#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _audit_creation_method Xtal3.6 _audit_creation_date 01-02-19 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _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 'Prof L Lindoy' _publ_contact_author_address ; Prof L Lindoy School of Chemistry University of Sydney Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_section_title ; Macrocyclic ligand design. A synthetic, solvent extraction, computational and NMR study of the effect of cryptand flixibility on sodium ion affinity #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Adam, Kenneth R.' 'Atkinson, Ian M.' 'Kim, Jeong' 'Lindoy, L.' 'Matthews, Owen A.' 'Meehan, George V.' 'Raciti, Fiona' 'Skelton, Brian W.' 'Svenstrup, Niels' 'White, Allan H.' _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_llpic _database_code_CSD 164829 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C45 H48 Cl2 N5 Na1 O13' _chemical_formula_moiety ? _chemical_formula_weight 960.8 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 12.299(10) _cell_length_b 14.264(11) _cell_length_c 15.317(19) _cell_angle_alpha 63.29(8) _cell_angle_beta 81.12(9) _cell_angle_gamma 77.38(6) _cell_volume 2338(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 7.6 _cell_measurement_theta_max 8.9 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .217 _exptl_crystal_description block _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Cad4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; ? ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 10081 _reflns_number_total 5782 _reflns_Friedel_coverage ? _reflns_number_gt 1228 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 22.21 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .066 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 14 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .132 _refine_ls_wR_factor_ref .139 _refine_ls_goodness_of_fit_ref 1.982 _refine_ls_number_reflns 1228 _refine_ls_number_parameters 303 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .043 _refine_diff_density_min -.411 _refine_diff_density_max .483 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection '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 90 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 96 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 10 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Na ? 0 2 .030029 .025024 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 26 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 4 .132019 .158997 '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 Na .7434(9) .6398(9) .2169(11) .076(16) Uani ? ? 1.00000 ? ? N0 .733(2) .704(2) .370(2) .079(10) Uiso ? ? 1.00000 ? ? C1a .616(3) .697(3) .427(3) .075(12) Uiso ? ? 1.00000 ? ? C2a .547(3) .705(3) .349(2) .065(11) Uiso ? ? 1.00000 ? ? O3a .5701(18) .6393(17) .3040(16) .072(8) Uiso ? ? 1.00000 ? ? C4a .548(3) .535(3) .367(3) .099(15) Uiso ? ? 1.00000 ? ? C4a' .573(3) .475(3) .317(3) .078(13) Uiso ? ? 1.00000 ? ? O3a' .6895(17) .4641(16) .2865(16) .066(7) Uiso ? ? 1.00000 ? ? C2a' .719(3) .407(2) .235(2) .054(10) Uiso ? ? 1.00000 ? ? C1a' .682(2) .454(2) .135(2) .050(10) Uiso ? ? 1.00000 ? ? C1b .745(3) .822(3) .334(2) .065(11) Uiso ? ? 1.00000 ? ? C2b .850(2) .845(2) .264(2) .051(10) Uiso ? ? 1.00000 ? ? C3b .921(4) .874(3) .307(3) .117(16) Uiso ? ? 1.00000 ? ? C4b 1.015(3) .904(3) .240(3) .087(13) Uiso ? ? 1.00000 ? ? C5b 1.032(3) .906(3) .153(3) .085(13) Uiso ? ? 1.00000 ? ? C6b .958(3) .886(3) .109(3) .095(14) Uiso ? ? 1.00000 ? ? C7b .861(3) .856(2) .169(2) .054(10) Uiso ? ? 