# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/255 data_global #------------------------------------------------------------------------------ _publ_requested_journal 'Journal of Materials Chemistry' _publ_contact_author_name 'Professor Gunzi Saito' _publ_contact_author_address ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; _publ_contact_author_email 'saito@kuchem.kyoto-u.ac.jp' #------------------------------------------------------------------------------ _publ_section_title ; A stable and flexible dianion: 2-Dicyanomethylene-1,1,3,4,5,5-hexacyanopentenediide (DHCP^2-^), and its complex formation ; loop_ _publ_author_name _publ_author_address 'Saito, Gunzi' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Sekizaki, Shuichi' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Konsha, Akihiko' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Yamochi, Hideki' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Matsumoto, Kiyoshi' ; Graduate School of Human and Environmental Studies, Kyoto University, Kyoto 606-8501, Japan ; 'Kusunoki, Masami' ; Institute for Protein Research, Osaka University, Suita, Osaka 565-0871, Japan ; 'Sakaguchi, Ken-ichi' ; Institute for Protein Research, Osaka University, Suita, Osaka 565-0871, Japan ; #------------------------------------------------------------------------------ data_ET1 #------------------------------------------------------------------------------ _chemical_name_common ? _chemical_formula_moiety '2(C10 H8 S8 1+),2(C10 H8 S8), C14 N8 2-, 2(C4 H8 O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H48 N8 O2 S32' _chemical_formula_weight 1963.23 _chemical_melting_point ? _chemical_compound_source 'Local laboratory' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.666(3) _cell_length_b 19.620(4) _cell_length_c 9.523(2) _cell_angle_alpha 96.38(4) _cell_angle_beta 112.72(2) _cell_angle_gamma 89.35(3) _cell_volume 1996.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 1.614 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'flotation in mixture of CHCl3 and CCl4' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC-4' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9650 _diffrn_reflns_av_R_equivalents 0.1693 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9644 _reflns_number_observed 5195 _reflns_observed_criterion >2sigma(F) #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku MSC/AFC diffractometer software' _computing_cell_refinement 'Rigaku MSC/AFC diffractometer software' _computing_data_reduction ? _computing_structure_solution 'SIR-92 for Crystan6.3.3 (MacScience, 1995)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _computing_publication_material ? #------------------------------------------------------------------------------ _refine_special_details ; Refinement on F^2^ using reflections with F^2^ > 2.0 sigma(F^2^). Weighted R-factors wR and goodnesses of fit S are based on F^2^, conventional R-factors R are based on F. