# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1839 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-10-03 _audit_update_record ? #======================================================================= # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'J.Chem.Soc.,Dalton' _publ_requested_category ? _publ_section_title ; Macrocyclic ligand design. Interaction of selected transition and post-transition metal ions with a new O~2N~2-donor macrocycle incorporating a methylpyridyl pendant arm ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Atkinson, Ian M.' . ; School of Biomedical and Molecular Science, James Cook University, Townsville, Qld 4811, Australia ; 'Chartres, Jy D.' . ; School of Biomedical and Molecular Science, James Cook University, Townsville, Qld 4811, Australia ; 'Everett, Grover W.' . ; Chemistry Department, University of Kansas, Lawrence, Kansas 66045, USA ; ' Ji, Xue-Kui' . ; School of Chemistry, University of Sydney, NSW 2006, Australia ; ' Lindoy, Leonard F.' . ; School of Chemistry, University of Sydney, NSW 2006, Australia ; 'Matthews, Owen A.' . ; School of Biomedical and Molecular Science, James Cook University, Townsville, Qld 4811, Australia ; 'Meehan, George V.' . ; School of Biomedical and Molecular Science, James Cook University, Townsville, Qld 4811, Australia ; 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; ' Wei, Gang' . ; School of Chemistry, University of Sydney, NSW 2006, 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 ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ge2a # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C35 H41 Cu1 N5 O10.8675' _chemical_formula_moiety ? _chemical_formula_weight 777.34 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_n _symmetry_space_group_name_Hall -p_2n_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2-y,1/2+z 1/2+x,1/2-y,-z -x,+y,1/2-z -x,-y,-z 1/2+x,1/2+y,1/2-z 1/2-x,1/2+y,+z +x,-y,1/2+z _cell_length_a 20.641(9) _cell_length_b 14.447(7) _cell_length_c 24.912(12) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 7429(6) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.39 _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 15.3 _cell_measurement_theta_max 15.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .653 _exptl_crystal_description fragment _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _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 0.88 _exptl_absorpt_correction_T_max 0.93 _diffrn_reflns_number 6457 _reflns_number_total 6457 _reflns_Friedel_coverage ? _reflns_number_gt 6457 _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 ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_matrix_type atomblock #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 11328(1087) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details ? #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 2813 #ActaC _refine_ls_number_parameters 486 #ActaC _refine_ls_number_restraints 12 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .142 #ActaC _refine_ls_R_factor_gt .07 #ActaC _refine_ls_wR_factor_all .077 #ActaC _refine_ls_wR_factor_ref .066 #ActaC _refine_ls_goodness_of_fit_all 1.705 #ActaC _refine_ls_goodness_of_fit_ref 1.934 #ActaC _refine_ls_shift/su_max .09 #ActaC _refine_ls_shift/su_mean .007 #ActaC _refine_diff_density_min -.56 #ActaC _refine_diff_density_max .631 #ActaC # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _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 ? 0 280 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 88 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 376 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 8 .263001 1.266 '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 Cu .71327(5) .55238(7) .31375(4) .0454(6) Uani ? ? 1.00000 ? ? N0 .6429(3) .5483(4) .3741(3) .041(4) Uani ? ? 1.00000 ? ? C0 .6650(4) .6125(6) .4173(3) .052(6) Uani ? ? 1.00000 ? ? N01 .7660(3) .6091(4) .3706(3) .043(4) Uani ? ? 1.00000 ? ? C02 .7360(4) .6225(5) .4177(3) .043(6) Uani ? ? 1.00000 ? ? C03 .7688(4) .6512(6) .4635(3) .060(7) Uani ? ? 1.00000 ? ? C04 .8346(5) .6675(6) .4593(4) .076(8) Uani ? ? 1.00000 ? ? C05 .8651(4) .6530(6) .4112(4) .070(7) Uani ? ? 1.00000 ? ? C06 .8299(4) .6242(6) .3685(4) .058(7) Uani ? ? 1.00000 ? ? C1 .5766(4) .5756(5) .3552(3) .047(6) Uani ? ? 1.00000 ? ? C11 .5705(4) .6748(5) .3371(3) .042(6) Uani ? ? 1.00000 ? ? C12 .5305(4) .7334(6) .3672(3) .051(6) Uani ? ? 1.00000 ? ? C13 .5241(4) .8291(6) .3512(3) .051(6) Uani ? ? 1.00000 ? ? C131 .4797(4) .8926(6) .3849(4) .065(7) Uani ? ? 1.00000 ? ? C132 .4110(5) .8553(9) .3845(5) .126(11) Uani ? ? 1.00000 ? ? C133 .4786(7) .9877(8) .3626(6) .176(14) Uani ? ? 1.00000 ? ? C134 .5040(7) .9006(10) .4395(5) .154(12) Uani ? ? 1.00000 ? ? C14 .5572(4) .8582(6) .3070(3) .055(6) Uani ? ? 1.00000 ? ? C15 .5965(4) .7987(6) .2785(3) .058(7) Uani ? ? 1.00000 ? ? C16 .6037(4) .7077(6) .2944(3) .047(6) Uani ? ? 1.00000 ? ? C1' .6382(4) .4501(5) .3966(3) .050(6) Uani ? ? 1.00000 ? ? C11' .6986(4) .4168(5) .4219(3) .039(5) Uani ? ? 1.00000 ? ? C12' .7048(4) .4096(5) .4772(3) .047(5) Uani ? ? 1.00000 ? ? C13' .7618(4) .3824(5) .5023(3) .046(6) Uani ? ? 1.00000 ? ? C131' .7677(4) .3817(6) .5625(3) .058(7) Uani ? ? 1.00000 ? ? C132' .7177(6) .3182(8) .5864(4) .110(10) Uani ? ? 1.00000 ? ? C133' .8342(5) .3560(9) .5819(5) .113(10) Uani ? ? 1.00000 ? ? C134' .7529(7) .4760(8) .5836(5) .127(11) Uani ? ? 1.00000 ? ? C14' .8123(4) .3585(6) .4689(4) .053(6) Uani ? ? 1.00000 ? ? C15' .8085(4) .3638(5) .4132(3) .045(6) Uani ? ? 1.00000 ? ? C16' .7518(4) .3931(5) .3906(3) .043(5) Uani ? ? 1.00000 ? ? O2 .6449(3) .6502(4) .2668(2) .056(4) Uani ? ? 1.00000 ? ? C3 .6185(5) .6072(7) .2208(4) .085(8) Uani ? ? 1.00000 ? ? O2' .7497(3) .4070(3) .3362(2) .052(4) Uani ? ? 1.00000 ? ? C3' .7203(5) .3373(6) .3034(4) .076(7) Uani ? ? 1.00000 ? ? N31 .6690(3) .4697(4) .2594(3) .047(5) Uani ? ? 1.00000 ? ? C32 .6369(4) .5044(6) .2182(3) .060(6) Uani ? ? 1.00000 ? ? C33 .6176(5) .4516(8) .1751(4) .095(9) Uani ? ? 1.00000 ? ? C34 .6346(6) .3604(7) .1732(4) .101(9) Uani ? ? 1.00000 ? ? C33' .6655(6) .3215(7) .2153(4) .088(8) Uani ? ? 1.00000 ? ? C32' .6848(4) .3771(6) .2580(4) .061(7) Uani ? ? 1.00000 ? ? N10 .8161(4) .5532(6) .2395(3) .090(6) Uani ? ? 1.00000 ? ? O101 .7761(3) .5975(4) .2585(3) .073(5) Uani ? ? 1.00000 ? ? O102 .8144(4) .4693(5) .2317(4) .152(8) Uani ? ? 1.00000 ? ? O103 .8704(5) .5856(7) .2267(5) .206(11) Uani ? ? 1.00000 ? ? N20 .5119(4) .6924(9) .5403(4) .112(6) Uiso ? ? .619(6) ? ? O201 .4643(8) .6902(11) .5279(6) .211(19) Uani ? ? .619(6) ? ? O202 .5255(5) .7436(10) .5757(5) .142(13) Uani ? ? .619(6) ? ? O203 .5538(6) .6631(11) .5088(5) .189(16) Uani ? ? .619(6) ? ? N20A .5338(4) .6505(15) .5460(3) .149(12) Uiso ? ? .381(6) ? ? O201A .4993(12) .647(3) .5088(12) .40(3) Uiso ? ? .381(6) ? ? O202A .5157(6) .6354(15) .5841(8) .140(9) Uiso ? ? .381(6) ? ? O203A .5819(15) .649(2) .5399(5) .285(18) Uiso ? ? .381(6) ? ? O01 .4580(5) .6959(6) .6760(4) .158(9) Uani ? ? 1.00000 ? ? O02 .5620(4) .4512(7) .5532(3) .148(8) Uani ? ? 1.00000 ? ? O03 .50000 .8338(9) .75000 .187(14) Uani ? ? 1.00000 ? ? O04 .50000 .5630(12) .75000 .163(19) Uani ? ? .74(2) ? ? H0a .64573 .66571 .41317 .07800 Uiso ? ? 1.00000 ? ? H0b .65033 .59105 .44805 .07800 Uiso ? ? 1.00000 ? ? H03 .74871 .65850 .49398 .08000 Uiso ? ? 1.00000 ? ? H04 .85884 .68515 .48562 .10200 Uiso ? ? 1.00000 ? ? H05 .90902 .66474 .40779 .09400 Uiso ? ? 1.00000 ? ? H06 .85366 .61725 .33427 .07900 Uiso ? ? 1.00000 ? ? H1a .54638 .56102 .38481 .07000 Uiso ? ? 1.00000 ? ? H1b .56469 .53425 .32643 .07000 Uiso ? ? 1.00000 ? ? H12 .50525 .70884 .39997 .07200 Uiso ? ? 1.00000 ? ? H132a .38131 .89048 .40398 .16500 Uiso ? ? 1.00000 ? ? H132b .39508 .84890 .34770 .16500 Uiso ? ? 1.00000 ? ? H132c .40956 .79135 .39889 .16500 Uiso ? ? 1.00000 ? ? H133a .45349 1.03003 .38331 .22700 Uiso ? ? 1.00000 ? ? H133b .52253 1.01243 .36096 .22700 Uiso ? ? 1.00000 ? ? H133c .46235 .98893 .32625 .22700 Uiso ? ? 1.00000 ? ? H134a .47696 .93580 .46221 .20900 Uiso ? ? 1.00000 ? ? H134b .50190 .83493 .45681 .20900 Uiso ? ? 1.00000 ? ? H134c .54653 .91709 .44129 .20900 Uiso ? ? 1.00000 ? ? H14 .54982 .92131 .29687 .06700 Uiso ? ? 1.00000 ? ? H15 .61786 .82312 .24713 .08200 Uiso ? ? 1.00000 ? ? H1'a .60254 .44655 .42205 .07600 Uiso ? ? 1.00000 ? ? H1'b .62590 .40802 .36724 .07600 Uiso ? ? 1.00000 ? ? H12' .66681 .42354 .49990 .06200 Uiso ? ? 1.00000 ? ? H132'a .71975 .31369 .62545 .16500 Uiso ? ? 1.00000 ? ? H132'b .67391 .34056 .57863 .16500 Uiso ? ? 1.00000 ? ? H132'c .71971 .25596 .57294 .16500 Uiso ? ? 1.00000 ? ? H133'a .83946 .35611 .62021 .15200 Uiso ? ? 1.00000 ? ? H133'b .84780 .29451 .56967 .15200 Uiso ? ? 1.00000 ? ? H133'c .86669 .39840 .56760 .15200 Uiso ? ? 1.00000 ? ? H134'a .75621 .48433 .62260 .16500 Uiso ? ? 1.00000 ? ? H134'b .78280 .52395 .56908 .16500 Uiso ? ? 1.00000 ? ? H134'c .71000 .49875 .57421 .16500 Uiso ? ? 1.00000 ? ? H14' .85389 .33947 .48468 .07200 Uiso ? ? 1.00000 ? ? H15' .84588 .34594 .38916 .07600 Uiso ? ? 1.00000 ? ? H3a .57547 .61174 .21833 .10400 Uiso ? ? 1.00000 ? ? H3b .63115 .63356 .18975 .10400 Uiso ? ? 1.00000 ? ? H3'a .69613 .30066 .32392 .11700 Uiso ? ? 1.00000 ? ? H3'b .75155 .29808 .29239 .11700 Uiso ? ? 1.00000 ? ? H33 .59223 .48436 .15018 .10800 Uiso ? ? 1.00000 ? ? H34 .62352 .33287 .14175 .12500 Uiso ? ? 1.00000 ? ? H33' .67169 .26329 .21239 .11400 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 Cu .0521(6) .0312(5) .0530(6) .0006(6) .0075(7) .0020(6) N0 .047(4) .024(4) .051(4) .001(4) .003(4) .002(4) C0 .062(7) .039(6) .054(6) .007(5) .011(5) -.005(5) N01 .042(5) .030(4) .058(5) -.006(3) .006(4) .007(4) C02 .047(6) .023(5) .061(6) .006(4) -.012(5) .000(4) C03 .071(8) .037(5) .072(7) .000(5) -.000(6) -.002(5) C04 .072(8) .054(7) .101(9) -.015(6) -.028(7) -.001(6) C05 .057(7) .046(6) .108(9) -.005(5) -.000(7) .008(6) C06 .062(7) .047(6) .065(7) .001(5) -.001(6) -.004(5) C1 .047(6) .034(6) .061(6) .006(5) .003(5) .003(5) C11 .039(6) .035(5) .053(6) .007(4) -.003(5) .001(4) C12 .045(6) .052(6) .056(6) .000(5) .003(5) .008(5) C13 .041(6) .039(6) .072(7) .012(5) -.013(5) -.000(5) C131 .079(8) .044(6) .071(7) .025(6) .000(6) -.005(5) C132 .065(8) .130(11) .182(14) .016(8) .040(9) -.062(10) C133 .207(16) .065(9) .256(18) .077(10) .124(15) .042(11) C134 .174(13) .180(14) .107(11) .125(12) -.033(10) -.063(10) C14 .070(7) .046(6) .048(6) .010(5) .001(6) .008(5) C15 .072(7) .057(6) .045(6) .002(6) .002(6) .021(5) C16 .052(6) .045(6) .044(6) .013(5) .005(5) .003(5) C1' .066(6) .024(5) .060(6) -.011(5) .007(5) .016(5) C11' .037(6) .022(5) .058(6) -.010(4) -.004(5) .006(4) C12' .066(6) .025(4) .050(6) -.013(5) -.001(6) .011(4) C13' .057(6) .035(5) .047(5) -.009(5) .001(5) .001(4) C131' .064(7) .042(6) .068(7) -.007(5) -.010(6) .004(5) C132' .150(12) .112(10) .067(8) -.030(10) .015(9) .020(7) C133' .084(9) .155(12) .100(10) .017(9) -.025(8) .025(9) C134' .179(13) .093(10) .108(10) -.001(9) -.033(11) -.037(8) C14' .042(6) .042(6) .076(7) -.007(5) -.009(5) .012(5) C15' .049(6) .025(5) .060(6) .007(4) .007(5) .006(5) C16' .069(6) .014(4) .045(5) .003(4) .005(5) .006(4) O2 .066(4) .047(4) .054(4) .014(3) .009(4) .003(3) C3 .113(9) .095(8) .047(6) .055(8) .002(7) .009(6) O2' .068(4) .034(3) .053(4) .003(3) .012(4) .005(3) C3' .116(9) .041(6) .070(7) .001(6) -.026(7) .001(5) N31 .051(5) .044(5) .044(5) -.006(4) .008(4) .000(4) C32 .075(7) .065(6) .040(6) .016(6) .004(6) -.002(5) C33 .093(9) .140(11) .051(7) .019(8) -.018(6) -.001(8) C34 .127(11) .084(9) .092(9) .030(8) -.026(8) -.028(8) C33' .131(10) .055(7) .077(8) .001(7) -.022(8) -.023(6) C32' .075(7) .040(6) .068(7) .004(5) .017(6) -.013(5) N10 .121(7) .084(6) .066(6) -.035(6) .023(5) -.004(6) O101 .074(5) .058(4) .086(5) .000(4) .028(4) .004(4) O102 .172(9) .085(6) .201(10) .038(6) .086(8) .037(6) O103 .142(9) .175(10) .302(14) -.046(8) .128(9) -.096(10) O201 .174(17) .174(17) .28(2) -.002(13) .084(17) -.023(16) O202 .097(11) .179(15) .149(13) -.008(10) -.014(10) -.025(12) O203 .126(13) .29(2) .156(15) .055(14) .081(12) .070(15) O01 .151(9) .144(8) .181(9) -.022(7) -.022(8) -.021(8) O02 .113(7) .202(10) .129(8) .030(7) -.004(6) -.034(7) O03 .239(17) .113(11) .208(16) .00000 .013(14) .00000 O04 .126(16) .123(16) .24(2) .00000 .063(15) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu N0 . . 2.090(6) ? Cu N01 . . 1.966(6) ? Cu O2 . . 2.315(5) ? Cu O2' . . 2.300(5) ? Cu N31 . . 2.024(6) ? Cu O101 . . 2.002(6) ? N0 C0 . . 1.494(10) ? N0 C1 . . 1.499(10) ? N0 C1' . . 1.530(10) ? C0 C02 . . 1.471(12) ? C0 H0a . . .872(8) ? C0 H0b . . .880(8) ? N01 C02 . . 1.340(10) ? N01 C06 . . 1.339(11) ? C02 C03 . . 1.389(12) ? C03 C04 . . 1.384(13) ? C03 H03 . . .872(9) ? C04 C05 . . 1.368(14) ? C04 H04 . . .864(10) ? C05 C06 . . 1.352(13) ? C05 H05 . . .927(9) ? C06 H06 . . .988(9) ? C1 C11 . . 1.508(11) ? C1 H1a . . .989(8) ? C1 H1b . . .966(8) ? C11 C12 . . 1.400(11) ? C11 C16 . . 1.353(11) ? C12 C13 . . 1.446(12) ? C12 H12 . . 1.031(8) ? C13 C131 . . 1.545(12) ? C13 C14 . . 1.361(12) ? C131 C132 . . 1.515(14) ? C131 C133 . . 1.481(15) ? C131 C134 . . 1.456(15) ? C132 H132a . . .933(12) ? C132 H132b . . .979(13) ? C132 H132c . . .992(13) ? C133 H133a . . .953(14) ? C133 H133b . . .976(14) ? C133 H133c . . .967(16) ? C134 H134a . . .944(13) ? C134 H134b . . 