1.00000 ? ? O8b .7759(19) .8289(18) .1508(17) .084(8) Uiso ? ? 1.00000 ? ? C9b .740(3) .892(3) .043(3) .089(14) Uiso ? ? 1.00000 ? ? C9b' .629(3) .879(3) .053(3) .082(13) Uiso ? ? 1.00000 ? ? O8b' .6273(18) .7731(17) .0662(16) .070(7) Uiso ? ? 1.00000 ? ? C7b' .532(2) .742(2) .073(2) .031(8) Uiso ? ? 1.00000 ? ? C6b' .430(3) .785(3) .103(3) .076(12) Uiso ? ? 1.00000 ? ? C5b' .340(3) .747(3) .108(3) .092(14) Uiso ? ? 1.00000 ? ? C4b' .340(3) .673(3) .072(3) .072(12) Uiso ? ? 1.00000 ? ? C3b' .443(3) .633(3) .041(3) .082(13) Uiso ? ? 1.00000 ? ? C2b' .538(2) .669(2) .036(2) .039(9) Uiso ? ? 1.00000 ? ? C1b' .646(2) .632(2) -.001(2) .041(9) Uiso ? ? 1.00000 ? ? C1c .817(3) .645(3) .454(3) .099(15) Uiso ? ? 1.00000 ? ? C2c .828(3) .523(3) .489(3) .079(13) Uiso ? ? 1.00000 ? ? C3c .783(3) .479(3) .586(3) .097(14) Uiso ? ? 1.00000 ? ? C4c .784(4) .371(4) .620(3) .129(18) Uiso ? ? 1.00000 ? ? C5c .821(3) .316(3) .571(3) .114(16) Uiso ? ? 1.00000 ? ? C6c .858(3) .360(3) .468(3) .111(16) Uiso ? ? 1.00000 ? ? C7c .862(3) .474(3) .436(3) .073(12) Uiso ? ? 1.00000 ? ? O8c .8949(17) .5305(16) .3353(16) .070(7) Uiso ? ? 1.00000 ? ? C9c .998(3) .488(3) .301(3) .074(12) Uiso ? ? 1.00000 ? ? C9c' 1.018(3) .570(3) .200(3) .088(13) Uiso ? ? 1.00000 ? ? O8c' .9381(18) .5879(17) .1435(16) .071(7) Uiso ? ? 1.00000 ? ? C7c' .951(3) .642(2) .043(2) .061(11) Uiso ? ? 1.00000 ? ? C6c' 1.025(3) .722(3) .003(3) .074(12) Uiso ? ? 1.00000 ? ? C5c' 1.034(3) .771(3) -.095(2) .064(11) Uiso ? ? 1.00000 ? ? C4c' .985(3) .748(3) -.153(3) .083(13) Uiso ? ? 1.00000 ? ? C3c' .911(3) .670(3) -.112(3) .087(13) Uiso ? ? 1.00000 ? ? C2c' .905(2) .621(2) -.010(2) .044(10) Uiso ? ? 1.00000 ? ? C1c' .834(2) .532(2) .032(2) .048(10) Uiso ? ? 1.00000 ? ? N0' .7251(18) .5562(17) .0764(17) .043(8) Uiso ? ? 1.00000 ? ? O101 .489(2) 1.011(2) -.186(2) .106(10) Uiso ? ? 1.00000 ? ? C101 .527(3) .937(3) -.214(3) .076(12) Uiso ? ? 1.00000 ? ? C102 .641(2) .922(2) -.239(2) .049(10) Uiso ? ? 1.00000 ? ? N102 .708(3) 1.001(3) -.251(3) .120(13) Uiso ? ? 1.00000 ? ? O1021 .697(3) 1.030(3) -.189(3) .195(16) Uiso ? ? 1.00000 ? ? O1022 .782(3) 1.012(3) -.313(3) .198(16) Uiso ? ? 1.00000 ? ? C103 .688(2) .846(2) -.266(2) .048(10) Uiso ? ? 1.00000 ? ? C104 .631(2) .771(2) -.262(2) .045(10) Uiso ? ? 1.00000 ? ? N104 .686(3) .682(3) -.283(3) .142(15) Uiso ? ? 1.00000 ? ? O1041 .779(3) .678(2) -.317(2) .151(13) Uiso ? ? 1.00000 ? ? O1042 .620(3) .627(3) -.281(3) .168(14) Uiso ? ? 1.00000 ? ? C105 .516(3) .781(2) -.231(2) .055(10) Uiso ? ? 1.00000 ? ? C106 .473(3) .862(3) -.206(3) .069(12) Uiso ? ? 1.00000 ? ? N106 .345(3) .870(2) -.175(2) .099(11) Uiso ? ? 1.00000 ? ? O1061 .314(2) .916(2) -.127(2) .122(11) Uiso ? ? 1.00000 ? ? O1062 .301(2) .818(2) -.198(2) .136(12) Uiso ? ? 1.00000 ? ? Cl11 .154(3) .915(3) .594(3) .43(11) Uani ? ? .50000 ? ? Cl12 .029(2) 1.104(2) .471(3) .32(9) Uani ? ? .50000 ? ? C10 .024(2) .983(6) .565(7) .29(8) Uiso ? ? .50000 ? ? Cl21 .347(3) .862(3) .512(3) .44(13) Uani ? ? .50000 ? ? Cl22 .401(2) 1.022(3) .525(4) .50(15) Uani ? ? .50000 ? ? C20 .448(3) .922(7) .502(10) .26(7) Uiso ? ? .50000 ? ? H1aA .58556 .75287 .44738 .08400 Uiso ? ? 1.00000 ? ? H1aB .61056 .63021 .48391 .08400 Uiso ? ? 1.00000 ? ? H2aA .54664 .77646 .29833 .08100 Uiso ? ? 1.00000 ? ? H2aB .47074 .70106 .37700 .08100 Uiso ? ? 1.00000 ? ? H4aA .47468 .53647 .40078 .08900 Uiso ? ? 1.00000 ? ? H4aB .59923 .50102 .42488 .08900 Uiso ? ? 1.00000 ? ? H4a'A .52388 .51053 .26126 .07900 Uiso ? ? 1.00000 ? ? H4a'B .54794 .40530 .35519 .07900 Uiso ? ? 1.00000 ? ? H2a'A .69525 .33737 .27266 .06700 Uiso ? ? 1.00000 ? ? H2a'B .80129 .38978 .23120 .06700 Uiso ? ? 