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6590 _refine_ls_number_parameters 937 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_obs 0.0521 _refine_ls_wR_factor_all 1.2934 _refine_ls_wR_factor_obs 0.1301 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.157 _refine_ls_restrained_S_all 8.085 _refine_ls_restrained_S_obs 1.157 _refine_ls_shift/esd_max 0.313 _refine_ls_shift/esd_mean 0.024 _refine_diff_density_max 0.418 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.113 #------------------------------------------------------------------------------ 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S21 S 0.0820(4) 0.4635(2) 0.3700(5) 0.0492(11) Uani 1 d . . S22 S 0.2153(4) 0.4641(2) 0.1641(4) 0.0452(10) Uani 1 d . . S23 S -0.0321(3) 0.6078(2) 0.2755(4) 0.0426(9) Uani 1 d . . S24 S 0.1082(4) 0.6148(2) 0.0786(4) 0.0485(11) Uani 1 d . . S25 S 0.1894(4) 0.3357(2) 0.4930(5) 0.0565(12) Uani 1 d . . S26 S 0.3345(4) 0.3332(2) 0.2373(5) 0.0621(13) Uani 1 d . . S27 S -0.1169(4) 0.7490(2) 0.2604(5) 0.0550(11) Uani 1 d . . S28 S 0.0514(4) 0.7582(2) 0.0240(5) 0.0543(11) Uani 1 d . . C21 C 0.1144(11) 0.5067(6) 0.2391(12) 0.032(3) Uani 1 d . . C22 C 0.0708(12) 0.5706(6) 0.2037(12) 0.034(3) Uani 1 d . . C23 C 0.1770(15) 0.3983(7) 0.3682(18) 0.054(4) Uani 1 d . . C24 C 0.2389(11) 0.3960(5) 0.2777(13) 0.031(3) Uani 1 d . . C25 C -0.0322(13) 0.6867(7) 0.2063(15) 0.041(3) Uani 1 d . . C26 C 0.0328(11) 0.6879(5) 0.1134(14) 0.031(3) Uani 1 d . . C27 C 0.2294(19) 0.2635(8) 0.4005(21) 0.077(6) Uani 1 d . . C28 C 0.3466(12) 0.2723(7) 0.3629(15) 0.047(4) Uani 1 d . . C29 C -0.1265(19) 0.8096(7) 0.1234(22) 0.086(6) Uani 1 d . . C30 C -0.0022(16) 0.8272(6) 0.1230(16) 0.058(4) Uani 1 d . . H29A H -0.1800 0.7900 0.0224 0.050 Uiso 1 calc . . H29B H -0.1630 0.8509 0.1484 0.050 Uiso 1 calc . . H27A H 0.2429 0.2268 0.4635 0.050 Uiso 1 calc . . H27B H 0.1600 0.2497 0.3064 0.050 Uiso 1 calc . . H28A H 0.3633 0.2288 0.3190 0.050 Uiso 1 calc . . H28B H 0.4165 0.2852 0.4570 0.050 Uiso 1 calc . . H30A H 0.0569 0.8365 0.2268 0.050 Uiso 1 calc . . H30B H -0.0079 0.8680 0.0740 0.050 Uiso 1 calc . . S31 S 0.4000(4) 0.3866(2) 0.9306(4) 0.0425(9) Uani 1 d . . S32 S 0.5382(4) 0.3903(2) 0.7329(4) 0.0473(10) Uani 1 d . . S33 S 0.2958(4) 0.5363(2) 0.8489(4) 0.0444(10) Uani 1 d . . S34 S 0.4229(4) 0.5349(2) 0.6351(4) 0.0459(10) Uani 1 d . . S35 S 0.4583(4) 0.2445(2) 0.9993(4) 0.0521(11) Uani 1 d . . S36 S 0.6237(4) 0.2493(2) 0.7604(5) 0.0560(12) Uani 1 d . . S37 S 0.1776(4) 0.6677(2) 0.7801(5) 0.0612(13) Uani 1 d . . S38 S 0.3226(4) 0.6641(2) 0.5175(5) 0.0592(13) Uani 1 d . . C31 C 0.4394(11) 0.4331(5) 0.8105(16) 0.038(3) Uani 1 d . . C32 C 0.3870(12) 0.4941(6) 0.7665(15) 0.042(4) Uani 1 d . . C33 C 0.4742(13) 0.3134(7) 0.9063(16) 0.053(4) Uani 1 d . . C34 C 0.5375(12) 0.3136(5) 0.8167(14) 0.039(4) Uani 1 d . . C35 C 0.2714(12) 0.6061(6) 0.7447(15) 0.045(4) Uani 1 d . . C36 C 0.3277(11) 0.6047(6) 0.6382(15) 0.036(3) Uani 1 d . . C37 C 0.4943(18) 0.1772(7) 0.8893(20) 0.075(5) Uani 1 d . . C38 