1.042(14) ? C134 H134c . . .910(14) ? C14 C15 . . 1.379(12) ? C14 H14 . . .958(8) ? C15 C16 . . 1.381(12) ? C15 H15 . . .965(8) ? C16 O2 . . 1.371(10) ? C1' C11' . . 1.477(11) ? C1' H1'a . . .973(8) ? C1' H1'b . . .984(8) ? C11' C12' . . 1.389(11) ? C11' C16' . . 1.389(11) ? C12' C13' . . 1.389(12) ? C12' H12' . . .987(8) ? C13' C131' . . 1.506(11) ? C13' C14' . . 1.377(12) ? C131' C132' . . 1.504(14) ? C131' C133' . . 1.502(14) ? C131' C134' . . 1.492(14) ? C132' H132'a . . .975(10) ? C132' H132'b . . .979(12) ? C132' H132'c . . .961(11) ? C133' H133'a . . .960(11) ? C133' H133'b . . .980(12) ? C133' H133'c . . .976(12) ? C134' H134'a . . .980(11) ? C134' H134'b . . .996(12) ? C134' H134'c . . .974(14) ? C14' C15' . . 1.393(12) ? C14' H14' . . .983(8) ? C15' C16' . . 1.365(12) ? C15' H15' . . 1.009(8) ? C16' O2' . . 1.371(9) ? O2 C3 . . 1.413(11) ? C3 C32 . . 1.535(14) ? C3 H3a . . .893(11) ? C3 H3b . . .900(9) ? O2' C3' . . 1.431(10) ? C3' C32' . . 1.465(13) ? C3' H3'a . . .890(9) ? C3' H3'b . . .901(10) ? N31 C32 . . 1.321(11) ? N31 C32' . . 1.376(10) ? C32 C33 . . 1.377(13) ? C33 C34 . . 1.365(16) ? C33 H33 . . .940(10) ? C34 C33' . . 1.350(15) ? C34 H34 . . .908(11) ? C33' C32' . . 1.391(13) ? C33' H33' . . .854(9) ? N10 O101 . . 1.146(10) ? N10 O102 . . 1.228(11) ? N10 O103 . . 1.255(13) ? N20 O201 . . 1.030(18) ? N20 O202 . . 1.186(18) ? N20 O203 . . 1.241(16) ? N20 N20A . . .77(2) ? N20 O201A . . 1.05(4) ? N20 O202A . . 1.37(2) ? N20 O203A . . 1.58(3) ? O201 O202 . . 1.90(2) ? O201 N20A . . 1.61(2) ? O201 O201A . . 1.07(4) ? O202 N20A . . 1.54(2) ? O202 O202A . . 1.59(3) ? O203 N20A . . 1.029(16) ? O203 O201A . . 1.15(3) ? O203 O203A . . .99(2) ? N20A O201A . . 1.17(3) ? N20A O202A . . 1.04(2) ? N20A O203A . . 1.00(3) ? O201A O203A . . 1.87(4) ? O202A O203A . . 1.76(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 N0 Cu N01 . . . 83.0(3) ? N0 Cu O2 . . . 87.5(2) ? N0 Cu O2' . . . 91.5(2) ? N0 Cu N31 . . . 98.6(3) ? N0 Cu O101 . . . 162.6(2) ? N01 Cu O2 . . . 116.6(2) ? N01 Cu O2' . . . 91.4(2) ? N01 Cu N31 . . . 168.0(3) ? N01 Cu O101 . . . 90.1(3) ? O2 Cu O2' . . . 151.6(2) ? O2 Cu N31 . . . 75.4(2) ? O2 Cu O101 . . . 81.3(2) ? O2' Cu N31 . . . 76.8(2) ? O2' Cu O101 . . . 104.7(2) ? N31 Cu O101 . . . 91.4(3) ? Cu N0 C0 . . . 106.8(5) ? Cu N0 C1 . . . 113.7(5) ? Cu N0 C1' . . . 109.5(4) ? C0 N0 C1 . . . 110.0(6) ? C0 N0 C1' . . . 109.3(6) ? C1 N0 C1' . . . 107.5(6) ? N0 C0 C02 . . . 111.7(7) ? N0 C0 H0a . . . 108.8(8) ? N0 C0 H0b . . . 107.7(7) ? C02 C0 H0a . . . 111.7(8) ? C02 C0 H0b . . . 111.8(8) ? H0a C0 H0b . . . 104.9(9) ? Cu N01 C02 . . . 115.8(5) ? Cu N01 C06 . . . 125.8(6) ? C02 N01 C06 . . . 117.8(7) ? C0 C02 N01 . . . 116.1(7) ? C0 C02 C03 . . . 121.3(7) ? N01 C02 C03 . . . 122.4(7) ? C02 C03 C04 . . . 117.8(8) ? C02 C03 H03 . . . 121.4(9) ? C04 C03 H03 . . . 120.8(9) ? C03 C04 C05 . . . 119.5(9) ? C03 C04 H04 . . . 124.1(10) ? C05 C04 H04 . . . 116.4(10) ? C04 C05 C06 . . . 119.3(9) ? C04 C05 H05 . . . 120.1(10) ? C06 C05 H05 . . . 120.6(10) ? N01 C06 C05 . . . 123.2(8) ? N01 C06 H06 . . . 120.4(8) ? C05 C06 H06 . . . 116.3(9) ? N0 C1 C11 . . . 114.8(6) ? N0 C1 H1a . . . 106.7(7) ? N0 C1 H1b . . . 107.6(7) ? C11 C1 H1a . . . 111.9(7) ? C11 C1 H1b . . . 110.1(7) ? H1a C1 H1b . . . 105.1(7) ? C1 C11 C12 . . . 117.6(7) ? C1 C11 C16 . . . 121.8(7) ? C12 C11 C16 . . . 120.6(7) ? C11 C12 C13 . . . 118.9(7) ? C11 C12 H12 . . . 121.0(8) ? C13 C12 H12 . . . 120.1(8) ? C12 C13 C131 . . . 118.2(7) ? C12 C13 C14 . . . 118.2(7) ? C131 C13 C14 . . . 123.6(7) ? C13 C131 C132 . . . 110.0(8) ? C13 C131 C133 . . . 110.9(9) ? C13 C131 C134 . . . 110.5(8) ? C132 C131 C133 . . . 108.2(9) ? C132 C131 C134 . . . 110.9(9) ? C133 C131 C134 . . . 106.3(10) ? C131 C132 H132a . . . 114.8(11) ? C131 C132 H132b . . . 110.7(10) ? C131 C132 H132c . . . 111.0(9) ? H132a C132 H132b . . . 108.5(11) ? H132a C132 H132c . . . 107.4(12) ? H132b C132 H132c . . . 103.9(11) ? C131 C133 H133a . . . 113.7(13) ? C131 C133 H133b . . . 110.0(12) ? C131 C133 H133c . . . 111.9(11) ? H133a C133 H133b . . . 107.0(12) ? H133a C133 H133c . . . 107.8(13) ? H133b C133 H133c . . . 106.0(14) ? C131 C134 H134a . . . 113.5(12) ? C131 C134 H134b . . . 107.5(11) ? C131 C134 H134c . . . 113.5(11) ? H134a C134 H134b . . . 102.6(12) ? H134a C134 H134c . . . 113.6(14) ? H134b C134 H134c . . . 105.0(13) ? C13 C14 C15 . . . 121.3(8) ? C13 C14 H14 . . . 115.3(8) ? C15 C14 H14 . . . 123.4(8) ? C14 C15 C16 . . . 120.7(8) ? C14 C15 H15 . . . 117.3(8) ? C16 C15 H15 . . . 122.0(8) ? C11 C16 C15 . . . 120.3(8) ? C11 C16 O2 . . . 119.7(7) ? C15 C16 O2 . . . 120.0(7) ? N0 C1' C11' . . . 113.9(6) ? N0 C1' H1'a . . . 109.6(7) ? N0 C1' H1'b . . . 108.4(7) ? C11' C1' H1'a . . . 110.1(7) ? C11' C1' H1'b . . . 109.5(7) ? H1'a C1' H1'b . . . 104.9(8) ? C1' C11' C12' . . . 121.7(7) ? C1' C11' C16' . . . 120.6(7) ? C12' C11' C16' . . . 117.7(7) ? C11' C12' C13' . . . 123.0(7) ? C11' C12' H12' . . . 118.6(8) ? C13' C12' H12' . . . 118.3(7) ? C12' C13' C131' . . . 121.2(7) ? C12' C13' C14' . . . 116.2(7) ? C131' C13' C14' . . . 122.6(7) ? C13' C131' C132' . . . 110.1(7) ? C13' C131' C133' . . . 113.4(8) ? C13' C131' C134' . . . 109.2(7) ? C132' C131' C133' . . . 110.4(8) ? C132' C131' C134' . . . 106.0(8) ? C133' C131' C134' . . . 107.4(9) ? C131' C132' H132'a . . . 114.0(10) ? C131' C132' H132'b . . . 110.7(9) ? C131' C132' H132'c . . . 113.7(10) ? H132'a C132' H132'b . . . 105.1(11) ? H132'a C132' H132'c . . . 106.5(10) ? H132'b C132' H132'c . . . 106.2(11) ? C131' C133' H133'a . . . 115.0(10) ? C131' C133' H133'b . . . 112.7(10) ? C131' C133' H133'c . . . 110.8(10) ? H133'a C133' H133'b . . . 106.2(11) ? H133'a C133' H133'c . . . 106.5(11) ? H133'b C133' H133'c . . . 105.0(10) ? C131' C134' H134'a . . . 116.6(10) ? C131' C134' H134'b . . . 112.3(11) ? C131' C134' H134'c . . . 114.2(11) ? H134'a C134' H134'b . . . 103.4(11) ? H134'a C134' H134'c . . . 105.1(12) ? H134'b C134' H134'c . . . 103.9(10) ? C13' C14' C15' . . . 123.0(8) ? C13' C14' H14' . . . 119.3(8) ? C15' C14' H14' . . . 117.6(8) ? C14' C15' C16' . . . 118.4(7) ? C14' C15' H15' . . . 122.2(8) ? C16' C15' H15' . . . 119.4(8) ? C11' C16' C15' . . . 121.6(7) ? C11' C16' O2' . . . 119.5(7) ? C15' C16' O2' . . . 118.7(7) ? Cu O2 C16 . . . 119.6(5) ? Cu O2 C3 . . . 112.1(5) ? C16 O2 C3 . . . 115.7(7) ? O2 C3 C32 . . . 111.4(7) ? O2 C3 H3a . . . 114.0(9) ? O2 C3 H3b . . . 113.6(10) ? C32 C3 H3a . . . 108.3(9) ? C32 C3 H3b . . . 107.6(9) ? H3a C3 H3b . . . 101.5(10) ? Cu O2' C16' . . . 112.6(4) ? Cu O2' C3' . . . 111.4(5) ? C16' O2' C3' . . . 118.4(6) ? O2' C3' C32' . . . 112.1(7) ? O2' C3' H3'a . . . 109.1(8) ? O2' C3' H3'b . . . 108.3(9) ? C32' C3' H3'a . . . 113.3(10) ? C32' C3' H3'b . . . 111.8(8) ? H3'a C3' H3'b . . . 101.6(9) ? Cu N31 C32 . . . 121.5(5) ? Cu N31 C32' . . . 118.9(5) ? C32 N31 C32' . . . 117.9(7) ? C3 C32 N31 . . . 117.4(7) ? C3 C32 C33 . . . 119.8(8) ? N31 C32 C33 . . . 122.8(9) ? C32 C33 C34 . . . 119.2(9) ? C32 C33 H33 . . . 113.4(11) ? C34 C33 H33 . . . 127.4(11) ? C33 C34 C33' . . . 119.8(10) ? C33 C34 H34 . . . 112.7(10) ? C33' C34 H34 . . . 127.5(11) ? C34 C33' C32' . . . 119.3(9) ? C34 C33' H33' . . . 114.4(10) ? C32' C33' H33' . . . 126.3(11) ? C3' C32' N31 . . . 118.7(8) ? C3' C32' C33' . . . 120.4(8) ? N31 C32' C33' . . . 120.8(8) ? O101 N10 O102 . . . 126.5(9) ? O101 N10 O103 . . . 122.6(9) ? O102 N10 O103 . . . 110.7(9) ? Cu O101 N10 . . . 124.7(6) ? O201 N20 O202 . . . 117.9(13) ? O201 N20 O203 . . . 117.8(14) ? O201 N20 N20A . . . 126(2) ? O201 N20 O201A . . . 61.6(18) ? O201 N20 O202A . . . 106.0(13) ? O201 N20 O203A . . . 149.4(17) ? O202 N20 O203 . . . 121.1(11) ? O202 N20 N20A . . . 102.3(15) ? O202 N20 O201A . . . 179(2) ? O202 N20 O202A . . . 76.6(12) ? O202 N20 O203A . . . 92.0(11) ? O203 N20 N20A . . . 55.8(11) ? O203 N20 O201A . . . 59.4(16) ? O203 N20 O202A . . . 104.9(13) ? O203 N20 O203A . . . 38.9(8) ? N20A N20 O201A . . . 78(2) ? N20A N20 O202A . . . 49.1(12) ? N20A N20 O203A . . . 31.4(16) ? O201A N20 O202A . . . 104(2) ? O201A N20 O203A . . . 89(2) ? O202A N20 O203A . . . 73.2(11) ? N20 O201 O202 . . . 33.5(9) ? N20 O201 N20A . . . 22.6(11) ? N20 O201 O201A . . . 60(2) ? O202 O201 N20A . . . 51.4(9) ? O202 O201 O201A . . . 93.8(19) ? N20A O201 O201A . . . 46.6(17) ? N20 O202 O201 . . . 28.6(7) ? N20 O202 N20A . . . 29.1(7) ? N20 O202 O202A . . . 56.9(11) ? O201 O202 N20A . . . 54.5(7) ? O201 O202 O202A . . . 66.3(9) ? N20A O202 O202A . . . 38.9(9) ? N20 O203 N20A . . . 38.1(12) ? N20 O203 O201A . . . 52.1(19) ? N20 O203 O203A . . . 89.2(18) ? N20A O203 O201A . . . 64.7(17) ? N20A O203 O203A . . . 59.6(17) ? O201A O203 O203A . . . 122(3) ? N20 N20A O201 . . . 31.0(11) ? N20 N20A O202 . . . 48.6(14) ? N20 N20A O203 . . . 86.1(17) ? N20 N20A O201A . . . 62(2) ? N20 N20A O202A . . . 97.0(17) ? N20 N20A O203A . . . 125(3) ? O201 N20A O202 . . . 74.1(10) ? O201 N20A O203 . . . 92.5(12) ? O201 N20A O201A . . . 41.5(17) ? O201 N20A O202A . . . 90.6(11) ? O201 N20A O203A . . . 148(2) ? O202 N20A O203 . . . 109(2) ? O202 N20A O201A . . . 110(2) ? O202 N20A O202A . . . 72.9(15) ? O202 N20A O203A . . . 102(2) ? O203 N20A O201A . . . 62.5(16) ? O203 N20A O202A . . . 177(2) ? O203 N20A O203A . . . 58.2(12) ? O201A N20A O202A . . . 119.6(18) ? O201A N20A O203A . . . 118.8(17) ? O202A N20A O203A . . . 119.0(15) ? N20 O201A O201 . . . 58(2) ? N20 O201A O203 . . . 69(2) ? N20 O201A N20A . . . 40.0(16) ? N20 O201A O203A . . . 57.3(15) ? O201 O201A O203 . . . 123(4) ? O201 O201A N20A . . . 92(3) ? O201 O201A O203A . . . 115(3) ? O203 O201A N20A . . . 52.7(14) ? O203 O201A O203A . . . 26.5(12) ? N20A O201A O203A . . . 28.0(9) ? N20 O202A O202 . . . 46.5(10) ? N20 O202A N20A . . . 33.8(12) ? N20 O202A O203A . . . 58.8(12) ? O202 O202A N20A . . . 68.2(17) ? O202 O202A O203A . . . 73.2(14) ? N20A O202A O203A . . . 29.9(10) ? N20 O203A O203 . . . 51.9(16) ? N20 O203A N20A . . . 23.5(16) ? N20 O203A O201A . . . 34.2(13) ? N20 O203A O202A . . . 48.0(11) ? O203 O203A N20A . . . 62(2) ? O203 O203A O201A . . . 31.2(16) ? O203 O203A O202A . . . 93(2) ? N20A O203A O201A . . . 33.2(12) ? N20A O203A O202A . . . 31.2(10) ? O201A O203A O202A . . . 63.4(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 Cu C0 2.899(9) . . ? Cu C02 2.820(8) . . ? Cu C06 2.956(9) . . ? Cu C1 3.022(8) . . ? Cu C11 3.485(8) . . ? Cu C16 3.222(8) . . ? Cu C1' 2.974(8) . . ? Cu C11' 3.345(8) . . ? Cu C16' 3.098(7) . . ? Cu C3 3.133(10) . . ? Cu C3' 3.121(9) . . ? Cu C32 2.938(9) . . ? Cu C32' 2.947(9) . . ? Cu N10 2.816(8) . . ? Cu O102 3.157(9) . . ? Cu H0a 3.2800(14) . . ? Cu H06 3.0882(16) . . ? Cu H1b 3.0942(17) . . ? Cu H1'b 3.0623(13) . . ? N0 N01 2.689(9) . . ? N0 C02 2.454(10) . . ? N0 C11 2.533(10) . . ? N0 C11' 2.521(9) . . ? N0 H0a 1.957(6) . . ? N0 H0b 1.950(6) . . ? N0 H1a 2.019(6) . . ? N0 H1b 2.014(6) . . ? N0 H1'a 2.071(6) . . ? N0 H1'b 2.064(6) . . ? C0 N01 2.387(11) . . ? C0 C03 2.493(12) . . ? C0 C1 2.451(12) . . ? C0 C11 2.934(12) . . ? C0 C1' 2.466(11) . . ? C0 C11' 2.914(11) . . ? N01 C03 2.392(11) . . ? N01 C04 2.755(12) . . ? N01 C05 2.368(11) . . ? N01 O101 2.807(9) . . ? N01 H06 2.027(6) . . ? C02 C04 2.375(13) . . ? C02 C05 2.706(12) . . ? C02 C06 2.295(12) . . ? C02 H0a 1.968(8) . . ? C02 H0b 1.975(8) . . ? C02 H03 1.987(8) . . ? C03 C05 2.377(13) . . ? C03 C06 2.710(13) . . ? C03 H04 2.001(9) . . ? C04 C06 2.348(14) . . ? C04 H03 1.978(10) . . ? C04 H05 2.001(10) . . ? C05 H04 1.916(10) . . ? C05 H06 1.998(10) . . ? C06 O101 2.983(11) . . ? C06 H05 1.991(9) . . ? C1 C12 2.487(11) . . ? C1 C16 2.501(11) . . ? C1 C1' 2.443(11) . . ? C1 O2 2.828(10) . . ? C1 H0a 2.411(8) . . ? C11 C13 2.452(11) . . ? C11 C14 2.767(11) . . ? C11 C15 2.371(11) . . ? C11 O2 2.355(10) . . ? C11 H0a 2.453(8) . . ? C11 H1a 2.089(8) . . ? C11 H1b 2.052(8) . . ? C11 H12 2.124(8) . . ? C12 C131 2.567(12) . . ? C12 C14 2.409(12) . . ? C12 C15 2.762(12) . . ? C12 C16 2.391(12) . . ? C13 C132 2.506(14) . . ? C13 C133 2.492(14) . . ? C13 C134 2.466(15) . . ? C13 C15 2.388(12) . . ? C13 C16 2.790(11) . . ? C13 H12 2.156(8) . . ? C13 H14 1.971(8) . . ? C131 C14 2.563(13) . . ? C131 H132a 2.086(9) . . ? C131 H132b 2.075(9) . . ? C131 H132c 2.087(9) . . ? C131 H133a 2.058(9) . . ? C131 H133b 2.033(9) . . ? C131 H133c 2.049(9) . . ? C131 H134a 2.026(9) . . ? C131 H134b 2.029(9) . . ? C131 H134c 2.002(9) . . ? C132 C133 2.428(17) . . ? C132 C134 2.447(18) . . ? C133 C134 2.35(2) . . ? C133 C14 2.838(16) . . ? C133 H14 2.401(15) . . ? C14 C16 2.398(12) . . ? C14 H15 2.013(9) . . ? C15 O2 2.384(10) . . ? C15 H14 2.067(9) . . ? C16 C3 2.358(12) . . ? C16 H15 2.062(8) . . ? C16 H3a 2.419(8) . . ? C1' C12' 2.503(11) . . ? C1' C16' 2.490(12) . . ? C1' O2' 2.819(10) . . ? C1' H0b 2.419(8) . . ? C1' H1a 2.500(8) . . ? C11' C13' 2.441(11) . . ? C11' C14' 2.755(11) . . ? C11' C15' 2.404(11) . . ? C11' O2' 2.385(9) . . ? C11' H1'a 2.029(7) . . ? C11' H1'b 2.030(8) . . ? C11' H12' 2.054(8) . . ? C12' C131' 2.522(12) . . ? C12' C134' 2.989(14) . . ? C12' C14' 2.348(12) . . ? C12' C15' 2.751(12) . . ? C12' C16' 2.378(11) . . ? C13' C132' 2.467(13) . . ? C13' C133' 2.513(14) . . ? C13' C134' 2.444(14) . . ? C13' C15' 2.435(11) . . ? C13' C16' 2.792(11) . . ? C13' H12' 2.050(8) . . ? C13' H14' 2.046(8) . . ? C131' C14' 2.529(12) . . ? C131' H132'a 2.099(8) . . ? C131' H132'b 2.065(8) . . ? C131' H132'c 2.086(8) . . ? C131' H133'a 