1.00000 ? ? H1a'A .60122 .46672 .13432 .04500 Uiso ? ? 1.00000 ? ? H1a'B .70837 .40773 .10063 .04500 Uiso ? ? 1.00000 ? ? H1bA .74823 .83998 .38947 .09700 Uiso ? ? 1.00000 ? ? H1bB .67989 .87047 .30068 .09700 Uiso ? ? 1.00000 ? ? H3b .91906 .86808 .37031 .12900 Uiso ? ? 1.00000 ? ? H4b 1.07753 .93042 .25435 .10600 Uiso ? ? 1.00000 ? ? H5b 1.10431 .92199 .11294 .10700 Uiso ? ? 1.00000 ? ? H6b .96605 .89193 .03701 .08900 Uiso ? ? 1.00000 ? ? H9bA .75663 .96526 .01525 .08900 Uiso ? ? 1.00000 ? ? H9bB .78608 .86117 .00135 .08900 Uiso ? ? 1.00000 ? ? H9b'A .59039 .89465 .10987 .11600 Uiso ? ? 1.00000 ? ? H9b'B .58730 .93814 -.00268 .11600 Uiso ? ? 1.00000 ? ? H6b' .42494 .84716 .11781 .07800 Uiso ? ? 1.00000 ? ? H5b' .26995 .76707 .14260 .11600 Uiso ? ? 1.00000 ? ? H4b' .27115 .65255 .06821 .07400 Uiso ? ? 1.00000 ? ? H3b' .44692 .57225 .02515 .10300 Uiso ? ? 1.00000 ? ? H1b'A .63507 .59653 -.04012 .04600 Uiso ? ? 1.00000 ? ? H1b'B .68090 .69224 -.04563 .04600 Uiso ? ? 1.00000 ? ? H1cA .78656 .66371 .50902 .09200 Uiso ? ? 1.00000 ? ? H1cB .88622 .66862 .43231 .09200 Uiso ? ? 1.00000 ? ? H3c .75896 .52023 .62508 .12400 Uiso ? ? 1.00000 ? ? H4c .75398 .33506 .69011 .13500 Uiso ? ? 1.00000 ? ? H5c .81680 .24060 .60456 .10800 Uiso ? ? 1.00000 ? ? H6c .87877 .31942 .42783 .09700 Uiso ? ? 1.00000 ? ? H9cA .99384 .42086 .29692 .07900 Uiso ? ? 1.00000 ? ? H9cB 1.05869 .46801 .34257 .07900 Uiso ? ? 1.00000 ? ? H9c'A 1.09219 .54790 .17334 .08600 Uiso ? ? 1.00000 ? ? H9c'B 1.02593 .63289 .20724 .08600 Uiso ? ? 1.00000 ? ? H6c' 1.06907 .73589 .04889 .07500 Uiso ? ? 1.00000 ? ? H5c' 1.07220 .83364 -.12851 .07700 Uiso ? ? 1.00000 ? ? H4c' 1.00412 .78301 -.22247 .09900 Uiso ? ? 1.00000 ? ? H3c' .87462 .65388 -.15772 .12200 Uiso ? ? 1.00000 ? ? H1c'A .87744 .46984 .08244 .06300 Uiso ? ? 1.00000 ? ? H1c'B .82682 .50941 -.01734 .06300 Uiso ? ? 1.00000 ? ? H103 .76373 .84218 -.29531 .05000 Uiso ? ? 1.00000 ? ? H105 .46883 .72762 -.22260 .07800 Uiso ? ? 1.00000 ? ? H10a -.01446 .94223 .54351 .40000 Uiso ? ? .50000 ? ? H10b -.01818 .98812 .61872 .40000 Uiso ? ? .50000 ? ? H20a .50725 .87480 .54442 .30000 Uiso ? ? .50000 ? ? H20b .48451 .94685 .43520 .30000 Uiso ? ? .50000 ? ? 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 Na .025(7) .026(8) .129(13) -.011(6) -.008(8) .014(8) Cl11 .64(11) .19(4) .24(6) .07(6) .02(6) .02(4) Cl12 .51(8) .14(3) .27(5) .09(4) -.09(5) -.10(3) Cl21 .48(9) .34(7) .28(6) -.12(7) -.07(6) .10(5) Cl22 1.1(2) .19(5) .13(5) .06(8) -.14(8) -.06(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 Na O3a . . 2.33(2) ? Na O3a' . . 2.44(3) ? Na O8b . . 2.52(3) ? Na O8b' . . 2.62(2) ? Na O8c . . 2.53(2) ? Na O8c' . . 2.59(2) ? N0 C1a . . 1.55(4) ? N0 C1b . . 1.56(5) ? N0 C1c . . 1.58(5) ? C1a C2a . . 1.52(6) ? C1a H1aA . . .97(4) ? C1a H1aB . . .97(3) ? C2a O3a . . 1.35(5) ? C2a H2aA . . .97(3) ? C2a H2aB . . .97(3) ? O3a C4a . . 1.42(4) ? C4a C4a' . . 1.35(7) ? C4a H4aA . . .97(4) ? C4a H4aB . . 1.04(4) ? C4a' O3a' . . 1.43(4) ? C4a' H4a'A . . .99(4) ? C4a' H4a'B . . .99(4) ? O3a' C2a' . . 1.34(5) ? C2a' C1a' . . 1.48(5) ? C2a' H2a'A . . .98(3) ? C2a' H2a'B . . .99(3) ? C1a' N0' . . 1.48(4) ? C1a' H1a'A . . .98(3) ? C1a' H1a'B . . .99(4) ? C1b C2b . . 1.54(4) ? C1b H1bA . . .99(4) ? C1b H1bB . . .98(3) ? C2b C3b . . 1.39(7) ? C2b C7b . . 1.37(5) ? C3b C4b . . 1.42(5) ? C3b H3b . . .94(5) ? C4b C5b . . 1.30(6) ? C4b H4b . . 1.02(5) ? C5b C6b . . 1.35(7) ? C5b H5b . . 1.01(4) ? C6b C7b . . 1.41(5) ? C6b H6b . . 1.06(5) ? C7b O8b . . 1.30(5) ? O8b C9b . . 1.57(4) ? C9b C9b' . . 1.40(6) ? C9b H9bA . . .99(4) ? C9b H9bB . . .98(4) ? C9b' O8b' . . 1.44(5) ? C9b' H9b'A . . 