# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email sst@ri.ac.uk _publ_contact_author_name 'Dr Scott Steven Turner' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Davy-Faraday Laboratory Royal Institution of Great Britiain 21 Albemarle Street London W1S 4BS UNITED KINGDOM ; _publ_contact_author_phone '020 7409 2992' _publ_contact_author_fax '020 7629 3569' _publ_section_title ; Superstructures of donor packing arrangements in a series of molecular charge transfer salts. ; loop_ _publ_author_name _publ_author_address 'Hiroki Akutsu' ; Graduate School and Faculty of Science Himeji Institute of Technology Hyogo, 678-1297, Japan ; 'Akane Akutsu-Sato' ; Department of Organic and Polymeric Materials Tokyo Institute of Technology O-akayama Tokyo, 152-8552, Japan ; 'Scott S. Turner' ; Davy-Faraday Research Laboratory Royal Institution of Great Britain 21 Albemarle Street London, W1S 4BS UK ; 'Peter Day' ; Davy-Faraday Research Laboratory Royal Institution of Great Britain 21 Albemarle Street London, W1S 4BS UK ; 'Enric Canadell' ; Institut de Ciencia de Materials de Barcelona Campus de la UAB E-08193, Bellaterra, Spain ; 'Steven Firth' ; Chemistry Department University College London 20 Gordon Street London, WC1H 0AJ, UK ; ; Robin J.H.Clark ; ; Chemistry Department University College London 20 Gordon Street London, WC1H 0AJ, UK ; 'Jun-ichi Yamada' ; Graduate School and Faculty of Science Himeji Institute of Technology Hyogo, 678-1297, Japan ; 'Shin-ichi Nakatsuji' ; Graduate School and Faculty of Science Himeji Institute of Technology Hyogo, 678-1297, Japan ; data_Compound_I _database_code_depnum_ccdc_archive 'CCDC 213252' _chemical_name_common ; Tetrakis(Bis(ethylenedithio)tetrathiafulvalenium) ammonium tris(oxalato) gallium N-methylformanilide solvate ; _chemical_name_systematic ; Tetrakis(Bis(ethylenedithio)tetrathiafulvalenium) ammonium tris(oxalato) gallium N-methylformanilide solvate ; _audit_creation_date 2003-02-27 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement ' CRYSTALS (Watkin et al 2001) ' _computing_publication_material 'teXsan (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.596(6) _cell_length_b 11.179(5) _cell_length_c 37.834(7) _cell_angle_alpha 82.17(2) _cell_angle_beta 84.53(2) _cell_angle_gamma 65.400(13) _cell_volume 3652.3(25) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description '_black_' _exptl_crystal_colour '_plate_' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_meas ? _chemical_formula_weight 2025.60 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H45 Ga N2 O13 S32 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2060.00 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_max 1.008 _exptl_absorpt_correction_T_min 0.664 #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Quantum CCD' _diffrn_measurement_device 'Rigaku ' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 14825 _reflns_number_total 14825 _reflns_number_gt 10225 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 0.544 _diffrn_reflns_theta_max 27.944 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga 0 2 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 64 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 26 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 108 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 90 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Ga1 Ga 0.53313(5) 0.67360(5) 0.247836(12) 0.0271 1.0000 Uani . S1 S 0.35722(14) -0.05620(12) 0.62874(3) 0.0423 1.0000 Uani . S2 S 0.02058(13) 0.21415(11) 0.60411(3) 0.0369 1.0000 Uani . S3 S 0.38825(14) -0.09332(12) 0.55198(3) 0.0390 1.0000 Uani . S4 S 0.09634(13) 0.12853(12) 0.53324(3) 0.0390 1.0000 Uani . S5 S 0.43522(14) -0.16236(12) 0.47051(3) 0.0398 1.0000 Uani . S6 S 0.14414(13) 0.06090(12) 0.45245(3) 0.0379 1.0000 Uani . S7 S 0.52130(14) -0.23074(12) 0.39813(3) 0.0430 1.0000 Uani . S8 S 0.17636(14) 0.03643(11) 0.37517(3) 0.0405 1.0000 Uani . S9 S 0.12704(14) 0.45174(12) 0.62664(3) 0.0396 1.0000 Uani . S10 S 0.20231(16) 0.72957(12) 0.60146(3) 0.0441 1.0000 Uani . S11 S 0.17168(14) 0.41978(12) 0.54961(3) 0.0377 1.0000 Uani . S12 S 0.24663(15) 0.64914(12) 0.53014(3) 0.0411 1.0000 Uani . S13 S 0.23549(14) 0.35099(12) 0.46935(3) 0.0385 1.0000 Uani . S14 S 0.30829(15) 0.58069(12) 0.44829(3) 0.0400 1.0000 Uani . S15 S 0.26846(15) 0.27057(12) 0.39840(3) 0.0388 1.0000 Uani . S16 S 0.34587(16) 0.54834(12) 0.37146(3) 0.0438 1.0000 Uani . S17 S 0.38814(13) 0.06380(14) 0.13962(3) 0.0486 1.0000 Uani . S18 S -0.00841(12) 0.23189(13) 0.14909(3) 0.0405 1.0000 Uani . S19 S 0.32472(13) 0.08709(13) 0.06369(3) 0.0411 1.0000 Uani . S20 S -0.00518(12) 0.22647(12) 0.07186(3) 0.0394 1.0000 Uani . S21 S 0.28183(13) 0.06423(13) -0.01919(3) 0.0435 1.0000 Uani . S22 S -0.04800(13) 0.19746(14) -0.00886(3) 0.0448 1.0000 Uani . S23 S 0.27198(15) 0.00370(14) -0.09116(3) 0.0532 1.0000 Uani . S24 S -0.11861(15) 0.16313(16) -0.08000(3) 0.0545 1.0000 Uani . S25 S 0.63579(14) 0.32294(15) 0.12035(4) 0.0547 1.0000 Uani . S26 S 0.24064(14) 0.48375(13) 0.13144(3) 0.0470 1.0000 Uani . S27 S 0.56741(13) 0.32601(14) 0.04618(3) 0.0447 1.0000 Uani . S28 S 0.23796(13) 0.46104(14) 0.05572(3) 0.0429 1.0000 Uani . S29 S 0.52309(13) 0.30202(14) -0.03548(3) 0.0445 1.0000 Uani . S30 S 0.19411(13) 0.43992(13) -0.02563(3) 0.0407 1.0000 Uani . S31 S 0.51514(14) 0.26424(14) -0.10997(3) 0.0490 1.0000 Uani . S32 S 0.12066(13) 0.43284(13) -0.09829(3) 0.0433 1.0000 Uani . O1 O 0.7906(3) 0.3313(3) 0.21380(9) 0.0432 1.0000 Uani . O2 O 0.6851(4) 0.2927(3) 0.28258(9) 0.0469 1.0000 Uani . O3 O 0.6813(3) 0.5482(3) 0.21791(8) 0.0363 1.0000 Uani . O4 O 0.5580(3) 0.5125(3) 0.27968(7) 0.0348 1.0000 Uani . O5 O 0.6469(4) 0.9686(3) 0.21002(9) 0.0481 1.0000 Uani . O6 O 0.7392(4) 0.8740(4) 0.27989(9) 0.0519 1.0000 Uani . O7 O 0.5423(3) 0.8238(3) 0.21513(7) 0.0317 1.0000 Uani . O8 O 0.6702(3) 0.7102(3) 0.27586(8) 0.0336 1.0000 Uani . O9 O 0.1284(4) 0.8303(4) 0.20655(9) 0.0496 1.0000 Uani . O10 O 0.1163(3) 0.9149(3) 0.27293(9) 0.0463 1.0000 Uani . O11 O 0.3675(3) 0.6858(3) 0.21839(8) 0.0367 1.0000 Uani . O12 O 0.3632(3) 0.7858(3) 0.27661(8) 0.0349 1.0000 Uani . O13 O 0.0375(5) 0.5361(5) 0.19654(11) 0.0756 1.0000 Uani . N1 N 0.0840(4) 0.5409(4) 0.2528(1) 0.0370 1.0000 Uani . N14 N 0.8513(4) 0.0590(4) 0.23421(12) 0.0473 1.0000 Uani . C1 C 0.1809(6) 0.0035(5) 0.65429(11) 0.0430 1.0000 Uani . C2 C 0.0941(6) 0.1497(5) 0.64820(12) 0.0436 1.0000 Uani . C3 C 0.2843(5) -0.0000(4) 0.58626(11) 0.0314 1.0000 Uani . C4 C 0.1523(5) 0.1017(4) 0.57736(11) 0.0289 1.0000 Uani . C5 C 0.2574(5) -0.0014(4) 0.51910(11) 0.0344 1.0000 Uani . C6 C 0.2771(5) -0.0300(4) 0.48483(11) 0.0335 1.0000 Uani . C7 C 0.3862(5) -0.1253(4) 0.42582(11) 0.0310 1.0000 Uani . C8 C 0.2533(5) -0.0233(4) 0.41739(11) 0.0322 1.0000 Uani . C9 C 0.4462(5) -0.1596(5) 0.35463(12) 0.0393 1.0000 Uani . C10 C 0.2771(5) -0.1094(4) 0.35306(11) 0.0335 1.0000 Uani . C11 C 0.2230(6) 0.5181(5) 0.65158(12) 0.0430 1.0000 Uani . C12 C 0.1612(6) 0.6655(5) 0.64526(12) 0.0460 1.0000 Uani . C13 C 0.1643(5) 0.5127(4) 0.58364(11) 0.0302 1.0000 Uani . C14 C 0.1962(5) 0.6180(4) 0.57452(11) 0.0307 1.0000 Uani . C15 C 0.2235(5) 0.5165(4) 0.51626(11) 0.0337 1.0000 Uani . C16 C 0.2508(5) 0.4885(4) 0.48196(11) 0.0337 1.0000 Uani . C17 C 0.2739(5) 0.3855(4) 0.4241(1) 0.0300 1.0000 Uani . C18 C 0.3055(5) 0.4905(4) 0.41434(11) 0.0325 1.0000 Uani . C19 C 0.2911(5) 0.3419(4) 0.35364(11) 0.0359 1.0000 Uani . C20 C 0.4059(5) 0.4000(4) 0.35036(12) 0.0368 1.0000 Uani . C21 C 0.2728(6) 0.0927(7) 0.17913(14) 0.0682 1.0000 Uani . C22 C 0.1339(6) 0.2112(7) 0.17866(14) 0.0652 1.0000 Uani . C23 C 0.2522(5) 0.1186(4) 0.10700(11) 0.0341 1.0000 Uani . C24 C 0.1002(5) 0.1824(4) 0.11052(11) 0.0334 1.0000 Uani . C25 C 0.1487(5) 0.1471(4) 0.04403(11) 0.0339 1.0000 Uani . C26 C 0.1304(5) 0.1373(4) 0.01007(11) 0.0352 1.0000 Uani . C27 C 0.1693(5) 0.0737(4) -0.05413(11) 0.0340 1.0000 Uani . C28 C 0.0198(5) 0.1339(4) -0.04917(11) 0.0347 1.0000 Uani . C29 C 0.1351(7) 0.0475(8) -0.12383(15) 0.0731 1.0000 Uani . C30 C -0.0067(8) 0.1591(7) -0.12125(15) 0.0763 1.0000 Uani . C31 C 0.5256(7) 0.3308(7) 0.16050(14) 0.0621 1.0000 Uani . C32 C 0.3865(7) 0.4582(7) 0.16170(14) 0.0623 1.0000 Uani . C33 C 0.4974(5) 0.3677(4) 0.08851(11) 0.0361 1.0000 Uani . C34 C 0.3471(5) 0.4296(4) 0.09313(11) 0.0342 1.0000 Uani . C35 C 0.3904(5) 0.3878(4) 0.02731(11) 0.0337 1.0000 Uani . C36 C 0.3724(5) 0.3772(4) -0.00702(11) 0.0337 1.0000 Uani . C37 C 0.4117(5) 0.3273(4) -0.07206(11) 0.0341 1.0000 Uani . C38 C 0.2609(5) 0.3897(4) -0.0674(1) 0.0306 1.0000 Uani . C39 C 0.3664(6) 0.2854(5) -0.13869(12) 0.0463 1.0000 Uani . C40 C 0.2304(5) 0.4138(5) -0.13946(12) 0.0427 1.0000 Uani . C41 C 0.7144(4) 0.4266(4) 0.22990(11) 0.0299 1.0000 Uani . C42 C 0.6497(5) 0.4046(4) 0.26719(11) 0.0302 1.0000 Uani . C43 C 0.6212(5) 0.8770(4) 0.22640(11) 0.0302 1.0000 Uani . C44 C 0.6837(4) 0.8183(4) 0.26392(11) 0.0317 1.0000 Uani . C45 C 0.2402(5) 0.7812(4) 0.22519(11) 0.0324 1.0000 Uani . C46 C 0.2362(5) 0.8338(4) 0.26082(11) 0.0290 1.0000 Uani . C47 C 0.1629(5) 0.3999(4) 0.26045(11) 0.0335 1.0000 Uani . C48 C 0.3187(5) 0.3411(5) 0.25923(13) 0.0432 1.0000 Uani . C49 C 0.3942(6) 0.2048(6) 0.26720(15) 0.0564 1.0000 Uani . C50 C 0.3138(7) 0.1298(5) 0.27594(14) 0.0560 1.0000 Uani . C51 C 0.1568(7) 0.1904(5) 0.27720(14) 0.0557 1.0000 Uani . C52 C 0.0816(6) 0.3248(5) 0.26972(13) 0.0446 1.0000 Uani . C53 C 0.0701(6) 0.6202(5) 0.28102(15) 0.0527 1.0000 Uani . C54 C 0.0217(6) 0.5968(5) 0.22140(14) 0.0480 1.0000 Uani . H1 H 0.1195 -0.0408 0.6482 0.0507 1.0000 Uiso . H2 H 0.2033 -0.0253 0.6792 0.0507 1.0000 Uiso . H3 H 0.1594 0.1910 0.6528 0.0507 1.0000 Uiso . H4 H 0.0078 0.1769 0.6653 0.0507 1.0000 Uiso . H5 H 0.4736 -0.0846 0.3469 0.0507 1.0000 Uiso . H6 H 0.4964 -0.2228 0.3377 0.0507 1.0000 Uiso . H7 H 0.2442 -0.1785 0.3636 0.0507 1.0000 Uiso . H8 H 0.2459 -0.0910 0.3282 0.0507 1.0000 Uiso . H9 H 0.2134 0.4931 0.6766 0.0507 1.0000 Uiso . H10 H 0.3309 0.4839 0.6448 0.0507 1.0000 Uiso . H11 H 0.2024 0.6968 0.6624 0.0507 1.0000 Uiso . H12 H 0.0527 0.6989 0.6494 0.0507 1.0000 Uiso . H13 H 0.3212 0.2722 0.3381 0.0507 1.0000 Uiso . H14 H 0.1948 0.4080 0.3467 0.0507 1.0000 Uiso . H15 H 0.4314 0.4178 0.3253 0.0507 1.0000 Uiso . H16 H 0.5018 0.3347 0.3605 0.0507 1.0000 Uiso . H17 H 0.2434 0.0175 0.1856 0.0507 1.0000 Uiso . H18 H 0.3343 0.0894 0.1983 0.0507 1.0000 Uiso . H19 H 0.1672 0.2816 0.1723 0.0507 1.0000 Uiso . H20 H 0.0900 0.2175 0.2022 0.0507 1.0000 Uiso . H21 H 0.1806 0.0627 -0.1468 0.0507 1.0000 Uiso . H22 H 0.1065 -0.0247 -0.1245 0.0507 1.0000 Uiso . H23 H -0.0693 0.1650 -0.1407 0.0507 1.0000 Uiso . H24 H 0.0145 0.2370 -0.1250 0.0507 1.0000 Uiso . H25 H 0.4903 0.2617 0.1635 0.0507 1.0000 Uiso . H26 H 0.5877 0.3191 0.1802 0.0507 1.0000 Uiso . H27 H 0.4217 0.5306 0.1557 0.0507 1.0000 Uiso . H28 H 0.3434 0.4669 0.1855 0.0507 1.0000 Uiso . H29 H 0.4094 0.2719 -0.1624 0.0507 1.0000 Uiso . H30 H 0.3302 0.2160 -0.1309 0.0507 1.0000 Uiso . H31 H 0.1655 0.4213 -0.1584 0.0507 1.0000 Uiso . H32 H 0.2643 0.4838 -0.1446 0.0507 1.0000 Uiso . H33 H 0.3805 0.3942 0.2525 0.0507 1.0000 Uiso . H34 H 0.5035 0.1630 0.2658 0.0507 1.0000 Uiso . H35 H 0.3682 0.0312 0.2803 0.0507 1.0000 Uiso . H36 H 0.0982 0.1345 0.2828 0.0507 1.0000 Uiso . H37 H -0.0320 0.3658 0.2711 0.0507 1.0000 Uiso . H38 H 0.0800 0.5698 0.3049 0.0507 1.0000 Uiso . H39 H 0.1490 0.6541 0.2794 0.0507 1.0000 Uiso . H40 H -0.0271 0.6962 0.2824 0.0507 1.0000 Uiso . H41 H -0.0370 0.6984 0.2194 0.0507 1.0000 Uiso . H42 H 0.8120 0.1396 0.2451 0.0507 1.0000 Uiso . H43 H 0.9587 0.0165 0.2364 0.0507 1.0000 Uiso . H44 H 0.8268 0.0777 0.2099 0.0507 1.0000 Uiso . H45 H 0.8049 0.0030 0.2462 0.0507 1.0000 Uiso . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0308(2) 0.0288(2) 0.0211(2) -0.00695(18) 0.00127(17) -0.01064(19) S1 0.0520(7) 0.0435(7) 0.0241(5) -0.0070(5) -0.0059(5) -0.0104(6) S2 0.0457(7) 0.0370(6) 0.0241(5) -0.0099(5) 0.0012(5) -0.0116(5) S3 0.0468(7) 0.0426(7) 0.0224(5) -0.0103(5) 0.0038(5) -0.0121(5) S4 0.0473(7) 0.0448(7) 0.0218(5) -0.0080(5) -0.0025(5) -0.0145(5) S5 0.0485(7) 0.0449(7) 0.0202(5) -0.0063(5) -0.0020(5) -0.0126(5) S6 0.0470(7) 0.0412(6) 0.0221(5) -0.0104(5) 0.0032(5) -0.0137(5) S7 0.0459(7) 0.0452(7) 0.0247(5) -0.0111(5) -0.0021(5) -0.0032(5) S8 0.0553(7) 0.0333(6) 0.0245(5) -0.0099(5) -0.0082(5) -0.0065(5) S9 0.0576(7) 0.0474(7) 0.0240(5) -0.0121(5) 0.0109(5) -0.0317(6) S10 0.0769(9) 0.0373(7) 0.0252(6) -0.0110(5) 0.0074(5) -0.0300(6) S11 0.0554(7) 0.0448(7) 0.0215(5) -0.0104(5) 0.0029(5) -0.0279(6) S12 0.0659(8) 0.0421(7) 0.0208(5) -0.0071(5) 0.0059(5) -0.0280(6) S13 0.0582(7) 0.0460(7) 0.0195(5) -0.0083(5) 0.0058(5) -0.0294(6) S14 0.0633(8) 0.0398(7) 0.0233(5) -0.0094(5) 0.0025(5) -0.0265(6) S15 0.0632(8) 0.0414(7) 0.0214(5) -0.0090(5) 0.0057(5) -0.0308(6) S16 0.0740(9) 0.0332(6) 0.0258(6) -0.0060(5) 0.0109(5) -0.0255(6) S17 0.0297(6) 0.0671(9) 0.0331(6) -0.0199(6) -0.0039(5) 0.0009(5) S18 0.0286(6) 0.0566(7) 0.0235(5) -0.0124(5) -0.0002(4) -0.0025(5) S19 0.0289(6) 0.0586(8) 0.0280(6) -0.0117(5) 0.0027(4) -0.0087(5) S20 0.0299(6) 0.0537(7) 0.0228(5) -0.0078(5) -0.0013(4) -0.0044(5) S21 0.0318(6) 0.0624(8) 0.0291(6) -0.0147(5) 0.0028(5) -0.0103(5) S22 0.0316(6) 0.0648(8) 0.0270(6) -0.0141(5) 0.0018(5) -0.0067(5) S23 0.0500(8) 0.0660(9) 0.0311(6) -0.0204(6) 0.0077(5) -0.0088(6) S24 0.0419(7) 0.082(1) 0.0356(7) -0.0120(7) -0.0073(5) -0.0188(7) S25 0.0389(7) 0.0737(9) 0.0421(7) -0.0238(7) -0.0142(5) -0.0059(6) S26 0.0446(7) 0.0597(8) 0.0246(6) -0.0126(5) 0.0000(5) -0.0073(6) S27 0.0306(6) 0.0679(8) 0.0299(6) -0.0132(6) -0.0007(5) -0.0124(6) S28 0.0311(6) 0.0675(8) 0.0228(5) -0.0094(5) -0.0004(4) -0.0117(5) S29 0.0315(6) 0.0677(8) 0.0248(5) -0.0130(5) -0.0005(5) -0.0087(6) S30 0.0310(6) 0.0628(8) 0.0216(5) -0.0102(5) 0.0013(4) -0.0113(5) S31 0.0383(7) 0.0649(8) 0.0301(6) -0.0208(6) 0.0001(5) -0.0030(6) S32 0.0335(6) 0.0655(8) 0.0271(6) -0.0122(5) -0.0034(5) -0.0138(6) O1 0.0446(18) 0.0377(18) 0.0403(18) -0.0170(15) 0.0091(14) -0.0084(14) O2 0.059(2) 0.0318(19) 0.045(2) 0.0017(15) 0.0051(16) -0.0173(16) O3 0.0429(17) 0.0340(17) 0.0271(15) -0.0061(13) 0.0118(13) -0.0128(14) O4 0.0410(17) 0.0374(17) 0.0249(15) -0.0070(13) 0.0124(12) -0.0168(14) O5 0.059(2) 0.050(2) 0.046(2) 0.0036(17) -0.0079(16) -0.0345(18) O6 0.063(2) 0.058(2) 0.049(2) -0.0054(17) -0.0187(17) -0.0354(18) O7 0.0440(17) 0.0325(16) 0.0221(14) -0.0012(12) -0.0067(12) -0.0183(13) O8 0.0355(16) 0.0386(18) 0.0278(15) 0.0015(13) -0.0072(12) -0.0164(13) O9 0.0411(19) 0.063(2) 0.044(2) -0.0063(17) -0.0164(16) -0.0178(17) O10 0.0349(18) 0.0413(19) 0.057(2) -0.0200(16) -0.0025(15) -0.0055(15) O11 0.0377(17) 0.0445(18) 0.0321(16) -0.0185(14) 0.0007(13) -0.0171(14) O12 0.0318(16) 0.0403(18) 0.0297(16) -0.0158(13) -0.0002(12) -0.0086(13) O13 0.080(3) 0.099(3) 0.046(2) -0.012(2) -0.009(2) -0.032(3) N1 0.038(2) 0.034(2) 0.036(2) -0.0030(16) -0.0033(16) -0.0113(16) N14 0.038(2) 0.039(2) 0.066(3) -0.002(2) -0.012(2) -0.0154(18) C1 0.072(3) 0.041(3) 0.018(2) -0.0005(18) 0.000(2) -0.026(2) C2 0.058(3) 0.046(3) 0.024(2) -0.012(2) 0.001(2) -0.017(2) C3 0.042(2) 0.032(2) 0.023(2) -0.0095(17) 0.0034(18) -0.0173(19) C4 0.043(2) 0.029(2) 0.022(2) -0.0057(16) 0.0004(17) -0.0217(19) C5 0.050(3) 0.041(3) 0.020(2) -0.0091(18) 0.0045(18) -0.025(2) C6 0.045(3) 0.037(2) 0.022(2) -0.0050(18) 0.0001(18) -0.020(2) C7 0.041(2) 0.032(2) 0.0193(19) -0.0019(16) -0.0028(17) -0.0146(19) C8 0.048(3) 0.032(2) 0.020(2) -0.0072(17) 0.0016(18) -0.019(2) C9 0.043(3) 0.048(3) 0.024(2) -0.011(2) 0.0037(19) -0.015(2) C10 0.048(3) 0.032(2) 0.022(2) -0.0098(17) -0.0014(18) -0.016(2) C11 0.058(3) 0.042(3) 0.027(2) -0.002(2) -0.005(2) -0.018(2) C12 0.075(3) 0.044(3) 0.024(2) -0.010(2) -0.002(2) -0.027(3) C13 0.032(2) 0.034(2) 0.025(2) -0.0113(17) 0.0037(17) -0.0120(18) C14 0.035(2) 0.034(2) 0.025(2) -0.0100(17) 0.0053(17) -0.0142(19) C15 0.038(2) 0.040(3) 0.022(2) -0.0107(18) -0.0004(17) -0.0125(19) C16 0.039(2) 0.037(2) 0.025(2) -0.0098(18) 0.0010(18) -0.0141(19) C17 0.034(2) 0.034(2) 0.021(2) -0.0076(17) 0.0032(16) -0.0115(18) C18 0.043(3) 0.030(2) 0.024(2) -0.0122(18) 0.0043(18) -0.0140(19) C19 0.051(3) 0.042(3) 0.018(2) -0.0047(18) -0.0013(18) -0.022(2) C20 0.043(3) 0.037(3) 0.030(2) -0.0131(19) 0.0123(19) -0.016(2) C21 0.039(3) 0.108(5) 0.035(3) -0.003(3) -0.009(2) -0.007(3) C22 0.043(3) 0.112(5) 0.036(3) -0.032(3) 0.008(2) -0.022(3) C23 0.032(2) 0.035(2) 0.026(2) -0.0061(18) -0.0025(17) -0.0037(19) C24 0.030(2) 0.038(2) 0.025(2) -0.0075(18) 0.0005(17) -0.0057(18) C25 0.031(2) 0.035(2) 0.031(2) -0.0041(18) 0.0001(18) -0.0087(18) C26 0.031(2) 0.041(3) 0.027(2) -0.0068(19) 0.0043(18) -0.0088(19) C27 0.036(2) 0.041(3) 0.023(2) -0.0061(18) 0.0033(17) -0.014(2) C28 0.038(3) 0.039(3) 0.022(2) -0.0049(18) -0.0002(18) -0.011(2) C29 0.068(4) 0.116(6) 0.037(3) -0.020(3) 0.006(3) -0.036(4) C30 0.084(4) 0.091(5) 0.029(3) -0.016(3) -0.009(3) -0.006(4) C31 0.061(4) 0.094(5) 0.038(3) 0.005(3) -0.021(3) -0.038(3) C32 0.065(4) 0.095(5) 0.039(3) -0.034(3) 0.007(3) -0.040(3) C33 0.034(2) 0.041(3) 0.029(2) -0.0133(19) -0.0047(18) -0.008(2) C34 0.038(3) 0.040(3) 0.020(2) -0.0047(18) -0.0027(17) -0.011(2) C35 0.032(2) 0.043(3) 0.022(2) -0.0051(18) 0.0018(17) -0.0126(19) C36 0.031(2) 0.044(3) 0.022(2) -0.0042(18) -0.0002(17) -0.0116(19) C37 0.040(3) 0.037(2) 0.021(2) -0.0076(18) -0.0018(18) -0.010(2) C38 0.034(2) 0.037(2) 0.0194(19) -0.0075(17) -0.0022(16) -0.0115(19) C39 0.052(3) 0.052(3) 0.027(2) -0.015(2) -0.004(2) -0.011(2) C40 0.043(3) 0.055(3) 0.026(2) -0.007(2) -0.0027(19) -0.013(2) C41 0.028(2) 0.035(2) 0.026(2) -0.0057(18) -0.0025(16) -0.0099(18) C42 0.030(2) 0.034(2) 0.029(2) -0.0041(18) -0.0025(17) -0.0146(18) C43 0.029(2) 0.031(2) 0.029(2) -0.0063(18) 0.0005(17) -0.0096(18) C44 0.025(2) 0.034(2) 0.033(2) -0.0096(19) -0.0006(17) -0.0073(18) C45 0.040(3) 0.035(2) 0.028(2) -0.0036(18) 0.0003(18) -0.021(2) C46 0.031(2) 0.025(2) 0.032(2) -0.0082(17) 0.0022(17) -0.0118(18) C47 0.040(3) 0.038(3) 0.025(2) -0.0042(18) -0.0021(18) -0.018(2) C48 0.035(3) 0.049(3) 0.043(3) -0.011(2) 0.002(2) -0.013(2) C49 0.046(3) 0.057(4) 0.048(3) -0.015(3) 0.003(2) -0.002(3) C50 0.083(4) 0.036(3) 0.039(3) -0.009(2) 0.003(3) -0.014(3) C51 0.091(4) 0.048(3) 0.042(3) -0.003(2) -0.004(3) -0.043(3) C52 0.048(3) 0.050(3) 0.043(3) -0.008(2) -0.002(2) -0.027(2) C53 0.064(3) 0.033(3) 0.058(3) -0.013(2) 0.008(3) -0.017(2) C54 0.047(3) 0.052(3) 0.036(3) -0.002(2) 0.005(2) -0.013(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 376. 332. 191. ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10225 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_all 0.0926 _refine_ls_wR_factor_ref 0.0631 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.0553 _refine_ls_shift/su_max 0.000982 _refine_diff_density_min -0.78 _refine_diff_density_max 0.78 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ga1 . O3 . 1.933(3) yes Ga1 . O4 . 1.964(3) yes Ga1 . O7 . 1.973(3) yes Ga1 . O8 . 1.963(3) yes Ga1 . O11 . 1.975(3) yes Ga1 . O12 . 1.936(3) yes S1 . C1 . 1.779(5) yes S1 . C3 . 1.744(4) yes S2 . C2 . 1.809(5) yes S2 . C4 . 1.727(4) yes S3 . C3 . 1.738(4) yes S3 . C5 . 1.748(5) yes S4 . C4 . 1.751(4) yes S4 . C5 . 1.723(4) yes S5 . C6 . 1.726(4) yes S5 . C7 . 1.746(4) yes S6 . C6 . 1.744(4) yes S6 . C8 . 1.731(4) yes S7 . C7 . 1.724(4) yes S7 . C9 . 1.804(5) yes S8 . C8 . 1.751(4) yes S8 . C10 . 1.789(4) yes S9 . C11 . 1.793(5) yes S9 . C13 . 1.740(4) yes S10 . C12 . 1.789(5) yes S10 . C14 . 1.737(4) yes S11 . C13 . 1.739(4) yes S11 . C15 . 1.722(5) yes S12 . C14 . 1.733(4) yes S12 . C15 . 1.741(4) yes S13 . C16 . 1.736(4) yes S13 . C17 . 1.741(4) yes S14 . C16 . 1.723(5) yes S14 . C18 . 1.746(4) yes S15 . C17 . 1.734(4) yes S15 . C19 . 1.805(4) yes S16 . C18 . 1.733(4) yes S16 . C20 . 1.788(4) yes S17 . C21 . 1.756(6) yes S17 . C23 . 1.742(4) yes S18 . C22 . 1.768(5) yes S18 . C24 . 1.724(4) yes S19 . C23 . 1.741(4) yes S19 . C25 . 1.737(4) yes S20 . C24 . 1.753(4) yes S20 . C25 . 1.716(4) yes S21 . C26 . 1.720(4) yes S21 . C27 . 1.750(4) yes S22 . C26 . 1.743(4) yes S22 . C28 . 1.725(4) yes S23 . C27 . 1.715(4) yes S23 . C29 . 1.761(6) yes S24 . C28 . 1.749(4) yes S24 . C30 . 1.803(6) yes S25 . C31 . 1.757(6) yes S25 . C33 . 1.747(4) yes S26 . C32 . 1.798(6) yes S26 . C34 . 1.719(4) yes S27 . C33 . 1.724(4) yes S27 . C35 . 1.730(4) yes S28 . C34 . 1.751(4) yes S28 . C35 . 1.705(4) yes S29 . C36 . 1.701(4) yes S29 . C37 . 1.750(4) yes S30 . C36 . 1.735(4) yes S30 . C38 . 1.724(4) yes S31 . C37 . 1.721(4) yes S31 . C39 . 1.794(5) yes S32 . C38 . 1.736(4) yes S32 . C40 . 1.781(5) yes O1 . C41 . 1.218(5) yes O2 . C42 . 1.226(5) yes O3 . C41 . 1.286(5) yes O4 . C42 . 1.283(5) yes O5 . C43 . 1.226(5) yes O6 . C44 . 1.215(5) yes O7 . C43 . 1.270(5) yes O8 . C44 . 1.286(5) yes O9 . C45 . 1.224(5) yes O10 . C46 . 1.225(5) yes O11 . C45 . 1.275(5) yes O12 . C46 . 1.279(5) yes O13 . C54 . 1.195(6) yes N1 . C47 . 1.437(6) yes N1 . C53 . 1.441(6) yes N1 . C54 . 1.335(6) yes N14 . H42 . 0.956 no N14 . H43 . 0.945 no N14 . H44 . 0.944 no N14 . H45 . 0.956 no C1 . C2 . 1.490(7) yes C1 . H1 . 0.973 no C1 . H2 . 0.968 no C2 . H3 . 0.958 no C2 . H4 . 0.970 no C3 . C4 . 1.338(6) yes C5 . C6 . 1.355(5) yes C7 . C8 . 1.340(6) yes C9 . C10 . 1.484(6) yes C9 . H5 . 0.980 no C9 . H6 . 0.961 no C10 . H7 . 0.975 no C10 . H8 . 0.984 no C11 . C12 . 1.494(7) yes C11 . H9 . 0.958 no C11 . H10 . 0.964 no C12 . H11 . 0.962 no C12 . H12 . 0.954 no C13 . C14 . 1.330(6) yes C15 . C16 . 1.352(5) yes C17 . C18 . 1.328(6) yes C19 . C20 . 1.483(6) yes C19 . H13 . 0.969 no C19 . H14 . 0.945 no C20 . H15 . 0.972 no C20 . H16 . 0.979 no C21 . C22 . 1.435(8) yes C21 . H17 . 0.987 no C21 . H18 . 0.964 no C22 . H19 . 0.960 no C22 . H20 . 0.948 no C23 . C24 . 1.333(6) yes C25 . C26 . 1.338(6) yes C27 . C28 . 1.313(6) yes C29 . C30 . 1.419(9) yes C29 . H21 . 0.960 no C29 . H22 . 0.958 no C30 . H23 . 0.973 no C30 . H24 . 0.963 no C31 . C32 . 1.495(9) yes C31 . H25 . 0.954 no C31 . H26 . 0.961 no C32 . H27 . 0.992 no C32 . H28 . 0.955 no C33 . C34 . 1.321(6) yes C35 . C36 . 1.354(5) yes C37 . C38 . 1.326(6) yes C39 . C40 . 1.483(7) yes C39 . H29 . 0.956 no C39 . H30 . 0.974 no C40 . H31 . 0.967 no C40 . H32 . 0.956 no C41 . C42 . 1.518(6) yes C43 . C44 . 1.545(6) yes C45 . C46 . 1.534(5) yes C47 . C48 . 1.359(6) yes C47 . C52 . 1.359(6) yes C48 . C49 . 