2.097(8) . . ? C131' H133'b 2.086(8) . . ? C131' H133'c 2.061(9) . . ? C131' H134'a 2.121(8) . . ? C131' H134'b 2.085(8) . . ? C131' H134'c 2.089(8) . . ? C132' C133' 2.469(17) . . ? C132' C134' 2.393(16) . . ? C133' C134' 2.413(17) . . ? C133' C14' 2.852(14) . . ? C133' H14' 2.468(11) . . ? C14' C16' 2.369(12) . . ? C14' H15' 2.112(9) . . ? C15' O2' 2.354(10) . . ? C15' H14' 2.043(8) . . ? C16' C3' 2.408(12) . . ? C16' H15' 2.058(9) . . ? C16' H3'a 2.423(8) . . ? O2 N31 2.662(8) . . ? O2 C32 2.435(10) . . ? O2 O101 2.823(8) . . ? O2 H3a 1.954(5) . . ? O2 H3b 1.955(5) . . ? C3 N31 2.442(12) . . ? C3 C33 2.521(15) . . ? O2' N31 2.693(8) . . ? O2' C32' 2.403(11) . . ? O2' H3'a 1.917(5) . . ? O2' H3'b 1.915(5) . . ? C3' N31 2.445(11) . . ? C3' C33' 2.479(14) . . ? N31 C33 2.368(12) . . ? N31 C34 2.758(12) . . ? N31 C33' 2.406(11) . . ? N31 O101 2.882(8) . . ? C32 C34 2.364(14) . . ? C32 C33' 2.708(13) . . ? C32 C32' 2.311(12) . . ? C32 H3a 2.003(9) . . ? C32 H3b 2.000(9) . . ? C32 H33 1.951(9) . . ? C33 C33' 2.348(15) . . ? C33 C32' 2.711(13) . . ? C33 H34 1.909(11) . . ? C34 C32' 2.365(14) . . ? C34 H33 2.075(11) . . ? C34 H33' 1.872(11) . . ? C33' H34 2.034(10) . . ? C32' H3'a 1.992(9) . . ? C32' H3'b 1.984(9) . . ? C32' H33' 2.017(9) . . ? O101 O102 2.120(10) . . ? O101 O103 2.107(11) . . ? O101 H06 2.492(6) . . ? O102 O103 2.043(12) . . ? O103 O03 2.976(11) . '2 664' ? O201 O203 1.95(2) . . ? O201 O202A 1.93(2) . . ? O201 O203A 2.52(3) . . ? O201 O02 2.925(17) . '5 666' ? O202 O203 2.11(2) . . ? O202 O201A 2.24(4) . . ? O202 O203A 2.01(3) . . ? O202 O01 2.943(16) . . ? O203 O202A 2.07(2) . . ? N20A O02 2.94(2) . . ? O201A O202A 1.91(3) . . ? O201A O02 2.45(3) . '5 666' ? O202A O01 2.73(2) . . ? O202A O02 2.93(2) . . ? O203A O02 2.90(4) . . ? O01 O03 2.849(13) . . ? O01 O04 2.800(15) . . ? H0a H0b 1.3883(5) . . ? H1a H1b 1.5516(7) . . ? H132a H132b 1.5516(6) . . ? H132a H132c 1.5515(6) . . ? H132b H132c 1.5514(5) . . ? H133a H133b 1.5509(6) . . ? H133a H133c 1.5513(6) . . ? H133b H133c 1.5511(5) . . ? H134a H134b 1.5514(7) . . ? H134a H134c 1.5514(6) . . ? H134b H134c 1.5514(5) . . ? H1'a H1'b 1.5514(6) . . ? H132'a H132'b 1.5513(5) . . ? H132'a H132'c 1.5514(6) . . ? H132'b H132'c 1.5516(5) . . ? H133'a H133'b 1.5514(6) . . ? H133'a H133'c 1.5514(6) . . ? H133'b H133'c 1.5516(7) . . ? H134'a H134'b 1.5513(6) . . ? H134'a H134'c 1.5513(5) . . ? H134'b H134'c 1.5514(6) . . ? H3a H3b 1.3882(5) . . ? H3'a H3'b 1.3881(5) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3272 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 11 9 6 -11 9 6 11 -9 6 11 9 -6 -11 -9 -6 11 -9 -6 -11 -9 6 -11 9 -6 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 12.456 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' #======================================================================= # 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 #==END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_ll200 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C35 H41 Ag1 N4 O5' _chemical_formula_moiety ? _chemical_formula_weight 705.6 _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 18.303(2) _cell_length_b 11.1770(10) _cell_length_c 15.940(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.221(2) _cell_angle_gamma 90.00000 _cell_volume 3260.9(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5036 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .666 _exptl_crystal_description leaf _exptl_crystal_size_max .25 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .025 _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 .651 _exptl_absorpt_correction_T_max .875 _diffrn_reflns_number 36819 _reflns_number_total 8120 _reflns_Friedel_coverage 0 _reflns_number_gt 4869 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.89 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .069 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _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 .049 _refine_ls_wR_factor_ref .046 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_number_reflns 4869 _refine_ls_number_parameters 459 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .056 _refine_diff_density_min -.707 _refine_diff_density_max 1.111 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _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 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 ? 0 140 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 164 0 0 '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 20 .008 .006 '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' 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 .873205(18) .95464(3) .63004(2) .03214(17) Uani ? ? 1.00000 ? ? N0 .74677(18) .8852(3) .6472(2) .029(2) Uani ? ? 1.00000 ? ? C0 .7536(2) .8147(4) .7248(3) .032(2) Uani ? ? 1.00000 ? ? N01 .87451(19) .8938(3) .7586(2) .032(2) Uani ? ? 1.00000 ? ? C02 .8083(2) .8620(4) .7880(3) .031(2) Uani ? ? 1.00000 ? ? C03 .7930(2) .8639(4) .8728(3) .033(2) Uani ? ? 1.00000 ? ? C04 .8467(3) .8948(4) .9300(3) .037(3) Uani ? ? 1.00000 ? ? C05 .9152(3) .9227(4) .9003(3) .036(3) Uani ? ? 1.00000 ? ? C06 .9269(2) .9240(4) .8148(3) .036(3) Uani ? ? 1.00000 ? ? C1 .7247(2) .8046(4) .5779(3) .033(2) Uani ? ? 1.00000 ? ? C11 .7183(2) .8620(4) .4923(2) .030(2) Uani ? ? 1.00000 ? ? C12 .6503(2) .8746(4) .4547(3) .036(3) Uani ? ? 1.00000 ? ? C13 .6406(2) .9187(4) .3738(3) .035(3) Uani ? ? 1.00000 ? ? C131 .5652(3) .9249(5) .3310(3) .047(3) Uani ? ? 1.00000 ? ? C132 .5091(5) .9650(16) .4006(7) .074(9) Uani ? ? .593(16) ? ? C133 .5639(8) 1.004(2) .2613(9) .097(13) Uani ? ? .593(16) ? ? C134 .5425(6) .7960(13) .3080(11) .092(11) Uani ? ? .593(16) ? ? C132A .5034(8) .872(2) .3772(10) .063(11) Uani ? ? .407(16) ? ? C133A .5438(12) 1.0613(15) .316(2) .12(2) Uani ? ? .407(16) ? ? C134A .5680(8) .863(2) .2435(11) .070(12) Uani ? ? .407(16) ? ? C14 .7030(2) .9535(4) .3310(3) .037(2) Uani ? ? 1.00000 ? ? C15 .7720(2) .9403(4) .3660(3) .035(2) Uani ? ? 1.00000 ? ? C16 .7804(2) .8928(4) .4455(2) .030(2) Uani ? ? 1.00000 ? ? C1' .6916(2) .9819(4) .6570(3) .035(3) Uani ? ? 1.00000 ? ? C11' .7082(2) 1.0703(4) .7264(3) .032(3) Uani ? ? 1.00000 ? ? C12' .6702(2) 1.0658(4) .8016(3) .038(3) Uani ? ? 1.00000 ? ? C13' .6832(3) 1.1440(5) .8687(3) .046(3) Uani ? ? 1.00000 ? ? C131' .6408(3) 1.1346(6) .9514(3) .058(4) Uani ? ? 1.00000 ? ? C132' .6570(6) 1.0222(10) .9937(5) .096(8) Uani ? ? .779(10) ? ? C133' .5569(4) 1.1403(10) .9307(5) .080(6) Uani ? ? .779(10) ? ? C134' .6552(5) 1.2425(9) 1.0096(5) .083(6) Uani ? ? .779(10) ? ? C132'A .7052(13) 1.103(3) 1.0264(14) .060(17) Uani ? ? .221(10) ? ? C133'A .5946(19) 1.002(3) .9571(18) .08(2) Uani ? ? .221(10) ? ? C134'A .5964(18) 1.223(3) .9702(18) .08(2) Uani ? ? .221(10) ? ? C14' .7360(3) 1.2301(5) .8563(3) .050(3) Uani ? ? 1.00000 ? ? C15' .7738(3) 1.2401(5) .7812(3) .048(3) Uani ? ? 1.00000 ? ? C16' .7602(2) 1.1599(4) .7165(3) .037(3) Uani ? ? 1.00000 ? ? O2 .84718(14) .8654(3) .48088(16) .0316(16) Uani ? ? 1.00000 ? ? C3 .9114(2) .9130(4) .4411(3) .036(3) Uani ? ? 1.00000 ? ? O2' .79431(16) 1.1630(3) .63954(18) .0399(19) Uani ? ? 1.00000 ? ? C3' .8589(3) 1.2351(4) .6298(3) .046(3) Uani ? ? 1.00000 ? ? N31 .89578(18) 1.0835(3) .5309(2) .033(2) Uani ? ? 1.00000 ? ? C32 .9166(2) 1.0460(5) .4544(3) .036(2) Uani ? ? 1.00000 ? ? C33 .9392(2) 1.1257(5) .3933(3) .044(3) Uani ? ? 1.00000 ? ? C34 .9390(3) 1.2464(5) .4112(3) .056(4) Uani ? ? 1.00000 ? ? C33' .9129(3) 1.2861(5) .4875(3) .051(3) Uani ? ? 1.00000 ? ? C32' .8906(2) 1.2017(4) .5467(3) .039(3) Uani ? ? 1.00000 ? ? N1 .8939(6) .5741(10) .6655(8) .051(4) Uiso ? ? .50000 ? ? N1' .8831(5) .5393(8) .6630(5) .021(2) Uiso ? ? .50000 ? ? O01 .8206(2) .5445(4) .6529(2) .066(3) Uani ? ? 1.00000 ? ? O02 .9265(6) .5879(10) .6075(7) .088(3) Uiso ? ? .50000 ? ? O02' .9295(3) .5349(6) .6017(4) .0290(15) Uiso ? ? .50000 ? ? O03 .9247(4) .5883(6) .7324(4) .0456(17) Uiso ? ? .50000 ? ? O03' .9040(4) .5146(7) .7317(5) .059(2) Uiso ? ? .50000 ? ? H0a .70710 .81214 .75175 .04200 Uiso ? ? 1.00000 ? ? H0b .76799 .73568 .71064 .04200 Uiso ? ? 1.00000 ? ? H03 .74383 .84746 .89178 .04300 Uiso ? ? 1.00000 ? ? H04 .83665 .89385 .98905 .04500 Uiso ? ? 1.00000 ? ? H05 .95475 .94192 .93857 .04400 Uiso ? ? 1.00000 ? ? H06 .97454 .94638 .79367 .04300 Uiso ? ? 1.00000 ? ? H1a .75951 .74180 .57405 .04200 Uiso ? ? 1.00000 ? ? H1b .67808 .77079 .59164 .04200 Uiso ? ? 1.00000 ? ? H12 .60763 .85208 .48712 .04200 Uiso ? ? 1.00000 ? ? H132a .46285 .97081 .37487 .10700 Uiso ? ? .593(16) ? ? H132b .50642 .89552 .43970 .10700 Uiso ? ? .593(16) ? ? H132c .52468 1.02984 .42727 .10700 Uiso ? ? .593(16) ? ? H133a .51525 1.01504 .24005 .14200 Uiso ? ? .593(16) ? ? H133b .57666 1.08842 .28338 .14200 Uiso ? ? .593(16) ? ? H133c .59657 .98778 .22050 .14200 Uiso ? ? .593(16) ? ? H134a .49427 .79827 .28484 .16300 Uiso ? ? .593(16) ? ? H134b .57489 .77062 .26213 .16300 Uiso ? ? .593(16) ? ? H134c .54669 .74577 .35208 .16300 Uiso ? ? .593(16) ? ? H132Aa .45818 .89161 .34954 .06600 Uiso ? ? .407(16) ? ? H132Ab .50788 .78768 .37982 .06600 Uiso ? ? .407(16) ? ? H132Ac .50128 .90325 .43310 .06600 Uiso ? ? .407(16) ? ? H133Aa .49498 1.06248 .29182 .11000 Uiso ? ? .407(16) ? ? H133Ab .54042 1.10013 .36979 .11000 Uiso ? ? .407(16) ? ? H133Ac .57646 1.09799 .28190 .11000 Uiso ? ? .407(16) ? ? H134Aa .52756 .87654 .21247 .07200 Uiso ? ? .407(16) ? ? H134Ab .61082 .90282 .21263 .07200 Uiso ? ? .407(16) ? ? H134Ac .58182 .78307 .24869 .07200 Uiso ? ? .407(16) ? ? H14 .69849 .98754 .27635 .04700 Uiso ? ? 1.00000 ? ? H15 .81441 .96369 .33486 .04300 Uiso ? ? 1.00000 ? ? H1'a .68872 1.02463 .60508 .04000 Uiso ? ? 1.00000 ? ? H1'b .64534 .94409 .66653 .04000 Uiso ? ? 1.00000 ? ? H12' .63253 1.00367 .80825 .04900 Uiso ? ? 1.00000 ? ? H132'a .63094 1.01298 1.04438 .11400 Uiso ? ? .779(10) ? ? H132'b .64589 .95429 .95798 .11400 Uiso ? ? .779(10) ? ? H132'c .70886 1.01686 1.00644 .11400 Uiso ? ? .779(10) ? ? H133'a .52864 1.13258 .98079 .11200 Uiso ? ? .779(10) ? ? H133'b .54429 1.21202 .90291 .11200 Uiso ? ? .779(10) ? ? H133'c .54254 1.07388 .89394 .11200 Uiso ? ? .779(10) ? ? H134'a .62629 1.23949 1.05790 .10300 Uiso ? ? .779(10) ? ? H134'b .70574 1.24543 1.02453 .10300 Uiso ? ? .779(10) ? ? H134'c .64396 1.31514 .97898 .10300 Uiso ? ? .779(10) ? ? H132'Aa .68264 1.08069 1.07840 .08800 Uiso ? ? .221(10) ? ? H132'Ab .72294 1.00963 1.00897 .08800 Uiso ? ? .221(10) ? ? H132'Ac .74377 1.14179 1.02660 .08800 Uiso ? ? .221(10) ? ? H133'Aa .56986 .99992 1.01064 .05700 Uiso ? ? .221(10) ? ? H133'Ab .56429 .99264 .91367 .05700 Uiso ? ? .221(10) ? ? H133'Ac .63144 .93856 .95970 .05700 Uiso ? ? .221(10) ? ? H134'Aa .57214 1.19802 1.01619 .10300 Uiso ? ? .221(10) ? ? H134'Ab .61636 1.28598 .96081 .10300 Uiso ? ? .221(10) ? ? H134'Ac .55788 1.20352 .92030 .10300 Uiso ? ? .221(10) ? ? H14' .74636 1.28592 .90085 .06200 Uiso ? ? 1.00000 ? ? H15' .81037 1.30293 .77269 .05800 Uiso ? ? 1.00000 ? ? H3a .95423 .87423 .46411 .04700 Uiso ? ? 1.00000 ? ? H3b .90990 .89552 .38233 .04700 Uiso ? ? 1.00000 ? ? H3'a .84777 1.31904 .63266 .05800 Uiso ? ? 1.00000 ? ? H3'b .89376 1.21895 .67476 .05800 Uiso ? ? 1.00000 ? ? H33 .95462 1.09581 .33886 .05700 Uiso ? ? 1.00000 ? ? H34 .95759 1.30308 .37042 .06800 Uiso ? ? 1.00000 ? ? H33' .90979 1.37081 .49996 .06700 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 .02891(17) .0413(2) .02622(16) -.00512(18) -.00134(12) .00235(19) N0 .0263(19) .034(2) .0259(18) -.0024(16) -.0034(15) -.0041(16) C0 .031(2) .037(3) .028(2) -.004(2) .0018(19) -.000(2) N01 .029(2) .039(2) .029(2) -.0019(17) -.0030(16) .0008(17) C02 .031(2) .029(2) .032(2) .0013(19) .001(2) .0011(19) C03 .034(3) .035(3) .030(2) -.005(2) .002(2) .003(2) C04 .045(3) .039(3) .027(2) -.001(2) .001(2) .001(2) C05 .042(3) .038(3) .029(2) -.005(2) -.010(2) .0009(19) C06 .032(2) .041(3) .036(2) -.003(2) -.001(2) .003(2) C1 .029(2) .039(3) .031(2) -.006(2) -.0005(19) -.005(2) C11 .031(2) .033(3) .027(2) -.004(2) .0006(19) -.0092(19) C12 .029(2) .045(3) .032(2) -.006(2) .001(2) -.012(2) C13 .027(3) .041(3) .036(2) .0022(18) -.002(2) -.011(2) C131 .029(3) .064(4) .049(3) .006(2) -.010(2) -.013(3) C132 .040(6) .107(14) .073(8) .022(7) -.008(5) .010(8) C133 .060(8) .14(2) .086(10) .002(9) -.039(7) .047(10) C134 .055(7) .088(10) .132(15) .001(7) -.046(9) -.046(9) C132A .043(9) .083(15) .063(10) -.002(9) -.013(7) .005(10) C133A .062(13) .031(11) .26(4) .007(8) -.09(2) .018(13) C134A .038(8) .110(17) .062(11) .003(9) -.025(8) -.029(11) C14 .037(3) .044(3) .031(2) .004(2) -.0095(19) -.002(2) C15 .031(2) .044(3) .031(2) -.008(2) .0004(18) -.003(2) C16 .026(2) .037(3) .028(2) -.004(2) -.0039(19) -.005(2) C1' .025(2) .049(3) .030(2) -.002(2) -.0034(18) -.002(2) C11' .024(2) .039(3) .033(2) .0067(19) -.0070(18) -.006(2) C12' .027(2) .050(3) .038(3) .002(2) -.006(2) -.007(2) C13' .034(3) .062(4) .042(3) .008(2) -.009(2) -.014(3) C131' .045(3) .085(5) .042(3) .001(3) .000(3) -.024(3) C132' .110(10) .133(10) .044(5) .032(8) .033(6) .002(6) C133' .046(5) .140(9) .055(5) .002(5) .007(4) -.040(5) C134' .064(6) .126(8) .057(5) -.002(5) -.004(4) -.051(5) C132'A .037(14) .12(3) .026(12) -.007(14) -.010(10) -.004(13) C133'A .07(2) .14(3) .048(17) .00(2) .018(16) .027(17) C134'A .08(3) .10(3) .052(19) .01(2) .032(19) -.000(17) C14' .043(3) .057(4) .049(3) .007(3) -.012(2) -.023(3) C15' .040(3) .046(3) .057(3) .001(2) -.007(3) -.013(3) C16' .031(3) .041(3) .040(3) .008(2) -.005(2) -.006(2) O2 .0217(15) .0448(19) .0281(15) -.0040(13) -.0004(12) .0009(14) C3 .027(2) .054(3) .029(2) -.004(2) -.001(2) .001(2) O2' .0365(18) .040(2) .0429(18) -.0036(15) -.0030(15) -.0037(15) C3' .042(3) .041(3) .057(3) -.008(2) -.005(3) -.001(3) N31 .026(2) .038(2) .035(2) -.0063(15) -.0034(16) .0027(16) C32 .021(2) .056(3) .030(2) -.005(2) -.0063(17) .010(3) C33 .036(3) .061(4) .035(3) -.011(2) -.007(2) .013(2) C34 .048(3) .073(4) .048(3) -.020(3) -.016(3) .031(3) C33' .044(3) .050(3) .059(3) -.014(2) -.017(3) .021(3) C32' .028(2) .046(3) .045(3) -.007(2) -.012(2) .010(2) O01 .052(2) .075(3) .071(3) .009(2) .014(2) .003(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ag N0 . . 