1.01(4) ? C9b' H9b'B . . 1.00(3) ? O8b' C7b' . . 1.31(4) ? C7b' C6b' . . 1.39(4) ? C7b' C2b' . . 1.37(5) ? C6b' C5b' . . 1.31(6) ? C6b' H6b' . . .99(5) ? C5b' C4b' . . 1.40(7) ? C5b' H5b' . . .99(4) ? C4b' C3b' . . 1.37(5) ? C4b' H4b' . . .97(4) ? C3b' C2b' . . 1.36(5) ? C3b' H3b' . . 1.00(5) ? C2b' C1b' . . 1.45(4) ? C1b' N0' . . 1.50(3) ? C1b' H1b'A . . .98(4) ? C1b' H1b'B . . .97(3) ? C1c C2c . . 1.56(6) ? C1c H1cA . . .99(5) ? C1c H1cB . . .94(4) ? C2c C3c . . 1.40(5) ? C2c C7c . . 1.26(6) ? C3c C4c . . 1.39(6) ? C3c H3c . . .99(5) ? C4c C5c . . 1.27(8) ? C4c H4c . . 1.01(4) ? C5c C6c . . 1.44(6) ? C5c H5c . . .98(4) ? C6c C7c . . 1.48(6) ? C6c H6c . . 1.00(5) ? C7c O8c . . 1.43(4) ? O8c C9c . . 1.42(4) ? C9c C9c' . . 1.48(4) ? C9c H9cA . . 1.00(4) ? C9c H9cB . . .97(4) ? C9c' O8c' . . 1.32(5) ? C9c' H9c'A . . .99(4) ? C9c' H9c'B . . .97(5) ? O8c' C7c' . . 1.37(4) ? C7c' C6c' . . 1.47(5) ? C7c' C2c' . . 1.23(6) ? C6c' C5c' . . 1.34(5) ? C6c' H6c' . . 1.06(5) ? C5c' C4c' . . 1.33(7) ? C5c' H5c' . . .99(3) ? C4c' C3c' . . 1.44(6) ? C4c' H4c' . . .97(4) ? C3c' C2c' . . 1.39(5) ? C3c' H3c' . . 1.01(5) ? C2c' C1c' . . 1.55(5) ? C1c' N0' . . 1.45(4) ? C1c' H1c'A . . .99(3) ? C1c' H1c'B . . .97(4) ? O101 C101 . . 1.29(5) ? C101 C102 . . 1.39(4) ? C101 C106 . . 1.33(6) ? C102 N102 . . 1.48(6) ? C102 C103 . . 1.32(5) ? N102 O1021 . . 1.16(7) ? N102 O1022 . . 1.19(5) ? C103 C104 . . 1.37(5) ? C103 H103 . . .97(3) ? C104 N104 . . 1.45(6) ? C104 C105 . . 1.41(4) ? N104 O1041 . . 1.19(5) ? N104 O1042 . . 1.23(6) ? C105 C106 . . 1.35(6) ? C105 H105 . . 1.01(4) ? C106 N106 . . 1.57(4) ? N106 O1061 . . 1.16(5) ? N106 O1062 . . 1.20(6) ? Cl11 C10 . . 1.69(5) ? Cl12 C10 . . 1.68(7) ? Cl12 C10 . '2 576' 1.82(11) ? Cl12 H10a . '2 576' .84(4) ? C10 H10a . . 1.00(10) ? C10 H10b . . .93(10) ? C10 C10 . '2 576' 1.97(15) ? Cl21 C20 . . 1.61(9) ? Cl22 C20 . . 1.59(14) ? Cl22 C20 . '2 676' 2.09(7) ? C20 H20a . . .98(8) ? C20 H20b . . .99(13) ? 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 O3a Na O3a' . . . 69.1(8) ? O3a Na O8b . . . 104.2(9) ? O3a Na O8b' . . . 83.6(8) ? O3a Na O8c . . . 109.5(9) ? O3a Na O8c' . . . 165.3(9) ? O3a' Na O8b . . . 173.3(9) ? O3a' Na O8b' . . . 110.7(10) ? O3a' Na O8c . . . 79.4(8) ? O3a' Na O8c' . . . 96.5(9) ? O8b Na O8b' . . . 66.4(9) ? O8b Na O8c . . . 104.6(10) ? O8b Na O8c' . . . 90.2(8) ? O8b' Na O8c . . . 166.0(8) ? O8b' Na O8c' . . . 105.4(9) ? O8c Na O8c' . . . 62.9(8) ? C1a N0 C1b . . . 104(3) ? C1a N0 C1c . . . 104(2) ? C1b N0 C1c . . . 101(3) ? N0 C1a C2a . . . 100(3) ? N0 C1a H1aA . . . 116(4) ? N0 C1a H1aB . . . 115(3) ? C2a C1a H1aA . . . 110(3) ? C2a C1a H1aB . . . 109(4) ? H1aA C1a H1aB . . . 106(4) ? C1a C2a O3a . . . 124(3) ? C1a C2a H2aA . . . 104(4) ? C1a C2a H2aB . . . 107(3) ? O3a C2a H2aA . . . 107(3) ? O3a C2a H2aB . . . 107(4) ? H2aA C2a H2aB . . . 107(3) ? Na O3a C2a . . . 116(2) ? Na O3a C4a . . . 113(2) ? C2a O3a C4a . . . 112(3) ? O3a C4a C4a' . . . 109(3) ? O3a C4a H4aA . . . 112(3) ? O3a C4a H4aB . . . 109(4) ? C4a' C4a H4aA . . . 117(5) ? C4a' C4a H4aB . . . 108(3) ? H4aA C4a H4aB . . . 101(4) ? C4a C4a' O3a' . . . 111(4) ? C4a C4a' H4a'A . . . 106(3) ? C4a C4a' H4a'B . . . 111(3) ? O3a' C4a' H4a'A . . . 113(3) ? O3a' C4a' H4a'B . . . 112(3) ? H4a'A C4a' H4a'B . . . 103(4) ? Na O3a' C4a' . . . 108(2) ? Na O3a' C2a' . . . 118.0(17) ? C4a' O3a' C2a' . . . 114(3) ? O3a' C2a' C1a' . . . 118(2) ? O3a' C2a' H2a'A . . . 109(3) ? O3a' C2a' H2a'B . . . 107(4) ? C1a' C2a' H2a'A . . . 110(4) ? C1a' C2a' H2a'B . . . 108(3) ? H2a'A C2a' H2a'B . . . 104(3) ? C2a' C1a' N0' . . . 109(3) ? C2a' C1a' H1a'A . . . 