C 0.6135(16) 0.1820(7) 0.8651(18) 0.061(4) Uani 1 d . . C39 C 0.1699(18) 0.7261(7) 0.6452(18) 0.084(6) Uani 1 d . . C40 C 0.2809(15) 0.7375(6) 0.6173(16) 0.053(4) Uani 1 d . . H37A H 0.4953 0.1361 0.9357 0.050 Uiso 1 calc . . H37B H 0.4274 0.1715 0.7902 0.050 Uiso 1 calc . . H38A H 0.6237 0.1393 0.8121 0.050 Uiso 1 calc . . H38B H 0.6812 0.1878 0.9635 0.050 Uiso 1 calc . . H39A H 0.1047 0.7097 0.5491 0.050 Uiso 1 calc . . H39B H 0.1457 0.7696 0.6798 0.050 Uiso 1 calc . . H40A H 0.3487 0.7499 0.7137 0.050 Uiso 1 calc . . H40B H 0.2687 0.7755 0.5581 0.050 Uiso 1 calc . . S41 S 0.5988(4) 0.4561(2) 0.3851(4) 0.0449(10) Uani 1 d . . S42 S 0.7251(4) 0.4578(2) 0.1729(4) 0.0488(10) Uani 1 d . . S43 S 0.4821(3) 0.6017(2) 0.2945(4) 0.0417(9) Uani 1 d . . S44 S 0.6170(4) 0.6075(2) 0.0912(4) 0.0446(10) Uani 1 d . . S45 S 0.6856(4) 0.3211(2) 0.4799(5) 0.0588(12) Uani 1 d . . S46 S 0.8274(4) 0.3220(2) 0.2178(5) 0.0584(12) Uani 1 d . . S47 S 0.3846(4) 0.7399(2) 0.2605(5) 0.0538(11) Uani 1 d . . S48 S 0.5457(4) 0.7472(2) 0.0178(5) 0.0503(11) Uani 1 d . . C41 C 0.6305(12) 0.5001(6) 0.2519(13) 0.037(3) Uani 1 d . . C42 C 0.5790(15) 0.5627(6) 0.2142(16) 0.048(4) Uani 1 d . . C43 C 0.6839(15) 0.3861(7) 0.3639(18) 0.057(4) Uani 1 d . . C44 C 0.7381(11) 0.3864(5) 0.2673(12) 0.032(3) Uani 1 d . . C45 C 0.4722(13) 0.6775(7) 0.2174(15) 0.040(3) Uani 1 d . . C46 C 0.5331(12) 0.6796(5) 0.1160(13) 0.037(3) Uani 1 d . . C47 C 0.7399(23) 0.2501(10) 0.3966(24) 0.107(8) Uani 1 d . . C48 C 0.8451(13) 0.2624(6) 0.3507(16) 0.047(3) Uani 1 d . . C491 C 0.4256(26) 0.8172(11) 0.2042(32) 0.023(7) Uiso 0.44(4) d P . C492 C 0.3694(22) 0.7999(10) 0.1156(27) 0.037(6) Uiso 0.56(4) d P . C501 C 0.5129(37) 0.8173(14) 0.1275(40) 0.036(9) Uiso 0.36(4) d P . C502 C 0.4415(25) 0.8073(9) 0.0607(25) 0.036(6) Uiso 0.64(4) d P . H47A H 0.7644 0.2165 0.4680 0.050 Uiso 1 calc . . H47B H 0.6715 0.2301 0.3074 0.050 Uiso 1 calc . . H48A H 0.8644 0.2192 0.3087 0.050 Uiso 1 calc . . H48B H 0.9161 0.2774 0.4421 0.050 Uiso 1 calc . . S51 S 0.8975(4) 0.3825(2) 0.9155(4) 0.0447(10) Uani 1 d . . S52 S 1.0325(4) 0.3929(2) 0.7169(4) 0.0439(10) Uani 1 d . . S53 S 0.7899(3) 0.5357(2) 0.8407(4) 0.0388(9) Uani 1 d . . S54 S 0.9200(4) 0.5365(2) 0.6311(4) 0.0441(10) Uani 1 d . . S55 S 0.9665(4) 0.2409(2) 0.9792(5) 0.0534(11) Uani 1 d . . S56 S 1.1248(4) 0.2531(2) 0.7359(5) 0.0565(12) Uani 1 d . . S57 S 0.6800(4) 0.6692(2) 0.7842(5) 0.0617(13) Uani 1 d . . S58 S 0.8263(4) 0.6687(2) 0.5234(5) 0.0567(12) Uani 1 d . . C51 C 0.9294(11) 0.4310(5) 0.7910(15) 0.033(3) Uani 1 d . . C52 C 0.8853(12) 0.4935(5) 0.7583(13) 0.041(4) Uani 1 d . . C53 C 0.9747(12) 0.3096(6) 0.8830(16) 0.040(4) Uani 1 d . . C54 C 1.0348(12) 0.3145(5) 0.7982(16) 0.037(3) Uani 1 d . . C55 C 0.7696(12) 0.6073(7) 0.7411(17) 0.050(4) Uani 1 d . . C56 C 0.8295(9) 0.6077(5) 0.6413(12) 0.021(2) Uani 1 d . . C571 C 1.1132(21) 0.1993(9) 0.9864(23) 0.010(6) Uiso 0.41(4) d P . C572 C 1.0443(40) 0.1759(17) 0.9269(42) 0.087(11) Uiso 0.59(4) d P . C581 C 1.1280(35) 