2.457(3) ? Ag N01 . . 2.160(3) ? Ag O2 . . 2.621(3) ? Ag O2' . . 2.745(3) ? Ag N31 . . 2.179(4) ? N0 C0 . . 1.472(5) ? N0 C1 . . 1.480(5) ? N0 C1' . . 1.488(5) ? C0 C02 . . 1.512(6) ? C0 H0a . . .955(4) ? C0 H0b . . .949(4) ? N01 C02 . . 1.349(5) ? N01 C06 . . 1.351(6) ? C02 C03 . . 1.382(6) ? C03 C04 . . 1.383(6) ? C03 H03 . . .968(4) ? C04 C05 . . 1.376(6) ? C04 H04 . . .960(4) ? C05 C06 . . 1.381(6) ? C05 H05 . . .969(4) ? C06 H06 . . .969(4) ? C1 C11 . . 1.512(6) ? C1 H1a . . .951(4) ? C1 H1b . . .959(4) ? C11 C12 . . 1.387(6) ? C11 C16 . . 1.405(6) ? C12 C13 . . 1.392(6) ? C12 H12 . . .971(4) ? C13 C131 . . 1.538(6) ? C13 C14 . . 1.389(6) ? C131 C132 . . 1.580(13) ? C131 C133 . . 1.423(18) ? C131 C134 . . 1.543(15) ? C131 C132A . . 1.475(17) ? C131 C133A . . 1.593(19) ? C131 C134A . . 1.56(2) ? C132 C132A . . 1.11(3) ? C132 C133A . . 1.84(3) ? C132 H132a . . .942(10) ? C132 H132b . . .996(16) ? C132 H132c . . .887(16) ? C132 H132Aa . . 1.483(13) ? C132 H132Ac . . .874(16) ? C133 C133A . . 1.14(4) ? C133 C134A . . 1.61(3) ? C133 H133a . . .959(14) ? C133 H133b . . 1.03(2) ? C133 H133c . . .904(15) ? C133 H133Ac . . 1.12(2) ? C134 C132A . . 1.57(2) ? C134 C134A . . 1.35(2) ? C134 H134a . . .957(13) ? C134 H134b . . .984(15) ? C134 H134c . . .902(16) ? C134 H132Ab . . 1.314(16) ? C134 H134Ac . . 1.199(16) ? C132A H132a . . 1.33(2) ? C132A H132b . . 1.032(17) ? C132A H132Aa . . .962(15) ? C132A H132Ab . . .95(2) ? C132A H132Ac . . .958(17) ? C133A H133a . . 1.41(3) ? C133A H133b . . .85(3) ? C133A H133Aa . . .97(3) ? C133A H133Ab . . .97(4) ? C133A H133Ac . . .91(3) ? C134A H134b . . 1.08(2) ? C134A H134Aa . . .902(16) ? C134A H134Ab . . 1.030(17) ? C134A H134Ac . . .93(2) ? C14 C15 . . 1.386(6) ? C14 H14 . . .954(4) ? C15 C16 . . 1.381(6) ? C15 H15 . . .960(4) ? C16 O2 . . 1.379(5) ? C1' C11' . . 1.513(6) ? C1' H1'a . . .956(4) ? C1' H1'b . . .959(4) ? C11' C12' . . 1.389(6) ? C11' C16' . . 1.391(6) ? C12' C13' . . 1.401(7) ? C12' H12' . . .984(4) ? C13' C131' . . 1.536(7) ? C13' C14' . . 1.378(7) ? C131' C132' . . 1.456(13) ? C131' C133' . . 1.571(9) ? C131' C134' . . 1.544(11) ? C131' C132'A . . 1.71(2) ? C131' C133'A . . 1.70(4) ? C131' C134'A . . 1.31(3) ? C132' C132'A . . 1.37(3) ? C132' C133'A . . 1.30(4) ? C132' H132'a . . .946(9) ? C132' H132'b . . .970(11) ? C132' H132'c . . .972(12) ? C132' H132'Ab . . 1.238(12) ? C132' H133'Ac . . 1.176(11) ? C133' C133'A . . 1.74(4) ? C133' C134'A . . 1.33(3) ? C133' H133'a . . .957(8) ? C133' H133'b . . .944(10) ? C133' H133'c . . .981(10) ? C133' H134'Ac . . .726(11) ? C134' C132'A . . 1.82(3) ? C134' C134'A . . 1.26(3) ? C134' H134'a . . .936(8) ? C134' H134'b . . .955(9) ? C134' H134'c . . .969(9) ? C134' H134'Ab . . 1.158(9) ? C132'A H132'c . . 1.02(3) ? C132'A H132'Aa . . .96(2) ? C132'A H132'Ab . . 1.13(3) ? C132'A H132'Ac . . .83(3) ? C133'A H132'b . . 1.08(4) ? C133'A H133'Aa . . .97(3) ? C133'A H133'Ab . . .89(3) ? C133'A H133'Ac . . .98(4) ? C134'A H133'b . . 1.44(3) ? C134'A H134'c . . 1.36(3) ? C134'A H134'Aa . . .90(3) ? C134'A H134'Ab . . .81(3) ? C134'A H134'Ac . . 1.08(3) ? C14' C15' . . 1.390(7) ? C14' H14' . . .964(5) ? C15' C16' . . 1.388(7) ? C15' H15' . . .979(5) ? C16' O2' . . 1.380(5) ? O2 C3 . . 1.440(5) ? C3 C32 . . 1.504(7) ? C3 H3a . . .967(4) ? C3 H3b . . .957(4) ? O2' C3' . . 1.439(6) ? C3' C32' . . 1.495(7) ? C3' H3'a . . .961(5) ? C3' H3'b . . .975(5) ? N31 C32 . . 1.346(5) ? N31 C32' . . 1.349(6) ? C32 C33 . . 1.384(7) ? C33 C34 . . 1.379(8) ? C33 H33 . . .973(5) ? C34 C33' . . 1.381(8) ? C34 H34 . . .970(6) ? C33' C32' . . 1.397(7) ? C33' H33' . . .969(5) ? N1 N1' . . .439(14) ? N1 O01 . . 1.396(12) ? N1 O02 . . 1.112(16) ? N1 O02' . . 1.287(13) ? N1 O03 . . 1.215(14) ? N1 O03' . . 1.259(14) ? N1' O01 . . 1.156(9) ? N1' O02 . . 1.308(14) ? N1' O02' . . 1.297(10) ? N1' O03 . . 1.449(11) ? N1' O03' . . 1.191(11) ? O02 O02' . . .602(13) ? O02 O03 . . 1.991(13) ? O03 O03' . . .908(11) ? H132a H132Aa . . .97656(7) ? H132b H132Ac . . .165248(11) ? H133b H133Ac . . .109593(9) ? H133c H134Ab . . .99285(8) ? H134b H134Ac . . .28558(2) ? H134c H132Ab . . .96018(7) ? H132'b H133'Ac . . .31885(3) ? H132'c H132'Ab . . .27293(3) ? H133'b H134'Ac . . .38367(3) ? H134'c H134'Ab . . .66646(5) ? 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 N0 Ag N01 . . . 78.56(12) ? N0 Ag O2 . . . 79.22(9) ? N0 Ag O2' . . . 76.47(10) ? N0 Ag N31 . . . 118.10(12) ? N01 Ag O2 . . . 137.94(12) ? N01 Ag O2' . . . 102.64(11) ? N01 Ag N31 . . . 153.52(13) ? O2 Ag O2' . . . 106.22(9) ? O2 Ag N31 . . . 68.16(11) ? O2' Ag N31 . . . 65.19(11) ? Ag N0 C0 . . . 100.7(2) ? Ag N0 C1 . . . 111.3(2) ? Ag N0 C1' . . . 114.9(2) ? C0 N0 C1 . . . 108.9(3) ? C0 N0 C1' . . . 110.9(3) ? C1 N0 C1' . . . 109.6(3) ? N0 C0 C02 . . . 115.2(3) ? N0 C0 H0a . . . 108.7(4) ? N0 C0 H0b . . . 108.7(4) ? C02 C0 H0a . . . 107.4(4) ? C02 C0 H0b . . . 107.5(4) ? H0a C0 H0b . . . 109.2(4) ? Ag N01 C02 . . . 113.9(3) ? Ag N01 C06 . . . 123.7(3) ? C02 N01 C06 . . . 118.2(3) ? C0 C02 N01 . . . 117.0(3) ? C0 C02 C03 . . . 121.4(4) ? N01 C02 C03 . . . 121.4(4) ? C02 C03 C04 . . . 120.1(4) ? C02 C03 H03 . . . 119.7(4) ? C04 C03 H03 . . . 120.1(4) ? C03 C04 C05 . . . 118.4(4) ? C03 C04 H04 . . . 120.3(4) ? C05 C04 H04 . . . 121.2(4) ? C04 C05 C06 . . . 119.1(4) ? C04 C05 H05 . . . 120.8(4) ? C06 C05 H05 . . . 120.1(4) ? N01 C06 C05 . . . 122.6(4) ? N01 C06 H06 . . . 118.2(4) ? C05 C06 H06 . . . 119.2(4) ? N0 C1 C11 . . . 115.8(3) ? N0 C1 H1a . . . 108.4(4) ? N0 C1 H1b . . . 108.1(4) ? C11 C1 H1a . . . 107.7(4) ? C11 C1 H1b . . . 107.9(4) ? H1a C1 H1b . . . 108.7(4) ? C1 C11 C12 . . . 119.9(4) ? C1 C11 C16 . . . 121.6(4) ? C12 C11 C16 . . . 118.2(4) ? C11 C12 C13 . . . 123.2(4) ? C11 C12 H12 . . . 117.8(4) ? C13 C12 H12 . . . 119.0(4) ? C12 C13 C131 . . . 122.6(4) ? C12 C13 C14 . . . 116.9(4) ? C131 C13 C14 . . . 120.5(4) ? C13 C131 C132 . . . 106.6(5) ? C13 C131 C133 . . . 112.7(7) ? C13 C131 C134 . . . 107.7(6) ? C13 C131 C132A . . . 116.6(7) ? C13 C131 C133A . . . 109.2(10) ? C13 C131 C134A . . . 110.2(6) ? C132 C131 C133 . . . 111.3(9) ? C132 C131 C134 . . . 104.9(9) ? C132 C131 C132A . . . 42.4(10) ? C132 C131 C133A . . . 71.1(14) ? C132 C131 C134A . . . 141.1(8) ? C133 C131 C134 . . . 113.2(10) ? C133 C131 C132A . . . 129.0(9) ? C133 C131 C133A . . . 44.0(16) ? C133 C131 C134A . . . 65.1(11) ? C134 C131 C132A . . . 62.5(10) ? C134 C131 C133A . . . 142.4(12) ? C134 C131 C134A . . . 51.8(10) ? C132A C131 C133A . . . 105.7(13) ? C132A C131 C134A . . . 107.2(10) ? C133A C131 C134A . . . 107.4(16) ? C131 C132 C132A . . . 63.7(10) ? C131 C132 C133A . . . 54.8(8) ? C131 C132 H132a . . . 107.4(10) ? C131 C132 H132b . . . 104.6(12) ? C131 C132 H132c . . . 111.1(10) ? C131 C132 H132Aa . . . 82.3(7) ? C131 C132 H132Ac . . . 107.5(13) ? C132A C132 C133A . . . 109.4(15) ? C132A C132 H132a . . . 80.5(13) ? C132A C132 H132b . . . 58.4(13) ? C132A C132 H132c . . . 163.1(16) ? C132A C132 H132Aa . . . 40.4(9) ? C132A C132 H132Ac . . . 56.3(13) ? C133A C132 H132a . . . 87.2(12) ? C133A C132 H132b . . . 158.6(13) ? C133A C132 H132c . . . 76.3(13) ? C133A C132 H132Aa . . . 97.9(11) ? C133A C132 H132Ac . . . 162.2(15) ? H132a C132 H132b . . . 106.3(13) ? H132a C132 H132c . . . 116.1(17) ? H132a C132 H132Aa . . . 40.2(6) ? H132a C132 H132Ac . . . 99.4(12) ? H132b C132 H132c . . . 110.8(12) ? H132b C132 H132Aa . . . 83.1(10) ? H132b C132 H132Ac . . . 6.85(14) ? H132c C132 H132Aa . . . 156.3(14) ? H132c C132 H132Ac . . . 114.5(13) ? H132Aa C132 H132Ac . . . 77.6(10) ? C131 C133 C133A . . . 76.0(16) ? C131 C133 C134A . . . 61.5(11) ? C131 C133 H133a . . . 111.4(14) ? C131 C133 H133b . . . 107.4(12) ? C131 C133 H133c . . . 115.1(17) ? C131 C133 H133Ac . . . 110.6(11) ? C133A C133 C134A . . . 134(2) ? C133A C133 H133a . . . 84.1(18) ? C133A C133 H133b . . . 45.8(13) ? C133A C133 H133c . . . 152(2) ? C133A C133 H133Ac . . . 47.2(13) ? C134A C133 H133a . . . 96.0(15) ? C134A C133 H133b . . . 161.2(14) ? C134A C133 H133c . . . 69.0(14) ? C134A C133 H133Ac . . . 163.8(13) ? H133a C133 H133b . . . 102.5(18) ? H133a C133 H133c . . . 112.8(15) ? H133a C133 H133Ac . . . 100.1(17) ? H133b C133 H133c . . . 106.5(16) ? H133b C133 H133Ac . . . 3.29(11) ? H133c C133 H133Ac . . . 105.5(16) ? C131 C134 C132A . . . 56.6(9) ? C131 C134 C134A . . . 64.7(11) ? C131 C134 H134a . . . 108.3(11) ? C131 C134 H134b . . . 106.5(11) ? C131 C134 H134c . . . 112.0(14) ? C131 C134 H132Ab . . . 89.4(9) ? C131 C134 H134Ac . . . 98.0(9) ? C132A C134 C134A . . . 113.2(15) ? C132A C134 H134a . . . 80.4(10) ? C132A C134 H134b . . . 163.0(15) ? C132A C134 H134c . . . 80.0(13) ? C132A C134 H132Ab . . . 37.1(9) ? C132A C134 H134Ac . . . 153.8(14) ? C134A C134 H134a . . . 90.7(14) ? C134A C134 H134b . . . 52.1(11) ? C134A C134 H134c . . . 154.9(14) ? C134A C134 H132Ab . . . 150.3(15) ? C134A C134 H134Ac . . . 42.2(10) ? H134a C134 H134b . . . 106.1(16) ? H134a C134 H134c . . . 113.1(14) ? H134a C134 H132Ab . . . 83.7(9) ? H134a C134 H134Ac . . . 104.7(15) ? H134b C134 H134c . . . 110.5(13) ? H134b C134 H132Ab . . . 157.0(14) ? H134b C134 H134Ac . . . 10.0(2) ? H134c C134 H132Ab . . . 46.9(8) ? H134c C134 H134Ac . . . 119.4(13) ? H132Ab C134 H134Ac . . . 166.3(13) ? C131 C132A C132 . . . 73.9(12) ? C131 C132A C134 . . . 60.8(8) ? C131 C132A H132a . . . 94.7(13) ? C131 C132A H132b . . . 110.0(14) ? C131 C132A H132Aa . . . 109.9(15) ? C131 C132A H132Ab . . . 110.8(14) ? C131 C132A H132Ac . . . 110.6(15) ? C132 C132A C134 . . . 134.6(16) ? C132 C132A H132a . . . 44.2(9) ? C132 C132A H132b . . . 55.3(12) ? C132 C132A H132Aa . . . 91.2(17) ? C132 C132A H132Ab . . . 155.5(19) ? C132 C132A H132Ac . . . 49.4(12) ? C134 C132A H132a . . . 133.3(14) ? C134 C132A H132b . . . 142.6(16) ? C134 C132A H132Aa . . . 101.3(14) ? C134 C132A H132Ab . . . 56.8(11) ? C134 C132A H132Ac . . . 150.8(16) ? H132a C132A H132b . . . 81.0(13) ? H132a C132A H132Aa . . . 47.1(9) ? H132a C132A H132Ab . . . 151.0(15) ? H132a C132A H132Ac . . . 72.5(13) ? H132b C132A H132Aa . . . 115.3(16) ? H132b C132A H132Ab . . . 101.9(17) ? H132b C132A H132Ac . . . 8.53(16) ? H132Aa C132A H132Ab . . . 108.7(18) ? H132Aa C132A H132Ac . . . 107.7(16) ? H132Ab C132A H132Ac . . . 109.0(18) ? C131 C133A C132 . . . 54.2(10) ? C131 C133A C133 . . . 60.1(13) ? C131 C133A H133a . . . 82.5(11) ? C131 C133A H133b . . . 105.1(18) ? C131 C133A H133Aa . . . 107.4(15) ? C131 C133A H133Ab . . . 108(3) ? C131 C133A H133Ac . . . 111.2(19) ? C132 C133A C133 . . . 110.3(16) ? C132 C133A H133a . . . 106.6(12) ? C132 C133A H133b . . . 154(2) ? C132 C133A H133Aa . . . 88.7(17) ? C132 C133A H133Ab . . . 65.5(19) ? C132 C133A H133Ac . . . 159(2) ? C133 C133A H133a . . . 42.5(14) ? C133 C133A H133b . . . 60(2) ? C133 C133A H133Aa . . . 90(3) ? C133 C133A H133Ab . . . 162(3) ? C133 C133A H133Ac . . . 65(2) ? H133a C133A H133b . . . 83(3) ? H133a C133A H133Aa . . . 48.0(15) ? H133a C133A H133Ab . . . 154(2) ? H133a C133A H133Ac . . . 84(3) ? H133b C133A H133Aa . . . 114(4) ? H133b C133A H133Ab . . . 115(2) ? H133b C133A H133Ac . . . 6.2(2) ? H133Aa C133A H133Ab . . . 106(2) ? H133Aa C133A H133Ac . . . 112(4) ? H133Ab C133A H133Ac . . . 112(2) ? C131 C134A C133 . . . 53.4(9) ? C131 C134A C134 . . . 63.5(10) ? C131 C134A H134b . . . 100.6(13) ? C131 C134A H134Aa . . . 112.7(15) ? C131 C134A H134Ab . . . 105.2(14) ? C131 C134A H134Ac . . . 111.0(15) ? C133 C134A C134 . . . 113.1(15) ? C133 C134A H134b . . . 153.6(17) ? C133 C134A H134Aa . . . 83.7(15) ? C133 C134A H134Ab . . . 72.1(13) ? C133 C134A H134Ac . . . 160.0(17) ? C134 C134A H134b . . . 46.0(10) ? C134 C134A H134Aa . . . 103.1(15) ? C134 C134A H134Ab . . . 150.1(16) ? C134 C134A H134Ac . . . 59.9(12) ? H134b C134A H134Aa . . . 114.1(19) ? H134b C134A H134Ab . . . 117.2(16) ? H134b C134A H134Ac . . . 14.0(3) ? H134Aa C134A H134Ab . . . 106.7(18) ? H134Aa C134A H134Ac . . . 116(2) ? H134Ab C134A H134Ac . . . 104.5(15) ? C13 C14 C15 . . . 121.5(4) ? C13 C14 H14 . . . 119.4(4) ? C15 C14 H14 . . . 119.1(4) ? C14 C15 C16 . . . 120.6(4) ? C14 C15 H15 . . . 120.0(4) ? C16 C15 H15 . . . 119.5(4) ? C11 C16 C15 . . . 119.6(4) ? C11 C16 O2 . . . 116.5(3) ? C15 C16 O2 . . . 123.8(4) ? N0 C1' C11' . . . 114.6(3) ? N0 C1' H1'a . . . 107.9(4) ? N0 C1' H1'b . . . 107.2(4) ? C11' C1' H1'a . . . 108.5(4) ? C11' C1' H1'b . . . 110.3(4) ? H1'a C1' H1'b . . . 108.2(4) ? C1' C11' C12' . . . 120.5(4) ? C1' C11' C16' . . . 121.5(4) ? C12' C11' C16' . . . 117.9(4) ? C11' C12' C13' . . . 123.5(4) ? C11' C12' H12' . . . 118.1(4) ? C13' C12' H12' . . . 118.4(4) ? C12' C13' C131' . . . 121.8(5) ? C12' C13' C14' . . . 