1.391(7) yes C48 . H33 . 0.996 no C49 . C50 . 1.349(8) yes C49 . H34 . 0.954 no C50 . C51 . 1.369(8) yes C50 . H35 . 1.002 no C51 . C52 . 1.371(7) yes C51 . H36 . 0.993 no C52 . H37 . 0.990 no C53 . H38 . 0.988 no C53 . H39 . 0.972 no C53 . H40 . 0.968 no C54 . H41 . 1.032 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 . Ga1 . O4 . 82.74(12) yes O3 . Ga1 . O7 . 91.28(12) yes O4 . Ga1 . O7 . 171.33(12) yes O3 . Ga1 . O8 . 100.54(12) yes O4 . Ga1 . O8 . 91.60(12) yes O7 . Ga1 . O8 . 83.29(12) yes O3 . Ga1 . O11 . 89.53(12) yes O4 . Ga1 . O11 . 100.02(13) yes O7 . Ga1 . O11 . 86.16(12) yes O8 . Ga1 . O11 . 165.54(12) yes O3 . Ga1 . O12 . 170.79(13) yes O4 . Ga1 . O12 . 93.21(12) yes O7 . Ga1 . O12 . 93.59(13) yes O8 . Ga1 . O12 . 87.80(12) yes O11 . Ga1 . O12 . 83.01(11) yes C1 . S1 . C3 . 98.5(2) yes C2 . S2 . C4 . 102.8(2) yes C3 . S3 . C5 . 95.5(2) yes C4 . S4 . C5 . 94.5(2) yes C6 . S5 . C7 . 94.4(2) yes C6 . S6 . C8 . 95.5(2) yes C7 . S7 . C9 . 102.2(2) yes C8 . S8 . C10 . 99.1(2) yes C11 . S9 . C13 . 99.5(2) yes C12 . S10 . C14 . 103.1(2) yes C13 . S11 . C15 . 95.2(2) yes C14 . S12 . C15 . 94.8(2) yes C16 . S13 . C17 . 94.8(2) yes C16 . S14 . C18 . 95.2(2) yes C17 . S15 . C19 . 102.1(2) yes C18 . S16 . C20 . 99.5(2) yes C21 . S17 . C23 . 102.2(2) yes C22 . S18 . C24 . 101.6(2) yes C23 . S19 . C25 . 96.6(2) yes C24 . S20 . C25 . 95.5(2) yes C26 . S21 . C27 . 95.7(2) yes C26 . S22 . C28 . 96.2(2) yes C27 . S23 . C29 . 105.0(3) yes C28 . S24 . C30 . 100.3(3) yes C31 . S25 . C33 . 101.9(2) yes C32 . S26 . C34 . 102.2(2) yes C33 . S27 . C35 . 96.0(2) yes C34 . S28 . C35 . 95.6(2) yes C36 . S29 . C37 . 95.5(2) yes C36 . S30 . C38 . 96.27(19) yes C37 . S31 . C39 . 102.0(2) yes C38 . S32 . C40 . 102.0(2) yes Ga1 . O3 . C41 . 113.8(3) yes Ga1 . O4 . C42 . 114.4(3) yes Ga1 . O7 . C43 . 113.5(3) yes Ga1 . O8 . C44 . 112.7(3) yes Ga1 . O11 . C45 . 112.4(2) yes Ga1 . O12 . C46 . 112.6(2) yes C47 . N1 . C53 . 117.1(4) yes C47 . N1 . C54 . 121.9(4) yes C53 . N1 . C54 . 120.9(4) yes H42 . N14 . H43 . 109.469 no H42 . N14 . H44 . 109.548 no H43 . N14 . H44 . 110.470 no H42 . N14 . H45 . 108.505 no H43 . N14 . H45 . 109.365 no H44 . N14 . H45 . 109.452 no S1 . C1 . C2 . 113.3(3) yes S1 . C1 . H1 . 107.668 no C2 . C1 . H1 . 110.137 no S1 . C1 . H2 . 107.939 no C2 . C1 . H2 . 111.319 no H1 . C1 . H2 . 106.114 no S2 . C2 . C1 . 115.8(3) yes S2 . C2 . H3 . 108.307 no C1 . C2 . H3 . 108.612 no S2 . C2 . H4 . 107.673 no C1 . C2 . H4 . 108.989 no H3 . C2 . H4 . 107.129 no S1 . C3 . S3 . 116.4(2) yes S1 . C3 . C4 . 127.4(3) yes S3 . C3 . C4 . 116.0(3) yes S2 . C4 . S4 . 112.7(2) yes S2 . C4 . C3 . 128.8(3) yes S4 . C4 . C3 . 118.5(3) yes S3 . C5 . S4 . 115.5(2) yes S3 . C5 . C6 . 123.3(3) yes S4 . C5 . C6 . 121.2(4) yes S5 . C6 . S6 . 115.3(2) yes S5 . C6 . C5 . 121.8(3) yes S6 . C6 . C5 . 122.9(3) yes S5 . C7 . S7 . 113.0(2) yes S5 . C7 . C8 . 118.2(3) yes S7 . C7 . C8 . 128.7(3) yes S6 . C8 . S8 . 115.7(2) yes S6 . C8 . C7 . 116.2(3) yes S8 . C8 . C7 . 128.1(3) yes S7 . C9 . C10 . 115.1(3) yes S7 . C9 . H5 . 108.217 no C10 . C9 . H5 . 107.206 no S7 . C9 . H6 . 109.342 no C10 . C9 . H6 . 110.418 no H5 . C9 . H6 . 106.170 no S8 . C10 . C9 . 112.9(3) yes S8 . C10 . H7 . 109.579 no C9 . C10 . H7 . 109.408 no S8 . C10 . H8 . 108.943 no C9 . C10 . H8 . 110.920 no H7 . C10 . H8 . 104.781 no S9 . C11 . C12 . 112.2(3) yes S9 . C11 . H9 . 110.468 no C12 . C11 . H9 . 108.621 no S9 . C11 . H10 . 110.243 no C12 . C11 . H10 . 107.477 no H9 . C11 . H10 . 107.656 no S10 . C12 . C11 . 114.9(3) yes S10 . C12 . H11 . 108.581 no C11 . C12 . H11 . 108.662 no S10 . C12 . H12 . 108.892 no C11 . C12 . H12 . 107.447 no H11 . C12 . H12 . 108.164 no S9 . C13 . S11 . 116.2(3) yes S9 . C13 . C14 . 126.7(3) yes S11 . C13 . C14 . 117.0(3) yes S10 . C14 . S12 . 113.3(2) yes S10 . C14 . C13 . 129.1(3) yes S12 . C14 . C13 . 117.6(3) yes S11 . C15 . S12 . 115.2(2) yes S11 . C15 . C16 . 122.5(3) yes S12 . C15 . C16 . 122.2(4) yes S13 . C16 . S14 . 115.3(2) yes S13 . C16 . C15 . 121.1(4) yes S14 . C16 . C15 . 123.5(3) yes S13 . C17 . S15 . 112.8(2) yes S13 . C17 . C18 . 117.6(3) yes S15 . C17 . C18 . 129.7(3) yes S14 . C18 . S16 . 115.8(3) yes S14 . C18 . C17 . 116.9(3) yes S16 . C18 . C17 . 127.3(3) yes S15 . C19 . C20 . 113.1(3) yes S15 . C19 . H13 . 107.197 no C20 . C19 . H13 . 110.275 no S15 . C19 . H14 . 108.375 no C20 . C19 . H14 . 109.560 no H13 . C19 . H14 . 108.232 no S16 . C20 . C19 . 114.0(3) yes S16 . C20 . H15 . 109.140 no C19 . C20 . H15 . 109.596 no S16 . C20 . H16 . 108.951 no C19 . C20 . H16 . 109.407 no H15 . C20 . H16 . 105.332 no S17 . C21 . C22 . 117.6(4) yes S17 . C21 . H17 . 107.692 no C22 . C21 . H17 . 107.037 no S17 . C21 . H18 . 108.832 no C22 . C21 . H18 . 109.634 no H17 . C21 . H18 . 105.305 no S18 . C22 . C21 . 118.4(4) yes S18 . C22 . H19 . 108.234 no C21 . C22 . H19 . 104.464 no S18 . C22 . H20 . 108.848 no C21 . C22 . H20 . 107.793 no H19 . C22 . H20 . 108.718 no S17 . C23 . S19 . 115.6(2) yes S17 . C23 . C24 . 129.0(3) yes S19 . C23 . C24 . 115.3(3) yes S18 . C24 . S20 . 114.7(2) yes S18 . C24 . C23 . 127.5(3) yes S20 . C24 . C23 . 117.8(3) yes S19 . C25 . S20 . 114.0(2) yes S19 . C25 . C26 . 124.6(3) yes S20 . C25 . C26 . 121.4(3) yes S21 . C26 . S22 . 113.5(2) yes S21 . C26 . C25 . 122.9(3) yes S22 . C26 . C25 . 123.6(3) yes S21 . C27 . S23 . 114.4(2) yes S21 . C27 . C28 . 117.2(3) yes S23 . C27 . C28 . 128.4(3) yes S22 . C28 . S24 . 116.1(2) yes S22 . C28 . C27 . 117.0(3) yes S24 . C28 . C27 . 126.8(3) yes S23 . C29 . C30 . 120.3(4) yes S23 . C29 . H21 . 108.899 no C30 . C29 . H21 . 105.522 no S23 . C29 . H22 . 109.169 no C30 . C29 . H22 . 104.345 no H21 . C29 . H22 . 107.959 no S24 . C30 . C29 . 116.5(5) yes S24 . C30 . H23 . 108.200 no C29 . C30 . H23 . 108.733 no S24 . C30 . H24 . 108.736 no C29 . C30 . H24 . 107.737 no H23 . C30 . H24 . 106.550 no S25 . C31 . C32 . 113.0(4) yes S25 . C31 . H25 . 110.014 no C32 . C31 . H25 . 106.794 no S25 . C31 . H26 . 109.527 no C32 . C31 . H26 . 109.110 no H25 . C31 . H26 . 108.227 no S26 . C32 . C31 . 115.4(4) yes S26 . C32 . H27 . 108.146 no C31 . C32 . H27 . 106.964 no S26 . C32 . H28 . 109.962 no C31 . C32 . H28 . 110.150 no H27 . C32 . H28 . 105.675 no S25 . C33 . S27 . 115.5(2) yes S25 . C33 . C34 . 127.7(3) yes S27 . C33 . C34 . 116.9(3) yes S26 . C34 . S28 . 114.3(2) yes S26 . C34 . C33 . 128.8(3) yes S28 . C34 . C33 . 116.9(3) yes S27 . C35 . S28 . 114.7(2) yes S27 . C35 . C36 . 123.2(3) yes S28 . C35 . C36 . 122.1(3) yes S29 . C36 . S30 . 114.6(2) yes S29 . C36 . C35 . 122.6(3) yes S30 . C36 . C35 . 122.8(3) yes S29 . C37 . S31 . 114.5(2) yes S29 . C37 . C38 . 117.4(3) yes S31 . C37 . C38 . 128.1(3) yes S30 . C38 . S32 . 115.2(2) yes S30 . C38 . C37 . 116.2(3) yes S32 . C38 . C37 . 128.6(3) yes S31 . C39 . C40 . 116.2(3) yes S31 . C39 . H29 . 108.810 no C40 . C39 . H29 . 109.169 no S31 . C39 . H30 . 107.992 no C40 . C39 . H30 . 107.276 no H29 . C39 . H30 . 106.957 no S32 . C40 . C39 . 112.3(3) yes S32 . C40 . H31 . 108.935 no C39 . C40 . H31 . 109.830 no S32 . C40 . H32 . 109.333 no C39 . C40 . H32 . 108.746 no H31 . C40 . H32 . 107.563 no O1 . C41 . O3 . 125.5(4) yes O1 . C41 . C42 . 119.1(4) yes O3 . C41 . C42 . 115.3(3) yes O2 . C42 . O4 . 125.9(4) yes O2 . C42 . C41 . 121.0(4) yes O4 . C42 . C41 . 113.1(4) yes O5 . C43 . O7 . 124.9(4) yes O5 . C43 . C44 . 120.6(4) yes O7 . C43 . C44 . 114.5(4) yes O6 . C44 . O8 . 125.0(4) yes O6 . C44 . C43 . 120.5(4) yes O8 . C44 . C43 . 114.5(4) yes O9 . C45 . O11 . 126.6(4) yes O9 . C45 . C46 . 120.4(4) yes O11 . C45 . C46 . 113.0(4) yes O10 . C46 . O12 . 123.8(4) yes O10 . C46 . C45 . 120.4(4) yes O12 . C46 . C45 . 115.8(3) yes N1 . C47 . C48 . 120.4(4) yes N1 . C47 . C52 . 120.0(4) yes C48 . C47 . C52 . 119.6(4) yes C47 . C48 . C49 . 120.0(5) yes C47 . C48 . H33 . 120.935 no C49 . C48 . H33 . 119.026 no C48 . C49 . C50 . 120.5(5) yes C48 . C49 . H34 . 120.179 no C50 . C49 . H34 . 119.305 no C49 . C50 . C51 . 118.9(5) yes C49 . C50 . H35 . 120.384 no C51 . C50 . H35 . 120.692 no C50 . C51 . C52 . 121.0(5) yes C50 . C51 . H36 . 118.582 no C52 . C51 . H36 . 120.386 no C47 . C52 . C51 . 120.0(5) yes C47 . C52 . H37 . 120.906 no C51 . C52 . H37 . 119.070 no N1 . C53 . H38 . 112.476 no N1 . C53 . H39 . 113.389 no H38 . C53 . H39 . 104.622 no N1 . C53 . H40 . 114.400 no H38 . C53 . H40 . 104.914 no H39 . C53 . H40 . 106.172 no O13 . C54 . N1 . 123.4(5) yes O13 . C54 . H41 . 121.351 no N1 . C54 . H41 . 115.176 no # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_Compound_II _database_code_depnum_ccdc_archive 'CCDC 213253' _chemical_name_common ; Tetrakis(Bis(ethylenedithio)tetrathiafulvalenium) ammonium tris(oxalato) galium phenylacetonitrile solvate ; _chemical_name_systematic ; Tetrakis(Bis(ethylenedithio)tetrathiafulvalenium) ammonium tris(oxalato) galium phenylacetonitrile solvate ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'CRYSTALS (Watkin et al 2001)' _computing_publication_material 'teXsan (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.8240(11) _cell_length_b 11.196(2) _cell_length_c 37.882(10) _cell_angle_alpha 81.469(5) _cell_angle_beta 87.657(3) _cell_angle_gamma 64.362(2) _cell_volume 3713.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description '_plate_' _exptl_crystal_colour '_black_' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_meas ? _chemical_formula_weight 2007.58 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H43 Ga N2 O12 S32 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2040.00 _exptl_absorpt_coefficient_mu 1.330 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.479 #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Quantum CCD' _diffrn_measurement_device 'Rigaku ' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 13242 _reflns_number_total 13242 _reflns_number_gt 8548 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 0.544 _diffrn_reflns_theta_max 27.571 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga 0 2 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 64 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 24 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 108 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 86 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Ga1 Ga -0.04340(8) 0.60040(7) 0.248978(16) 0.0403 1.0000 Uani . S1 S 0.4845(2) -0.32288(17) 0.60436(4) 0.0530 1.0000 Uani . S2 S 0.1456(2) -0.07434(19) 0.62865(4) 0.0611 1.0000 Uani . S3 S 0.4079(2) -0.16849(18) 0.53318(4) 0.0550 1.0000 Uani . S4 S 0.1133(2) 0.03594(18) 0.55173(4) 0.0555 1.0000 Uani . S5 S 0.3593(2) -0.01890(18) 0.45227(4) 0.0551 1.0000 Uani . S6 S 0.0661(2) 0.18723(18) 0.47038(4) 0.0555 1.0000 Uani . S7 S 0.3279(2) 0.08398(17) 0.37509(4) 0.0591 1.0000 Uani . S8 S -0.0192(2) 0.32931(18) 0.39803(4) 0.0583 1.0000 Uani . S9 S 0.7094(3) -0.16812(18) 0.39976(4) 0.0640 1.0000 Uani . S10 S 0.6293(2) -0.41801(19) 0.37391(4) 0.0591 1.0000 Uani . S11 S 0.7524(2) -0.32032(18) 0.47085(4) 0.0562 1.0000 Uani . S12 S 0.6742(2) -0.52777(18) 0.45085(4) 0.0545 1.0000 Uani . S13 S 0.8139(2) -0.47042(18) 0.55244(4) 0.0543 1.0000 Uani . S14 S 0.7351(2) -0.67675(18) 0.53173(4) 0.0563 1.0000 Uani . S15 