0.1843(13) 0.8530(42) 0.031(9) Uiso 0.44(5) d P . C582 C 1.0700(30) 0.1750(11) 0.7801(36) 0.049(8) Uiso 0.56(5) d P . C59 C 0.6808(22) 0.7281(8) 0.6535(23) 0.106(8) Uani 1 d . . C60 C 0.7816(13) 0.7417(6) 0.6234(16) 0.044(3) Uani 1 d . . H59A H 0.6156 0.7125 0.5569 0.050 Uiso 1 calc . . H59B H 0.6561 0.7713 0.6889 0.050 Uiso 1 calc . . H60A H 0.8501 0.7558 0.7181 0.050 Uiso 1 calc . . H60B H 0.7646 0.7792 0.5623 0.050 Uiso 1 calc . . N1 N 0.7896(12) 0.1059(7) 0.6277(18) 0.081(4) Uani 1 d . . N2 N 0.8352(14) -0.0899(8) 0.8219(18) 0.126(6) Uani 1 d . . N3 N 0.5518(16) -0.1394(7) 0.8256(17) 0.099(5) Uani 1 d . . N4 N 0.2717(12) -0.1045(6) 0.4019(16) 0.087(4) Uani 1 d . . N5 N 0.3289(12) 0.1013(6) 0.5151(15) 0.087(4) Uani 1 d . . N6 N 0.3838(14) 0.1221(6) 0.1555(15) 0.087(4) Uani 1 d . . N7 N 0.6016(19) 0.0264(8) 0.0193(19) 0.144(8) Uani 1 d . . N8 N 0.7370(14) -0.0993(7) 0.3855(15) 0.087(4) Uani 1 d . . C1 C 0.5573(12) -0.0183(5) 0.5762(12) 0.046(3) Uani 1 d . . C2 C 0.6864(11) -0.0047(5) 0.6593(13) 0.056(3) Uani 1 d . . C3 C 0.4843(12) -0.0710(5) 0.5947(14) 0.051(3) Uani 1 d . . C4 C 0.4914(11) 0.0275(5) 0.4556(13) 0.049(3) Uani 1 d . . C5 C 0.5142(12) 0.0317(5) 0.3231(12) 0.052(3) Uani 1 d . . C6 C 0.5964(13) -0.0023(6) 0.2670(14) 0.062(3) Uani 1 d . . C7 C 0.7470(12) 0.0578(6) 0.6421(13) 0.059(3) Uani 1 d . . C8 C 0.7651(16) -0.0499(8) 0.7564(18) 0.090(5) Uani 1 d . . C9 C 0.5280(16) -0.1094(8) 0.7259(18) 0.078(5) Uani 1 d . . C10 C 0.3658(12) -0.0880(5) 0.4879(14) 0.054(3) Uani 1 d . . C11 C 0.4000(11) 0.0681(6) 0.4858(12) 0.050(3) Uani 1 d . . C12 C 0.4401(14) 0.0830(6) 0.2282(14) 0.060(4) Uani 1 d . . C13 C 0.5961(17) 0.0129(7) 0.1237(19) 0.093(5) Uani 1 d . . C14 C 0.6696(12) -0.0564(6) 0.3339(14) 0.056(3) Uani 1 d . . C61 C -0.0424(25) 0.1263(8) 0.2039(31) 0.108(8) Uani 1 d . . C62 C 0.0136(29) 0.1017(12) 0.3125(50) 0.260(24) Uani 1 d . . C63 C -0.0207(37) 0.0270(18) 0.3246(38) 0.216(17) Uani 1 d . . C64 C -0.0239(43) 0.0134(13) 0.1893(47) 0.259(21) Uani 1 d . . C65 C -0.0910(31) 0.0735(16) 0.1172(32) 0.195(13) Uani 1 d . . C71 C 0.1086(31) -0.0131(13) 0.7856(61) 0.264(24) Uani 1 d . . C72 C 0.1119(36) -0.0923(13) 0.7075(38) 0.209(15) Uani 1 d . . C73 C 0.1819(26) -0.1136(10) 0.8259(29) 0.121(8) Uani 1 d . . C74 C 0.2303(39) -0.0637(14) 0.9057(37) 0.279(24) Uani 1 d . . C75 C 0.2080(32) -0.0017(13) 0.7934(48) 0.212(15) Uani 1 d . . #------------------------------------------------------------------------------ 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 S21 0.065(3) 0.037(2) 0.070(3) 0.023(2) 0.048(2) 0.013(2) S22 0.062(3) 0.043(2) 0.045(2) 0.012(2) 0.035(2) 0.010(2) S23 0.041(2) 0.036(2) 0.059(2) 0.014(2) 0.027(2) 0.006(2) S24 0.069(3) 0.036(2) 0.060(2) 0.019(2) 0.044(2) 0.007(2) S25 0.070(3) 0.054(2) 0.066(3) 0.032(2) 0.043(2) 0.022(2) S26 0.087(3) 0.045(2) 0.089(3) 0.020(2) 0.069(3) 0.028(2) S27 0.072(3) 0.047(2) 0.068(3) 0.030(2) 0.045(2) 0.031(2) S28 0.060(3) 0.044(2) 0.078(3) 0.033(2) 0.041(2) 0.021(2) C21 0.032(7) 