111(3) ? C2a' C1a' H1a'B . . . 113(2) ? N0' C1a' H1a'A . . . 110(2) ? N0' C1a' H1a'B . . . 109(3) ? H1a'A C1a' H1a'B . . . 104(4) ? N0 C1b C2b . . . 109(3) ? N0 C1b H1bA . . . 112(3) ? N0 C1b H1bB . . . 111(3) ? C2b C1b H1bA . . . 111(3) ? C2b C1b H1bB . . . 109(3) ? H1bA C1b H1bB . . . 104(3) ? C1b C2b C3b . . . 106(3) ? C1b C2b C7b . . . 126(3) ? C3b C2b C7b . . . 126(3) ? C2b C3b C4b . . . 108(4) ? C2b C3b H3b . . . 131(4) ? C4b C3b H3b . . . 120(5) ? C3b C4b C5b . . . 126(5) ? C3b C4b H4b . . . 123(5) ? C5b C4b H4b . . . 111(3) ? C4b C5b C6b . . . 125(4) ? C4b C5b H5b . . . 121(5) ? C6b C5b H5b . . . 115(4) ? C5b C6b C7b . . . 113(4) ? C5b C6b H6b . . . 127(4) ? C7b C6b H6b . . . 120(4) ? C2b C7b C6b . . . 121(4) ? C2b C7b O8b . . . 110(3) ? C6b C7b O8b . . . 129(4) ? Na O8b C7b . . . 124.4(17) ? Na O8b C9b . . . 109(2) ? C7b O8b C9b . . . 115(2) ? O8b C9b C9b' . . . 102(3) ? O8b C9b H9bA . . . 109(4) ? O8b C9b H9bB . . . 110(3) ? C9b' C9b H9bA . . . 119(3) ? C9b' C9b H9bB . . . 112(5) ? H9bA C9b H9bB . . . 104(3) ? C9b C9b' O8b' . . . 108(3) ? C9b C9b' H9b'A . . . 108(4) ? C9b C9b' H9b'B . . . 110(3) ? O8b' C9b' H9b'A . . . 114(3) ? O8b' C9b' H9b'B . . . 116(4) ? H9b'A C9b' H9b'B . . . 101(3) ? Na O8b' C9b' . . . 108(2) ? Na O8b' C7b' . . . 110.2(14) ? C9b' O8b' C7b' . . . 120(2) ? O8b' C7b' C6b' . . . 125(3) ? O8b' C7b' C2b' . . . 115(3) ? C6b' C7b' C2b' . . . 120(3) ? C7b' C6b' C5b' . . . 120(4) ? C7b' C6b' H6b' . . . 119(4) ? C5b' C6b' H6b' . . . 121(4) ? C6b' C5b' C4b' . . . 122(4) ? C6b' C5b' H5b' . . . 120(5) ? C4b' C5b' H5b' . . . 118(4) ? C5b' C4b' C3b' . . . 116(4) ? C5b' C4b' H4b' . . . 121(3) ? C3b' C4b' H4b' . . . 123(4) ? C4b' C3b' C2b' . . . 124(4) ? C4b' C3b' H3b' . . . 117(4) ? C2b' C3b' H3b' . . . 119(3) ? C7b' C2b' C3b' . . . 117(3) ? C7b' C2b' C1b' . . . 118(3) ? C3b' C2b' C1b' . . . 125(4) ? C2b' C1b' N0' . . . 115(2) ? C2b' C1b' H1b'A . . . 109(3) ? C2b' C1b' H1b'B . . . 110(3) ? N0' C1b' H1b'A . . . 108(2) ? N0' C1b' H1b'B . . . 109(3) ? H1b'A C1b' H1b'B . . . 105(3) ? N0 C1c C2c . . . 108(4) ? N0 C1c H1cA . . . 108(3) ? N0 C1c H1cB . . . 111(3) ? C2c C1c H1cA . . . 110(3) ? C2c C1c H1cB . . . 113(3) ? H1cA C1c H1cB . . . 107(5) ? C1c C2c C3c . . . 108(4) ? C1c C2c C7c . . . 126(3) ? C3c C2c C7c . . . 126(4) ? C2c C3c C4c . . . 111(4) ? C2c C3c H3c . . . 123(4) ? C4c C3c H3c . . . 126(4) ? C3c C4c C5c . . . 126(4) ? C3c C4c H4c . . . 114(5) ? C5c C4c H4c . . . 121(4) ? C4c C5c C6c . . . 125(4) ? C4c C5c H5c . . . 116(4) ? C6c C5c H5c . . . 118(5) ? C5c C6c C7c . . . 108(4) ? C5c C6c H6c . . . 125(4) ? C7c C6c H6c . . . 127(4) ? C2c C7c C6c . . . 124(3) ? C2c C7c O8c . . . 120(3) ? C6c C7c O8c . . . 115(4) ? Na O8c C7c . . . 118.3(18) ? Na O8c C9c . . . 119(2) ? C7c O8c C9c . . . 117(2) ? O8c C9c C9c' . . . 105(2) ? O8c C9c H9cA . . . 111(3) ? O8c C9c H9cB . . . 114(4) ? C9c' C9c H9cA . . . 108(4) ? C9c' C9c H9cB . . . 114(3) ? H9cA C9c H9cB . . . 104(3) ? C9c C9c' O8c' . . . 112(3) ? C9c C9c' H9c'A . . . 109(3) ? C9c C9c' H9c'B . . . 106(4) ? O8c' C9c' H9c'A . . . 112(4) ? O8c' C9c' H9c'B . . . 114(3) ? H9c'A C9c' H9c'B . . . 105(4) ? Na O8c' C9c' . . . 112(2) ? Na O8c' C7c' . . . 113.7(17) ? C9c' O8c' C7c' . . . 121(3) ? O8c' C7c' C6c' . . . 118(4) ? O8c' C7c' C2c' . . . 121(3) ? C6c' C7c' C2c' . . . 121(3) ? C7c' C6c' C5c' . . . 114(4) ? C7c' C6c' H6c' . . . 121(3) ? C5c' C6c' H6c' . . . 125(4) ? C6c' C5c' C4c' . . . 125(3) ? C6c' C5c' H5c' . . . 119(4) ? C4c' C5c' H5c' . . . 116(3) ? C5c' C4c' C3c' . . . 121(3) ? C5c' C4c' H4c' . . . 116(4) ? C3c' C4c' H4c' . . . 123(5) ? C4c' C3c' C2c' . . . 113(4) ? C4c' C3c' H3c' . . . 119(3) ? C2c' C3c' H3c' . . . 