116.4(4) ? C131' C13' C14' . . . 121.8(5) ? C13' C131' C132' . . . 110.8(6) ? C13' C131' C133' . . . 108.3(4) ? C13' C131' C134' . . . 112.1(5) ? C13' C131' C132'A . . . 105.4(8) ? C13' C131' C133'A . . . 111.0(11) ? C13' C131' C134'A . . . 117.3(14) ? C132' C131' C133' . . . 109.2(7) ? C132' C131' C134' . . . 111.2(6) ? C132' C131' C132'A . . . 50.3(11) ? C132' C131' C133'A . . . 47.7(12) ? C132' C131' C134'A . . . 131.9(14) ? C133' C131' C134' . . . 105.0(6) ? C133' C131' C132'A . . . 145.6(9) ? C133' C131' C133'A . . . 64.0(12) ? C133' C131' C134'A . . . 54.0(15) ? C134' C131' C132'A . . . 68.0(11) ? C134' C131' C133'A . . . 136.7(11) ? C134' C131' C134'A . . . 51.7(14) ? C132'A C131' C133'A . . . 97.2(15) ? C132'A C131' C134'A . . . 114.8(16) ? C133'A C131' C134'A . . . 109.4(19) ? C131' C132' C132'A . . . 74.6(13) ? C131' C132' C133'A . . . 76.2(17) ? C131' C132' H132'a . . . 112.8(10) ? C131' C132' H132'b . . . 111.2(8) ? C131' C132' H132'c . . . 110.3(10) ? C131' C132' H132'Ab . . . 112.7(8) ? C131' C132' H133'Ac . . . 113.1(7) ? C132'A C132' C133'A . . . 148(2) ? C132'A C132' H132'a . . . 94.2(12) ? C132'A C132' H132'b . . . 151.2(15) ? C132'A C132' H132'c . . . 48.1(13) ? C132'A C132' H132'Ab . . . 51.2(12) ? C132'A C132' H133'Ac . . . 163.2(15) ? C133'A C132' H132'a . . . 85.4(16) ? C133'A C132' H132'b . . . 54.7(17) ? C133'A C132' H132'c . . . 160.0(18) ? C133'A C132' H132'Ab . . . 157.4(18) ? C133'A C132' H133'Ac . . . 46.4(17) ? H132'a C132' H132'b . . . 108.1(11) ? H132'a C132' H132'c . . . 108.1(9) ? H132'a C132' H132'Ab . . . 108.3(8) ? H132'a C132' H133'Ac . . . 96.1(9) ? H132'b C132' H132'c . . . 106.1(11) ? H132'b C132' H132'Ab . . . 103.2(10) ? H132'b C132' H133'Ac . . . 13.05(19) ? H132'c C132' H132'Ab . . . 3.07(15) ? H132'c C132' H133'Ac . . . 115.7(10) ? H132'Ab C132' H133'Ac . . . 112.7(9) ? C131' C133' C133'A . . . 61.8(12) ? C131' C133' C134'A . . . 53.1(15) ? C131' C133' H133'a . . . 110.7(6) ? C131' C133' H133'b . . . 111.8(8) ? C131' C133' H133'c . . . 110.8(8) ? C131' C133' H134'Ac . . . 93.7(8) ? C133'A C133' C134'A . . . 106.7(19) ? C133'A C133' H133'a . . . 86.2(12) ? C133'A C133' H133'b . . . 164.2(12) ? C133'A C133' H133'c . . . 65.1(12) ? C133'A C133' H134'Ac . . . 155.2(14) ? C134'A C133' H133'a . . . 87.9(14) ? C134'A C133' H133'b . . . 76.4(15) ? C134'A C133' H133'c . . . 162.2(16) ? C134'A C133' H134'Ac . . . 54.5(15) ? H133'a C133' H133'b . . . 109.6(9) ? H133'a C133' H133'c . . . 106.5(9) ? H133'a C133' H134'Ac . . . 107.0(10) ? H133'b C133' H133'c . . . 107.3(7) ? H133'b C133' H134'Ac . . . 22.0(3) ? H133'c C133' H134'Ac . . . 127.4(9) ? C131' C134' C132'A . . . 60.4(9) ? C131' C134' C134'A . . . 54.8(16) ? C131' C134' H134'a . . . 111.8(8) ? C131' C134' H134'b . . . 109.8(8) ? C131' C134' H134'c . . . 108.5(7) ? C131' C134' H134'Ab . . . 79.7(5) ? C132'A C134' C134'A . . . 110.6(18) ? C132'A C134' H134'a . . . 97.7(10) ? C132'A C134' H134'b . . . 60.5(10) ? C132'A C134' H134'c . . . 153.4(10) ? C132'A C134' H134'Ab . . . 139.7(10) ? C134'A C134' H134'a . . . 85.4(15) ? C134'A C134' H134'b . . . 162.3(16) ? C134'A C134' H134'c . . . 73.5(16) ? C134'A C134' H134'Ab . . . 38.7(15) ? H134'a C134' H134'b . . . 110.2(8) ? H134'a C134' H134'c . . . 109.0(9) ? H134'a C134' H134'Ab . . . 102.7(8) ? H134'b C134' H134'c . . . 107.5(9) ? H134'b C134' H134'Ab . . . 138.1(9) ? H134'c C134' H134'Ab . . . 35.1(3) ? C131' C132'A C132' . . . 55.1(10) ? C131' C132'A C134' . . . 51.7(8) ? C131' C132'A H132'c . . . 91.2(16) ? C131' C132'A H132'Aa . . . 111.1(19) ? C131' C132'A H132'Ab . . . 102.4(16) ? C131' C132'A H132'Ac . . . 119(2) ? C132' C132'A C134' . . . 100.8(15) ? C132' C132'A H132'c . . . 45.2(12) ? C132' C132'A H132'Aa . . . 83(2) ? C132' C132'A H132'Ab . . . 58.5(15) ? C132' C132'A H132'Ac . . . 154(3) ? C134' C132'A H132'c . . . 143(2) ? C134' C132'A H132'Aa . . . 98(2) ? C134' C132'A H132'Ab . . . 153.9(18) ? C134' C132'A H132'Ac . . . 89(2) ? H132'c C132'A H132'Aa . . . 93(3) ? H132'c C132'A H132'Ab . . . 13.3(4) ? H132'c C132'A H132'Ac . . . 116(3) ? H132'Aa C132'A H132'Ab . . . 95(2) ? H132'Aa C132'A H132'Ac . . . 120(3) ? H132'Ab C132'A H132'Ac . . . 104(2) ? C131' C133'A C132' . . . 56.0(14) ? C131' C133'A C133' . . . 54.2(12) ? C131' C133'A H132'b . . . 90(2) ? C131' C133'A H133'Aa . . . 108(3) ? C131' C133'A H133'Ab . . . 112(3) ? C131' C133'A H133'Ac . . . 107(3) ? C132' C133'A C133' . . . 108(2) ? C132' C133'A H132'b . . . 47.0(14) ? C132' C133'A H133'Aa . . . 91(2) ? C132' C133'A H133'Ab . . . 156(3) ? C132' C133'A H133'Ac . . . 60.2(18) ? C133' C133'A H132'b . . . 142(3) ? C133' C133'A H133'Aa . . . 93(2) ? C133' C133'A H133'Ab . . . 71(2) ? C133' C133'A H133'Ac . . . 158(3) ? H132'b C133'A H133'Aa . . . 113(3) ? H132'b C133'A H133'Ab . . . 119(3) ? H132'b C133'A H133'Ac . . . 16.9(6) ? H133'Aa C133'A H133'Ab . . . 113(4) ? H133'Aa C133'A H133'Ac . . . 105(3) ? H133'Ab C133'A H133'Ac . . . 112(3) ? C131' C134'A C133' . . . 72.9(18) ? C131' C134'A C134' . . . 73.6(18) ? C131' C134'A H133'b . . . 100(2) ? C131' C134'A H134'c . . . 101(2) ? C131' C134'A H134'Aa . . . 105(3) ? C131' C134'A H134'Ab . . . 109(3) ? C131' C134'A H134'Ac . . . 95(2) ? C133' C134'A C134' . . . 145(3) ? C133' C134'A H133'b . . . 39.6(10) ? C133' C134'A H134'c . . . 158(2) ? C133' C134'A H134'Aa . . . 84(2) ? C133' C134'A H134'Ab . . . 140(3) ? C133' C134'A H134'Ac . . . 33.0(10) ? C134' C134'A H133'b . . . 161(3) ? C134' C134'A H134'c . . . 43.3(12) ? C134' C134'A H134'Aa . . . 94(2) ? C134' C134'A H134'Ab . . . 64(2) ? C134' C134'A H134'Ac . . . 162(3) ? H133'b C134'A H134'c . . . 124(2) ? H133'b C134'A H134'Aa . . . 105(3) ? H133'b C134'A H134'Ab . . . 104(3) ? H133'b C134'A H134'Ac . . . 6.7(5) ? H134'c C134'A H134'Aa . . . 118(3) ? H134'c C134'A H134'Ab . . . 20.9(11) ? H134'c C134'A H134'Ac . . . 130(3) ? H134'Aa C134'A H134'Ab . . . 130(4) ? H134'Aa C134'A H134'Ac . . . 102(3) ? H134'Ab C134'A H134'Ac . . . 109(3) ? C13' C14' C15' . . . 122.1(5) ? C13' C14' H14' . . . 118.9(5) ? C15' C14' H14' . . . 119.0(5) ? C14' C15' C16' . . . 119.9(4) ? C14' C15' H15' . . . 121.3(5) ? C16' C15' H15' . . . 118.8(5) ? C11' C16' C15' . . . 120.2(4) ? C11' C16' O2' . . . 115.5(4) ? C15' C16' O2' . . . 124.3(4) ? Ag O2 C16 . . . 116.4(2) ? Ag O2 C3 . . . 96.5(2) ? C16 O2 C3 . . . 117.5(3) ? O2 C3 C32 . . . 110.8(3) ? O2 C3 H3a . . . 109.2(4) ? O2 C3 H3b . . . 109.6(4) ? C32 C3 H3a . . . 109.8(4) ? C32 C3 H3b . . . 109.9(4) ? H3a C3 H3b . . . 107.5(4) ? Ag O2' C16' . . . 105.5(2) ? Ag O2' C3' . . . 92.1(2) ? C16' O2' C3' . . . 119.0(3) ? O2' C3' C32' . . . 106.1(4) ? O2' C3' H3'a . . . 111.6(4) ? O2' C3' H3'b . . . 110.6(4) ? C32' C3' H3'a . . . 111.6(4) ? C32' C3' H3'b . . . 110.5(4) ? H3'a C3' H3'b . . . 106.5(5) ? Ag N31 C32 . . . 120.4(3) ? Ag N31 C32' . . . 119.9(3) ? C32 N31 C32' . . . 119.7(4) ? C3 C32 N31 . . . 114.7(4) ? C3 C32 C33 . . . 123.8(4) ? N31 C32 C33 . . . 121.5(4) ? C32 C33 C34 . . . 118.9(4) ? C32 C33 H33 . . . 119.7(5) ? C34 C33 H33 . . . 121.4(5) ? C33 C34 C33' . . . 119.9(5) ? C33 C34 H34 . . . 119.9(5) ? C33' C34 H34 . . . 120.2(6) ? C34 C33' C32' . . . 118.8(5) ? C34 C33' H33' . . . 121.1(5) ? C32' C33' H33' . . . 120.2(5) ? C3' C32' N31 . . . 116.0(4) ? C3' C32' C33' . . . 123.1(4) ? N31 C32' C33' . . . 120.9(4) ? N1' N1 O01 . . . 48.9(17) ? N1' N1 O02 . . . 107(2) ? N1' N1 O02' . . . 82(2) ? N1' N1 O03 . . . 114(2) ? N1' N1 O03' . . . 71.0(18) ? O01 N1 O02 . . . 115.5(11) ? O01 N1 O02' . . . 107.1(9) ? O01 N1 O03 . . . 126.9(10) ? O01 N1 O03' . . . 97.6(9) ? O02 N1 O02' . . . 27.9(7) ? O02 N1 O03 . . . 117.6(12) ? O02 N1 O03' . . . 133.8(12) ? O02' N1 O03 . . . 120.3(10) ? O02' N1 O03' . . . 114.2(10) ? O03 N1 O03' . . . 43.0(6) ? N1 N1' O01 . . . 114(2) ? N1 N1' O02 . . . 54.5(19) ? N1 N1' O02' . . . 79(2) ? N1 N1' O03 . . . 50.0(18) ? N1 N1' O03' . . . 89(2) ? O01 N1' O02 . . . 119.2(8) ? O01 N1' O02' . . . 123.2(7) ? O01 N1' O03 . . . 127.1(7) ? O01 N1' O03' . . . 117.0(8) ? O02 N1' O02' . . . 26.7(6) ? O02 N1' O03 . . . 92.3(8) ? O02 N1' O03' . . . 121.6(9) ? O02' N1' O03 . . . 104.3(7) ? O02' N1' O03' . . . 118.4(8) ? O03 N1' O03' . . . 38.7(5) ? N1 O01 N1' . . . 16.6(6) ? N1 O02 N1' . . . 18.7(7) ? N1 O02 O02' . . . 92.4(15) ? N1 O02 O03 . . . 32.7(7) ? N1' O02 O02' . . . 75.6(12) ? N1' O02 O03 . . . 46.7(5) ? O02' O02 O03 . . . 99.2(13) ? N1 O02' N1' . . . 19.5(6) ? N1 O02' O02 . . . 59.7(13) ? N1' O02' O02 . . . 77.7(13) ? N1 O03 N1' . . . 16.1(6) ? N1 O03 O02 . . . 29.7(7) ? N1 O03 O03' . . . 71.1(8) ? N1' O03 O02 . . . 41.0(5) ? N1' O03 O03' . . . 55.1(7) ? O02 O03 O03' . . . 89.6(7) ? N1 O03' N1' . . . 20.4(7) ? N1 O03' O03 . . . 65.9(8) ? N1' O03' O03 . . . 86.2(8) ? C132 H132a C132A . . . 55.2(13) ? C132 H132a H132Aa . . . 101.2(10) ? C132A H132a H132Aa . . . 46.2(7) ? C132 H132b C132A . . . 66.3(15) ? C132 H132b H132Ac . . . 39.1(6) ? C132A H132b H132Ac . . . 59.4(11) ? C133 H133a C133A . . . 53.4(13) ? C133 H133b C133A . . . 73.9(19) ? C133 H133b H133Ac . . . 144.0(9) ? C133A H133b H133Ac . . . 117.1(12) ? C133 H133c H134Ab . . . 117.5(13) ? C134 H134b C134A . . . 81.9(13) ? C134 H134b H134Ac . . . 133.4(8) ? C134A H134b H134Ac . . . 51.7(9) ? C134 H134c H132Ab . . . 89.7(9) ? C132 H132Aa C132A . . . 48.4(14) ? C132 H132Aa H132a . . . 38.5(6) ? C132A H132Aa H132a . . . 86.7(13) ? C134 H132Ab C132A . . . 86.1(11) ? C134 H132Ab H134c . . . 43.4(6) ? C132A H132Ab H134c . . . 121.9(9) ? C132 H132Ac C132A . . . 74.3(16) ? C132 H132Ac H132b . . . 134.0(7) ? C132A H132Ac H132b . . . 112.1(11) ? C133 H133Ac C133A . . . 67.5(18) ? C133 H133Ac H133b . . . 32.7(8) ? C133A H133Ac H133b . . . 56.7(12) ? C134A H134Ab H133c . . . 98.9(11) ? C134 H134Ac C134A . . . 77.9(13) ? C134 H134Ac H134b . . . 36.6(7) ? C134A H134Ac H134b . . . 114.3(11) ? C132' H132'b C133'A . . . 78(2) ? C132' H132'b H133'Ac . . . 123.6(7) ? C133'A H132'b H133'Ac . . . 64(2) ? C132' H132'c C132'A . . . 86.7(15) ? C132' H132'c H132'Ab . . . 165.9(7) ? C132'A H132'c H132'Ab . . . 107.3(13) ? C133' H133'b C134'A . . . 64.0(15) ? C133' H133'b H134'Ac . . . 45.1(5) ? C134'A H133'b H134'Ac . . . 19.2(14) ? C134' H134'c C134'A . . . 63.3(14) ? C134' H134'c H134'Ab . . . 88.2(5) ? C134'A H134'c H134'Ab . . . 25.6(13) ? C132' H132'Ab C132'A . . . 70.3(13) ? C132' H132'Ab H132'c . . . 11.0(5) ? C132'A H132'Ab H132'c . . . 59.4(12) ? C132' H133'Ac C133'A . . . 73(2) ? C132' H133'Ac H132'b . . . 43.4(5) ? C133'A H133'Ac H132'b . . . 100(2) ? C134' H134'Ab C134'A . . . 78(2) ? C134' H134'Ab H134'c . . . 56.7(5) ? C134'A H134'Ab H134'c . . . 134(2) ? C133' H134'Ac C134'A . . . 92.5(19) ? C133' H134'Ac H133'b . . . 113.0(6) ? C134'A H134'Ac H133'b . . . 154.1(18) ? 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 C0 3.090(4) . . ? Ag C02 2.974(4) . . ? Ag C06 3.119(4) . . ? Ag C1 3.298(4) . . ? Ag C11 3.726(4) . . ? Ag C16 3.461(4) . . ? Ag C1' 3.367(4) . . ? Ag C11' 3.631(4) . . ? Ag C16' 3.386(5) . . ? Ag C3 3.129(4) . . ? Ag C3' 3.146(5) . . ? Ag C32 3.087(4) . . ? Ag C33 3.569(5) . '3 776' ? Ag C32' 3.082(5) . . ? Ag H0b 3.3716(4) . . ? Ag H06 3.1959(4) . . ? Ag H1a 3.2821(4) . . ? Ag H1'a 3.4873(5) . . ? Ag H3a 3.1675(4) . . ? Ag H3'b 3.0618(4) . . ? Ag H33 3.2377(5) . '3 776' ? N0 N01 2.932(5) . . ? N0 C02 2.519(5) . . ? N0 C11 2.535(5) . . ? N0 C11' 2.525(5) . . ? N0 H0a 1.995(3) . . ? N0 H0b 1.990(3) . . ? N0 H1a 1.996(3) . . ? N0 H1b 1.998(3) . . ? N0 H1'a 2.001(3) . . ? N0 H1'b 1.995(3) . . ? C0 N01 2.442(5) . . ? C0 C03 2.524(6) . . ? C0 C1 2.402(6) . . ? C0 C1' 2.438(6) . . ? C0 C11' 2.975(6) . . ? C0 H03 2.693(4) . . ? C0 H1a 2.540(4) . . ? C0 H1b 2.576(4) . . ? C0 H1'b 2.621(4) . . ? N01 C03 2.382(5) . . ? N01 C04 2.780(5) . . ? N01 C05 2.397(5) . . ? N01 H06 2.000(3) . . ? C02 C04 2.396(6) . . ? C02 C05 2.732(6) . . ? C02 C06 2.317(6) . . ? C02 H0a 2.016(4) . . ? C02 H0b 2.013(4) . . ? C02 H03 2.042(4) . . ? C03 C05 2.371(6) . . ? C03 C06 2.708(6) . . ? C03 H0a 2.550(4) . . ? C03 H04 2.043(4) . . ? C04 C06 2.377(6) . . ? C04 H03 2.047(5) . . ? C04 H05 2.050(5) . . ? C05 H04 2.046(4) . . ? C05 H06 2.038(4) . . ? C06 H05 2.046(4) . . ? C1 C12 2.510(6) . . ? C1 C16 2.546(6) . . ? C1 C1' 2.426(6) . . ? C1 O2 2.812(5) . . ? C1 H0b 2.384(4) . . ? C1 H12 2.635(4) . . ? C1 H1'a 2.582(4) . . ? C1 H1'b 2.559(4) . . ? C11 C13 2.444(6) . . ? C11 C14 2.781(6) . . ? C11 C15 2.408(6) . . ? C11 C1' 2.989(6) . . ? C11 O2 2.367(5) . . ? C11 H1a 2.016(4) . . ? C11 H1b 2.024(4) . . ? C11 H12 2.030(4) . . ? C11 H1'a 2.614(4) . . ? C12 C131 2.570(6) . . ? C12 C132 2.903(12) . . ? C12 C132A 2.954(15) . . ? C12 C14 2.370(6) . . ? C12 C15 2.743(6) . . ? C12 C16 2.395(6) . . ? C12 H1b 2.522(4) . . ? C12 H132b 2.654(4) . . ? C13 C132 2.500(11) . . ? C13 C133 2.466(16) . . ? C13 C134 2.487(14) . . ? C13 C132A 2.565(15) . . ? C13 C133A 2.55(2) . . ? C13 C134A 2.539(18) . . ? C13 C15 2.421(6) . . ? C13 C16 2.814(6) . . ? C13 H12 2.047(4) . . ? C13 H132b 2.687(4) . . ? C13 H132c 2.604(4) . . ? C13 H133b 2.651(4) . . ? C13 H133c 2.683(4) . . ? C13 H134c 2.609(4) . . ? C13 H134Ab 2.630(4) . . ? C13 H14 2.035(4) . . ? C131 C14 2.543(6) . . ? C131 H132a 2.067(5) . . ? C131 H132b 2.069(5) . . ? C131 H132c 2.071(5) . . ? C131 H133a 1.986(5) . . ? C131 H133b 1.991(5) . . ? C131 H133c 1.983(5) . . ? C131 H134a 2.054(5) . . ? C131 H134b 2.052(5) . . ? C131 H134c 2.058(5) . . ? C131 H132Aa 2.016(5) . . ? C131 H132Ab 