S 0.8567(3) -0.58077(19) 0.62915(4) 0.0661 1.0000 Uani . S16 S 0.7719(2) -0.82834(18) 0.60287(4) 0.0608 1.0000 Uani . S17 S 0.2668(2) -0.11281(19) 0.13333(4) 0.0623 1.0000 Uani . S18 S -0.1267(2) 0.0664(2) 0.12351(5) 0.0687 1.0000 Uani . S19 S 0.26542(19) -0.01936(18) 0.05682(4) 0.0527 1.0000 Uani . S20 S -0.0638(2) 0.12960(19) 0.04831(4) 0.0560 1.0000 Uani . S21 S 0.30367(19) 0.08098(18) -0.02496(4) 0.0509 1.0000 Uani . S22 S -0.02510(19) 0.23159(19) -0.03402(4) 0.0540 1.0000 Uani . S23 S 0.3724(2) 0.16335(19) -0.09806(4) 0.0545 1.0000 Uani . S24 S -0.0211(2) 0.3462(2) -0.10851(4) 0.0626 1.0000 Uani . S25 S 0.50598(19) 0.12602(18) 0.14971(4) 0.0519 1.0000 Uani . S26 S 0.1096(2) 0.29700(19) 0.13917(4) 0.0568 1.0000 Uani . S27 S 0.50455(19) 0.20480(18) 0.07255(4) 0.0500 1.0000 Uani . S28 S 0.17558(19) 0.34895(18) 0.06306(4) 0.0518 1.0000 Uani . S29 S 0.54888(19) 0.31035(18) -0.00834(4) 0.0538 1.0000 Uani . S30 S 0.2198(2) 0.45147(19) -0.01980(4) 0.0544 1.0000 Uani . S31 S 0.6198(2) 0.4139(2) -0.07952(5) 0.0634 1.0000 Uani . S32 S 0.2313(2) 0.58022(19) -0.09222(4) 0.0636 1.0000 Uani . O1 O -0.1428(6) 0.3309(5) 0.21318(13) 0.0587 1.0000 Uani . O2 O -0.2770(7) 0.3926(6) 0.27852(13) 0.0734 1.0000 Uani . O3 O -0.0477(5) 0.4773(4) 0.2173(1) 0.0426 1.0000 Uani . O4 O -0.1873(5) 0.5455(4) 0.2757(1) 0.0486 1.0000 Uani . O5 O -0.1890(5) 0.7587(4) 0.21912(11) 0.0488 1.0000 Uani . O6 O -0.0649(5) 0.7300(4) 0.28093(11) 0.0476 1.0000 Uani . O7 O -0.3015(5) 0.9812(4) 0.21546(12) 0.0576 1.0000 Uani . O8 O -0.1901(6) 0.9511(5) 0.28366(12) 0.0614 1.0000 Uani . O9 O 0.3566(5) 0.4703(5) 0.20738(12) 0.0599 1.0000 Uani . O10 O 0.3725(6) 0.3315(5) 0.27545(13) 0.0645 1.0000 Uani . O11 O 0.1225(5) 0.6128(4) 0.2196(1) 0.0464 1.0000 Uani . O12 O 0.1261(5) 0.4588(4) 0.2787(1) 0.0490 1.0000 Uani . N1 N 0.5318(9) -0.3310(8) 0.19476(18) 0.0815 1.0000 Uani . N2 N 0.6375(6) 0.2372(6) 0.23481(16) 0.0569 1.0000 Uani . C1 C 0.410(1) -0.3034(8) 0.64847(17) 0.0680 1.0000 Uani . C2 C 0.3208(11) -0.1659(8) 0.65440(18) 0.0759 1.0000 Uani . C3 C 0.3518(8) -0.1851(6) 0.57748(15) 0.0447 1.0000 Uani . C4 C 0.2193(8) -0.0915(6) 0.58598(14) 0.0436 1.0000 Uani . C5 C 0.2451(8) -0.0234(7) 0.51909(15) 0.0483 1.0000 Uani . C6 C 0.2262(8) 0.0405(7) 0.48476(15) 0.0493 1.0000 Uani . C7 C 0.2512(9) 0.1000(7) 0.41735(15) 0.0515 1.0000 Uani . C8 C 0.1164(8) 0.1955(6) 0.42552(15) 0.0473 1.0000 Uani . C9 C 0.0577(9) 0.2999(7) 0.35400(16) 0.0564 1.0000 Uani . C10 C 0.2240(8) 0.2514(7) 0.35327(15) 0.0513 1.0000 Uani . C11 C 0.678(1) -0.1917(8) 0.35521(17) 0.0683 1.0000 Uani . C12 C 0.726(1) -0.3275(8) 0.34957(18) 0.0692 1.0000 Uani . C13 C 0.7004(8) -0.3056(6) 0.42614(15) 0.0470 1.0000 Uani . C14 C 0.6685(7) -0.4009(7) 0.41737(15) 0.0483 1.0000 Uani . C15 C 0.7309(7) -0.4669(6) 0.48447(15) 0.0458 1.0000 Uani . C16 C 0.7548(7) -0.5286(6) 0.51891(15) 0.0436 1.0000 Uani . C17 C 0.8126(7) -0.5945(6) 0.58611(15) 0.0464 1.0000 Uani . C18 C 0.7781(7) -0.6882(6) 0.57690(15) 0.0453 1.0000 Uani . C20 C 0.796(1) -0.8023(7) 0.64725(17) 0.0642 1.0000 Uani . C21 C 0.1238(12) -0.1250(11) 0.1619(2) 0.0914 1.0000 Uani . C22 C -0.0148(12) 0.0010(13) 0.1631(2) 0.0967 1.0000 Uani . C23 C 0.0092(7) 0.0504(7) 0.09116(16) 0.0488 1.0000 Uani . C24 C 0.1576(8) -0.0183(6) 0.09491(14) 0.0495 1.0000 Uani . C25 C 0.1117(7) 0.0841(6) 0.02906(15) 0.0446 1.0000 Uani . C26 C 0.1270(7) 0.1294(6) -0.00604(16) 0.0476 1.0000 Uani . C27 C 0.2347(7) 0.1740(6) -0.06669(15) 0.0434 1.0000 Uani . C28 C 0.0823(8) 0.2436(6) -0.07067(15) 0.0464 1.0000 Uani . C29 C 0.2588(8) 0.2147(7) -0.13866(16) 0.0533 1.0000 Uani . C30 C 0.1226(8) 0.3471(7) -0.13892(17) 0.0568 1.0000 Uani . C31 C 0.364(1) 0.123(1) 0.18018(19) 0.0830 1.0000 Uani . C32 C 0.2242(9) 0.241(1) 0.17847(19) 0.0778 1.0000 Uani . C33 C 0.3989(7) 0.2089(6) 0.11055(15) 0.0446 1.0000 Uani . C34 C 0.2482(7) 0.2751(6) 0.10633(15) 0.0442 1.0000 Uani . C35 C 0.3513(7) 0.3065(6) 0.04378(15) 0.0442 1.0000 Uani . C36 C 0.3713(7) 0.3510(6) 0.00965(15) 0.0472 1.0000 Uani . C37 C 0.3319(8) 0.4759(7) -0.05438(15) 0.0493 1.0000 Uani . C38 C 0.4821(8) 0.4124(6) -0.04941(14) 0.0444 1.0000 Uani . C39 C 0.5146(13) 0.4688(13) -0.1200(2) 0.1135 0.9470 Uani . C40 C 0.3711(12) 0.5459(16) -0.1246(2) 0.1339 0.9860 Uani . C41 C -0.1262(7) 0.4150(6) 0.22852(15) 0.0429 1.0000 Uani . C42 C -0.2035(7) 0.4512(6) 0.26387(16) 0.0463 1.0000 Uani . C43 C -0.2228(7) 0.8682(6) 0.23112(16) 0.0421 1.0000 Uani . C44 C -0.1559(7) 0.8528(7) 0.26848(15) 0.0451 1.0000 Uani . C45 C 0.2472(8) 0.5064(6) 0.22623(15) 0.0425 1.0000 Uani . C46 C 0.2536(7) 0.4240(6) 0.26324(15) 0.0416 1.0000 Uani . C47 C 0.3394(8) -0.1634(7) 0.26348(16) 0.0509 1.0000 Uani . C48 C 0.1857(9) -0.0965(8) 0.26078(18) 0.0582 1.0000 Uani . C49 C 0.1155(9) 0.0369(9) 0.2658(2) 0.0742 1.0000 Uani . C50 C 0.2002(12) 0.1007(7) 0.2740(2) 0.0693 1.0000 Uani . C51 C 0.3536(11) 0.0329(8) 0.2767(2) 0.0668 1.0000 Uani . C52 C 0.4247(8) -0.0997(8) 0.27171(19) 0.0612 1.0000 Uani . C53 C 0.420(1) -0.3090(8) 0.2573(2) 0.0683 1.0000 Uani . C54 C 0.4818(9) -0.3233(7) 0.2225(2) 0.0590 1.0000 Uani . C191 C 0.771(2) -0.6618(19) 0.6560(5) 0.0489 0.336(18) Uani . C192 C 0.8950(15) -0.7487(12) 0.6510(2) 0.0584 0.664(18) Uani . H1 H 0.3543 -0.3516 0.6535 0.0507 1.0000 Uiso . H2 H 0.4951 -0.3362 0.6649 0.0507 1.0000 Uiso . H3 H 0.3756 -0.1179 0.6502 0.0507 1.0000 Uiso . H4 H 0.2900 -0.1708 0.6788 0.0507 1.0000 Uiso . H5 H 0.0308 0.2362 0.3468 0.0507 1.0000 Uiso . H6 H 0.0117 0.3826 0.3388 0.0507 1.0000 Uiso . H7 H 0.2526 0.3083 0.3643 0.0507 1.0000 Uiso . H8 H 0.2527 0.2540 0.3289 0.0507 1.0000 Uiso . H9 H 0.7246 -0.1510 0.3394 0.0507 1.0000 Uiso . H10 H 0.5676 -0.1427 0.3508 0.0507 1.0000 Uiso . H11 H 0.7059 -0.3243 0.3251 0.0507 1.0000 Uiso . H12 H 0.8256 -0.3729 0.3559 0.0507 1.0000 Uiso . H15 H 0.8500 -0.8893 0.6609 0.0507 1.0000 Uiso . H16 H 0.7002 -0.7593 0.6566 0.0507 1.0000 Uiso . H17 H 0.0941 -0.1872 0.1537 0.0507 1.0000 Uiso . H18 H 0.1658 -0.1577 0.1851 0.0507 1.0000 Uiso . H19 H 0.0167 0.0662 0.1682 0.0507 1.0000 Uiso . H20 H -0.0736 -0.0153 0.1817 0.0507 1.0000 Uiso . H21 H 0.3212 0.2219 -0.1582 0.0507 1.0000 Uiso . H22 H 0.2266 0.1486 -0.1412 0.0507 1.0000 Uiso . H23 H 0.0825 0.3741 -0.1624 0.0507 1.0000 Uiso . H24 H 0.1594 0.4085 -0.1330 0.0507 1.0000 Uiso . H25 H 0.3449 0.0527 0.1773 0.0507 1.0000 Uiso . H26 H 0.4059 0.1138 0.2034 0.0507 1.0000 Uiso . H27 H 0.2450 0.3118 0.1823 0.0507 1.0000 Uiso . H28 H 0.1664 0.2211 0.1966 0.0507 1.0000 Uiso . H29 H 0.5596 0.5150 -0.1347 0.0507 1.0000 Uiso . H30 H 0.5272 0.3898 -0.1284 0.0507 1.0000 Uiso . H31 H 0.3369 0.5088 -0.1415 0.0507 1.0000 Uiso . H32 H 0.3629 0.6307 -0.1348 0.0507 1.0000 Uiso . H33 H 0.1249 -0.1395 0.2550 0.0507 1.0000 Uiso . H34 H 0.0079 0.0894 0.2632 0.0507 1.0000 Uiso . H35 H 0.1538 0.1901 0.2779 0.0507 1.0000 Uiso . H36 H 0.4126 0.0771 0.2824 0.0507 1.0000 Uiso . H37 H 0.5325 -0.1472 0.2732 0.0507 1.0000 Uiso . H38 H 0.4959 -0.3593 0.2751 0.0507 1.0000 Uiso . H39 H 0.3455 -0.3462 0.2596 0.0507 1.0000 Uiso . H40 H 0.7285 0.2001 0.2487 0.0507 1.0000 Uiso . H41 H 0.6326 0.1713 0.2225 0.0507 1.0000 Uiso . H42 H 0.6339 0.3107 0.2181 0.0507 1.0000 Uiso . H43 H 0.5536 0.2677 0.2501 0.0507 1.0000 Uiso . H131 H 0.7975 -0.6637 0.6792 0.0507 0.336(18) Uiso . H132 H 0.9936 -0.8100 0.6417 0.0507 0.664(18) Uiso . H141 H 0.6616 -0.5997 0.6522 0.0507 0.336(18) Uiso . H142 H 0.9149 -0.7540 0.6759 0.0507 0.664(18) Uiso . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0460(4) 0.0373(4) 0.0328(3) -0.0002(3) 0.0012(3) -0.0151(3) S1 0.0630(12) 0.051(1) 0.0349(8) 0.0031(7) 0.0004(7) -0.0177(9) S2 0.0733(13) 0.0583(11) 0.0357(8) 0.0021(7) 0.0076(8) -0.017(1) S3 0.0671(12) 0.0611(11) 0.0312(7) 0.0039(7) 0.0016(7) -0.0257(9) S4 0.0672(12) 0.056(1) 0.0332(8) 0.0040(7) -0.0038(7) -0.0198(9) S5 0.0659(12) 0.055(1) 0.0341(8) 0.0052(7) -0.0014(7) -0.0196(9) S6 0.0694(12) 0.058(1) 0.0302(7) 0.0011(7) 0.0034(7) -0.0220(9) S7 0.0790(14) 0.047(1) 0.0354(8) 0.0035(7) 0.0112(8) -0.0159(9) S8 0.0658(12) 0.054(1) 0.0360(8) 0.0039(7) 0.0031(7) -0.0119(9) S9 0.1107(17) 0.047(1) 0.0363(8) 0.0042(7) -0.0075(9) -0.0383(11) S10 0.0828(14) 0.0650(11) 0.0362(8) 0.0036(8) -0.0122(8) -0.0403(11) S11 0.0843(14) 0.056(1) 0.0286(7) 0.0011(7) -0.0047(8) -0.032(1) S12 0.0742(13) 0.059(1) 0.0344(8) 0.0025(7) -0.0014(7) -0.035(1) S13 0.0759(13) 0.053(1) 0.0336(7) 0.0021(7) 0.0001(7) -0.0298(9) S14 0.0799(13) 0.0608(11) 0.0319(8) 0.0028(7) -0.0052(8) -0.036(1) S15 0.1099(17) 0.0528(11) 0.0343(8) 0.0011(7) -0.0124(9) -0.0351(11) S16 0.0950(15) 0.050(1) 0.0373(8) 0.0043(7) -0.0006(8) -0.035(1) S17 0.0668(13) 0.0658(12) 0.0339(8) 0.0080(8) -0.0022(8) -0.014(1) S18 0.0602(13) 0.0734(13) 0.056(1) 0.0083(9) 0.0186(9) -0.020(1) S19 0.047(1) 0.0650(11) 0.0323(7) 0.0031(7) 0.0002(7) -0.0139(9) S20 0.0469(11) 0.0710(12) 0.0405(8) 0.0002(8) 0.0027(7) -0.0191(9) S21 0.045(1) 0.061(1) 0.0327(7) 0.0027(7) 0.0003(6) -0.0129(8) S22 0.044(1) 0.0684(11) 0.0333(7) 0.0053(7) 0.0008(7) -0.0132(9) S23 0.045(1) 0.0684(11) 0.0393(8) 0.0034(8) 0.0063(7) -0.0181(9) S24 0.0524(11) 0.0677(12) 0.0384(8) 0.0129(8) 0.0010(7) -0.0051(9) S25 0.041(1) 0.061(1) 0.0340(7) 0.0045(7) 0.0008(6) -0.0074(8) S26 0.040(1) 0.0651(11) 0.0445(9) 0.0063(8) 0.0040(7) -0.0083(9) S27 0.042(1) 0.059(1) 0.0335(7) 0.0010(7) 0.0012(6) -0.0098(8) S28 0.045(1) 0.061(1) 0.0364(8) 0.0027(7) -0.0032(7) -0.0134(8) S29 0.043(1) 0.0642(11) 0.0360(8) 0.0036(7) -0.0011(7) -0.0091(9) S30 0.0464(11) 0.0653(11) 0.0389(8) 0.0035(7) -0.0042(7) -0.0153(9) S31 0.0515(12) 0.0811(13) 0.0470(9) 0.0015(9) 0.0054(8) -0.023(1) S32 0.0615(12) 0.0639(11) 0.0397(9) 0.0088(8) -0.0072(8) -0.008(1) O1 0.067(3) 0.051(3) 0.068(3) -0.016(2) 0.012(2) -0.033(3) O2 0.095(4) 0.093(4) 0.059(3) -0.009(3) 0.018(3) -0.068(4) O3 0.048(3) 0.038(2) 0.039(2) -0.0041(17) 0.0102(18) -0.017(2) O4 0.054(3) 0.057(3) 0.038(2) -0.011(2) 0.0113(19) -0.026(2) O5 0.054(3) 0.044(3) 0.040(2) -0.0044(19) -0.0069(19) -0.013(2) O6 0.057(3) 0.042(2) 0.041(2) -0.0024(19) -0.0100(19) -0.020(2) O7 0.056(3) 0.041(3) 0.057(3) 0.004(2) -0.009(2) -0.005(2) O8 0.075(4) 0.049(3) 0.057(3) -0.023(2) 0.001(2) -0.019(3) O9 0.057(3) 0.064(3) 0.058(3) -0.005(2) 0.015(2) -0.028(3) O10 0.049(3) 0.061(3) 0.060(3) 0.014(2) 0.001(2) -0.008(3) O11 0.048(3) 0.041(2) 0.045(2) 0.0081(19) -0.0004(19) -0.018(2) O12 0.053(3) 0.049(3) 0.036(2) 0.0050(19) 0.0006(19) -0.017(2) N1 0.098(6) 0.105(6) 0.059(4) -0.030(4) 0.023(4) -0.057(5) N2 0.050(4) 0.047(3) 0.070(4) -0.013(3) 0.007(3) -0.017(3) C1 0.083(6) 0.068(5) 0.033(3) 0.005(3) -0.003(3) -0.018(4) C2 0.120(7) 0.069(5) 0.034(3) 0.004(3) -0.003(4) -0.039(5) C3 0.063(5) 0.042(3) 0.031(3) 0.004(3) -0.004(3) -0.027(3) C4 0.058(4) 0.044(3) 0.028(3) 0.005(2) -0.002(3) -0.024(3) C5 0.059(4) 0.051(4) 0.036(3) 0.004(3) -0.006(3) -0.027(3) C6 0.064(5) 0.055(4) 0.032(3) -0.000(3) -0.002(3) -0.030(4) C7 0.077(5) 0.050(4) 0.027(3) -0.001(3) 0.000(3) -0.028(4) C8 0.066(5) 0.042(4) 0.032(3) -0.001(3) 0.002(3) -0.023(3) C9 0.077(5) 0.055(4) 0.031(3) 0.008(3) -0.005(3) -0.027(4) C10 0.063(5) 0.049(4) 0.034(3) 0.005(3) 0.000(3) -0.021(3) C11 0.112(7) 0.061(5) 0.038(3) -0.000(3) 0.002(4) -0.045(5) C12 0.092(6) 0.071(5) 0.037(3) -0.003(3) 0.003(4) -0.030(5) C13 