128(4) ? C7c' C2c' C3c' . . . 127(3) ? C7c' C2c' C1c' . . . 122(3) ? C3c' C2c' C1c' . . . 112(3) ? C2c' C1c' N0' . . . 116(3) ? C2c' C1c' H1c'A . . . 106(3) ? C2c' C1c' H1c'B . . . 110(3) ? N0' C1c' H1c'A . . . 109(2) ? N0' C1c' H1c'B . . . 111(3) ? H1c'A C1c' H1c'B . . . 105(3) ? C1a' N0' C1b' . . . 110(2) ? C1a' N0' C1c' . . . 107(2) ? C1b' N0' C1c' . . . 111(2) ? O101 C101 C102 . . . 117(4) ? O101 C101 C106 . . . 127(3) ? C102 C101 C106 . . . 116(4) ? C101 C102 N102 . . . 120(3) ? C101 C102 C103 . . . 121(4) ? N102 C102 C103 . . . 118(3) ? C102 N102 O1021 . . . 117(3) ? C102 N102 O1022 . . . 113(4) ? O1021 N102 O1022 . . . 127(5) ? C102 C103 C104 . . . 123(3) ? C102 C103 H103 . . . 122(4) ? C104 C103 H103 . . . 115(3) ? C103 C104 N104 . . . 123(3) ? C103 C104 C105 . . . 117(3) ? N104 C104 C105 . . . 120(3) ? C104 N104 O1041 . . . 121(4) ? C104 N104 O1042 . . . 113(3) ? O1041 N104 O1042 . . . 124(5) ? C104 C105 C106 . . . 117(3) ? C104 C105 H105 . . . 123(3) ? C106 C105 H105 . . . 120(3) ? C101 C106 C105 . . . 126(3) ? C101 C106 N106 . . . 119(3) ? C105 C106 N106 . . . 114(3) ? C106 N106 O1061 . . . 115(4) ? C106 N106 O1062 . . . 112(3) ? O1061 N106 O1062 . . . 133(3) ? C10 Cl12 C10 . . '2 576' 68(5) ? C10 Cl12 H10a . . '2 576' 65(4) ? C10 Cl12 H10a '2 576' . '2 576' 8.8(16) ? Cl11 C10 Cl12 . . . 110(3) ? Cl11 C10 H10a . . . 109(6) ? Cl11 C10 H10b . . . 111(7) ? Cl11 C10 Cl12 . . '2 576' 101(5) ? Cl11 C10 C10 . . '2 576' 118(6) ? Cl12 C10 H10a . . . 108(7) ? Cl12 C10 H10b . . . 111(6) ? Cl12 C10 Cl12 . . '2 576' 112(6) ? Cl12 C10 C10 . . '2 576' 59(4) ? H10a C10 H10b . . . 107(4) ? H10a C10 Cl12 . . '2 576' 7.4(17) ? H10a C10 C10 . . '2 576' 49(5) ? H10b C10 Cl12 . . '2 576' 111(4) ? H10b C10 C10 . . '2 576' 130(4) ? Cl12 C10 C10 '2 576' . '2 576' 52(4) ? C20 Cl22 C20 . . '2 676' 97(4) ? Cl21 C20 Cl22 . . . 110(4) ? Cl21 C20 H20a . . . 112(7) ? Cl21 C20 H20b . . . 111(12) ? Cl21 C20 Cl22 . . '2 676' 167(9) ? Cl22 C20 H20a . . . 111(13) ? Cl22 C20 H20b . . . 109(7) ? Cl22 C20 Cl22 . . '2 676' 83(5) ? H20a C20 H20b . . . 105(5) ? H20a C20 Cl22 . . '2 676' 64(3) ? H20b C20 Cl22 . . '2 676' 61(3) ? C10 H10a Cl12 . . '2 576' 164(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Na N0 2.85(4) . . ? Na C1a 3.70(5) . . ? Na C2a 3.16(4) . . ? Na C4a 3.17(4) . . ? Na C4a' 3.19(4) . . ? Na C2a' 3.29(4) . . ? Na C1a' 3.65(5) . . ? Na C7b 3.43(4) . . ? Na C9b 3.38(3) . . ? Na C9b' 3.35(3) . . ? Na C7b' 3.31(3) . . ? Na C7c 3.45(4) . . ? Na C9c 3.45(3) . . ? Na C9c' 3.31(4) . . ? Na C7c' 3.38(4) . . ? Na N0' 2.95(4) . . ? N0 C2a 2.36(5) . . ? N0 O3a 2.86(5) . . ? N0 C2b 2.53(4) . . ? N0 C2c 2.54(4) . . ? N0 H1aA 2.17(3) . . ? N0 H1aB 2.15(3) . . ? N0 H2aA 2.50(3) . . ? N0 H1bA 2.14(4) . . ? N0 H1bB 2.12(3) . . ? N0 H1cA 2.11(3) . . ? N0 H1cB 2.10(3) . . ? C1a O3a 2.54(6) . . ? C1a C1b 2.45(5) . . ? C1a C1c 2.46(5) . . ? C1a H2aA 2.00(4) . . ? C1a H2aB 2.03(4) . . ? C1a H1cA 2.46(4) . . ? C2a C4a 2.30(6) . . ? C2a H1aA 2.07(4) . . ? C2a H1aB 2.04(3) . . ? C2a H4aA 2.48(4) . . ? O3a C4a' 2.25(5) . . ? O3a O3a' 2.71(3) . . ? O3a H2aA 1.88(3) . . ? O3a H2aB 1.88(2) . . ? O3a H4aA 2.00(2) . . ? O3a H4aB 2.015(18) . . ? O3a H4a'A 2.40(3) . . ? C4a O3a' 2.30(5) . . ? C4a H2aB 2.41(4) . . ? C4a H4a'A 1.88(5) . . ? C4a H4a'B 1.94(5) . . ? C4a' C2a' 2.32(5) . . ? C4a' H4aA 1.99(4) . . ? C4a' H4aB 1.94(5) . . ? C4a' H2a'A 2.48(4) . . ? O3a' C1a' 2.41(5) . . ? O3a' N0' 2.88(3) . . ? O3a' H4aB 2.45(3) . . ? O3a' H4a'A 2.04(2) . . ? O3a' H4a'B 2.03(2) . . ? O3a' H2a'A 1.90(3) . . ? O3a' H2a'B 1.88(2) . . ? C2a' N0' 2.41(3) . . ? C2a' H1a'A 2.04(3) . . ? C2a' H1a'B 