2.016(5) . . ? C131 H132Ac 2.022(5) . . ? C131 H133Aa 2.098(5) . . ? C131 H133Ab 2.104(5) . . ? C131 H133Ac 2.098(5) . . ? C131 H134Aa 2.080(5) . . ? C131 H134Ab 2.081(5) . . ? C131 H134Ac 2.080(5) . . ? C131 H14 2.687(5) . . ? C132 C133 2.481(19) . . ? C132 C134 2.48(2) . . ? C132 C134A 2.96(2) . . ? C132 H12 2.593(13) . . ? C132 H133a 2.623(12) . . ? C132 H133b 2.635(13) . . ? C132 H134a 2.636(15) . . ? C132 H134c 2.661(17) . . ? C132 H132Ab 2.009(18) . . ? C132 H133Aa 2.064(14) . . ? C132 H133Ab 1.690(17) . . ? C133 C134 2.48(3) . . ? C133 C132A 2.62(2) . . ? C133 C14 2.832(15) . . ? C133 H132a 2.621(14) . . ? C133 H134a 2.66(2) . . ? C133 H134b 2.62(2) . . ? C133 H133Aa 1.502(16) . . ? C133 H133Ab 2.081(17) . . ? C133 H134Aa 1.76(2) . . ? C133 H134Ab 1.622(18) . . ? C133 H134Ac 2.50(2) . . ? C133 H14 2.481(14) . . ? C134 C133A 2.97(2) . . ? C134 H132a 2.663(14) . . ? C134 H132b 2.468(16) . . ? C134 H132Aa 1.993(13) . . ? C134 H132Ac 2.448(16) . . ? C134 H134Aa 1.789(17) . . ? C134 H134Ab 2.305(15) . . ? C132A C133A 2.45(3) . . ? C132A C134A 2.44(2) . . ? C132A H12 2.595(15) . . ? C132A H132c 1.97(2) . . ? C132A H134a 1.695(18) . . ? C132A H134b 2.525(17) . . ? C132A H134c 1.67(2) . . ? C132A H133Aa 2.53(2) . . ? C132A H133Ab 2.64(2) . . ? C132A H134Aa 2.665(16) . . ? C132A H134Ac 2.695(17) . . ? C133A C134A 2.54(3) . . ? C133A H132a 2.03(3) . . ? C133A H132c 1.85(4) . . ? C133A H133c 1.98(3) . . ? C133A H132Aa 2.52(2) . . ? C133A H132Ac 2.69(3) . . ? C133A H134Aa 2.66(3) . . ? C134A H133a 1.96(2) . . ? C134A H133b 2.61(2) . . ? C134A H133c 1.54(2) . . ? C134A H134a 1.668(17) . . ? C134A H134c 2.20(2) . . ? C134A H132Aa 2.650(16) . . ? C134A H132Ab 2.579(18) . . ? C14 C16 2.404(6) . . ? C14 H133c 2.649(4) . . ? C14 H134Ab 2.589(4) . . ? C14 H15 2.042(4) . . ? C15 O2 2.435(5) . . ? C15 C3 2.831(6) . . ? C15 H14 2.029(4) . . ? C15 H3b 2.586(4) . . ? C16 C3 2.410(6) . . ? C16 H1a 2.683(4) . . ? C16 H15 2.033(4) . . ? C16 H3b 2.579(4) . . ? C1' C12' 2.520(6) . . ? C1' C16' 2.535(6) . . ? C1' O2' 2.777(5) . . ? C1' H0a 2.441(4) . . ? C1' H1b 2.591(4) . . ? C1' H12' 2.658(4) . . ? C11' C13' 2.458(6) . . ? C11' C14' 2.780(7) . . ? C11' C15' 2.409(6) . . ? C11' O2' 2.344(5) . . ? C11' H1'a 2.030(4) . . ? C11' H1'b 2.053(4) . . ? C11' H12' 2.047(4) . . ? C12' C131' 2.568(7) . . ? C12' C133'A 2.93(3) . . ? C12' C14' 2.361(7) . . ? C12' C15' 2.740(7) . . ? C12' C16' 2.382(6) . . ? C12' H1'b 2.585(4) . . ? C13' C132' 2.462(11) . . ? C13' C133' 2.518(9) . . ? C13' C134' 2.555(9) . . ? C13' C132'A 2.59(2) . . ? C13' C133'A 2.67(3) . . ? C13' C134'A 2.44(3) . . ? C13' C15' 2.422(7) . . ? C13' C16' 2.815(6) . . ? C13' H12' 2.060(5) . . ? C13' H132'b 2.646(5) . . ? C13' H132'c 2.656(5) . . ? C13' H134'c 2.697(5) . . ? C13' H134'Ab 2.487(5) . . ? C13' H134'Ac 2.529(5) . . ? C13' H14' 2.027(5) . . ? C131' C14' 2.547(7) . . ? C131' H132'a 2.020(6) . . ? C131' H132'b 2.020(7) . . ? C131' H132'c 2.011(6) . . ? C131' H133'a 2.108(5) . . ? C131' H133'b 2.111(6) . . ? C131' H133'c 2.127(5) . . ? C131' H134'a 2.081(6) . . ? C131' H134'b 2.072(6) . . ? C131' H134'c 2.066(7) . . ? C131' H132'Aa 2.244(5) . . ? C131' H132'Ab 2.245(6) . . ? C131' H132'Ac 2.231(5) . . ? C131' H133'Aa 2.203(6) . . ? C131' H133'Ab 2.199(6) . . ? C131' H133'Ac 2.202(7) . . ? C131' H134'Aa 1.778(6) . . ? C131' H134'Ab 1.757(7) . . ? C131' H134'Ac 1.772(6) . . ? C131' H14' 2.693(6) . . ? C132' C133' 2.468(14) . . ? C132' C134' 2.476(15) . . ? C132' C134'A 2.53(4) . . ? C132' H133'a 2.661(12) . . ? C132' H133'c 2.688(11) . . ? C132' H134'a 2.696(11) . . ? C132' H134'b 2.694(11) . . ? C132' H132'Aa 1.570(9) . . ? C132' H132'Ac 2.140(12) . . ? C132' H133'Aa 1.638(12) . . ? C132' H133'Ab 2.144(11) . . ? C132' H134'Aa 2.531(12) . . ? C133' C134' 2.470(12) . . ? C133' H132'a 2.669(9) . . ? C133' H132'b 2.675(10) . . ? C133' H134'a 2.633(8) . . ? C133' H134'c 2.634(10) . . ? C133' H133'Aa 2.035(10) . . ? C133' H133'Ab 1.678(11) . . ? C133' H133'Ac 2.675(10) . . ? C133' H134'Aa 1.532(8) . . ? C133' H134'Ab 2.015(10) . . ? C134' C14' 2.864(9) . . ? C134' H132'a 2.662(10) . . ? C134' H133'a 2.660(9) . . ? C134' H133'b 2.665(8) . . ? C134' H132'Aa 2.173(9) . . ? C134' H132'Ac 1.991(9) . . ? C134' H134'Aa 1.603(9) . . ? C134' H134'Ac 2.317(8) . . ? C134' H14' 2.459(8) . . ? C132'A C133'A 2.56(4) . . ? C132'A C134'A 2.56(4) . . ? C132'A H132'a 1.72(3) . . ? C132'A H132'b 2.27(3) . . ? C132'A H134'a 2.16(3) . . ? C132'A H134'b 1.59(3) . . ? C132'A H133'Ac 2.52(3) . . ? C132'A H134'Aa 2.66(3) . . ? C133'A C134'A 2.47(5) . . ? C133'A H12' 2.47(3) . . ? C133'A H132'a 1.54(3) . . ? C133'A H132'c 2.24(3) . . ? C133'A H133'a 1.93(4) . . ? C133'A H133'b 2.66(4) . . ? C133'A H133'c 1.60(3) . . ? C133'A H132'Aa 2.66(3) . . ? C133'A H132'Ab 2.49(3) . . ? C133'A H134'Aa 2.42(4) . . ? C133'A H134'Ac 2.42(4) . . ? C134'A H133'a 1.61(3) . . ? C134'A H133'c 2.28(3) . . ? C134'A H134'a 1.51(3) . . ? C134'A H134'b 2.19(3) . . ? C134'A H133'Aa 2.62(3) . . ? C14' C16' 2.405(7) . . ? C14' H15' 2.076(5) . . ? C15' O2' 2.447(6) . . ? C15' C3' 2.877(7) . . ? C15' H14' 2.040(5) . . ? C16' C3' 2.429(6) . . ? C16' H1'a 2.671(4) . . ? C16' H15' 2.048(5) . . ? C16' H3'b 2.621(4) . . ? O2 N31 2.714(5) . . ? O2 C32 2.424(6) . . ? O2 H1a 2.590(3) . . ? O2 H15 2.641(3) . . ? O2 H3a 1.981(3) . . ? O2 H3b 1.978(3) . . ? C3 N31 2.401(6) . . ? C3 C33 2.548(7) . . ? C3 H15 2.513(4) . . ? O2' N31 2.695(5) . . ? O2' C32' 2.346(5) . . ? O2' H1'a 2.534(3) . . ? O2' H134'b 2.648(3) . '4 574' ? O2' H15' 2.652(3) . . ? O2' H3'a 2.003(3) . . ? O2' H3'b 2.003(3) . . ? C3' N31 2.413(6) . . ? C3' C33' 2.543(7) . . ? C3' H15' 2.563(5) . . ? N31 C33 2.383(6) . . ? N31 C34 2.755(7) . . ? N31 C33' 2.389(6) . . ? C32 C34 2.379(8) . . ? C32 C33' 2.736(7) . . ? C32 C32' 2.330(7) . . ? C32 H3a 2.045(5) . . ? C32 H3b 2.040(5) . . ? C32 H33 2.048(4) . . ? C33 C33' 2.389(7) . . ? C33 C32' 2.741(6) . . ? C33 H3b 2.634(5) . . ? C33 H34 2.044(5) . . ? C34 C32' 2.391(7) . . ? C34 H33 2.061(6) . . ? C34 H33' 2.056(6) . . ? C33' H3'a 2.633(5) . . ? C33' H34 2.049(5) . . ? C32' H3'a 2.054(5) . . ? C32' H3'b 2.051(5) . . ? C32' H33' 2.062(5) . . ? N1' H3'a 2.590(9) . '1 545' ? O01 O02 2.127(12) . . ? O01 O02' 2.159(7) . . ? O01 O03 2.337(8) . . ? O01 O03' 2.001(8) . . ? O01 H0b 2.519(4) . . ? O01 H3'a 2.589(4) . '1 545' ? O02 O03' 2.182(13) . . ? O02 H04 2.508(11) . '4 564' ? O02 H34 2.470(11) . '3 776' ? O02' O03 2.170(9) . . ? O02' O03' 2.138(10) . . ? O02' H04 2.592(6) . '4 564' ? O02' H05 2.448(6) . '2 746' ? O02' H05 2.655(6) . '4 564' ? O02' H06 2.612(6) . '2 746' ? O02' H33' 2.474(6) . '1 545' ? O03 H06 2.469(7) . '2 746' ? O03 H15 2.665(7) . '4 565' ? O03 H3b 2.412(7) . '4 565' ? O03' H06 2.386(8) . '2 746' ? O03' H15 2.340(8) . '4 565' ? O03' H3b 2.605(8) . '4 565' ? O03' H33 2.300(8) . '4 565' ? H0a H0b 1.55159(10) . . ? H0a H03 2.3619(3) . . ? H0a H1'b 2.29919(14) . . ? H0b H1a 2.1832(3) . . ? H03 H04 2.35345(18) . . ? H04 H05 2.3711(2) . . ? H05 H06 2.3398(3) . . ? H1a H1b 1.55182(16) . . ? H1b H12 2.29071(17) . . ? H1b H1'b 2.35404(16) . . ? H12 H132b 2.05617(19) . . ? H12 H132Ac 2.2010(2) . . ? H132a H132b 1.55101(11) . . ? H132a H132c 1.55124(11) . . ? H132a H132Ab 2.20784(17) . . ? H132a H132Ac 1.38616(9) . . ? H132a H133Aa 1.77599(14) . . ? H132a H133Ab 2.02790(14) . . ? H132a H1'b 2.2916(2) . '3 676' ? H132b H132c 2.3507(2) . '3 676' ? H132b H132c 1.55092(13) . . ? H132b H134c 2.30290(15) . . ? H132b H132Aa 1.68437(16) . . ? H132b H132Ab 1.53778(11) . . ? H132c H132Aa 2.32207(14) . . ? H132c H132Ac 2.3973(3) . '3 676' ? H132c H132Ac 1.48132(12) . . ? H132c H133Aa 2.2541(3) . . ? H132c H133Ab 1.24166(10) . . ? H133a H133b 1.55147(10) . . ? H133a H133c 1.55205(16) . . ? H133a H133Aa 1.04982(9) . . ? H133a H133Ab 2.3208(2) . . ? H133a H133Ac 1.59811(10) . . ? H133a H134Aa 1.62516(13) . . ? H133a H134Ab 2.19771(17) . . ? H133b H133c 1.55098(11) . . ? H133b H133Aa 1.52928(16) . . ? H133b H133Ab 1.53665(16) . . ? H133c H133Aa 2.33735(18) . . ? H133c H133Ac 1.61664(11) . . ? H133c H134Aa 1.77663(13) . . ? H133c H134Ac 2.3475(2) . . ? H133c H14 2.0639(2) . . ? H134a H134b 1.55178(15) . . ? H134a H134c 1.55103(11) . . ? H134a H132Aa 1.61047(11) . . ? H134a H132Ab 1.53795(19) . . ? H134a H134Aa 1.57249(12) . . ? H134a H134Ac 1.71342(17) . . ? H134b H134c 1.55082(17) . . ? H134b H132Ab 2.2534(2) . . ? H134b H134Aa 1.66532(10) . . ? H134b H134Ab 1.80065(12) . . ? H134c H132Aa 2.29839(16) . . ? H134c H132Ac 2.33775(15) . . ? H134c H134Ac 1.81974(19) . . ? H132Aa H132Ab 1.55127(10) . . ? H132Aa H132Ac 1.55087(15) . . ? H132Aa H133Aa 2.22539(16) . . ? H132Ab H132Ac 1.55088(11) . . ? H133Aa H133Ab 1.55096(13) . . ? H133Aa H133Ac 1.55191(16) . . ? H133Ab H133Ac 1.55098(16) . . ? H133Ab H133'b 2.16605(18) . '4 574' ? H133Ab H134'Ab 2.37523(15) . '4 574' ? H133Ab H134'Ac 2.35895(19) . '4 574' ? H134Aa H134Ab 1.55195(16) . . ? H134Aa H134Ac 1.55133(10) . . ? H134Aa H133'c 2.19397(18) . '3 676' ? H134Ab H134Ac 1.55110(11) . . ? H134Ab H14 2.11909(15) . . ? H14 H15 2.3296(2) . . ? H15 H3b 2.04879(17) . . ? H1'a H1'b 1.55119(10) . . ? H1'b H12' 2.3676(3) . . ? H12' H133'c 2.28292(17) . . ? H12' H133'Ab 2.10122(19) . . ? H132'a H132'b 1.55075(16) . . ? H132'a H132'c 1.55185(15) . . ? H132'a H132'Aa 1.32600(9) . . ? H132'a H132'Ab 1.77841(18) . . ? H132'a H133'Aa 1.24729(11) . . ? H132'a H133'Ac 1.58556(15) . . ? H132'a H134'Aa 2.37357(17) . . ? H132'b H132'c 1.55153(11) . . ? H132'b H132'Ab 1.73872(13) . . ? H132'b H133'Aa 1.70593(14) . . ? H132'b H133'Ab 1.70443(15) . . ? H132'c H132'Aa 1.43501(12) . . ? H132'c H132'Ac 1.56835(12) . . ? H132'c H133'Ac 1.82230(13) . . ? H133'a H133'b 1.55379(13) . . ? H133'a H133'c 1.55384(16) . . ? H133'a H133'Aa 1.72955(12) . . ? H133'a H133'Aa 2.33753(17) . '3 677' ? H133'a H133'Ab 2.00556(13) . . ? H133'a H134'Aa 1.21812(8) . . ? H133'a H134'Ab 2.37125(16) . . ? H133'a H134'Ac 1.35970(10) . . ? H133'b H133'c 1.55092(14) . . ? H133'b H134'Aa 1.8809(2) . . ? H133'b H134'Ab 1.80714(12) . . ? H133'c H133'Aa 2.0944(2) . . ? H133'c H133'Ab 1.03967(7) . . ? H133'c H134'Ac 1.53429(12) . . ? H134'a H134'b 1.55175(15) . . ? H134'a H134'c 1.55087(13) . . ? H134'a H132'Aa 2.07803(15) . . ? H134'a H134'Aa 1.27831(10) . . ? H134'a H134'Ab 1.64194(18) . . ? H134'b H134'c 1.55130(11) . . ? H134'b H132'Aa 2.07588(15) . . ? H134'b H132'Ac 1.35177(10) . . ? H134'b H134'Ab 1.97496(16) . . ? H134'b H14' 2.1577(2) . . ? H134'c H134'Aa 1.94920(13) . . ? H134'c H134'Ac 2.21410(15) . . ? H134'c H14' 2.27781(19) . . ? H132'Aa H132'Ab 1.55113(11) . . ? H132'Aa H132'Ac 1.55149(11) . . ? H132'Ab H132'Ac 1.55096(13) . . ? H132'Ab H133'Ac 2.01056(16) . . ? H133'Aa H133'Ab 1.5508(2) . . ? H133'Aa H133'Ac 1.55148(11) . . ? H133'Aa H134'Aa 2.2163(2) . . ? H133'Ab H133'Ac 1.55155(12) . . ? H133'Ab H134'Ac 2.3623(2) . . ? H134'Aa H134'Ab 1.55125(10) . . ? H134'Aa H134'Ac 1.55084(19) . . ? H134'Ab H134'Ac 1.55137(10) . . ? H14' H15' 2.3665(2) . . ? H15' H3'a 2.3441(3) . . ? H15' H3'b 2.38028(17) . . ? H3a H3b 1.55116(14) . . ? H3'a H3'b 1.55114(9) . . ? H33 H34 2.3712(2) . . ? H34 H33' 2.3698(2) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1464 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 24 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .736 _reflns_d_resolution_low 18.229 _diffrn_reflns_av_sigmaI/netI .151 _diffrn_reflns_theta_min 1.11 _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 ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .106 _refine_ls_wR_factor_all .068 _refine_ls_goodness_of_fit_all 1.363 _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 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #==END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_ll100 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C35 H41 Cl1 N4 O9 Pb1' _chemical_formula_moiety ? _chemical_formula_weight 904.39 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_c_c_n _symmetry_space_group_name_Hall -p_2ab_2ac loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2-y,+z 1/2+x,-y,1/2-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z 1/2-x,+y,1/2+z +x,1/2-y,1/2+z _cell_length_a 26.4940(17) _cell_length_b 12.4426(8) _cell_length_c 22.0460(14) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 7267.6(8) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8013 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 4.775 _exptl_crystal_description plate _exptl_crystal_size_max .40 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .10 _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 .327 _exptl_absorpt_correction_T_max .564 _diffrn_reflns_number 84511 _reflns_number_total 9438 _reflns_Friedel_coverage ? _reflns_number_gt 5639 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.15 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .032 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _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 #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 5639 #ActaC _refine_ls_number_parameters 464 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .077 #ActaC _refine_ls_R_factor_gt .033 #ActaC _refine_ls_wR_factor_all .045 #ActaC _refine_ls_wR_factor_ref .04 #ActaC _refine_ls_goodness_of_fit_all 1.104 #ActaC _refine_ls_goodness_of_fit_ref 1.276 #ActaC _refine_ls_shift/su_max .052 #ActaC _refine_ls_shift/su_mean .003 #ActaC _refine_diff_density_min -.714 #ActaC _refine_diff_density_max 1.132 #ActaC # 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' _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 ? 