0.058(4) 0.042(4) 0.034(3) -0.002(3) -0.003(3) -0.016(3) C14 0.051(4) 0.056(4) 0.033(3) -0.002(3) -0.002(3) -0.020(3) C15 0.052(4) 0.047(4) 0.033(3) 0.000(3) 0.001(3) -0.018(3) C16 0.043(4) 0.043(3) 0.040(3) -0.002(3) 0.005(3) -0.016(3) C17 0.051(4) 0.042(4) 0.033(3) 0.004(3) -0.005(3) -0.011(3) C18 0.053(4) 0.040(3) 0.037(3) -0.005(3) -0.001(3) -0.014(3) C20 0.093(6) 0.058(4) 0.040(4) -0.001(3) 0.006(4) -0.033(4) C21 0.098(8) 0.123(8) 0.061(5) 0.037(5) -0.019(5) -0.068(7) C22 0.093(7) 0.172(11) 0.040(4) -0.012(5) 0.022(4) -0.074(8) C23 0.039(4) 0.049(4) 0.043(3) 0.001(3) 0.002(3) -0.007(3) C24 0.068(5) 0.043(4) 0.026(3) 0.001(3) 0.005(3) -0.015(4) C25 0.042(4) 0.053(4) 0.035(3) -0.004(3) 0.002(3) -0.018(3) C26 0.044(4) 0.052(4) 0.037(3) -0.004(3) 0.001(3) -0.012(3) C27 0.041(4) 0.045(3) 0.032(3) 0.001(3) 0.001(2) -0.009(3) C28 0.056(5) 0.042(3) 0.033(3) 0.003(3) 0.003(3) -0.017(3) C29 0.058(5) 0.057(4) 0.039(3) 0.003(3) 0.004(3) -0.023(4) C30 0.065(5) 0.051(4) 0.042(3) 0.005(3) 0.002(3) -0.019(4) C31 0.060(6) 0.130(8) 0.041(4) 0.019(4) -0.004(3) -0.033(6) C32 0.055(5) 0.115(7) 0.050(4) -0.015(4) 0.010(3) -0.023(5) C33 0.041(4) 0.049(4) 0.033(3) -0.004(3) 0.002(2) -0.010(3) C34 0.043(4) 0.041(3) 0.039(3) -0.002(3) 0.001(3) -0.009(3) C35 0.044(4) 0.044(3) 0.038(3) -0.003(3) -0.005(3) -0.013(3) C36 0.047(4) 0.052(4) 0.033(3) -0.007(3) -0.004(3) -0.013(3) C37 0.052(5) 0.055(4) 0.034(3) -0.008(3) -0.003(3) -0.017(3) C38 0.053(5) 0.047(4) 0.030(3) -0.005(3) 0.001(3) -0.018(3) C39 0.089(8) 0.15(1) 0.036(4) 0.015(5) 0.024(5) -0.004(7) C40 0.065(7) 0.248(16) 0.042(5) -0.003(7) 0.002(4) -0.030(9) C41 0.043(4) 0.037(3) 0.041(3) 0.000(3) -0.005(3) -0.012(3) C42 0.049(4) 0.046(4) 0.042(3) 0.002(3) 0.002(3) -0.022(3) C43 0.039(4) 0.040(4) 0.044(3) -0.010(3) 0.009(3) -0.014(3) C44 0.049(4) 0.057(4) 0.036(3) -0.011(3) 0.010(3) -0.028(3) C45 0.050(4) 0.048(4) 0.037(3) -0.007(3) 0.001(3) -0.029(4) C46 0.047(4) 0.041(3) 0.036(3) -0.006(3) 0.003(3) -0.017(3) C47 0.057(5) 0.057(4) 0.036(3) -0.001(3) 0.007(3) -0.025(4) C48 0.062(5) 0.065(5) 0.050(4) -0.003(3) -0.000(3) -0.031(4) C49 0.056(5) 0.074(6) 0.062(5) 0.003(4) -0.005(4) -0.004(5) C50 0.100(7) 0.044(4) 0.054(4) -0.005(3) 0.008(4) -0.023(5) C51 0.103(7) 0.062(5) 0.059(4) -0.018(4) 0.009(4) -0.056(5) C52 0.059(5) 0.071(5) 0.057(4) -0.004(4) 0.003(3) -0.034(4) C53 0.081(6) 0.059(5) 0.060(4) -0.012(4) 0.010(4) -0.025(4) C54 0.058(5) 0.049(4) 0.065(5) -0.009(3) -0.004(4) -0.017(4) C191 0.041(14) 0.033(11) 0.04(1) 0.003(8) -0.012(8) 0.01(1) C192 0.08(1) 0.068(8) 0.028(5) 0.008(5) -0.015(5) -0.032(8) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 15.8 -2.54 10.8 3.42 ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8548 _refine_ls_number_parameters 920 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1377 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_all 0.1042 _refine_ls_wR_factor_ref 0.0673 _refine_ls_goodness_of_fit_ref 1.1923 _refine_ls_shift/su_max 0.000673 _refine_diff_density_min -0.73 _refine_diff_density_max 0.71 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ga1 . O3 . 1.972(4) yes Ga1 . O4 . 1.963(4) yes Ga1 . O5 . 1.952(4) yes Ga1 . O6 . 1.963(4) yes Ga1 . O11 . 1.979(4) yes Ga1 . O12 . 1.973(4) yes S1 . C1 . 1.802(7) yes S1 . C3 . 1.738(6) yes S2 . C2 . 1.810(9) yes S2 . C4 . 1.746(6) yes S3 . C3 . 1.754(6) yes S3 . C5 . 1.746(7) yes S4 . C4 . 1.755(6) yes S4 . C5 . 1.736(7) yes S5 . C6 . 1.739(7) yes S5 . C7 . 1.738(6) yes S6 . C6 . 1.743(7) yes S6 . C8 . 1.751(6) yes S7 . C7 . 1.741(6) yes S7 . C10 . 1.787(6) yes S8 . C8 . 1.740(7) yes S8 . C9 . 1.818(7) yes S9 . C11 . 1.805(7) yes S9 . C13 . 1.741(7) yes S10 . C12 . 1.806(8) yes S10 . C14 . 1.762(6) yes S11 . C13 . 1.752(6) yes S11 . C15 . 1.745(7) yes S12 . C14 . 1.741(6) yes S12 . C15 . 1.744(6) yes S13 . C16 . 1.734(6) yes S13 . C17 . 1.745(6) yes S14 . C16 . 1.748(6) yes S14 . C18 . 1.752(6) yes S15 . C17 . 1.749(6) yes S15 . C191 . 1.70(2) yes S15 . C192 . 1.819(11) yes S16 . C18 . 1.747(6) yes S16 . C20 . 1.790(7) yes S17 . C21 . 1.78(1) yes S17 . C24 . 1.754(6) yes S18 . C22 . 1.76(1) yes S18 . C23 . 1.744(6) yes S19 . C24 . 1.753(6) yes S19 . C25 . 1.727(6) yes S20 . C23 . 1.747(6) yes S20 . C25 . 1.735(6) yes S21 . C26 . 1.738(7) yes S21 . C27 . 1.741(6) yes S22 . C26 . 1.719(6) yes S22 . C28 . 1.734(6) yes S23 . C27 . 1.740(6) yes S23 . C29 . 1.807(7) yes S24 . C28 . 1.740(6) yes S24 . C30 . 1.787(7) yes S25 . C31 . 1.783(8) yes S25 . C33 . 1.744(6) yes S26 . C32 . 1.768(8) yes S26 . C34 . 1.768(6) yes S27 . C33 . 1.735(6) yes S27 . C35 . 1.742(6) yes S28 . C34 . 1.750(6) yes S28 . C35 . 1.740(7) yes S29 . C36 . 1.738(7) yes S29 . C38 . 1.751(6) yes S30 . C36 . 1.744(6) yes S30 . C37 . 1.744(7) yes S31 . C38 . 1.737(6) yes S31 . C39 . 1.76(1) yes S32 . C37 . 1.737(6) yes S32 . C40 . 1.75(1) yes O1 . C41 . 1.246(7) yes O2 . C42 . 1.236(8) yes O3 . C41 . 1.270(7) yes O4 . C42 . 1.279(7) yes O5 . C43 . 1.273(7) yes O6 . C44 . 1.300(8) yes O7 . C43 . 1.232(7) yes O8 . C44 . 1.227(7) yes O9 . C45 . 1.214(7) yes O10 . C46 . 1.227(7) yes O11 . C45 . 1.287(7) yes O12 . C46 . 1.284(7) yes N1 . C54 . 1.141(9) yes N2 . H40 . 0.948 no N2 . H41 . 0.948 no N2 . H42 . 0.950 no N2 . H43 . 0.953 no C1 . C2 . 1.451(11) yes C1 . H1 . 0.917 no C1 . H2 . 0.965 no C2 . H3 . 0.908 no C2 . H4 . 0.964 no C3 . C4 . 1.335(9) yes C5 . C6 . 1.366(8) yes C7 . C8 . 1.353(9) yes C9 . C10 . 1.48(1) yes C9 . H5 . 0.938 no C9 . H6 . 0.947 no C10 . H7 . 0.949 no C10 . H8 . 0.954 no C11 . C12 . 1.43(1) yes C11 . H9 . 0.923 no C11 . H10 . 0.989 no C12 . H11 . 0.947 no C12 . H12 . 0.909 no C13 . C14 . 1.323(9) yes C15 . C16 . 1.361(8) yes C17 . C18 . 1.328(9) yes C20 . C191 . 1.57(2) yes C20 . C192 . 1.367(14) yes C20 . H15 . 0.960 no C20 . H16 . 0.935 no C21 . C22 . 1.483(14) yes C21 . H17 . 0.955 no C21 . H18 . 0.939 no C22 . H19 . 0.952 no C22 . H20 . 0.939 no C23 . C24 . 1.324(9) yes C25 . C26 . 1.378(8) yes C27 . C28 . 1.359(9) yes C29 . C30 . 1.51(1) yes C29 . H21 . 0.958 no C29 . H22 . 0.940 no C30 . H23 . 0.938 no C30 . H24 . 0.960 no C31 . C32 . 1.428(12) yes C31 . H25 . 0.910 no C31 . H26 . 0.958 no C32 . H27 . 0.930 no C32 . H28 . 0.938 no C33 . C34 . 1.342(9) yes C35 . C36 . 1.354(9) yes C37 . C38 . 1.339(9) yes C39 . C40 . 1.298(14) yes C39 . H29 . 0.932 no C39 . H30 . 0.940 no C40 . H31 . 0.957 no C40 . H32 . 0.941 no C41 . C42 . 1.532(8) yes C43 . C44 . 1.540(8) yes C45 . C46 . 1.547(8) yes C47 . C48 . 1.36(1) yes C47 . C52 . 1.38(1) yes C47 . C53 . 1.52(1) yes C48 . C49 . 1.387(11) yes C48 . H33 . 0.963 no C49 . C50 . 1.379(12) yes C49 . H34 . 0.963 no C50 . C51 . 1.362(12) yes C50 . H35 . 0.935 no C51 . C52 . 1.379(11) yes C51 . H36 . 0.959 no C52 . H37 . 0.957 no C53 . C54 . 1.431(11) yes C53 . H38 . 0.944 no C53 . H39 . 0.981 no C191 . C192 . 1.22(2) yes C191 . H131 . 0.919 no C191 . H141 . 0.997 no C192 . H132 . 1.000 no C192 . H142 . 0.959 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 . Ga1 . O4 . 82.39(17) yes O3 . Ga1 . O5 . 93.20(17) yes O4 . Ga1 . O5 . 98.14(19) yes O3 . Ga1 . O6 . 173.26(18) yes O4 . Ga1 . O6 . 92.51(18) yes O5 . Ga1 . O6 . 83.12(17) yes O3 . Ga1 . O11 . 86.68(17) yes O4 . Ga1 . O11 . 166.80(18) yes O5 . Ga1 . O11 . 89.82(18) yes O6 . Ga1 . O11 . 98.92(18) yes O3 . Ga1 . O12 . 93.43(18) yes O4 . Ga1 . O12 . 90.72(18) yes O5 . Ga1 . O12 . 169.57(19) yes O6 . Ga1 . O12 . 91.03(17) yes O11 . Ga1 . O12 . 82.53(17) yes C1 . S1 . C3 . 103.5(3) yes C2 . S2 . C4 . 98.5(3) yes C3 . S3 . C5 . 94.8(3) yes C4 . S4 . C5 . 94.9(3) yes C6 . S5 . C7 . 95.4(3) yes C6 . S6 . C8 . 95.0(3) yes C7 . S7 . C10 . 99.7(3) yes C8 . S8 . C9 . 102.0(3) yes C11 . S9 . C13 . 102.8(3) yes C12 . S10 . C14 . 98.0(3) yes C13 . S11 . C15 . 94.9(3) yes C14 . S12 . C15 . 94.6(3) yes C16 . S13 . C17 . 94.7(3) yes C16 . S14 . C18 . 94.4(3) yes C17 . S15 . C191 . 103.5(7) yes C17 . S15 . C192 . 99.0(4) yes C191 . S15 . C192 . 40.3(7) yes C18 . S16 . C20 . 102.4(3) yes C21 . S17 . C24 . 100.3(4) yes C22 . S18 . C23 . 101.8(4) yes C24 . S19 . C25 . 94.5(3) yes C23 . S20 . C25 . 94.7(3) yes C26 . S21 . C27 . 94.9(3) yes C26 . S22 . C28 . 95.1(3) yes C27 . S23 . C29 . 99.9(3) yes C28 . S24 . C30 . 102.9(3) yes C31 . S25 . C33 . 101.4(3) yes C32 . S26 . C34 . 100.4(3) yes C33 . S27 . C35 . 95.7(3) yes C34 . S28 . C35 . 95.1(3) yes C36 . S29 . C38 . 95.4(3) yes C36 . S30 . C37 . 94.8(3) yes C38 . S31 . C39 . 100.7(4) yes C37 . S32 . C40 . 102.3(4) yes Ga1 . O3 . C41 . 114.3(4) yes Ga1 . O4 . C42 . 113.7(4) yes Ga1 . O5 . C43 . 114.3(4) yes Ga1 . O6 . C44 . 113.8(4) yes Ga1 . O11 . C45 . 111.9(4) yes Ga1 . O12 . C46 . 113.1(4) yes H40 . N2 . H41 . 109.807 no H40 . N2 . H42 . 109.639 no H41 . N2 . H42 . 109.529 no H40 . N2 . H43 . 109.407 no H41 . N2 . H43 . 109.303 no H42 . N2 . H43 . 109.139 no S1 . C1 . C2 . 115.0(5) yes S1 . C1 . H1 . 109.492 no C2 . C1 . H1 . 110.061 no S1 . C1 . H2 . 106.900 no C2 . C1 . H2 . 104.281 no H1 . C1 . H2 . 110.997 no S2 . C2 . C1 . 116.2(6) yes S2 . C2 . H3 . 107.445 no C1 . C2 . H3 . 110.800 no S2 . C2 . H4 . 104.510 no C1 . C2 . H4 . 105.844 no H3 . C2 . H4 . 111.921 no S1 . C3 . S3 . 113.1(4) yes S1 . C3 . C4 . 129.6(5) yes S3 . C3 . C4 . 117.3(5) yes S2 . C4 . S4 . 115.7(4) yes S2 . C4 . C3 . 126.7(5) yes S4 . C4 . C3 . 117.4(4) yes S3 . C5 . S4 . 115.7(3) yes S3 . C5 . C6 . 121.5(5) yes S4 . C5 . C6 . 122.8(5) yes S5 . C6 . S6 . 115.2(3) yes S5 . C6 . C5 . 122.6(6) yes S6 . C6 . C5 . 122.2(5) yes S5 . C7 . S7 . 116.3(4) yes S5 . C7 . C8 . 117.2(5) yes S7 . C7 . C8 . 126.4(5) yes S6 . C8 . S8 . 113.1(4) yes S6 . C8 . C7 . 116.9(5) yes S8 . C8 . C7 . 129.9(5) yes S8 . C9 . C10 . 113.4(5) yes S8 . C9 . H5 . 106.872 no C10 . C9 . H5 . 109.891 no S8 . C9 . H6 . 106.700 no C10 . C9 . H6 . 109.084 no H5 . C9 . H6 . 110.819 no S7 . C10 . C9 . 114.3(5) yes S7 . C10 . H7 . 107.864 no C9 . C10 . H7 . 109.809 no S7 . C10 . H8 . 107.562 no C9 . C10 . H8 . 107.994 no H7 . C10 . H8 . 109.176 no S9 . C11 . C12 . 115.8(5) yes S9 . C11 . H9 . 108.252 no C12 . C11 . H9 . 110.073 no S9 . C11 . H10 . 105.129 no C12 . C11 . H10 . 108.852 no H9 . C11 . H10 . 108.404 no S10 . C12 . C11 . 116.8(6) yes S10 . C12 . H11 . 105.560 no C11 . C12 . H11 . 106.256 no S10 . C12 . H12 . 107.439 no C11 . C12 . H12 . 107.595 no H11 . C12 . H12 . 113.395 no S9 . C13 . S11 . 112.6(4) yes S9 . C13 . C14 . 130.4(5) yes S11 . C13 . C14 . 116.9(5) yes S10 . C14 . S12 . 115.4(4) yes S10 . C14 . C13 . 126.1(5) yes S12 . C14 . C13 . 118.4(5) yes S11 . C15 . S12 . 115.2(3) yes S11 . C15 . C16 . 122.5(5) yes S12 . C15 . C16 . 122.3(5) yes S13 . C16 . S14 . 115.6(3) yes S13 . C16 . C15 . 122.7(5) yes S14 . C16 . C15 . 121.6(5) yes S13 . C17 . S15 . 115.5(4) yes S13 . C17 . C18 . 117.8(5) yes S15 . C17 . C18 . 126.7(5) yes S14 . C18 . S16 . 112.5(4) yes S14 . C18 . C17 . 117.3(5) yes S16 . C18 . C17 . 130.2(5) yes S16 . C20 . C191 . 121.9(8) yes S16 . C20 . C192 . 115.4(6) yes C191 . C20 . C192 . 48.4(9) yes S16 . C20 . H15 . 106.861 no C191 . C20 . H15 . 129.162 no C192 . C20 . H15 . 99.608 no S16 . C20 . H16 . 107.967 no C191 . C20 . H16 . 69.837 no C192 . C20 . H16 . 116.395 no H15 . C20 . H16 . 109.836 no S17 . C21 . C22 . 