2.08(4) . . ? C1a' C1b' 2.44(3) . . ? C1a' C1c' 2.36(4) . . ? C1a' H2a'A 2.02(3) . . ? C1a' H2a'B 2.01(3) . . ? C1a' H1c'A 2.43(3) . . ? C1b C3b 2.34(6) . . ? C1b C7b 2.59(5) . . ? C1b O8b 2.74(5) . . ? C1b C1c 2.43(4) . . ? C1b Cl22 3.76(7) . '2 676' ? C1b H1aA 2.47(3) . . ? C1b H1cB 2.50(3) . . ? C2b C4b 2.28(5) . . ? C2b C5b 2.64(5) . . ? C2b C6b 2.41(5) . . ? C2b O8b 2.19(5) . . ? C2b H1bA 2.11(3) . . ? C2b H1bB 2.07(3) . . ? C2b H3b 2.13(4) . . ? C3b C5b 2.44(6) . . ? C3b C6b 2.92(7) . . ? C3b C7b 2.46(7) . . ? C3b Cl11 3.83(7) . '2 676' ? C3b Cl12 3.71(7) . '2 676' ? C3b H1bA 2.32(4) . . ? C3b H4b 2.16(4) . . ? C4b C6b 2.35(7) . . ? C4b C7b 2.66(6) . . ? C4b H3b 2.06(4) . . ? C4b H5b 2.02(4) . . ? C5b C7b 2.31(5) . . ? C5b H4b 1.92(5) . . ? C5b H6b 2.16(5) . . ? C6b O8b 2.44(5) . . ? C6b C9b 2.98(6) . . ? C6b H5b 1.99(4) . . ? C7b C9b 2.43(6) . . ? C7b H6b 2.14(3) . . ? O8b C9b' 2.31(5) . . ? O8b O8b' 2.82(4) . . ? O8b H9bA 2.11(2) . . ? O8b H9bB 2.11(3) . . ? O8b H9b'A 2.34(2) . . ? C9b O8b' 2.29(5) . . ? C9b H9b'A 1.96(4) . . ? C9b H9b'B 1.97(4) . . ? C9b' C7b' 2.39(6) . . ? C9b' C6b' 2.88(6) . . ? C9b' H9bA 2.06(4) . . ? C9b' H9bB 1.98(4) . . ? O8b' C6b' 2.40(4) . . ? O8b' C2b' 2.26(5) . . ? O8b' C1b' 2.60(5) . . ? O8b' H9bB 2.39(2) . . ? O8b' H9b'A 2.06(3) . . ? O8b' H9b'B 2.08(2) . . ? O8b' H1b'B 2.41(3) . . ? C7b' C5b' 2.34(5) . . ? C7b' C4b' 2.76(5) . . ? C7b' C3b' 2.33(6) . . ? C7b' C1b' 2.42(5) . . ? C7b' H6b' 2.06(3) . . ? C6b' C4b' 2.38(7) . . ? C6b' C3b' 2.70(7) . . ? C6b' C2b' 2.39(5) . . ? C6b' H5b' 2.00(3) . . ? C5b' C3b' 2.34(6) . . ? C5b' C2b' 2.74(5) . . ? C5b' H6b' 2.01(5) . . ? C5b' H4b' 2.08(5) . . ? C4b' C2b' 2.41(4) . . ? C4b' H5b' 2.06(4) . . ? C4b' H3b' 2.03(4) . . ? C3b' C1b' 2.49(5) . . ? C3b' H4b' 2.07(4) . . ? C2b' N0' 2.49(3) . . ? C2b' H3b' 2.04(4) . . ? C2b' H1b'A 1.99(3) . . ? C2b' H1b'B 1.99(3) . . ? C1b' C1c' 2.42(4) . . ? C1b' H1a'A 2.44(3) . . ? C1c C3c 2.40(5) . . ? C1c C7c 2.51(6) . . ? C1c O8c 2.89(6) . . ? C1c H1bA 2.48(4) . . ? C2c C4c 2.30(5) . . ? C2c C5c 2.65(6) . . ? C2c C6c 2.42(7) . . ? C2c O8c 2.33(5) . . ? C2c H1cA 2.11(4) . . ? C2c H1cB 2.11(4) . . ? C2c H3c 2.11(4) . . ? C3c C5c 2.37(7) . . ? C3c C6c 2.92(7) . . ? C3c C7c 2.38(6) . . ? C3c H1cA 2.37(4) . . ? C3c H4c 2.02(3) . . ? C4c C6c 2.41(7) . . ? C4c C7c 2.65(5) . . ? C4c H3c 2.13(6) . . ? C4c H5c 1.92(6) . . ? C5c C7c 2.36(5) . . ? C5c H4c 1.99(5) . . ? C5c H6c 2.18(5) . . ? C6c O8c 2.45(4) . . ? C6c C9c 2.95(5) . . ? C6c Cl12 3.78(6) . '1 645' ? C6c H5c 2.09(4) . . ? C7c C9c 2.42(5) . . ? C7c H6c 2.23(4) . . ? O8c C9c' 2.30(4) . . ? O8c O8c' 2.67(3) . . ? O8c H9cA 2.01(2) . . ? O8c H9cB 2.01(2) . . ? O8c H9c'B 2.46(2) . . ? C9c O8c' 2.32(4) . . ? C9c H9c'A 2.02(3) . . ? C9c H9c'B 1.98(3) . . ? C9c' C7c' 2.35(5) . . ? C9c' C6c' 2.82(5) . . ? C9c' H9cA 2.03(3) . . ? C9c' H9cB 2.08(4) . . ? O8c' C6c' 2.44(4) . . ? O8c' C2c' 2.27(4) . . ? O8c' C1c' 2.75(5) . . ? O8c' H9c'A 1.92(2) . . ? O8c' H9c'B 1.93(3) . . ? C7c' C5c' 2.36(4) . . ? C7c' C4c' 2.70(5) . . ? C7c' C3c' 2.34(6) . . ? C7c' C1c' 2.43(6) . . ? C7c' H6c' 2.21(4) . . ? C6c' C4c' 2.36(6) . . ? C6c' C3c' 2.83(7) . . ? C6c' C2c' 2.36(6) . . ? C6c' H5c' 2.02(3) . . ? C5c' C3c' 2.41(6) . . ? C5c' C2c' 2.66(5) . . ? C5c' H6c' 2.13(4) . . ? C5c' H4c' 1.96(4) . . ? C4c' C2c' 2.36(4) . . ? C4c' H5c' 1.98(5) . . ? C4c' H3c' 2.13(5) . . ? C3c' C1c' 2.43(4) . . ? C3c' H4c' 2.13(3) . . ? C3c' H1c'B 2.45(4) . . ? C2c' N0' 2.53(4) . . ? C2c' H3c' 2.17(4) . . ? C2c' H1c'A 2.05(3) . . ? C2c' H1c'B 2.09(4) . . ? C1c' H1a'B 2.37(3) . . ? N0' H1a'A 2.04(2) . . ? N0' H1a'B 2.03(3) . . ? N0' H1b'A 2.04(3) . . ? N0' H1b'B 