0.052(7) 0.015(5) -0.005(5) 0.015(5) 0.005(6) C22 0.047(8) 0.031(6) 0.010(5) 0.000(4) -0.005(5) 0.001(5) C23 0.076(11) 0.042(7) 0.069(10) 0.031(7) 0.049(9) 0.008(7) C24 0.029(7) 0.023(5) 0.027(6) -0.006(4) -0.002(5) 0.006(5) C25 0.039(8) 0.052(7) 0.043(7) 0.028(6) 0.021(6) 0.013(6) C26 0.034(8) 0.021(5) 0.039(7) -0.002(5) 0.016(6) -0.004(5) C27 0.127(16) 0.052(9) 0.082(12) 0.006(8) 0.073(12) 0.025(9) C28 0.031(7) 0.057(8) 0.045(8) -0.007(6) 0.009(6) 0.007(6) C29 0.102(14) 0.036(7) 0.100(13) 0.030(8) 0.014(11) 0.033(8) C30 0.089(11) 0.030(6) 0.057(9) 0.021(6) 0.026(8) 0.017(7) S31 0.058(3) 0.037(2) 0.044(2) 0.0138(15) 0.030(2) 0.014(2) S32 0.074(3) 0.034(2) 0.055(2) 0.018(2) 0.045(2) 0.015(2) S33 0.065(3) 0.030(2) 0.054(2) 0.017(2) 0.038(2) 0.013(2) S34 0.059(3) 0.040(2) 0.056(2) 0.018(2) 0.038(2) 0.014(2) S35 0.068(3) 0.049(2) 0.055(2) 0.029(2) 0.035(2) 0.019(2) S36 0.074(3) 0.044(2) 0.071(3) 0.021(2) 0.048(2) 0.026(2) S37 0.062(3) 0.050(2) 0.102(4) 0.040(2) 0.057(3) 0.025(2) S38 0.084(3) 0.053(2) 0.074(3) 0.038(2) 0.059(3) 0.027(2) C31 0.034(7) 0.023(5) 0.072(9) 0.010(6) 0.036(7) 0.003(5) C32 0.033(8) 0.027(5) 0.070(9) 0.028(6) 0.020(7) 0.004(5) C33 0.044(9) 0.073(9) 0.060(9) 0.049(8) 0.029(7) 0.030(7) C34 0.050(8) 0.020(5) 0.038(7) -0.003(5) 0.009(6) 0.024(5) C35 0.045(8) 0.051(7) 0.060(9) 0.033(7) 0.035(7) -0.006(6) C36 0.039(8) 0.029(6) 0.045(7) 0.014(5) 0.019(6) 0.018(5) C37 0.100(14) 0.050(8) 0.083(12) 0.001(7) 0.046(11) -0.026(8) C38 0.092(12) 0.041(7) 0.080(11) 0.027(7) 0.062(10) 0.018(7) C39 0.147(17) 0.065(9) 0.076(11) 0.051(8) 0.072(12) 0.071(10) C40 0.077(11) 0.032(6) 0.058(9) 0.022(6) 0.031(8) 0.002(7) S41 0.064(3) 0.037(2) 0.051(2) 0.015(2) 0.039(2) 0.015(2) S42 0.071(3) 0.045(2) 0.048(2) 0.021(2) 0.037(2) 0.023(2) S43 0.049(2) 0.036(2) 0.051(2) 0.015(2) 0.029(2) 0.010(2) S44 0.054(2) 0.037(2) 0.055(2) 0.018(2) 0.031(2) 0.014(2) S45 0.071(3) 0.049(2) 0.082(3) 0.037(2) 0.050(3) 0.022(2) S46 0.078(3) 0.046(2) 0.071(3) 0.011(2) 0.050(3) 0.024(2) S47 0.064(3) 0.052(2) 0.071(3) 0.034(2) 0.048(2) 0.027(2) S48 0.063(3) 0.042(2) 0.069(3) 0.033(2) 0.045(2) 0.025(2) C41 0.054(9) 0.044(7) 0.036(7) 0.010(5) 0.042(7) 0.016(6) C42 0.078(11) 0.035(7) 0.039(8) 0.006(6) 0.033(8) 0.005(7) C43 0.079(12) 0.045(8) 0.065(10) 0.022(7) 0.043(9) -0.002(8) C44 0.046(8) 0.018(5) 0.024(6) -0.006(4) 0.006(5) 0.014(5) C45 0.050(8) 0.047(7) 0.033(7) 0.015(5) 0.026(6) -0.006(6) C46 0.054(8) 0.019(5) 0.029(6) -0.005(4) 0.008(6) 0.024(5) C47 0.159(21) 0.083(12) 0.109(16) 0.060(11) 0.074(15) 0.039(13) C48 0.055(8) 0.040(6) 0.054(8) -0.001(6) 0.030(7) 0.013(6) S51 0.063(3) 0.036(2) 0.052(2) 0.016(2) 0.039(2) 0.015(2) S52 0.065(3) 0.028(2) 0.055(2) 0.011(2) 0.039(2) 0.012(2) S53 0.048(2) 0.031(2) 0.053(2) 0.012(2) 0.034(2) 0.0068(15) S54 0.060(3) 0.035(2) 0.055(2) 0.015(2) 0.040(2) 0.015(2) S55 0.052(3) 0.049(2) 0.071(3) 0.033(2) 0.030(2) 0.014(2) S56 0.068(3) 0.041(2) 0.077(3) 0.024(2) 0.043(2) 0.023(2) S57 0.072(3) 0.043(2) 0.096(4) 0.025(2) 0.058(3) 0.023(2) S58 