116.0(6) yes S17 . C21 . H17 . 107.462 no C22 . C21 . H17 . 107.273 no S17 . C21 . H18 . 107.858 no C22 . C21 . H18 . 108.243 no H17 . C21 . H18 . 109.934 no S18 . C22 . C21 . 115.6(6) yes S18 . C22 . H19 . 107.703 no C21 . C22 . H19 . 106.927 no S18 . C22 . H20 . 108.695 no C21 . C22 . H20 . 107.641 no H19 . C22 . H20 . 110.192 no S18 . C23 . S20 . 114.7(4) yes S18 . C23 . C24 . 128.1(5) yes S20 . C23 . C24 . 117.2(5) yes S17 . C24 . S19 . 113.3(4) yes S17 . C24 . C23 . 129.1(5) yes S19 . C24 . C23 . 117.6(5) yes S19 . C25 . S20 . 115.8(3) yes S19 . C25 . C26 . 122.3(5) yes S20 . C25 . C26 . 121.9(5) yes S21 . C26 . S22 . 116.1(3) yes S21 . C26 . C25 . 121.2(5) yes S22 . C26 . C25 . 122.8(5) yes S21 . C27 . S23 . 114.8(4) yes S21 . C27 . C28 . 116.5(4) yes S23 . C27 . C28 . 128.6(5) yes S22 . C28 . S24 . 114.9(4) yes S22 . C28 . C27 . 117.4(4) yes S24 . C28 . C27 . 127.8(5) yes S23 . C29 . C30 . 112.9(5) yes S23 . C29 . H21 . 107.717 no C30 . C29 . H21 . 108.983 no S23 . C29 . H22 . 108.560 no C30 . C29 . H22 . 109.073 no H21 . C29 . H22 . 109.603 no S24 . C30 . C29 . 115.4(5) yes S24 . C30 . H23 . 109.765 no C29 . C30 . H23 . 106.842 no S24 . C30 . H24 . 108.945 no C29 . C30 . H24 . 106.175 no H23 . C30 . H24 . 109.587 no S25 . C31 . C32 . 117.8(6) yes S25 . C31 . H25 . 107.916 no C32 . C31 . H25 . 109.126 no S25 . C31 . H26 . 105.175 no C32 . C31 . H26 . 104.542 no H25 . C31 . H26 . 112.296 no S26 . C32 . C31 . 119.4(6) yes S26 . C32 . H27 . 106.246 no C31 . C32 . H27 . 108.106 no S26 . C32 . H28 . 105.823 no C31 . C32 . H28 . 105.030 no H27 . C32 . H28 . 112.325 no S25 . C33 . S27 . 114.4(4) yes S25 . C33 . C34 . 128.7(5) yes S27 . C33 . C34 . 116.9(5) yes S26 . C34 . S28 . 114.4(4) yes S26 . C34 . C33 . 128.3(5) yes S28 . C34 . C33 . 117.3(5) yes S27 . C35 . S28 . 114.6(3) yes S27 . C35 . C36 . 121.3(5) yes S28 . C35 . C36 . 124.1(5) yes S29 . C36 . S30 . 115.1(3) yes S29 . C36 . C35 . 122.8(5) yes S30 . C36 . C35 . 122.1(5) yes S30 . C37 . S32 . 114.4(4) yes S30 . C37 . C38 . 118.0(5) yes S32 . C37 . C38 . 127.6(5) yes S29 . C38 . S31 . 115.7(4) yes S29 . C38 . C37 . 116.5(5) yes S31 . C38 . C37 . 127.8(5) yes S31 . C39 . C40 . 127.0(7) yes S31 . C39 . H29 . 105.186 no C40 . C39 . H29 . 103.723 no S31 . C39 . H30 . 104.746 no C40 . C39 . H30 . 104.176 no H29 . C39 . H30 . 111.990 no S32 . C40 . C39 . 127.8(7) yes S32 . C40 . H31 . 103.323 no C39 . C40 . H31 . 104.960 no S32 . C40 . H32 . 104.343 no C39 . C40 . H32 . 106.112 no H31 . C40 . H32 . 109.621 no O1 . C41 . O3 . 125.3(6) yes O1 . C41 . C42 . 120.4(6) yes O3 . C41 . C42 . 114.3(5) yes O2 . C42 . O4 . 124.7(6) yes O2 . C42 . C41 . 120.5(6) yes O4 . C42 . C41 . 114.8(5) yes O5 . C43 . O7 . 125.8(6) yes O5 . C43 . C44 . 114.9(5) yes O7 . C43 . C44 . 119.2(6) yes O6 . C44 . O8 . 126.2(6) yes O6 . C44 . C43 . 113.5(5) yes O8 . C44 . C43 . 120.3(6) yes O9 . C45 . O11 . 126.8(6) yes O9 . C45 . C46 . 119.6(6) yes O11 . C45 . C46 . 113.5(5) yes O10 . C46 . O12 . 124.7(5) yes O10 . C46 . C45 . 120.8(6) yes O12 . C46 . C45 . 114.5(5) yes C48 . C47 . C52 . 120.4(7) yes C48 . C47 . C53 . 120.7(7) yes C52 . C47 . C53 . 118.9(7) yes C47 . C48 . C49 . 119.5(7) yes C47 . C48 . H33 . 121.336 no C49 . C48 . H33 . 119.173 no C48 . C49 . C50 . 120.2(8) yes C48 . C49 . H34 . 122.528 no C50 . C49 . H34 . 117.211 no C49 . C50 . C51 . 119.8(7) yes C49 . C50 . H35 . 120.854 no C51 . C50 . H35 . 119.355 no C50 . C51 . C52 . 120.5(7) yes C50 . C51 . H36 . 119.855 no C52 . C51 . H36 . 119.642 no C47 . C52 . C51 . 119.6(7) yes C47 . C52 . H37 . 119.738 no C51 . C52 . H37 . 120.667 no C47 . C53 . C54 . 112.8(6) yes C47 . C53 . H38 . 110.561 no C54 . C53 . H38 . 110.466 no C47 . C53 . H39 . 107.808 no C54 . C53 . H39 . 107.668 no H38 . C53 . H39 . 107.356 no N1 . C54 . C53 . 177.7(8) yes S15 . C191 . C20 . 116.4(12) yes S15 . C191 . C192 . 75.2(13) yes C20 . C191 . C192 . 57.1(10) yes S15 . C191 . H131 . 106.975 no C20 . C191 . H131 . 113.398 no C192 . C191 . H131 . 91.778 no S15 . C191 . H141 . 102.884 no C20 . C191 . H141 . 108.331 no C192 . C191 . H141 . 159.495 no H131 . C191 . H141 . 108.071 no S15 . C192 . C20 . 120.7(8) yes S15 . C192 . C191 . 64.6(11) yes C20 . C192 . C191 . 74.5(13) yes S15 . C192 . H132 . 106.139 no C20 . C192 . H132 . 106.512 no C191 . C192 . H132 . 168.229 no S15 . C192 . H142 . 108.308 no C20 . C192 . H142 . 109.332 no C191 . C192 . H142 . 85.717 no H132 . C192 . H142 . 104.629 no # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_Compound_III _database_code_depnum_ccdc_archive 'CCDC 213254' _chemical_name_common ; Tetrakis(Bis(ethylenedithio)tetrathiafulvalenium) ammonium tris(oxalato) iron acetophenone solvate ; _chemical_name_systematic ; Tetrakis(Bis(ethylenedithio)tetrathiafulvalenium) ammonium tris(oxalato) iron acetophenone solvate ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'CRYSTALS (Watkin et al 2001)' _computing_publication_material 'teXsan (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 10.132(2) _cell_length_b 11.261(1) _cell_length_c 36.651(4) _cell_angle_alpha 82.957(6) _cell_angle_beta 86.413(3) _cell_angle_gamma 63.4770(12) _cell_volume 3713.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description '_black_' _exptl_crystal_colour '_plate_' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.005 _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_meas ? _chemical_formula_weight 1996.71 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H44 Fe N O13 S32 ' _chemical_formula_moiety 'C54 H44 Fe N O13 S32 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2034.00 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_max 1.998 _exptl_absorpt_correction_T_min 0.3044 #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector quantum _diffrn_measurement_device 'Rigaku ' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 15212 _reflns_number_total 15212 _reflns_number_gt 6401 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.050 _diffrn_reflns_theta_max 27.529 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe 0 2 0.301 0.845 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 64 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 26 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 2 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 108 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 88 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Fe1 Fe 0.47653(15) 0.08920(14) 0.24146(3) 0.0490 1.0000 Uani . S1 S 0.6130(3) 0.8155(2) 0.10493(6) 0.0524 1.0000 Uani . S2 S 0.4249(3) 0.6330(3) 0.13220(6) 0.0597 1.0000 Uani . S3 S 0.4377(3) 0.8971(2) 0.03686(6) 0.0478 1.0000 Uani . S4 S 0.2780(3) 0.7388(3) 0.06029(6) 0.0502 1.0000 Uani . S5 S 0.2656(3) 0.9901(2) -0.04067(6) 0.0486 1.0000 Uani . S6 S 0.1120(3) 0.8270(3) -0.01678(6) 0.0509 1.0000 Uani . S7 S 0.1305(3) 1.0818(3) -0.11419(6) 0.0567 1.0000 Uani . S8 S -0.0547(3) 0.8914(3) -0.08450(7) 0.0712 1.0000 Uani . S9 S 0.4739(3) 0.6409(3) -0.07521(6) 0.0566 1.0000 Uani . S10 S 0.6798(3) 0.8169(3) -0.10298(6) 0.0561 1.0000 Uani . S11 S 0.6366(3) 0.5705(3) -0.00639(6) 0.0505 1.0000 Uani . S12 S 0.8058(3) 0.7219(3) -0.02842(6) 0.0505 1.0000 Uani . S13 S 0.7962(3) 0.4786(2) 0.07264(6) 0.0524 1.0000 Uani . S14 S 0.9635(3) 0.6310(2) 0.05049(6) 0.0484 1.0000 Uani . S15 S 0.9109(4) 0.3937(3) 0.14759(7) 0.0711 1.0000 Uani . S16 S 1.1196(3) 0.5657(3) 0.12059(7) 0.0622 1.0000 Uani . S17 S 0.6485(4) 0.0756(3) 0.36620(7) 0.0859 1.0000 Uani . S18 S 0.7317(4) 0.3212(3) 0.39315(7) 0.0744 1.0000 Uani . S19 S 0.6875(4) -0.0279(3) 0.44455(7) 0.0746 1.0000 Uani . S20 S 0.7663(4) 0.1747(3) 0.46601(7) 0.0723 1.0000 Uani . S21 S 0.7422(4) -0.1710(3) 0.52802(7) 0.0781 1.0000 Uani . S22 S 0.8200(4) 0.0326(3) 0.54888(7) 0.0715 1.0000 Uani . S23 S 0.7781(4) -0.3165(3) 0.60124(7) 0.0854 1.0000 Uani . S24 S 0.8606(4) -0.0722(3) 0.62773(7) 0.0790 1.0000 Uani . S25 S 0.8450(4) 0.5772(3) 0.37298(7) 0.0814 1.0000 Uani . S26 S 0.4965(4) 0.8197(3) 0.39699(7) 0.0800 1.0000 Uani . S27 S 0.8632(3) 0.4767(3) 0.45153(7) 0.0711 1.0000 Uani . S28 S 0.5709(3) 0.6812(3) 0.47088(7) 0.0737 1.0000 Uani . S29 S 0.9026(3) 0.3331(3) 0.53432(7) 0.0732 1.0000 Uani . S30 S 0.6102(4) 0.5364(3) 0.55397(7) 0.0762 1.0000 Uani . S31 S 0.9731(4) 0.1850(3) 0.60732(7) 0.0751 1.0000 Uani . S32 S 0.6339(4) 0.4349(3) 0.63283(7) 0.0852 1.0000 Uani . O1 O 0.6550(7) 0.0266(7) 0.27281(16) 0.0554 1.0000 Uani . O2 O 0.6292(7) -0.0365(7) 0.20901(16) 0.0597 1.0000 Uani . O3 O 0.8871(8) -0.1381(8) 0.27825(19) 0.0748 1.0000 Uani . O4 O 0.8669(8) -0.1803(7) 0.20664(18) 0.0652 1.0000 Uani . O5 O 0.3232(7) 0.0860(7) 0.20972(17) 0.0600 1.0000 Uani . O6 O 0.4296(7) -0.0460(6) 0.27238(16) 0.0532 1.0000 Uani . O7 O 0.2226(8) -0.0476(8) 0.20086(19) 0.0775 1.0000 Uani . O8 O 0.3227(8) -0.1790(7) 0.2694(2) 0.0739 1.0000 Uani . O9 O 0.4860(7) 0.2441(7) 0.21058(16) 0.0573 1.0000 Uani . O10 O 0.3545(8) 0.2356(7) 0.27230(17) 0.0621 1.0000 Uani . O11 O 0.3877(8) 0.4692(7) 0.20612(18) 0.0726 1.0000 Uani . O12 O 0.2575(9) 0.4562(7) 0.2731(2) 0.0779 1.0000 Uani . O13 O 1.0468(12) 0.1319(11) 0.2744(3) 0.1242 1.0000 Uani . N1 N 1.1576(9) -0.2786(8) 0.2362(2) 0.0625 1.0000 Uani . C1 C 0.5355(15) 0.8064(15) 0.1489(3) 0.0897 1.0000 Uani . C2 C 0.5098(14) 0.6930(14) 0.1611(3) 0.0810 1.0000 Uani . C3 C 0.4827(9) 0.8028(8) 0.0794(2) 0.0421 1.0000 Uani . C4 C 0.4089(9) 0.7299(8) 0.0908(2) 0.0406 1.0000 Uani . C5 C 0.3130(9) 0.8412(9) 0.0266(2) 0.0447 1.0000 Uani . C6 C 0.2370(9) 0.8831(9) -0.0071(2) 0.0417 1.0000 Uani . C7 C 0.1443(9) 0.9872(8) -0.0717(2) 0.0388 1.0000 Uani . C8 C 0.0699(9) 0.9153(9) -0.0603(2) 0.0417 1.0000 Uani . C10 C -0.0374(18) 0.9615(15) -0.1275(3) 0.1091 1.0000 Uani . C11 C 0.5012(11) 0.706(1) -0.1207(2) 0.0552 1.0000 Uani . C12 C 0.519(1) 0.8322(9) -0.1236(2) 0.0506 1.0000 Uani . C13 C 0.6048(9) 0.6562(9) -0.0505(2) 0.0444 1.0000 Uani . C14 C 0.6825(9) 0.7262(8) -0.0602(2) 0.0436 1.0000 Uani . C15 C 0.767(1) 0.6199(9) 0.0054(2) 0.0448 1.0000 Uani . C16 C 0.8351(9) 0.5799(9) 0.0388(2) 0.0418 1.0000 Uani . C17 C 0.9147(9) 0.4807(9) 0.1047(2) 0.0442 1.0000 Uani . C18 C 0.9926(9) 0.5484(8) 0.0942(2) 0.0415 1.0000 Uani . C19 C 1.0500(14) 0.4051(15) 0.1721(3) 0.0873 1.0000 Uani . C20 C 1.0670(14) 0.5292(16) 0.1649(3) 0.0900 1.0000 Uani . C21 C 0.638(2) 0.2206(18) 0.3422(3) 0.1444 1.0000 Uani . C22 C 0.7275(14) 0.2819(13) 0.3476(3) 0.0770 1.0000 Uani . C23 C 0.6863(12) 0.0951(11) 0.4100(3) 0.0660 1.0000 Uani . C24 C 0.7252(12) 0.1868(11) 0.4192(3) 0.0668 1.0000 Uani . C25 C 0.7419(13) 0.0312(11) 0.4794(2) 0.0672 1.0000 Uani . C26 C 0.7646(11) -0.0275(11) 0.5141(3) 0.0614 1.0000 Uani . C27 C 0.7884(11) -0.184(1) 0.5743(3) 0.0577 1.0000 Uani . C28 C 0.8234(11) -0.0907(11) 0.5834(2) 0.0615 1.0000 Uani . C29 C 0.8127(18) -0.2924(13) 0.6464(3) 0.0985 1.0000 Uani . C30 C 0.7710(18) -0.1562(14) 0.6532(3) 0.0978 1.0000 Uani . C31 C 0.7408(15) 0.7404(12) 0.3512(3) 0.0757 1.0000 Uani . C32 C 0.5759(15) 0.7884(12) 0.3521(3) 0.0761 1.0000 Uani . C33 C 0.7622(13) 0.592(1) 0.4163(2) 0.0609 1.0000 Uani . C34 C 0.6302(13) 0.6877(12) 0.4244(3) 0.0641 1.0000 Uani . C35 C 0.7282(13) 0.5374(11) 0.4857(3) 0.0669 1.0000 Uani . C36 C 0.7437(12) 0.4765(11) 0.5200(2) 