(5) . . ? Ag N 3.018(4) . . ? Ag N 3.574(5) . '3 666' ? Ag O2' 3.95(4) . . ? Ag O2' 3.70(3) . '3 666' ? Ag H2 3.287(2) . . ? Ag H5 3.4567(15) . . ? Ag H112 3.1533(14) . . ? Ag H122 3.0505(17) . . ? Ag H132 3.413(2) . . ? Ag' Ag' 3.792(7) . '3 666' ? Ag' C2a 3.482(8) . . ? Ag' C5a 3.163(7) . . ? Ag' C111 3.232(5) . . ? Ag' C112 3.288(6) . . ? Ag' C121 3.699(6) . . ? Ag' C131 3.559(6) . . ? Ag' C132 3.687(7) . . ? Ag' N 2.925(8) . '3 666' ? Ag' N 3.537(6) . . ? Ag' O2 3.990(8) . '3 666' ? Ag' O2 3.370(6) . . ? Ag' O2' 2.98(3) . '3 666' ? Ag' H5 3.157(5) . . ? Ag' H112 2.789(4) . . ? Ag' H122 3.659(6) . . ? Ag' H132 3.135(6) . . ? N1a N3a 2.168(5) . . ? N1a C4a 2.204(5) . . ? N1a H2 2.028(3) . . ? N1a H5 2.067(3) . . ? C2a C4a 2.156(5) . . ? C2a C5a 2.116(5) . . ? C2a H3 2.061(4) . . ? N3a C5a 2.138(5) . . ? N3a O2 2.752(5) . '2 645' ? N3a H2 2.040(3) . . ? N3a H4 2.088(3) . . ? C4a H3 2.073(4) . . ? C4a H5 2.048(4) . . ? C5a H4 2.041(4) . . ? P1 C112 2.743(5) . . ? P1 C116 2.818(3) . . ? P1 C122 2.759(5) . . ? P1 C126 2.835(4) . . ? P1 C132 2.743(5) . . ? P1 C136 2.834(4) . . ? P1 H112 2.7718(13) . . ? P1 H122 2.831(3) . . ? P1 H132 2.8192(18) . . ? C111 C113 2.412(7) . . ? C111 C114 2.753(6) . . ? C111 C115 2.391(5) . . ? C111 C121 2.885(5) . . ? C111 C131 2.886(4) . . ? C111 H112 2.001(4) . . ? C111 H116 2.044(4) . . ? C112 C114 2.352(7) . . ? C112 C115 2.738(7) . . ? C112 C116 2.368(7) . . ? C112 H113 2.027(5) . . ? C113 C115 2.368(10) . . ? C113 C116 2.756(8) . . ? C113 H112 2.033(6) . . ? C113 H114 1.927(6) . . ? C114 C116 2.394(8) . . ? C114 H113 2.064(8) . . ? C114 H115 1.999(8) . . ? C115 H114 2.053(6) . . ? C115 H116 2.077(5) . . ? C116 H115 2.086(3) . . ? C121 C123 2.399(5) . . ? C121 C124 2.777(6) . . ? C121 C125 2.396(6) . . ? C121 C131 2.889(5) . . ? C121 H122 2.058(3) . . ? C121 H126 2.041(3) . . ? C121 H136 2.700(3) . . ? C122 C124 2.370(7) . . ? C122 C125 2.727(6) . . ? C122 C126 2.369(4) . . ? C122 H123 2.048(4) . . ? C123 C125 2.343(5) . . ? C123 C126 2.729(5) . . ? C123 H122 2.031(5) . . ? C123 H124 2.005(5) . . ? C124 C126 2.384(6) . . ? C124 H123 2.010(4) . . ? C124 H125 2.007(4) . . ? C125 H124 2.002(4) . . ? C125 H126 2.027(5) . . ? C126 H125 2.035(4) . . ? C131 C133 2.391(7) . . ? C131 C134 2.772(6) . . ? C131 C135 2.394(5) . . ? C131 H116 2.689(3) . . ? C131 H132 2.036(3) . . ? C131 H136 2.044(3) . . ? C132 C134 2.380(6) . . ? C132 C135 2.729(6) . . ? C132 C136 2.356(6) . . ? C132 H133 2.029(5) . . ? C133 C135 2.350(7) . . ? C133 C136 2.718(8) . . ? C133 H132 2.029(6) . . ? C133 H134 2.020(6) . . ? C134 C136 2.366(7) . . ? C134 H133 2.002(5) . . ? C134 H135 2.010(5) . . ? C135 H134 2.021(5) . . ? C135 H136 2.008(5) . . ? C136 H135 2.017(4) . . ? N H3 2.466(5) . '2 655' ? O1 O1 2.975(5) . '3 666' ? O1 O2 2.010(6) . . ? O2 O2' 2.06(4) . . ? O2 H3 1.793(3) . '2 655' ? O2' H3 2.65(4) . '2 655' ? O2' H115 2.38(3) . '4 464' ? H112 H113 2.3015(10) . . ? H113 H114 2.2973(13) . . ? H114 H115 2.3246(11) . . ? H122 H123 2.3468(15) . . ? H123 H124 2.2987(9) . . ? H124 H125 2.2955(16) . . ? H125 H126 2.3205(16) . . ? H132 H133 2.3241(9) . . ? H133 H134 2.3050(12) . . ? H134 H135 2.3161(13) . . ? H135 H136 2.2978(8) . . ? _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 [(Ph3P)Ag(C3H4N2)(NO3)]2 _exptl_crystal_F_000 976 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 5 8 5 -5 8 -5 -5 -8 -5 5 -8 6 5 -12 6 -5 -12 6 -5 12 -6 5 12 10 0 0 0 12 0 0 0 14 -10 0 0 0 -12 0 0 0 -14 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -20 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 11.159 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression Zachariasen _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 3 _refine_ls_R_factor_all .045 _refine_ls_wR_factor_all .057 _refine_ls_goodness_of_fit_all 1.539 _refine_ls_shift/su_mean .003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end