0 280 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 328 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 72 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132019 .158997 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pb ? 0 8 -4.133 10.102 '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 Pb .388835(7) .772195(17) .426444(8) .04649(12) Uani ? ? 1.00000 ? ? N0 .39310(13) .7815(3) .31069(17) .038(2) Uani ? ? 1.00000 ? ? C0 .41710(18) .8871(4) .2984(2) .048(3) Uani ? ? 1.00000 ? ? N01 .46254(16) .8756(3) .3935(2) .053(3) Uani ? ? 1.00000 ? ? C02 .4630(2) .9104(4) .3356(2) .047(3) Uani ? ? 1.00000 ? ? C03 .5024(2) .9688(4) .3134(2) .061(4) Uani ? ? 1.00000 ? ? C04 .5427(2) .9922(5) .3515(3) .079(5) Uani ? ? 1.00000 ? ? C05 .5416(2) .9607(6) .4097(3) .081(5) Uani ? ? 1.00000 ? ? C06 .5020(2) .9005(5) .4301(2) .069(4) Uani ? ? 1.00000 ? ? C1 .34030(16) .7881(4) .2859(2) .044(3) Uani ? ? 1.00000 ? ? C11 .31294(15) .6816(4) .2791(2) .042(3) Uani ? ? 1.00000 ? ? C12 .30469(16) .6417(4) .2215(2) .044(3) Uani ? ? 1.00000 ? ? C13 .27953(17) .5457(4) .2105(2) .048(3) Uani ? ? 1.00000 ? ? C131 .2699(2) .5039(5) .1472(2) .061(4) Uani ? ? 1.00000 ? ? C132 .3056(6) .4215(12) .1313(4) .256(14) Uani ? ? 1.00000 ? ? C133 .2730(5) .5874(7) .0997(4) .187(10) Uani ? ? 1.00000 ? ? C134 .2189(4) .4606(14) .1420(4) .285(16) Uani ? ? 1.00000 ? ? C14 .26312(18) .4890(4) .2612(2) .052(3) Uani ? ? 1.00000 ? ? C15 .2702(2) .5272(5) .3200(2) .051(3) Uani ? ? 1.00000 ? ? C16 .29455(17) .6245(4) .3286(2) .043(3) Uani ? ? 1.00000 ? ? C1' .42076(15) .6949(3) .2779(2) .035(2) Uani ? ? 1.00000 ? ? C11' .47677(16) .6886(4) .29144(19) .037(2) Uani ? ? 1.00000 ? ? C12' .51247(17) .7186(4) .2477(2) .042(3) Uani ? ? 1.00000 ? ? C13' .56364(17) .7064(4) .2559(2) .045(3) Uani ? ? 1.00000 ? ? C131' .5999(2) .7420(5) .2053(3) .061(4) Uani ? ? 1.00000 ? ? C132' .5993(2) .8660(6) .2024(3) .082(5) Uani ? ? 1.00000 ? ? C133' .5829(2) .6979(5) .1438(3) .073(4) Uani ? ? 1.00000 ? ? C134' .6541(2) .7040(6) .2167(3) .092(5) Uani ? ? 1.00000 ? ? C14' .57919(18) .6612(5) .3092(3) .057(4) Uani ? ? 1.00000 ? ? C15' .5451(2) .6297(5) .3541(2) .058(3) Uani ? ? 1.00000 ? ? C16' .49478(17) .6447(4) .3450(2) .042(3) Uani ? ? 1.00000 ? ? O2 .29998(11) .6733(3) .38525(14) .049(2) Uani ? ? 1.00000 ? ? C3 .2885(2) .6094(5) .4373(2) .059(3) Uani ? ? 1.00000 ? ? O2' .45794(12) .6205(3) .38737(15) .056(2) Uani ? ? 1.00000 ? ? C3' .4654(2) .5299(4) .4256(2) .052(3) Uani ? ? 1.00000 ? ? N31 .37571(15) .5560(3) .43452(16) .045(3) Uani ? ? 1.00000 ? ? C32 .3285(2) .5245(4) .4485(2) .050(3) Uani ? ? 1.00000 ? ? C33 .3195(2) .4249(5) .4735(2) .063(4) Uani ? ? 1.00000 ? ? C34 .3593(3) .3574(5) .4854(2) .069(4) Uani ? ? 1.00000 ? ? C33' .4079(2) .3902(5) .4712(2) .058(4) Uani ? ? 1.00000 ? ? C32' .4145(2) .4903(4) .4453(2) .045(3) Uani ? ? 1.00000 ? ? Cl1 .41858(7) .69826(14) .58115(7) .0721(11) Uani ? ? 1.00000 ? ? O11 .4507(2) .7172(5) .5306(2) .128(5) Uani ? ? 1.00000 ? ? O12 .3666(3) .6995(10) .5606(4) .126(8) Uani ? ? 0.65000 ? ? O13 .4275(8) .6065(15) .6100(11) .32(2) Uani ? ? 0.65000 ? ? O14 .4187(6) .7798(11) .6205(6) .196(13) Uani ? ? 0.65000 ? ? O12' .3993(7) .5923(17) .5730(7) .098(6) Uiso ? ? 0.35000 ? ? O13' .4516(6) .6716(15) .6295(7) .085(6) Uiso ? ? 0.35000 ? ? O14' .3891(8) .769(2) .5815(11) .122(8) Uiso ? ? 0.35000 ? ? N .34502(15) 1.0086(3) .44734(18) .039(2) Uani ? ? 1.00000 ? ? O01 .33627(15) .9439(4) .4041(2) .082(3) Uani ? ? 1.00000 ? ? O02 .3794(2) .9851(5) .4782(2) .126(5) Uani ? ? 1.00000 ? ? O03 .3178(2) 1.0816(4) .4549(2) .095(4) Uani ? ? 1.00000 ? ? H0a .39235 .94341 .30566 .05900 Uiso ? ? 1.00000 ? ? H0b .42583 .89117 .25603 .05900 Uiso ? ? 1.00000 ? ? H03 .50295 .99153 .27084 .07400 Uiso ? ? 1.00000 ? ? H04 .57048 1.03574 .33665 .09500 Uiso ? ? 1.00000 ? ? H05 .56880 .97674 .43712 .10100 Uiso ? ? 1.00000 ? ? H06 .50150 .87498 .47158 .08600 Uiso ? ? 1.00000 ? ? H1a .34103 .82274 .24693 .05300 Uiso ? ? 1.00000 ? ? H1b .32024 .83323 .31245 .05300 Uiso ? ? 1.00000 ? ? H1'a .41582 .70377 .23552 .04800 Uiso ? ? 1.00000 ? ? H1'b .40583 .62680 .28956 .04800 Uiso ? ? 1.00000 ? ? H12 .31711 .68162 .18670 .05700 Uiso ? ? 1.00000 ? ? H132a .29661 .39221 .09225 .34200 Uiso ? ? 1.00000 ? ? H132b .29850 .36058 .16029 .34200 Uiso ? ? 1.00000 ? ? H132c .33728 .44195 .13438 .34200 Uiso ? ? 1.00000 ? ? H133a .26497 .55706 .06139 .23700 Uiso ? ? 1.00000 ? ? H133b .30475 .61877 .09951 .23700 Uiso ? ? 1.00000 ? ? H133c .24771 .64188 .10861 .23700 Uiso ? ? 1.00000 ? ? H134a .21502 .43185 .10138 .36100 Uiso ? ? 1.00000 ? ? H134b .19533 .50712 .15225 .36100 Uiso ? ? 1.00000 ? ? H134c .21843 .39633 .16871 .36100 Uiso ? ? 1.00000 ? ? H12' .49960 .75046 .21011 .05200 Uiso ? ? 1.00000 ? ? H132'a .62193 .89267 .17114 .11200 Uiso ? ? 1.00000 ? ? H132'b .61073 .89703 .24017 .11200 Uiso ? ? 1.00000 ? ? H132'c .56656 .89369 .19401 .11200 Uiso ? ? 1.00000 ? ? H133'a .60616 .71700 .11250 .11100 Uiso ? ? 1.00000 ? ? H133'b .55032 .72330 .13338 .11100 Uiso ? ? 1.00000 ? ? H133'c .58157 .62003 .14541 .11100 Uiso ? ? 1.00000 ? ? H134'a .67706 .73104 .18655 .13900 Uiso ? ? 1.00000 ? ? H134'b .65669 .62842 .21815 .13900 Uiso ? ? 1.00000 ? ? H134'c .66624 .73188 .25571 .13900 Uiso ? ? 1.00000 ? ? H14 .24628 .42102 .25536 .06500 Uiso ? ? 1.00000 ? ? H15 .25831 .48618 .35428 .06400 Uiso ? ? 1.00000 ? ? H14' .61507 .64893 .31612 .07100 Uiso ? ? 1.00000 ? ? H15' .55766 .59873 .39166 .07200 Uiso ? ? 1.00000 ? ? H3a .25626 .57420 .43178 .07200 Uiso ? ? 1.00000 ? ? H3b .28587 .65421 .47235 .07200 Uiso ? ? 1.00000 ? ? H3'a .48362 .47454 .40412 .06800 Uiso ? ? 1.00000 ? ? H3'b .48544 .54892 .46055 .06800 Uiso ? ? 1.00000 ? ? H33 .28465 .40251 .48252 .07900 Uiso ? ? 1.00000 ? ? H34 .35349 .28779 .50308 .08700 Uiso ? ? 1.00000 ? ? H33' .43616 .34334 .47964 .07100 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 Pb .04992(12) .05250(13) .03706(10) .00211(10) -.00168(9) -.00401(9) N0 .038(2) .039(2) .036(2) .0031(18) -.0058(16) -.0028(16) C0 .049(3) .040(3) .054(3) .005(2) -.004(2) -.001(2) N01 .054(3) .054(3) .051(3) .000(2) -.005(2) -.010(2) C02 .051(3) .039(3) .052(3) .003(2) -.003(2) -.003(2) C03 .072(4) .051(4) .061(3) -.013(3) -.007(3) .004(3) C04 .069(4) .084(5) .085(5) -.033(4) -.006(4) .001(4) C05 .063(4) .096(5) .085(5) -.025(4) -.025(4) -.006(4) C06 .068(4) .085(5) .053(3) -.010(3) -.016(3) -.016(3) C1 .037(3) .047(3) .047(3) .011(2) -.009(2) .000(2) C11 .026(2) .049(3) .050(3) .004(2) -.003(2) .000(2) C12 .034(3) .058(3) .041(3) -.003(2) -.008(2) .002(2) C13 .036(3) .063(4) .045(3) .000(2) -.006(2) -.002(2) C131 .063(4) .070(4) .049(3) -.016(3) -.010(3) -.005(3) C132 .334(17) .337(17) .096(7) .231(15) -.092(9) -.120(9) C133 .374(16) .118(8) .070(5) -.092(9) -.094(8) .014(5) C134 .220(12) .58(3) .055(5) -.281(16) -.013(7) -.028(10) C14 .038(3) .064(4) .055(3) -.010(2) -.005(2) -.004(3) C15 .043(3) .068(4) .043(3) -.004(3) -.001(2) .006(2) C16 .031(3) .054(3) .044(3) .007(2) -.003(2) -.003(2) C1' .032(2) .035(3) .039(2) .0016(19) .000(2) -.004(2) C11' .040(3) .033(2) .037(2) .002(2) -.003(2) -.0002(19) C12' .046(3) .040(3) .040(2) .000(2) -.003(2) .006(2) C13' .041(3) .038(3) .056(3) .003(2) .001(2) .007(2) C131' .043(3) .061(4) .080(4) .001(2) .014(3) .022(3) C132' .075(4) .069(5) .101(5) -.009(3) .012(4) .025(4) C133' .081(4) .076(5) .061(4) -.005(3) .030(3) .015(3) C134' .047(4) .111(6) .119(6) .009(3) .018(4) .044(5) C14' .032(3) .075(4) .064(4) .008(3) -.004(2) .010(3) C15' .053(3) .076(4) .046(3) .013(3) -.006(3) .018(3) C16' .041(3) .050(3) .036(2) .010(2) .004(2) .008(2) O2 .0413(19) .063(2) .0416(19) .0053(17) .0022(14) -.0042(17) C3 .050(3) .087(4) .040(3) .000(3) .008(2) -.004(3) O2' .046(2) .069(3) .053(2) .0186(18) .0097(17) .0267(18) C3' .054(3) .055(3) .046(3) .009(3) -.001(3) .018(3) N31 .051(3) .048(3) .037(2) -.002(2) .0011(18) -.0004(18) C32 .056(3) .061(4) .032(2) -.010(3) .008(2) -.009(2) C33 .070(4) .071(4) .047(3) -.017(3) .014(3) -.005(3) C34 .103(5) .050(4) .055(4) -.011(4) .012(3) .001(3) C33' .078(4) .051(4) .045(3) .005(3) .005(3) .004(2) C32' .056(3) .047(3) .031(2) .006(3) -.004(2) .000(2) Cl1 .0883(12) .0736(12) .0545(9) .0088(9) -.0039(8) -.0071(8) O11 .096(4) .219(7) .068(3) -.020(4) .008(3) .006(4) O12 .072(6) .222(13) .085(6) -.031(7) .003(4) -.031(6) O13 .28(2) .172(16) .50(3) .068(17) -.02(2) .19(2) O14 .241(14) .202(14) .144(10) -.056(11) .006(10) -.128(10) N .029(2) .046(3) .042(2) .007(2) .0070(17) .000(2) O01 .065(3) .093(3) .089(3) .021(2) -.019(2) -.029(3) O02 .103(4) .166(6) .108(4) .033(4) -.036(3) -.063(4) O03 .110(4) .071(3) .104(4) -.007(3) .018(3) -.008(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 Pb N0 . . 2.557(4) ? Pb N01 . . 2.449(4) ? Pb O2 . . 2.807(3) ? Pb O2' . . 2.767(3) ? Pb N31 . . 2.718(4) ? Pb O11 . . 2.903(5) ? Pb O01 . . 2.597(5) ? Pb O02 . . 2.895(6) ? N0 C0 . . 1.485(6) ? N0 C1 . . 1.504(6) ? N0 C1' . . 1.490(5) ? C0 C02 . . 1.495(7) ? C0 H0a . . .973(5) ? C0 H0b . . .964(4) ? N01 C02 . . 1.348(6) ? N01 C06 . . 1.356(7) ? C02 C03 . . 1.363(7) ? C03 C04 . . 1.389(8) ? C03 H03 . . .980(4) ? C04 C05 . . 1.342(9) ? C04 H04 . . .971(6) ? C05 C06 . . 1.365(8) ? C05 H05 . . .962(6) ? C06 H06 . . .968(5) ? C1 C11 . . 1.518(7) ? C1 H1a . . .961(5) ? C1 H1b . . .970(5) ? C11 C12 . . 1.381(6) ? C11 C16 . . 1.390(6) ? C12 C13 . . 1.389(7) ? C12 H12 . . .971(5) ? C13 C131 . . 1.511(6) ? C13 C14 . . 1.391(6) ? C131 C132 . . 1.438(16) ? C131 C133 . . 1.477(10) ? C131 C134 . . 1.459(13) ? C132 H132a . . .965(10) ? C132 H132b . . 1.009(13) ? C132 H132c . . .880(16) ? C133 H133a . . .949(9) ? C133 H133b . . .927(13) ? C133 H133c . . .973(11) ? C134 H134a . . .970(10) ? C134 H134b . . .881(14) ? C134 H134c . . .993(15) ? C14 C15 . . 1.393(6) ? C14 H14 . . .965(5) ? C15 C16 . . 1.385(8) ? C15 H15 . . .965(5) ? C16 O2 . . 1.396(6) ? C1' C11' . . 1.516(6) ? C1' H1'a . . .950(4) ? C1' H1'b . . .970(4) ? C11' C12' . . 1.401(6) ? C11' C16' . . 1.386(6) ? C12' C13' . . 1.376(6) ? C12' H12' . . .980(5) ? C13' C131' . . 1.537(8) ? C13' C14' . . 1.366(8) ? C131' C132' . . 1.544(10) ? C131' C133' . . 1.530(9) ? C131' C134' . . 1.533(8) ? C132' H132'a . . .972(6) ? C132' H132'b . . .967(7) ? C132' H132'c . . .951(6) ? C133' H133'a . . .955(6) ? C133' H133'b . . .947(5) ? C133' H133'c . . .970(6) ? C134' H134'a . . .962(6) ? C134' H134'b . . .943(7) ? C134' H134'c . . .982(7) ? C14' C15' . . 1.396(8) ? C14' H14' . . .975(5) ? C15' C16' . . 1.361(7) ? C15' H15' . . .972(5) ? C16' O2' . . 1.384(6) ? O2 C3 . . 1.429(6) ? C3 C32 . . 1.517(8) ? C3 H3a . . .968(5) ? C3 H3b . . .955(5) ? O2' C3' . . 1.421(6) ? C3' C32' . . 1.500(7) ? C3' H3'a . . .965(5) ? C3' H3'b . . .965(5) ? N31 C32 . . 1.347(7) ? N31 C32' . . 1.335(6) ? C32 C33 . . 1.377(8) ? C33 C34 . . 1.373(9) ? C33 H33 . . .985(5) ? C34 C33' . . 1.387(9) ? C34 H34 . . .962(6) ? C33' C32' . . 1.381(8) ? C33' H33' . . .967(6) ? Cl1 O11 . . 1.422(5) ? Cl1 O12 . . 1.450(8) ? Cl1 O13 . . 1.33(2) ? Cl1 O14 . . 1.335(14) ? Cl1 O12' . . 1.43(2) ? Cl1 O13' . . 1.418(16) ? Cl1 O14' . . 1.18(2) ? O12 O12' . . 1.61(2) ? O12 O14' . . 1.15(3) ? O13 O12' . . 1.12(3) ? O13 O13' . . 1.12(3) ? O14 O13' . . 1.62(2) ? O14 O14' . . 1.17(3) ? N O01 . . 1.269(6) ? N O02 . . 1.174(6) ? N O03 . . 1.172(6) ? 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 N0 Pb N01 . . . 69.20(13) ? N0 Pb O2 . . . 74.58(10) ? N0 Pb O2' . . . 72.00(11) ? N0 Pb N31 . . . 96.65(11) ? N0 Pb O11 . . . 140.82(13) ? N0 Pb O01 . . . 78.30(13) ? N0 Pb O02 . . . 110.84(13) ? N01 Pb O2 . . . 143.43(12) ? N01 Pb O2' . . . 74.84(12) ? N01 Pb N31 . . . 129.90(12) ? N01 Pb O11 . . . 84.73(15) ? N01 Pb O01 . . . 86.51(13) ? N01 Pb O02 . . . 72.84(14) ? O2 Pb O2' . . . 98.93(10) ? O2 Pb N31 . . . 58.68(11) ? O2 Pb O11 . . . 128.76(13) ? O2 Pb O01 . . . 81.35(12) ? O2 Pb O02 . . . 117.14(13) ? O2' Pb N31 . . . 55.25(11) ? O2' Pb O11 . . . 73.25(13) ? O2' Pb O01 . . . 148.96(12) ? O2' Pb O02 . . . 143.51(13) ? N31 Pb O11 . . . 77.71(14) ? N31 Pb O01 . . . 139.27(13) ? N31 Pb O02 . . . 150.30(12) ? O11 Pb O01 . . . 130.29(15) ? O11 Pb O02 . . . 87.29(15) ? O01 Pb O02 . . . 43.60(14) ? Pb N0 C0 . . . 104.0(3) ? Pb N0 C1 . . . 108.9(2) ? Pb N0 C1' . . . 118.2(3) ? C0 N0 C1 . . . 106.5(3) ? C0 N0 C1' . . . 109.9(3) ? C1 N0 C1' . . . 108.7(3) ? N0 C0 C02 . . . 114.8(4) ? N0 C0 H0a . . . 108.6(4) ? N0 C0 H0b . . . 109.0(4) ? C02 C0 H0a . . . 108.6(4) ? C02 C0 H0b . . . 109.0(4) ? H0a C0 H0b . . . 106.5(4) ? Pb N01 C02 . . . 117.2(3) ? Pb N01 C06 . . . 123.9(3) ? C02 N01 C06 . . . 118.9(4) ? C0 C02 N01 . . . 116.7(4) ? C0 C02 C03 . . . 122.0(4) ? N01 C02 C03 . . . 121.2(5) ? C02 C03 C04 . . . 118.9(5) ? C02 C03 H03 . . . 120.6(5) ? C04 C03 H03 . . . 120.5(5) ? C03 C04 C05 . . . 120.0(5) ? C03 C04 H04 . . . 119.7(6) ? C05 C04 H04 . . . 120.1(6) ? C04 C05 C06 . . . 119.5(5) ? C04 C05 H05 . . . 121.6(6) ? C06 C05 H05 . . . 118.9(6) ? N01 C06 C05 . . . 121.4(5) ? N01 C06 H06 . . . 118.5(5) ? C05 C06 H06 . . . 120.1(5) ? N0 C1 C11 . . . 115.6(4) ? N0 C1 H1a . . . 109.3(4) ? N0 C1 H1b . . . 108.8(4) ? C11 C1 H1a . . . 108.2(4) ? C11 C1 H1b . . . 107.7(4) ? H1a C1 H1b . . . 106.9(5) ? C1 C11 C12 . . . 118.7(4) ? C1 C11 C16 . . . 