0.0615 1.0000 Uani . C37 C 0.8460(12) 0.3220(11) 0.5795(2) 0.0590 1.0000 Uani . C38 C 0.7130(14) 0.4145(12) 0.5884(3) 0.0659 1.0000 Uani . C39 C 0.8946(15) 0.2059(14) 0.6525(3) 0.0888 1.0000 Uani . C40 C 0.793(2) 0.3368(17) 0.6596(4) 0.1384 1.0000 Uani . C41 C 0.7693(13) -0.0690(11) 0.2615(2) 0.0578 1.0000 Uani . C42 C 0.7611(11) -0.103(1) 0.2225(2) 0.0479 1.0000 Uani . C43 C 0.290(1) -0.012(1) 0.2191(2) 0.0536 1.0000 Uani . C44 C 0.3472(11) -0.085(1) 0.2569(2) 0.0557 1.0000 Uani . C45 C 0.4077(12) 0.3591(11) 0.2215(2) 0.0584 1.0000 Uani . C46 C 0.3316(11) 0.353(1) 0.2593(2) 0.0525 1.0000 Uani . C47 C 0.8614(12) 0.3471(11) 0.2588(3) 0.0667 1.0000 Uani . C48 C 0.7119(13) 0.4138(12) 0.2514(3) 0.0742 1.0000 Uani . C49 C 0.6360(13) 0.5494(14) 0.2566(3) 0.0861 1.0000 Uani . C50 C 0.714(2) 0.6130(13) 0.2660(3) 0.0964 1.0000 Uani . C51 C 0.8617(18) 0.5475(15) 0.2732(3) 0.0933 1.0000 Uani . C52 C 0.9360(13) 0.4100(14) 0.2694(3) 0.0772 1.0000 Uani . C53 C 0.9393(14) 0.1999(13) 0.2546(3) 0.0778 1.0000 Uani . C54 C 0.8882(15) 0.1464(12) 0.2282(4) 0.0885 1.0000 Uani . C91 C 0.050(7) 1.007(7) -0.1415(6) 0.0873 0.52(5) Uani . C92 C -0.016(3) 1.082(3) -0.1344(7) 0.0527 0.52(5) Uani . H1 H 0.4421 0.8828 0.1493 0.0507 1.0000 Uiso . H2 H 0.5985 0.8114 0.1662 0.0507 1.0000 Uiso . H3 H 0.6039 0.6207 0.1664 0.0507 1.0000 Uiso . H4 H 0.4526 0.7095 0.1835 0.0507 1.0000 Uiso . H7 H -0.1379 1.0110 -0.1357 0.0507 1.0000 Uiso . H8 H 0.0110 0.8877 -0.1413 0.0507 1.0000 Uiso . H9 H 0.5920 0.6394 -0.1299 0.0507 1.0000 Uiso . H10 H 0.4230 0.7180 -0.1358 0.0507 1.0000 Uiso . H11 H 0.4355 0.8956 -0.1120 0.0507 1.0000 Uiso . H12 H 0.5216 0.8627 -0.1488 0.0507 1.0000 Uiso . H13 H 1.0309 0.3911 0.1977 0.0507 1.0000 Uiso . H14 H 1.1426 0.3356 0.1660 0.0507 1.0000 Uiso . H15 H 1.1346 0.5296 0.1821 0.0507 1.0000 Uiso . H16 H 0.9722 0.5997 0.1690 0.0507 1.0000 Uiso . H17 H 0.6557 0.2002 0.3175 0.0507 1.0000 Uiso . H18 H 0.5312 0.2894 0.3427 0.0507 1.0000 Uiso . H19 H 0.6960 0.3596 0.3310 0.0507 1.0000 Uiso . H20 H 0.8329 0.2243 0.3403 0.0507 1.0000 Uiso . H21 H 0.7683 -0.3339 0.6640 0.0507 1.0000 Uiso . H22 H 0.9160 -0.3357 0.6493 0.0507 1.0000 Uiso . H23 H 0.7811 -0.1533 0.6787 0.0507 1.0000 Uiso . H24 H 0.6684 -0.1093 0.6472 0.0507 1.0000 Uiso . H25 H 0.7632 0.8002 0.3625 0.0507 1.0000 Uiso . H26 H 0.7709 0.7400 0.3261 0.0507 1.0000 Uiso . H27 H 0.5529 0.7230 0.3436 0.0507 1.0000 Uiso . H28 H 0.5323 0.8688 0.3364 0.0507 1.0000 Uiso . H29 H 0.8606 0.1399 0.6585 0.0507 1.0000 Uiso . H30 H 0.9761 0.1857 0.6684 0.0507 1.0000 Uiso . H31 H 0.8414 0.3918 0.6618 0.0507 1.0000 Uiso . H32 H 0.7513 0.3245 0.6832 0.0507 1.0000 Uiso . H33 H 0.6681 0.3656 0.2414 0.0507 1.0000 Uiso . H34 H 0.5320 0.5917 0.2545 0.0507 1.0000 Uiso . H35 H 0.6660 0.7075 0.2659 0.0507 1.0000 Uiso . H36 H 0.9081 0.5962 0.2823 0.0507 1.0000 Uiso . H37 H 1.0386 0.3652 0.2729 0.0507 1.0000 Uiso . H38 H 0.8435 0.0956 0.2403 0.0507 1.0000 Uiso . H39 H 0.8237 0.2171 0.2122 0.0507 1.0000 Uiso . H40 H 0.9739 0.0903 0.2149 0.0507 1.0000 Uiso . H41 H 1.0614 -0.2397 0.2257 0.0507 1.0000 Uiso . H42 H 1.1652 -0.3499 0.2544 0.0507 1.0000 Uiso . H43 H 1.2288 -0.3153 0.2173 0.0507 1.0000 Uiso . H44 H 1.1737 -0.2150 0.2466 0.0507 1.0000 Uiso . H51 H 0.0401 1.0355 -0.1671 0.0507 0.52(5) Uiso . H52 H -0.1184 1.1677 -0.1288 0.0507 0.52(5) Uiso . H61 H 0.1219 0.9219 -0.1364 0.0507 0.52(5) Uiso . H62 H -0.0050 1.0938 -0.1584 0.0507 0.52(5) Uiso . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0580(9) 0.0484(8) 0.0451(7) -0.0062(6) -0.0025(6) -0.0271(7) S1 0.0571(15) 0.0549(15) 0.0593(13) -0.0009(11) -0.0139(11) -0.0371(13) S2 0.0887(19) 0.0631(17) 0.0467(12) 0.0056(11) -0.0181(12) -0.0516(16) S3 0.0537(14) 0.0533(14) 0.0507(12) 0.002(1) -0.011(1) -0.0368(12) S4 0.0612(15) 0.0648(16) 0.0451(11) 0.0018(11) -0.010(1) -0.0468(14) S5 0.0579(15) 0.0596(15) 0.0451(11) 0.004(1) -0.012(1) -0.0420(13) S6 0.0587(15) 0.0668(16) 0.0433(11) 0.0053(11) -0.011(1) -0.0436(14) S7 0.0613(16) 0.0608(16) 0.0587(13) 0.0180(12) -0.0222(12) -0.0398(14) S8 0.092(2) 0.101(2) 0.0577(14) 0.0169(14) -0.0265(14) -0.079(2) S9 0.0600(16) 0.0692(17) 0.0612(14) -0.0020(12) -0.0133(12) -0.0465(14) S10 0.0651(16) 0.0621(16) 0.0527(13) 0.0094(12) -0.0190(11) -0.0400(14) S11 0.0526(14) 0.0634(16) 0.0522(12) -0.0016(11) -0.004(1) -0.0414(13) S12 0.0545(14) 0.0629(15) 0.0500(12) 0.0038(11) -0.010(1) -0.0414(13) S13 0.0613(16) 0.0600(16) 0.0537(13) -0.0008(11) -0.0050(11) -0.0434(14) S14 0.0516(14) 0.0511(14) 0.0543(12) -0.001(1) -0.006(1) -0.0335(12) S15 0.099(2) 0.0757(19) 0.0524(14) 0.0110(13) -0.0117(14) -0.0543(18) S16 0.0653(17) 0.0579(16) 0.0719(16) -0.0004(12) -0.0245(13) -0.0335(14) S17 0.143(3) 0.080(2) 0.0501(14) -0.0013(14) -0.0196(16) -0.062(2) S18 0.115(2) 0.0712(19) 0.0499(13) 0.0002(13) -0.0067(14) -0.0534(19) S19 0.112(2) 0.077(2) 0.0494(14) -0.0014(13) -0.0051(14) -0.0558(19) S20 0.106(2) 0.083(2) 0.0469(13) -0.0013(13) -0.0086(13) -0.0589(19) S21 0.117(3) 0.079(2) 0.0506(14) -0.0002(13) -0.0107(15) -0.055(2) S22 0.100(2) 0.079(2) 0.0495(13) 0.0034(13) -0.0053(13) -0.0542(18) S23 0.140(3) 0.069(2) 0.0569(15) 0.0056(14) -0.0129(17) -0.057(2) S24 0.106(2) 0.097(2) 0.0526(14) 0.0075(14) -0.0160(15) -0.064(2) S25 0.107(2) 0.0624(19) 0.0557(15) 0.0035(13) 0.0127(15) -0.0247(18) S26 0.090(2) 0.080(2) 0.0519(14) 0.0059(14) -0.0080(14) -0.0245(18) S27 0.088(2) 0.0689(19) 0.0523(14) 0.0017(13) -0.0087(13) -0.0317(17) S28 0.086(2) 0.082(2) 0.0454(13) -0.0026(13) 0.0007(13) -0.0320(17) S29 0.086(2) 0.079(2) 0.0509(14) 0.0019(13) -0.0077(13) -0.0352(17) S30 0.092(2) 0.078(2) 0.0504(14) 0.0043(14) -0.0092(14) -0.0328(18) S31 0.091(2) 0.076(2) 0.0560(15) 0.0067(14) -0.0144(14) -0.0357(17) S32 0.103(2) 0.085(2) 0.0513(15) 0.0037(14) 0.0007(15) -0.0301(19) O1 0.056(4) 0.058(4) 0.054(4) -0.019(3) 0.001(3) -0.024(4) O2 0.060(4) 0.066(5) 0.049(3) -0.013(3) -0.009(3) -0.023(4) O3 0.068(5) 0.087(6) 0.069(4) -0.002(4) -0.015(4) -0.033(4) O4 0.056(5) 0.066(5) 0.063(4) -0.014(4) 0.007(4) -0.018(4) O5 0.057(4) 0.056(4) 0.061(4) -0.002(3) -0.011(3) -0.019(4) O6 0.063(4) 0.048(4) 0.056(3) -0.002(3) -0.015(3) -0.030(3) O7 0.081(5) 0.106(6) 0.071(4) -0.023(4) -0.011(4) -0.060(5) O8 0.090(5) 0.061(5) 0.084(5) 0.013(4) -0.021(4) -0.048(4) O9 0.064(4) 0.046(4) 0.056(4) -0.012(3) 0.011(3) -0.019(4) O10 0.086(5) 0.048(4) 0.057(4) -0.009(3) 0.012(3) -0.035(4) O11 0.090(5) 0.062(5) 0.065(4) 0.014(4) -0.003(4) -0.037(4) O12 0.099(6) 0.053(5) 0.083(5) -0.023(4) 0.029(4) -0.036(5) O13 0.104(8) 0.102(8) 0.128(8) -0.027(6) -0.025(6) -0.005(6) N1 0.055(5) 0.059(5) 0.075(5) -0.002(4) -0.012(4) -0.027(4) C1 0.135(11) 0.145(12) 0.044(5) -0.025(6) -0.005(6) -0.107(11) C2 0.11(1) 0.11(1) 0.047(5) 0.005(6) -0.014(6) -0.075(9) C3 0.039(5) 0.041(5) 0.048(5) -0.006(4) -0.010(4) -0.018(4) C4 0.047(5) 0.038(5) 0.050(5) -0.004(4) -0.006(4) -0.030(4) C5 0.048(5) 0.055(6) 0.046(4) -0.000(4) -0.008(4) -0.036(5) C6 0.044(5) 0.054(6) 0.042(4) -0.002(4) -0.008(4) -0.035(5) C7 0.043(5) 0.035(5) 0.042(4) 0.001(4) -0.004(4) -0.021(4) C8 0.046(5) 0.049(5) 0.034(4) -0.000(4) -0.004(4) -0.025(5) C10 0.171(14) 0.125(12) 0.092(8) 0.032(8) -0.065(9) -0.122(12) C11 0.058(6) 0.059(6) 0.057(5) -0.009(5) -0.006(4) -0.033(5) C12 0.055(6) 0.053(6) 0.048(5) -0.000(4) -0.007(4) -0.029(5) C13 0.049(5) 0.056(6) 0.036(4) -0.008(4) -0.008(4) -0.029(5) C14 0.046(5) 0.043(5) 0.056(5) -0.001(4) -0.014(4) -0.032(5) C15 0.058(6) 0.048(5) 0.045(4) -0.013(4) -0.001(4) -0.036(5) C16 0.041(5) 0.046(5) 0.048(4) -0.003(4) -0.003(4) -0.028(4) C17 0.041(5) 0.035(5) 0.052(5) -0.011(4) 0.003(4) -0.011(4) C18 0.041(5) 0.027(4) 0.053(5) -0.005(4) -0.007(4) -0.011(4) C19 0.092(9) 0.110(11) 0.056(6) 0.001(7) -0.004(6) -0.044(8) C20 0.075(8) 0.136(13) 0.080(8) -0.042(8) -0.003(6) -0.057(9) C21 0.30(2) 0.161(16) 0.047(7) 0.003(8) -0.02(1) -0.172(18) C22 0.107(9) 0.094(9) 0.049(5) -0.009(6) -0.007(6) -0.060(8) C23 0.083(8) 0.051(6) 0.060(6) 0.005(5) -0.011(5) -0.027(6) C24 0.069(7) 0.072(8) 0.053(6) -0.004(5) -0.010(5) -0.026(6) C25 0.088(8) 0.074(7) 0.038(5) 0.002(5) 0.004(5) -0.038(7) C26 0.068(7) 0.060(7) 0.057(6) -0.013(5) 0.008(5) -0.028(6) C27 0.061(6) 0.057(6) 0.064(6) -0.007(5) -0.000(5) -0.033(5) C28 0.054(6) 0.077(7) 0.050(5) 0.010(5) -0.001(4) -0.030(6) C29 0.163(14) 0.072(9) 0.057(7) -0.006(6) 0.009(7) -0.052(9) C30 0.158(13) 0.095(11) 0.053(6) 0.004(6) -0.007(7) -0.07(1) C31 0.11(1) 0.066(7) 0.046(5) -0.003(5) 0.005(6) -0.035(7) C32 0.11(1) 0.063(7) 0.061(6) -0.005(5) -0.006(6) -0.038(7) C33 0.090(8) 0.045(6) 0.048(5) -0.001(4) 0.003(5) -0.031(6) C34 0.088(8) 0.068(8) 0.051(5) -0.003(5) -0.008(5) -0.047(7) C35 0.093(8) 0.076(7) 0.048(5) -0.000(5) -0.003(5) -0.054(7) C36 0.075(7) 0.068(7) 0.047(5) -0.010(5) -0.003(5) -0.036(6) C37 0.066(7) 0.062(7) 0.054(5) 0.000(5) -0.016(5) -0.032(6) C38 0.095(9) 0.070(8) 0.050(5) 0.014(5) -0.023(6) -0.053(7) C39 0.11(1) 0.09(1) 0.056(6) -0.004(6) -0.022(6) -0.032(9) C40 0.208(19) 0.092(12) 0.059(8) 0.008(8) -0.017(9) -0.018(12) C41 0.085(8) 0.056(7) 0.051(5) -0.000(5) -0.016(6) -0.047(7) C42 0.047(6) 0.052(6) 0.053(5) 0.001(5) -0.003(5) -0.031(5) C43 0.053(6) 0.050(6) 0.058(5) -0.009(5) 0.001(4) -0.022(5) C44 0.078(7) 0.045(6) 0.049(5) -0.005(4) -0.007(5) -0.030(6) C45 0.076(7) 0.064(8) 0.043(5) 0.014(5) -0.016(5) -0.041(7) C46 0.064(7) 0.042(6) 0.062(5) -0.012(5) -0.003(5) -0.030(5) C47 0.065(7) 0.066(8) 0.060(6) -0.012(5) 0.009(5) -0.021(6) C48 0.077(8) 0.060(7) 0.081(7) -0.002(6) -0.019(6) -0.025(7) C49 0.069(8) 0.09(1) 0.087(8) -0.026(7) -0.004(6) -0.016(7) C50 0.146(14) 0.063(9) 0.070(8) -0.010(6) 0.005(8) -0.04(1) C51 0.113(12) 0.08(1) 0.083(8) -0.028(7) 0.011(8) -0.04(1) C52 0.067(8) 0.111(11) 0.066(7) -0.026(6) 0.011(5) -0.047(8) C53 0.076(8) 0.075(9) 0.078(7) -0.010(6) -0.006(6) -0.028(7) C54 0.11(1) 0.067(8) 0.105(9) -0.015(7) 0.018(8) -0.051(8) C91 0.17(4) 0.14(4) 0.020(9) 0.009(15) -0.021(15) -0.14(4) C92 0.064(14) 0.023(12) 0.063(14) -0.02(1) -0.02(1) -0.005(11) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 15.8 6.16 13.2 5.02 ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6401 _refine_ls_number_parameters 920 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.2138 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_all 0.1529 _refine_ls_wR_factor_ref 0.0746 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.1524 _refine_ls_shift/su_max 0.000390 _refine_diff_density_min -0.64 _refine_diff_density_max 0.74 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 . 2.004(6) yes Fe1 . O2 . 2.009(7) yes Fe1 . O5 . 2.015(6) yes Fe1 . O6 . 1.995(6) yes Fe1 . O9 . 1.994(6) yes Fe1 . O10 . 2.002(7) yes S1 . C1 . 1.760(11) yes S1 . C3 . 1.732(7) yes S2 . C2 . 1.78(1) yes S2 . C4 . 1.731(8) yes S3 . C3 . 1.737(8) yes S3 . C5 . 1.722(7) yes S4 . C4 . 1.747(7) yes S4 . C5 . 1.718(8) yes S5 . C6 . 1.717(8) yes S5 . C7 . 1.739(7) yes S6 . C6 . 1.721(7) yes S6 . C8 . 1.741(7) yes S7 . C7 . 1.748(7) yes S7 . C9 . 1.71(1) yes S8 . C8 . 1.719(8) yes S8 . C10 . 1.693(12) yes S9 . C11 . 1.799(9) yes S9 . C13 . 1.733(7) yes S10 . C12 . 1.768(8) yes S10 . C14 . 1.757(8) yes S11 . C13 . 1.746(8) yes S11 . C15 . 1.742(7) yes S12 . C14 . 1.746(7) yes S12 . C15 . 1.726(8) yes S13 . C16 . 