0.075(3) 0.049(2) 0.069(3) 0.031(2) 0.048(3) 0.023(2) C51 0.037(8) 0.027(6) 0.046(8) 0.012(5) 0.024(6) 0.003(5) C52 0.046(9) 0.021(5) 0.033(7) 0.008(5) -0.012(6) -0.009(5) C53 0.031(7) 0.039(7) 0.064(9) 0.028(6) 0.028(7) 0.000(5) C54 0.038(8) 0.017(5) 0.050(8) 0.006(5) 0.011(6) 0.012(5) C55 0.050(9) 0.047(7) 0.084(11) 0.026(7) 0.056(8) 0.006(6) C56 0.006(5) 0.020(5) 0.028(6) -0.002(4) -0.001(4) 0.007(4) C59 0.179(22) 0.066(10) 0.114(16) 0.057(10) 0.091(15) 0.071(12) C60 0.056(9) 0.022(5) 0.050(8) 0.003(5) 0.014(7) -0.016(5) N1 0.050(8) 0.064(7) 0.123(12) 0.005(7) 0.026(8) -0.029(6) N2 0.110(12) 0.108(11) 0.121(12) 0.048(9) -0.007(10) 0.015(10) N3 0.165(15) 0.077(8) 0.099(10) 0.060(8) 0.085(11) 0.043(9) N4 0.059(8) 0.085(9) 0.110(10) -0.003(7) 0.030(8) -0.034(7) N5 0.086(9) 0.077(8) 0.105(10) 0.025(7) 0.041(8) 0.039(7) N6 0.123(12) 0.077(8) 0.086(9) 0.042(7) 0.061(9) 0.040(8) N7 0.223(21) 0.153(15) 0.137(13) 0.067(12) 0.148(15) 0.084(14) N8 0.117(13) 0.072(8) 0.087(10) 0.013(7) 0.056(10) 0.025(9) C1 0.079(9) 0.024(5) 0.039(6) 0.008(4) 0.027(6) 0.006(5) C2 0.060(8) 0.047(6) 0.055(7) 0.009(5) 0.016(6) 0.002(6) C3 0.067(8) 0.029(5) 0.066(8) 0.014(5) 0.034(7) 0.002(5) C4 0.051(8) 0.038(6) 0.054(7) 0.011(5) 0.013(6) 0.004(5) C5 0.079(9) 0.025(5) 0.046(6) 0.010(4) 0.017(6) 0.002(5) C6 0.085(10) 0.044(6) 0.068(8) 0.013(5) 0.040(7) 0.019(6) C7 0.049(8) 0.063(7) 0.043(7) -0.011(6) -0.001(6) -0.022(6) C8 0.098(13) 0.086(10) 0.087(11) 0.037(9) 0.028(10) 0.013(9) C9 0.101(13) 0.073(10) 0.087(11) 0.032(9) 0.060(11) 0.023(9) C10 0.048(8) 0.041(6) 0.073(8) -0.011(5) 0.027(7) -0.011(5) C11 0.048(7) 0.066(7) 0.040(6) 0.022(5) 0.019(5) 0.014(6) C12 0.096(11) 0.040(6) 0.058(8) 0.017(6) 0.043(8) 0.020(7) C13 0.139(15) 0.077(9) 0.114(12) 0.049(9) 0.096(12) 0.055(10) C14 0.061(8) 0.044(6) 0.072(8) 0.012(6) 0.035(7) 0.013(6) C61 0.139(21) 0.041(9) 0.160(23) 0.018(11) 0.077(18) 0.023(11) C62 0.167(27) 0.058(13) 0.371(49) 0.004(21) -0.091(29) -0.018(15) C63 0.286(42) 0.188(32) 0.180(32) 0.068(25) 0.082(31) -0.063(29) C64 0.442(61) 0.085(16) 0.294(44) 0.053(23) 0.184(46) 0.134(27) C65 0.260(37) 0.141(23) 0.170(26) 0.041(19) 0.062(25) -0.026(24) C71 0.174(30) 0.086(17) 0.618(76) 0.113(29) 0.228(43) 0.049(19) C72 0.313(46) 0.094(17) 0.205(32) -0.044(19) 0.099(32) 0.023(23) C73 0.165(22) 0.058(10) 0.123(18) 0.023(11) 0.035(16) 0.045(13) C74 0.356(50) 0.101(19) 0.227(35) 0.023(21) -0.052(33) 0.075(27) C75 0.187(32) 0.095(17) 0.376(47) 0.088(22) 0.115(35) 0.008(20) #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S21 C23 1.686(15) . ? S21 C21 1.738(11) . ? S22 C21 1.757(11) . ? S22 C24 1.763(12) . ? S23 C22 1.716(13) . ? S23 C25 1.749(12) . ? S24 C22 1.731(12) . ? S24 C26 1.742(11) . ? S25 C27 1.740(15) . ? S25 C23 1.769(13) . ? S26 C28 1.750(15) . ? S26 C24 1.761(11) . ? S27 C25 1.720(13) . ? S27 C29 1.83(2) . ? S28 C26 1.756(11) . ? S28 C30 1.808(13) . ? C21 C22 1.38(2) . ? C23 C24 1.32(2) . ? C25 C26 1.37(2) . ? C27 C28 1.56(2) . ? C29 C30 1.50(2) . ? S31 C33 