2.036(19) . . ? N0' H1c'A 1.99(2) . . ? N0' H1c'B 2.00(3) . . ? O101 C102 2.28(4) . . ? O101 N102 2.72(4) . . ? O101 O1021 2.62(5) . . ? O101 C106 2.34(6) . . ? O101 N106 2.90(5) . . ? O101 O1061 2.63(4) . . ? O101 H9b'A 2.14(3) . '2 675' ? C101 N102 2.48(5) . . ? C101 O1021 2.86(6) . . ? C101 C103 2.36(5) . . ? C101 C104 2.78(5) . . ? C101 C105 2.39(6) . . ? C101 N106 2.51(5) . . ? C101 O1061 2.76(4) . . ? C102 O1021 2.26(7) . . ? C102 O1022 2.24(5) . . ? C102 C104 2.36(5) . . ? C102 C105 2.74(5) . . ? C102 C106 2.31(5) . . ? C102 Cl21 3.92(5) . '2 675' ? C102 H103 2.01(3) . . ? N102 C103 2.40(6) . . ? N102 Cl21 3.68(6) . '2 675' ? O1021 O1022 2.11(6) . . ? O1022 C103 2.63(6) . . ? O1022 Cl11 3.94(6) . '2 675' ? O1022 Cl12 3.77(6) . '2 675' ? O1022 Cl21 3.22(6) . '2 675' ? O1022 H4b 2.50(5) . '2 775' ? O1022 H103 2.37(5) . . ? C103 N104 2.47(6) . . ? C103 O1041 2.80(5) . . ? C103 C105 2.38(5) . . ? C103 C106 2.66(4) . . ? C103 Cl22 3.78(6) . '2 675' ? C104 O1041 2.30(5) . . ? C104 O1042 2.24(6) . . ? C104 C106 2.36(5) . . ? C104 Cl22 3.80(5) . '2 675' ? C104 H103 1.99(3) . . ? C104 H105 2.14(3) . . ? N104 C105 2.48(5) . . ? O1041 O1042 2.14(5) . . ? O1041 H103 2.47(4) . . ? O1042 C105 2.65(5) . . ? O1042 H105 2.41(4) . . ? C105 N106 2.46(4) . . ? C105 O1062 2.60(4) . . ? C106 O1061 2.31(4) . . ? C106 O1062 2.30(5) . . ? C106 Cl22 3.84(6) . '1 554' ? C106 H105 2.05(4) . . ? O1061 O1062 2.16(6) . . ? O1062 Cl11 3.47(6) . '1 554' ? O1062 H105 2.25(3) . . ? Cl11 Cl11 4.66(6) . '2 576' ? Cl11 Cl12 2.72(6) . '2 576' ? Cl11 Cl12 2.77(4) . . ? Cl11 C10 3.15(9) . '2 576' ? Cl11 Cl21 2.64(6) . . ? Cl11 Cl22 3.50(5) . . ? Cl11 C20 3.67(6) . . ? Cl11 H3b 3.28(5) . '2 676' ? Cl11 H4c' 3.17(4) . '1 456' ? Cl11 H10a 2.22(4) . . ? Cl11 H10a 2.70(4) . '2 576' ? Cl11 H10b 2.21(4) . . ? Cl12 Cl12 2.90(5) . '2 576' ? Cl12 Cl21 4.53(5) . '2 576' ? Cl12 Cl21 4.53(4) . . ? Cl12 Cl22 4.57(4) . . ? Cl12 H3b 2.82(5) . '2 676' ? Cl12 H6c 3.07(3) . '1 465' ? Cl12 H103 3.35(3) . '2 675' ? Cl12 H10a 2.21(3) . . ? Cl12 H10b 2.19(3) . . ? Cl12 H10b 2.32(5) . '2 576' ? C10 H10a 1.52(9) . '2 576' ? Cl21 Cl22 2.62(7) . . ? Cl21 Cl22 3.67(6) . '2 676' ? Cl21 H1aA 3.23(4) . . ? Cl21 H2a'A 3.30(4) . '2 666' ? Cl21 H20a 2.17(4) . . ? Cl21 H20b 2.17(4) . . ? Cl22 Cl22 2.47(4) . '2 676' ? Cl22 H1bA 2.99(5) . '2 676' ? Cl22 H20a 2.14(4) . . ? Cl22 H20a 1.87(4) . '2 676' ? Cl22 H20b 2.13(5) . . ? Cl22 H20b 1.82(5) . '2 676' ? C20 C20 2.77(16) . '2 676' ? H1aA H1aB 1.5514(13) . . ? H2aA H2aB 1.5513(9) . . ? H4aA H4aB 1.5514(12) . . ? H4a'A H4a'B 1.5513(11) . . ? H2a'A H2a'B 1.5513(10) . . ? H1a'A H1a'B 1.5514(9) . . ? H1bA H1bB 1.5513(15) . . ? H9bA H9bB 1.5512(11) . . ? H9b'A H9b'B 1.551(2) . . ? H1b'A H1b'B 1.5513(10) . . ? H1cA H1cB 1.5514(11) . . ? H9cA H9cB 1.5514(9) . . ? H9c'A H9c'B 1.5514(9) . . ? H1c'A H1c'B 1.5514(17) . . ? H10a H10a 1.6596(10) . '2 576' ? H10a H10b 1.5512(14) . . ? H20a H20b 1.5513(17) . . ? _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 1004 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 5 2 2 4 -2 3 -2 2 -4 2 1 5 0 -1 0 5 -1 -1 1 -5 -3 -5 2 -2 -4 2 -3 2 -2 4 -2 -1 0 -5 1 -5 0 1 1 -1 5 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min -14 _reflns_limit_k_max 15 _reflns_limit_l_min -15 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high .94 _reflns_d_resolution_low 13.654 _diffrn_reflns_av_sigmaI/netI .104 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 6 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .281 _refine_ls_wR_factor_all .139 _refine_ls_goodness_of_fit_all 2.034 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end