122.4(4) ? C12 C11 C16 . . . 118.9(4) ? C11 C12 C13 . . . 123.1(4) ? C11 C12 H12 . . . 119.3(5) ? C13 C12 H12 . . . 117.7(4) ? C12 C13 C131 . . . 122.6(4) ? C12 C13 C14 . . . 116.5(4) ? C131 C13 C14 . . . 121.0(4) ? C13 C131 C132 . . . 111.1(6) ? C13 C131 C133 . . . 113.8(6) ? C13 C131 C134 . . . 110.9(5) ? C132 C131 C133 . . . 107.0(7) ? C132 C131 C134 . . . 109.1(10) ? C133 C131 C134 . . . 104.8(8) ? C131 C132 H132a . . . 108.9(12) ? C131 C132 H132b . . . 105.0(10) ? C131 C132 H132c . . . 113.7(13) ? H132a C132 H132b . . . 103.6(14) ? H132a C132 H132c . . . 114.4(13) ? H132b C132 H132c . . . 110.3(13) ? C131 C133 H133a . . . 109.8(8) ? C131 C133 H133b . . . 110.5(9) ? C131 C133 H133c . . . 108.0(9) ? H133a C133 H133b . . . 111.5(11) ? H133a C133 H133c . . . 107.6(11) ? H133b C133 H133c . . . 109.4(9) ? C131 C134 H134a . . . 107.9(8) ? C131 C134 H134b . . . 113.2(14) ? C131 C134 H134c . . . 105.2(9) ? H134a C134 H134b . . . 113.8(11) ? H134a C134 H134c . . . 104.4(16) ? H134b C134 H134c . . . 111.6(10) ? C13 C14 C15 . . . 122.2(5) ? C13 C14 H14 . . . 118.8(4) ? C15 C14 H14 . . . 119.0(5) ? C14 C15 C16 . . . 119.2(5) ? C14 C15 H15 . . . 120.3(6) ? C16 C15 H15 . . . 120.5(5) ? C11 C16 C15 . . . 120.2(4) ? C11 C16 O2 . . . 116.3(4) ? C15 C16 O2 . . . 123.4(4) ? N0 C1' C11' . . . 115.0(3) ? N0 C1' H1'a . . . 109.0(3) ? N0 C1' H1'b . . . 107.6(4) ? C11' C1' H1'a . . . 109.5(4) ? C11' C1' H1'b . . . 107.6(4) ? H1'a C1' H1'b . . . 107.8(4) ? C1' C11' C12' . . . 120.8(4) ? C1' C11' C16' . . . 121.7(4) ? C12' C11' C16' . . . 117.3(4) ? C11' C12' C13' . . . 123.0(4) ? C11' C12' H12' . . . 117.1(4) ? C13' C12' H12' . . . 119.9(4) ? C12' C13' C131' . . . 119.2(4) ? C12' C13' C14' . . . 117.1(4) ? C131' C13' C14' . . . 123.7(4) ? C13' C131' C132' . . . 108.1(5) ? C13' C131' C133' . . . 110.8(4) ? C13' C131' C134' . . . 112.2(5) ? C132' C131' C133' . . . 108.6(5) ? C132' C131' C134' . . . 108.9(5) ? C133' C131' C134' . . . 108.1(5) ? C131' C132' H132'a . . . 111.4(6) ? C131' C132' H132'b . . . 111.1(6) ? C131' C132' H132'c . . . 112.3(6) ? H132'a C132' H132'b . . . 106.3(6) ? H132'a C132' H132'c . . . 107.5(7) ? H132'b C132' H132'c . . . 108.0(6) ? C131' C133' H133'a . . . 111.2(5) ? C131' C133' H133'b . . . 111.3(6) ? C131' C133' H133'c . . . 109.7(6) ? H133'a C133' H133'b . . . 109.2(6) ? H133'a C133' H133'c . . . 107.4(6) ? H133'b C133' H133'c . . . 108.0(6) ? C131' C134' H134'a . . . 111.8(6) ? C131' C134' H134'b . . . 112.4(5) ? C131' C134' H134'c . . . 110.0(6) ? H134'a C134' H134'b . . . 109.0(6) ? H134'a C134' H134'c . . . 105.9(6) ? H134'b C134' H134'c . . . 107.4(6) ? C13' C14' C15' . . . 122.0(5) ? C13' C14' H14' . . . 119.5(6) ? C15' C14' H14' . . . 118.4(6) ? C14' C15' C16' . . . 119.4(5) ? C14' C15' H15' . . . 119.6(5) ? C16' C15' H15' . . . 121.0(5) ? C11' C16' C15' . . . 121.1(4) ? C11' C16' O2' . . . 114.7(4) ? C15' C16' O2' . . . 124.2(4) ? Pb O2 C16 . . . 124.5(2) ? Pb O2 C3 . . . 99.4(3) ? C16 O2 C3 . . . 117.0(4) ? O2 C3 C32 . . . 111.7(4) ? O2 C3 H3a . . . 109.8(4) ? O2 C3 H3b . . . 109.9(5) ? C32 C3 H3a . . . 108.8(5) ? C32 C3 H3b . . . 109.0(4) ? H3a C3 H3b . . . 107.5(5) ? Pb O2' C16' . . . 121.9(3) ? Pb O2' C3' . . . 116.6(3) ? C16' O2' C3' . . . 118.3(4) ? O2' C3' C32' . . . 107.9(4) ? O2' C3' H3'a . . . 110.2(4) ? O2' C3' H3'b . . . 110.8(4) ? C32' C3' H3'a . . . 110.9(5) ? C32' C3' H3'b . . . 110.1(4) ? H3'a C3' H3'b . . . 106.9(5) ? Pb N31 C32 . . . 115.0(3) ? Pb N31 C32' . . . 121.3(3) ? C32 N31 C32' . . . 119.8(4) ? C3 C32 N31 . . . 114.1(4) ? C3 C32 C33 . . . 124.8(5) ? N31 C32 C33 . . . 121.0(5) ? C32 C33 C34 . . . 119.6(5) ? C32 C33 H33 . . . 119.9(5) ? C34 C33 H33 . . . 120.6(6) ? C33 C34 C33' . . . 119.3(5) ? C33 C34 H34 . . . 120.3(7) ? C33' C34 H34 . . . 120.3(7) ? C34 C33' C32' . . . 118.4(5) ? C34 C33' H33' . . . 119.9(6) ? C32' C33' H33' . . . 121.7(5) ? C3' C32' N31 . . . 116.1(4) ? C3' C32' C33' . . . 122.0(5) ? N31 C32' C33' . . . 121.9(5) ? O11 Cl1 O12 . . . 108.8(4) ? O11 Cl1 O13 . . . 114.3(10) ? O11 Cl1 O14 . . . 112.5(7) ? O11 Cl1 O12' . . . 105.6(7) ? O11 Cl1 O13' . . . 105.0(7) ? O11 Cl1 O14' . . . 106.2(12) ? O12 Cl1 O13 . . . 109.1(10) ? O12 Cl1 O14 . . . 101.4(8) ? O12 Cl1 O12' . . . 68.3(9) ? O12 Cl1 O13' . . . 145.4(8) ? O12 Cl1 O14' . . . 50.5(12) ? O13 Cl1 O14 . . . 110.0(12) ? O13 Cl1 O12' . . . 47.9(12) ? O13 Cl1 O13' . . . 47.9(12) ? O13 Cl1 O14' . . . 139.3(15) ? O14 Cl1 O12' . . . 141.8(9) ? O14 Cl1 O13' . . . 71.8(10) ? O14 Cl1 O14' . . . 55.2(13) ? O12' Cl1 O13' . . . 95.7(10) ? O12' Cl1 O14' . . . 117.1(14) ? O13' Cl1 O14' . . . 125.4(14) ? Pb O11 Cl1 . . . 108.7(3) ? Cl1 O12 O12' . . . 55.1(8) ? Cl1 O12 O14' . . . 52.3(12) ? O12' O12 O14' . . . 106.0(14) ? Cl1 O13 O12' . . . 70.6(16) ? Cl1 O13 O13' . . . 70.3(14) ? O12' O13 O13' . . . 141(2) ? Cl1 O14 O13' . . . 56.5(8) ? Cl1 O14 O14' . . . 55.5(13) ? O13' O14 O14' . . . 110.8(16) ? Cl1 O12' O12 . . . 56.6(8) ? Cl1 O12' O13 . . . 61.5(14) ? O12 O12' O13 . . . 110.6(18) ? Cl1 O13' O13 . . . 61.8(13) ? Cl1 O13' O14 . . . 51.7(8) ? O13 O13' O14 . . . 104.4(16) ? Cl1 O14' O12 . . . 77.2(16) ? Cl1 O14' O14 . . . 69.3(14) ? O12 O14' O14 . . . 137(2) ? O01 N O02 . . . 114.8(5) ? O01 N O03 . . . 119.1(4) ? O02 N O03 . . . 126.0(5) ? Pb O01 N . . . 106.3(3) ? Pb O02 N . . . 93.8(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 Pb C0 3.252(5) . . ? Pb C02 3.291(5) . . ? Pb C06 3.398(6) . . ? Pb C1 3.360(4) . . ? Pb C16 3.778(5) . . ? Pb C1' 3.516(4) . . ? Pb C16' 3.690(5) . . ? Pb C3 3.351(6) . . ? Pb C3' 3.634(5) . . ? Pb C32 3.506(5) . . ? Pb C32' 3.597(5) . . ? Pb Cl1 3.6194(16) . . ? Pb O12 3.148(9) . . ? Pb O14' 3.42(2) . . ? Pb N 3.196(4) . . ? Pb H0a 3.4114(2) . . ? Pb H06 3.3964(3) . . ? Pb H1b 3.1930(2) . . ? Pb H1'b 3.5472(3) . . ? Pb H3b 3.2590(2) . . ? N0 N01 2.844(6) . . ? N0 C02 2.511(6) . . ? N0 C11 2.557(6) . . ? N0 C11' 2.536(6) . . ? N0 H0a 2.018(4) . . ? N0 H0b 2.016(4) . . ? N0 H1a 2.035(4) . . ? N0 H1b 2.035(3) . . ? N0 H1'a 2.011(4) . . ? N0 H1'b 2.009(4) . . ? C0 N01 2.422(6) . . ? C0 C03 2.500(7) . . ? C0 C1 2.394(7) . . ? C0 C1' 2.436(6) . . ? C0 C11' 2.936(7) . . ? C0 H03 2.689(5) . . ? C0 H1a 2.448(5) . . ? C0 H1b 2.670(5) . . ? C0 H1'a 2.670(5) . . ? N01 C03 2.362(6) . . ? N01 C04 2.734(7) . . ? N01 C05 2.374(7) . . ? N01 H06 2.007(4) . . ? C02 C04 2.370(8) . . ? C02 C05 2.720(8) . . ? C02 C06 2.329(7) . . ? C02 C11' 2.949(7) . . ? C02 H0a 2.027(5) . . ? C02 H0b 2.026(5) . . ? C02 H03 2.044(5) . . ? C03 C05 2.366(8) . . ? C03 C06 2.710(6) . . ? C03 H0b 2.578(5) . . ? C03 H04 2.052(5) . . ? C04 C06 2.338(8) . . ? C04 H03 2.067(6) . . ? C04 H05 2.019(6) . . ? C05 H04 2.013(7) . . ? C05 H06 2.032(7) . . ? C06 H05 2.014(6) . . ? C1 C12 2.495(7) . . ? C1 C16 2.549(7) . . ? C1 C1' 2.433(6) . . ? C1 O2 2.825(6) . . ? C1 H0a 2.414(5) . . ? C1 H0b 2.686(4) . . ? C1 H1'a 2.518(4) . . ? C1 H1'b 2.655(5) . . ? C1 H12 2.630(5) . . ? C11 C13 2.435(7) . . ? C11 C14 2.764(7) . . ? C11 C15 2.405(7) . . ? C11 C1' 2.861(6) . . ? C11 O2 2.367(5) . . ? C11 H1a 2.035(5) . . ? C11 H1b 2.034(5) . . ? C11 H1'b 2.564(4) . . ? C11 H12 2.040(4) . . ? C12 C131 2.544(7) . . ? C12 C133 2.893(10) . . ? C12 C14 2.364(7) . . ? C12 C15 2.753(7) . . ? C12 C16 2.386(6) . . ? C12 H1a 2.513(5) . . ? C13 C132 2.432(13) . . ? C13 C133 2.503(10) . . ? C13 C134 2.446(12) . . ? C13 C15 2.438(6) . . ? C13 C16 2.810(6) . . ? C13 H12 2.031(5) . . ? C13 H132b 2.605(5) . . ? C13 H132c 2.612(5) . . ? C13 H133b 2.694(4) . . ? C13 H133c 2.681(5) . . ? C13 H134b 2.618(4) . . ? C13 H134c 2.631(5) . . ? C13 H14 2.040(5) . . ? C131 C14 2.526(6) . . ? C131 H12 2.686(6) . . ? C131 H132a 1.975(5) . . ? C131 H132b 1.959(6) . . ? C131 H132c 1.965(5) . . ? C131 H133a 2.008(5) . . ? C131 H133b 2.000(6) . . ? C131 H133c 2.004(6) . . ? C131 H134a 1.984(5) . . ? C131 H134b 1.979(5) . . ? C131 H134c 1.969(6) . . ? C131 H14 2.672(5) . . ? C132 C133 2.344(17) . . ? C132 C134 2.36(2) . . ? C132 H133a 2.526(13) . . ? C132 H133b 2.553(15) . . ? C132 H134a 2.492(16) . . ? C132 H134c 2.472(15) . . ? C133 C134 2.327(18) . . ? C133 H12 2.534(10) . . ? C133 H132a 2.513(9) . . ? C133 H132c 2.600(11) . . ? C133 H134a 2.471(11) . . ? C133 H134b 2.564(12) . . ? C134 C14 2.899(10) . . ? C134 H132a 2.483(11) . . ? C134 H132b 2.482(13) . . ? C134 H133a 2.467(12) . . ? C134 H133c 2.492(16) . . ? C134 H14 2.648(9) . . ? C14 C16 2.397(7) . . ? C14 H134c 2.625(5) . . ? C14 H15 2.056(4) . . ? C15 O2 2.449(7) . . ? C15 C3 2.823(7) . . ? C15 H14 2.044(5) . . ? C15 H3a 2.560(5) . . ? C16 C3 2.409(6) . . ? C16 H15 2.050(5) . . ? C16 H3a 2.568(4) . . ? C1' C12' 2.537(6) . . ? C1' C16' 2.535(6) . . ? C1' O2' 2.766(5) . . ? C1' H0b 2.493(4) . . ? C1' H12' 2.660(4) . . ? C11' C13' 2.441(6) . . ? C11' C14' 2.763(6) . . ? C11' C15' 2.392(7) . . ? C11' O2' 2.332(5) . . ? C11' H1'a 2.040(4) . . ? C11' H1'b 2.031(4) . . ? C11' H12' 2.043(4) . . ? C12' C131' 2.515(7) . . ? C12' C133' 2.966(8) . . ? C12' C14' 2.339(7) . . ? C12' C15' 2.734(7) . . ? C12' C16' 2.380(6) . . ? C12' H1'a 2.581(5) . . ? C13' C132' 2.495(8) . . ? C13' C133' 2.526(8) . . ? C13' C134' 2.548(7) . . ? C13' C15' 2.416(7) . . ? C13' C16' 2.789(6) . . ? C13' H12' 2.049(5) . . ? C13' H14' 2.032(5) . . ? C131' C14' 2.561(9) . . ? C131' H12' 2.662(5) . . ? C131' H132'a 2.103(6) . . ? C131' H132'b 2.096(6) . . ? C131' H132'c 2.099(6) . . ? C131' H133'a 2.076(7) . . ? C131' H133'b 2.072(6) . . ? C131' H133'c 2.069(6) . . ? C131' H134'a 2.090(5) . . ? C131' H134'b 2.084(6) . . ? C131' H134'c 2.083(6) . . ? C132' C133' 2.497(10) . . ? C132' C134' 2.504(10) . . ? C132' H133'b 2.674(7) . . ? C132' H134'a 2.681(6) . . ? C133' C134' 2.479(8) . . ? C133' H134'a 2.698(6) . . ? C133' H134'b 2.694(6) . . ? C134' C14' 2.895(8) . . ? C134' H132'a 2.692(7) . . ? C134' H133'a 2.630(6) . . ? C134' H133'c 2.693(6) . . ? C134' H14' 2.519(6) . . ? C14' C16' 2.380(7) . . ? C14' H15' 2.058(6) . . ? C15' O2' 2.426(6) . . ? C15' C3' 2.913(7) . . ? C15' H14' 2.048(5) . . ? C16' C3' 2.409(7) . . ? C16' H1'b 2.664(4) . . ? C16' H15' 2.040(5) . . ? C16' H3'a 2.504(5) . . ? O2 N31 2.708(5) . . ? O2 C32 2.438(6) . . ? O2 H1b 2.612(3) . . ? O2 H15 2.666(4) . . ? O2 H3a 1.978(3) . . ? O2 H3b 1.971(3) . . ? C3 N31 2.405(7) . . ? C3 C33 2.565(8) . . ? C3 H15 2.518(5) . . ? O2' N31 2.544(5) . . ? O2' C32' 2.362(6) . . ? O2' H1'b 2.562(3) . . ? O2' H15' 2.658(3) . . ? O2' H3'a 1.974(4) . . ? O2' H3'b 1.982(3) . . ? C3' N31 2.406(7) . . ? C3' C33' 2.520(8) . . ? C3' H15' 2.696(5) . . ? N31 C33 2.370(7) . . ? N31 C34 2.748(7) . . ? N31 C33' 2.374(7) . . ? C32 C34 2.377(8) . . ? C32 C33' 2.733(8) . . ? C32 C32' 2.319(7) . . ? C32 H3a 2.045(5) . . ? C32 H3b 2.039(5) . . ? C32 H33 2.053(5) . . ? C33 C33' 2.382(8) . . ? C33 C32' 2.717(7) . . ? C33 H3a 2.665(6) . . ? C33 H34 2.036(6) . . ? C34 C32' 2.378(8) . . ? C34 H33 2.057(8) . . ? C34 H33' 2.048(8) . . ? C33' H34 2.048(6) . . ? C32' H3'a 2.053(5) . . ? C32' H3'b 2.044(5) . . ? C32' H33' 2.061(5) . . ? O11 O12 2.335(10) . . ? O11 O13 2.31(2) . . ? O11 O14 2.292(14) . . ? O11 O12' 2.27(2) . . ? O11 O13' 2.253(16) . . ? O11 O14' 2.08(2) . . ? O12 O13 2.26(2) . . ? O12 O14 2.156(17) . . ? O12 O13' 2.738(18) . . ? O13 O14 2.18(2) . . ? O13 O14' 2.35(3) . . ? O13 H15' 2.584(19) . '5 666' ? O13 H3'a 2.58(2) . '5 666' ? O14 O12' 2.61(2) . . ? O14 H04 2.498(14) . '5 676' ? O14 H1'a 2.545(13) . '8 565' ? O12' O13' 2.11(2) . . ? O12' O14' 2.22(3) . . ? O13' O14' 2.31(3) . . ? O13' H12' 2.391(16) . '8 565' ? O13' H3'a 2.608(17) . '5 666' ? O14' H133b 2.66(2) . '8 565' ? O01 O02 2.058(6) . . ? O01 O03 2.105(7) . . ? O01 H0a 2.630(4) . . ? O01 H1b 2.482(5) . . ? O01 H3a 2.536(4) . '2 565' ? O02 O03 2.090(8) . . ? O02 H05 2.365(5) . '5 676' ? H0a H0b 1.55128(6) . . ? H0a H1b 2.35622(11) . . ? H0b H1'a 2.38994(15) . . ? H03 H04 2.36824(10) . . ? H04 H05 2.33387(13) . . ? H05 H06 2.31507(10) . . ? H1a H1b 1.55141(9) . . ? H1a H12 2.29084(10) . . ? H1'a H1'b 1.55132(7) . . ? H1'a H12' 2.36183(13) . . ? H12 H133b 2.10086(11) . . ? H132a H132b 1.55159(9) . . ? H132a H132c 1.55136(6) . . ? H132a H133a 2.31794(12) . . ? H132a H134a 2.22632(13) . . ? H132b H132c 1.55144(6) . . ? H132b H134c 2.17544(13) . . ? H133a H133b 1.55132(6) . . ? H133a H133c 1.55134(6) . . ? H133a H134a 2.22615(9) . . ? H133b H133c 1.55136(9) . . ? H133c H134b 2.37971(10) . . ? H134a H134b 1.55145(6) . . ? H134a H134c 1.55139(9) . . ? H134b H134c 1.55130(8) . . ? H134c H14 2.07075(11) . . ? H12' H133'b 2.18664(10) . . ? H132'a H132'b 1.55144(9) . . ? H132'a H132'c 1.55125(9) . . ? H132'b H132'c 1.55138(7) . . ? H133'a H133'b 1.55137(9) . . ? H133'a H133'c 1.55133(7) . . ? H133'b H133'c 1.55142(7) . . ? H134'a H134'b 1.55144(7) . . ? H134'a H134'c 1.55145(10) . . ? H134'b H134'c 1.55140(7) . . ? H134'c H14' 2.16261(8) . . ? H14 H15 2.34835(13) . . ? H15 H3a 2.03017(10) . . ? H14' H15' 2.34031(10) . . ? H3a H3b 1.55128(6) . . ? H3'a H3'b 1.55129(7) . . ? H3'b H3'b 2.25895(10) . '5 666' ? H33 H34 2.35995(11) . . ? H34 H33' 2.35415(13) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3600 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 36 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 13.247 _diffrn_reflns_av_sigmaI/netI .115 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' #======================================================================= # 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 #==END