1.708(13) . ? S31 C31 1.732(12) . ? S32 C31 1.755(11) . ? S32 C34 1.781(12) . ? S33 C32 1.708(13) . ? S33 C35 1.737(11) . ? S34 C32 1.737(12) . ? S34 C36 1.757(11) . ? S35 C37 1.74(2) . ? S35 C33 1.744(12) . ? S36 C34 1.768(11) . ? S36 C38 1.772(13) . ? S37 C35 1.713(14) . ? S37 C39 1.791(14) . ? S38 C36 1.712(12) . ? S38 C40 1.803(14) . ? C31 C32 1.371(14) . ? C33 C34 1.33(2) . ? C35 C36 1.40(2) . ? C37 C38 1.50(2) . ? C39 C40 1.44(2) . ? S41 C43 1.72(2) . ? S41 C41 1.762(11) . ? S42 C41 1.720(10) . ? S42 C44 1.722(12) . ? S43 C45 1.713(12) . ? S43 C42 1.723(14) . ? S44 C42 1.727(14) . ? S44 C46 1.756(10) . ? S45 C47 1.76(2) . ? S45 C43 1.773(14) . ? S46 C44 1.766(11) . ? S46 C48 1.771(14) . ? S47 C45 1.702(14) . ? S47 C491 1.79(2) . ? S47 C492 1.87(2) . ? S48 C46 1.743(12) . ? S48 C501 1.76(3) . ? S48 C502 1.81(2) . ? C41 C42 1.38(2) . ? C43 C44 1.30(2) . ? C45 C46 1.41(2) . ? C47 C48 1.48(2) . ? C491 C502 1.44(3) . ? C491 C501 1.47(3) . ? C492 C502 1.17(3) . ? C492 C501 1.67(4) . ? S51 C53 1.743(13) . ? S51 C51 1.746(12) . ? S52 C51 1.738(12) . ? S52 C54 1.793(12) . ? S53 C55 1.744(12) . ? S53 C52 1.747(14) . ? S54 C52 1.720(12) . ? S54 C56 1.759(10) . ? S55 C572 1.70(3) . ? S55 C53 1.734(11) . ? S55 C571 1.87(2) . ? S56 C54 1.790(12) . ? S56 C582 1.82(2) . ? S56 C581 1.84(2) . ? S57 C55 1.712(13) . ? S57 C59 1.79(2) . ? S58 C56 1.719(11) . ? S58 C60 1.814(14) . ? C51 C52 1.347(14) . ? C53 C54 1.27(2) . ? C55 C56 1.381(14) . ? C571 C581 1.35(3) . ? C571 C582 1.84(4) . ? C572 C581 1.43(4) . ? C572 C582 1.54(4) . ? C59 C60 1.35(2) . ? N1 C7 1.12(2) . ? N2 C8 1.17(2) . ? N3 C9 1.11(2) . ? N4 C10 1.11(2) . ? N5 C11 1.146(14) . ? N6 C12 1.120(15) . ? N7 C13 1.08(2) . ? N8 C14 1.161(15) . ? C1 C2 1.42(2) . ? C1 C3 1.416(14) . ? C1 C4 1.499(12) . ? C2 C8 1.41(2) . ? C2 C7 1.48(2) . ? C3 C10 1.38(2) . ? C3 C9 1.45(2) . ? C4 C5 1.40(2) . ? C4 C11 1.42(2) . ? C5 C6 1.40(2) . ? C5 C12 1.468(14) . ? C6 C14 1.403(15) . ? C6 C13 1.43(2) . ? C61 C62 1.15(4) . ? C61 C65 1.24(3) . ? C62 C63 1.55(4) . ? C63 C64 1.27(4) . ? C64 C65 1.49(4) . ? C71 C75 1.16(3) . ? C71 C72 1.65(4) . ? C72 C73 1.22(3) . ? C73 C74 1.17(3) . ? C74 C75 1.66(4) . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 S21 C21 95.4(6) . . ? C21 S22 C24 94.2(6) . . ? C22 S23 C25 95.5(6) . . ? C22 S24 C26 93.1(6) . . ? C27 S25 C23 102.3(7) . . ? C28 S26 C24 104.5(6) . . ? C25 S27 C29 99.3(7) . . ? C26 S28 C30 101.3(6) . . ? C22 C21 S21 123.0(9) . . ? C22 C21 S22 122.7(9) . . ? S21 C21 S22 114.3(7) . . ? C21 C22 S23 120.1(9) . . ? C21 C22 S24 122.7(10) . . ? S23 C22 S24 117.1(7) . . ? C24 C23 S21 120.0(10) . . ? C24 C23 S25 123.0(11) . . ? S21 C23 S25 117.0(8) . . ? C23 C24 S26 131.5(10) . . ? C23 C24 S22 115.9(9) . . ? S26 C24 S22 112.4(7) . . ? C26 C25 S27 130.6(9) . . ? C26 C25 S23 114.1(9) . . ? S27 C25 S23 115.3(7) . . ? C25 C26 S24 119.3(9) . . ? C25 C26 S28 126.2(9) . . ? S24 C26 S28 114.4(7) . . ? C28 C27 S25 115.7(12) . . ? C27 C28 S26 114.8(10) . . ? C30 C29 S27 112.6(11) . . ? C29 C30 