1.732(8) yes S13 . C17 . 1.740(8) yes S14 . C16 . 1.737(8) yes S14 . C18 . 1.724(8) yes S15 . C17 . 1.754(8) yes S15 . C19 . 1.777(12) yes S16 . C18 . 1.743(8) yes S16 . C20 . 1.735(13) yes S17 . C21 . 1.719(15) yes S17 . C23 . 1.74(1) yes S18 . C22 . 1.79(1) yes S18 . C24 . 1.713(11) yes S19 . C23 . 1.76(1) yes S19 . C25 . 1.73(1) yes S20 . C24 . 1.768(9) yes S20 . C25 . 1.75(1) yes S21 . C26 . 1.74(1) yes S21 . C27 . 1.76(1) yes S22 . C26 . 1.74(1) yes S22 . C28 . 1.754(9) yes S23 . C27 . 1.72(1) yes S23 . C29 . 1.790(12) yes S24 . C28 . 1.74(1) yes S24 . C30 . 1.738(12) yes S25 . C31 . 1.768(12) yes S25 . C33 . 1.73(1) yes S26 . C32 . 1.782(12) yes S26 . C34 . 1.749(11) yes S27 . C33 . 1.73(1) yes S27 . C35 . 1.752(11) yes S28 . C34 . 1.77(1) yes S28 . C35 . 1.743(12) yes S29 . C36 . 1.749(11) yes S29 . C37 . 1.73(1) yes S30 . C36 . 1.735(11) yes S30 . C38 . 1.74(1) yes S31 . C37 . 1.749(11) yes S31 . C39 . 1.779(13) yes S32 . C38 . 1.766(11) yes S32 . C40 . 1.753(17) yes O1 . C41 . 1.269(13) yes O2 . C42 . 1.312(11) yes O3 . C41 . 1.242(12) yes O4 . C42 . 1.193(12) yes O5 . C43 . 1.292(11) yes O6 . C44 . 1.30(1) yes O7 . C43 . 1.21(1) yes O8 . C44 . 1.23(1) yes O9 . C45 . 1.288(13) yes O10 . C46 . 1.273(11) yes O11 . C45 . 1.230(11) yes O12 . C46 . 1.215(12) yes O13 . C53 . 1.217(13) yes N1 . H41 . 0.974 no N1 . H42 . 1.023 no N1 . H43 . 1.026 no N1 . H44 . 0.815 no C1 . C2 . 1.420(15) yes C1 . H1 . 0.980 no C1 . H2 . 0.964 no C2 . H3 . 0.965 no C2 . H4 . 0.927 no C3 . C4 . 1.35(1) yes C5 . C6 . 1.41(1) yes C7 . C8 . 1.35(1) yes C9 . C10 . 1.275(15) yes C9 . H5 . 1.011 no C9 . H6 . 0.882 no C10 . H7 . 0.962 no C10 . H8 . 0.988 no C11 . C12 . 1.495(12) yes C11 . H9 . 0.996 no C11 . H10 . 0.935 no C12 . H11 . 0.950 no C12 . H12 . 0.962 no C13 . C14 . 1.345(11) yes C15 . C16 . 1.366(11) yes C17 . C18 . 1.340(11) yes C19 . C20 . 1.467(18) yes C19 . H13 . 0.969 no C19 . H14 . 0.959 no C20 . H15 . 0.932 no C20 . H16 . 1.009 no C21 . C22 . 1.385(17) yes C21 . H17 . 1.009 no C21 . H18 . 0.863 no C22 . H19 . 0.917 no C22 . H20 . 0.969 no C23 . C24 . 1.335(14) yes C25 . C26 . 1.340(12) yes C27 . C28 . 1.339(13) yes C29 . C30 . 1.440(18) yes C29 . H21 . 0.930 no C29 . H22 . 1.025 no C30 . H23 . 0.940 no C30 . H24 . 0.987 no C31 . C32 . 1.514(16) yes C31 . H25 . 0.922 no C31 . H26 . 0.951 no C32 . H27 . 0.948 no C32 . H28 . 0.956 no C33 . C34 . 1.341(15) yes C35 . C36 . 1.340(12) yes C37 . C38 . 1.336(16) yes C39 . C40 . 1.42(2) yes C39 . H29 . 0.929 no C39 . H30 . 0.965 no C40 . H31 . 0.849 no C40 . H32 . 0.965 no C41 . C42 . 1.548(13) yes C43 . C44 . 1.518(12) yes C45 . C46 . 1.545(14) yes C47 . C48 . 1.390(15) yes C47 . C52 . 1.349(14) yes C47 . C53 . 1.518(17) yes C48 . C49 . 1.386(17) yes C48 . H33 . 0.916 no C49 . C50 . 1.354(17) yes C49 . H34 . 1.003 no C50 . C51 . 1.356(19) yes C50 . H35 . 0.957 no C51 . C52 . 1.425(19) yes C51 . H36 . 0.932 no C52 . H37 . 0.947 no C53 . C54 . 1.440(16) yes C54 . H38 . 0.934 no C54 . H39 . 0.927 no C54 . H40 . 0.970 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Fe1 . O2 . 80.2(3) yes O1 . Fe1 . O5 . 160.7(3) yes O2 . Fe1 . O5 . 87.3(3) yes O1 . Fe1 . O6 . 86.6(2) yes O2 . Fe1 . O6 . 97.4(3) yes O5 . Fe1 . O6 . 80.5(2) yes O1 . Fe1 . O9 . 101.1(3) yes O2 . Fe1 . O9 . 90.1(3) yes O5 . Fe1 . O9 . 93.5(3) yes O6 . Fe1 . O9 . 170.1(3) yes O1 . Fe1 . O10 . 93.0(3) yes O2 . Fe1 . O10 . 166.6(3) yes O5 . Fe1 . O10 . 102.0(3) yes O6 . Fe1 . O10 . 93.6(3) yes O9 . Fe1 . O10 . 79.9(3) yes C1 . S1 . C3 . 98.7(4) yes C2 . S2 . C4 . 103.5(4) yes C3 . S3 . C5 . 94.5(4) yes C4 . S4 . C5 . 95.0(4) yes C6 . S5 . C7 . 94.9(3) yes C6 . S6 . C8 . 94.8(4) yes C7 . S7 . C9 . 101.4(5) yes C8 . S8 . C10 . 101.5(4) yes C11 . S9 . C13 . 101.9(4) yes C12 . S10 . C14 . 102.9(4) yes C13 . S11 . C15 . 95.4(4) yes C14 . S12 . C15 . 95.2(4) yes C16 . S13 . C17 . 94.9(4) yes C16 . S14 . C18 . 95.5(4) yes C17 . S15 . C19 . 102.2(5) yes C18 . S16 . C20 . 101.4(4) yes C21 . S17 . C23 . 100.6(6) yes C22 . S18 . C24 . 101.3(5) yes C23 . S19 . C25 . 95.6(5) yes C24 . S20 . C25 . 95.7(5) yes C26 . S21 . C27 . 96.1(4) yes C26 . S22 . C28 . 95.8(5) yes C27 . S23 . C29 . 102.9(5) yes C28 . S24 . C30 . 99.3(5) yes C31 . S25 . C33 . 100.3(5) yes C32 . S26 . C34 . 101.6(6) yes C33 . S27 . C35 . 96.1(5) yes C34 . S28 . C35 . 95.3(5) yes C36 . S29 . C37 . 95.4(5) yes C36 . S30 . C38 . 94.7(6) yes C37 . S31 . C39 . 104.9(6) yes C38 . S32 . C40 . 99.9(7) yes Fe1 . O1 . C41 . 114.8(6) yes Fe1 . O2 . C42 . 116.8(6) yes Fe1 . O5 . C43 . 114.0(5) yes Fe1 . O6 . C44 . 114.8(5) yes Fe1 . O9 . C45 . 116.3(6) yes Fe1 . O10 . C46 . 116.3(6) yes H41 . N1 . H42 . 109.636 no H41 . N1 . H43 . 109.284 no H42 . N1 . H43 . 114.753 no H41 . N1 . H44 . 108.916 no H42 . N1 . H44 . 108.405 no H43 . N1 . H44 . 105.653 no S1 . C1 . C2 . 118.9(9) yes S1 . C1 . H1 . 106.277 no C2 . C1 . H1 . 108.135 no S1 . C1 . H2 . 107.243 no C2 . C1 . H2 . 109.682 no H1 . C1 . H2 . 105.860 no S2 . C2 . C1 . 121.2(7) yes S2 . C2 . H3 . 104.493 no C1 . C2 . H3 . 104.928 no S2 . C2 . H4 . 107.004 no C1 . C2 . H4 . 108.734 no H3 . C2 . H4 . 110.113 no S1 . C3 . S3 . 117.1(4) yes S1 . C3 . C4 . 125.1(6) yes S3 . C3 . C4 . 117.7(6) yes S2 . C4 . S4 . 116.2(4) yes S2 . C4 . C3 . 127.8(6) yes S4 . C4 . C3 . 116.0(6) yes S3 . C5 . S4 . 116.5(4) yes S3 . C5 . C6 . 121.9(6) yes S4 . C5 . C6 . 121.5(6) yes S5 . C6 . S6 . 116.5(4) yes S5 . C6 . C5 . 122.4(5) yes S6 . C6 . C5 . 121.1(6) yes S5 . C7 . S7 . 115.7(4) yes S5 . C7 . C8 . 116.9(5) yes S7 . C7 . C8 . 127.5(6) yes S6 . C8 . S8 . 115.1(4) yes S6 . C8 . C7 . 116.9(6) yes S8 . C8 . C7 . 127.9(6) yes S7 . C9 . C10 . 129.2(9) yes S7 . C9 . H5 . 102.516 no C10 . C9 . H5 . 99.503 no S7 . C9 . H6 . 108.910 no C10 . C9 . H6 . 105.507 no H5 . C9 . H6 . 109.901 no S8 . C10 . C9 . 130.2(9) yes S8 . C10 . H7 . 104.368 no C9 . C10 . H7 . 103.423 no S8 . C10 . H8 . 103.889 no C9 . C10 . H8 . 107.468 no H7 . C10 . H8 . 105.357 no S9 . C11 . C12 . 116.0(6) yes S9 . C11 . H9 . 106.760 no C12 . C11 . H9 . 106.085 no S9 . C11 . H10 . 109.920 no C12 . C11 . H10 . 110.663 no H9 . C11 . H10 . 106.851 no S10 . C12 . C11 . 115.0(6) yes S10 . C12 . H11 . 110.189 no C11 . C12 . H11 . 106.111 no S10 . C12 . H12 . 109.135 no C11 . C12 . H12 . 107.709 no H11 . C12 . H12 . 108.514 no S9 . C13 . S11 . 114.6(5) yes S9 . C13 . C14 . 129.0(6) yes S11 . C13 . C14 . 116.4(6) yes S10 . C14 . S12 . 115.2(4) yes S10 . C14 . C13 . 127.1(6) yes S12 . C14 . C13 . 117.7(6) yes S11 . C15 . S12 . 115.4(4) yes S11 . C15 . C16 . 122.0(6) yes S12 . C15 . C16 . 122.6(6) yes S13 . C16 . S14 . 115.1(4) yes S13 . C16 . C15 . 122.9(6) yes S14 . C16 . C15 . 122.0(6) yes S13 . C17 . S15 . 113.9(5) yes S13 . C17 . C18 . 117.4(6) yes S15 . C17 . C18 . 128.7(6) yes S14 . C18 . S16 . 116.0(5) yes S14 . C18 . C17 . 117.1(6) yes S16 . C18 . C17 . 126.9(6) yes S15 . C19 . C20 . 117.8(9) yes S15 . C19 . H13 . 107.945 no C20 . C19 . H13 . 109.193 no S15 . C19 . H14 . 108.403 no C20 . C19 . H14 . 105.945 no H13 . C19 . H14 . 107.138 no S16 . C20 . C19 . 116.6(9) yes S16 . C20 . H15 . 112.063 no C19 . C20 . H15 . 109.517 no S16 . C20 . H16 . 107.823 no C19 . C20 . H16 . 103.907 no H15 . C20 . H16 . 106.034 no S17 . C21 . C22 . 125.9(13) yes S17 . C21 . H17 . 97.434 no C22 . C21 . H17 . 104.528 no S17 . C21 . H18 . 103.867 no C22 . C21 . H18 . 112.302 no H17 . C21 . H18 . 111.686 no S18 . C22 . C21 . 116.8(9) yes S18 . C22 . H19 . 110.063 no C21 . C22 . H19 . 104.157 no S18 . C22 . H20 . 107.162 no C21 . C22 . H20 . 107.990 no H19 . C22 . H20 . 110.619 no S17 . C23 . S19 . 115.0(6) yes S17 . C23 . C24 . 126.8(7) yes S19 . C23 . C24 . 118.0(7) yes S18 . C24 . S20 . 113.6(6) yes S18 . C24 . C23 . 130.5(7) yes S20 . C24 . C23 . 115.8(8) yes S19 . C25 . S20 . 114.7(5) yes S19 . C25 . C26 . 123.6(8) yes S20 . C25 . C26 . 121.6(8) yes S21 . C26 . S22 . 114.3(5) yes S21 . C26 . C25 . 122.5(8) yes S22 . C26 . C25 . 123.2(8) yes S21 . C27 . S23 . 114.1(5) yes S21 . C27 . C28 . 116.3(7) yes S23 . C27 . C28 . 129.5(7) yes S22 . C28 . S24 . 116.2(6) yes S22 . C28 . C27 . 117.5(7) yes S24 . C28 . C27 . 126.2(7) yes S23 . C29 . C30 . 116.6(9) yes S23 . C29 . H21 . 110.085 no C30 . C29 . H21 . 114.107 no S23 . C29 . H22 . 105.560 no C30 . C29 . H22 . 104.309 no H21 . C29 . H22 . 104.862 no S24 . C30 . C29 . 118.1(11) yes S24 . C30 . H23 . 113.507 no C29 . C30 . H23 . 105.892 no S24 . C30 . H24 . 110.780 no C29 . C30 . H24 . 100.106 no H23 . C30 . H24 . 107.203 no S25 . C31 . C32 . 115.3(8) yes S25 . C31 . H25 . 109.550 no C32 . C31 . H25 . 107.164 no S25 . C31 . H26 . 107.684 no C32 . C31 . H26 . 105.313 no H25 . C31 . H26 . 111.864 no S26 . C32 . C31 . 113.3(7) yes S26 . C32 . H27 . 108.272 no C31 . C32 . H27 . 109.844 no S26 . C32 . H28 . 107.886 no C31 . C32 . H28 . 108.296 no H27 . C32 . H28 . 109.175 no S25 . C33 . S27 . 116.7(7) yes S25 . C33 . C34 . 125.7(8) yes S27 . C33 . C34 . 117.5(8) yes S26 . C34 . S28 . 112.1(7) yes S26 . C34 . C33 . 131.1(8) yes S28 . C34 . C33 . 116.8(8) yes S27 . C35 . S28 . 114.3(5) yes S27 . C35 . C36 . 122.5(9) yes S28 . C35 . C36 . 123.2(9) yes S29 . C36 . S30 . 115.0(5) yes S29 . C36 . C35 . 122.3(8) yes S30 . C36 . C35 . 122.7(9) yes S29 . C37 . S31 . 114.2(7) yes S29 . C37 . C38 . 116.8(7) yes S31 . C37 . C38 . 129.0(8) yes S30 . C38 . S32 . 115.1(7) yes S30 . C38 . C37 . 118.2(8) yes S32 . C38 . C37 . 126.6(7) yes S31 . C39 . C40 . 117.2(9) yes S31 . C39 . H29 . 109.473 no C40 . C39 . H29 . 110.875 no S31 . C39 . H30 . 107.633 no C40 . C39 . H30 . 101.279 no H29 . C39 . H30 . 109.941 no S32 . C40 . C39 . 124.4(13) yes S32 . C40 . H31 . 104.232 no C39 . C40 . H31 . 110.230 no S32 . C40 . H32 . 98.778 no C39 . C40 . H32 . 102.284 no H31 . C40 . H32 . 117.333 no O1 . C41 . O3 . 126.9(9) yes O1 . C41 . C42 . 116.6(9) yes O3 . C41 . C42 . 116.5(11) yes O2 . C42 . O4 . 125.9(9) yes O2 . C42 . C41 . 110.7(10) yes O4 . C42 . C41 . 123.4(9) yes O5 . C43 . O7 . 125.8(9) yes O5 . C43 . C44 . 114.2(8) yes O7 . C43 . C44 . 120.0(9) yes O6 . C44 . O8 . 123.9(8) yes O6 . C44 . C43 . 114.6(8) yes O8 . C44 . C43 . 121.1(8) yes O9 . C45 . O11 . 128.1(10) yes O9 . C45 . C46 . 113.1(8) yes O11 . C45 . C46 . 118.8(11) yes O10 . C46 . O12 . 126.8(9) yes O10 . C46 . C45 . 113.9(9) yes O12 . C46 . C45 . 119.3(9) yes C48 . C47 . C52 . 122.2(11) yes C48 . C47 . C53 . 118.3(10) yes C52 . C47 . C53 . 119.5(11) yes C47 . C48 . C49 . 119.5(10) yes C47 . C48 . H33 . 114.629 no C49 . C48 . H33 . 125.637 no C48 . C49 . C50 . 118.3(12) yes C48 . C49 . H34 . 121.446 no C50 . C49 . H34 . 120.245 no C49 . C50 . C51 . 123.0(13) yes C49 . C50 . H35 . 120.029 no C51 . C50 . H35 . 116.651 no C50 . C51 . C52 . 119.3(12) yes C50 . C51 . H36 . 117.164 no C52 . C51 . H36 . 123.343 no C47 . C52 . C51 . 117.6(11) yes C47 . C52 . H37 . 122.281 no C51 . C52 . H37 . 119.727 no O13 . C53 . C47 . 116.9(11) yes O13 . C53 . C54 . 123.5(13) yes C47 . C53 . C54 . 119.6(11) yes C53 . C54 . H38 . 110.129 no C53 . C54 . H39 . 108.583 no H38 . C54 . H39 . 112.925 no C53 . C54 . H40 . 106.123 no H38 . C54 . H40 . 109.175 no H39 . C54 . H40 . 109.680 no # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================