S28 111.4(11) . . ? C33 S31 C31 97.5(6) . . ? C31 S32 C34 94.4(6) . . ? C32 S33 C35 95.5(6) . . ? C32 S34 C36 94.4(6) . . ? C37 S35 C33 100.0(7) . . ? C34 S36 C38 102.0(6) . . ? C35 S37 C39 101.9(6) . . ? C36 S38 C40 98.9(6) . . ? C32 C31 S31 123.0(8) . . ? C32 C31 S32 122.9(9) . . ? S31 C31 S32 113.7(6) . . ? C31 C32 S33 121.9(9) . . ? C31 C32 S34 120.4(9) . . ? S33 C32 S34 117.5(6) . . ? C34 C33 S31 117.1(9) . . ? C34 C33 S35 125.8(10) . . ? S31 C33 S35 117.1(8) . . ? C33 C34 S36 131.2(10) . . ? C33 C34 S32 117.2(8) . . ? S36 C34 S32 111.6(8) . . ? C36 C35 S37 127.5(8) . . ? C36 C35 S33 116.4(9) . . ? S37 C35 S33 116.1(7) . . ? C35 C36 S38 128.6(8) . . ? C35 C36 S34 115.9(9) . . ? S38 C36 S34 115.4(7) . . ? C38 C37 S35 118.8(11) . . ? C37 C38 S36 115.1(11) . . ? C40 C39 S37 117.6(11) . . ? C39 C40 S38 113.7(10) . . ? C43 S41 C41 94.1(6) . . ? C41 S42 C44 95.1(6) . . ? C45 S43 C42 96.5(6) . . ? C42 S44 C46 94.0(6) . . ? C47 S45 C43 103.0(8) . . ? C44 S46 C48 103.3(6) . . ? C45 S47 C491 106.2(8) . . ? C45 S47 C492 101.9(8) . . ? C46 S48 C501 100.9(9) . . ? C46 S48 C502 100.8(7) . . ? C42 C41 S42 124.4(9) . . ? C42 C41 S41 121.1(8) . . ? S42 C41 S41 114.5(7) . . ? C41 C42 S43 122.2(10) . . ? C41 C42 S44 120.7(10) . . ? S43 C42 S44 116.9(8) . . ? C44 C43 S41 118.1(10) . . ? C44 C43 S45 127.7(11) . . ? S41 C43 S45 114.2(8) . . ? C43 C44 S42 118.1(9) . . ? C43 C44 S46 128.6(10) . . ? S42 C44 S46 113.3(7) . . ? C46 C45 S47 126.6(9) . . ? C46 C45 S43 115.1(10) . . ? S47 C45 S43 118.2(7) . . ? C45 C46 S48 128.6(8) . . ? C45 C46 S44 117.3(9) . . ? S48 C46 S44 114.0(7) . . ? C48 C47 S45 117.5(14) . . ? C47 C48 S46 118.6(11) . . ? C502 C491 S47 113.8(16) . . ? C501 C491 S47 121.4(17) . . ? C502 C492 S47 125.3(18) . . ? C501 C492 S47 106.9(16) . . ? C491 C501 S48 126.6(22) . . ? C492 C501 S48 104.6(21) . . ? C492 C502 S48 130.4(16) . . ? C491 C502 S48 124.8(15) . . ? C53 S51 C51 96.7(5) . . ? C51 S52 C54 93.8(6) . . ? C55 S53 C52 95.4(5) . . ? C52 S54 C56 95.7(6) . . ? C572 S55 C53 107.4(12) . . ? C53 S55 C571 98.3(7) . . ? C54 S56 C582 99.8(8) . . ? C54 S56 C581 100.6(9) . . ? C55 S57 C59 99.0(7) . . ? C56 S58 C60 99.1(6) . . ? C52 C51 S52 121.5(9) . . ? C52 C51 S51 125.0(9) . . ? S52 C51 S51 113.5(6) . . ? C51 C52 S54 121.4(10) . . ? C51 C52 S53 122.6(9) . . ? S54 C52 S53 116.0(6) . . ? C54 C53 S55 128.0(10) . . ? C54 C53 S51 116.1(9) . . ? S55 C53 S51 115.8(7) . . ? C53 C54 S56 130.6(10) . . ? C53 C54 S52 119.4(9) . . ? S56 C54 S52 110.0(7) . . ? C56 C55 S57 128.4(9) . . ? C56 C55 S53 116.6(9) . . ? S57 C55 S53 115.0(7) . . ? C55 C56 S58 128.5(8) . . ? C55 C56 S54 116.2(8) . . ? S58 C56 S54 115.3(6) . . ? C581 C571 S55 117.6(19) . . ? C582 C571 S55 98.8(13) . . ? C581 C572 S55 124.1(23) . . ? C582 C572 S55 120.8(20) . . ? C571 C581 S56 119.7(18) . . ? C572 C581 S56 125.5(21) . . ? C572 C582 S56 119.8(22) . . ? S56 C582 C571 98.2(15) . . ? C60 C59 S57 123.4(13) . . ? C59 C60 S58 113.1(10) . . ? C2 C1 C3 126.6(10) . . ? C2 C1 C4 116.8(10) . . ? C3 C1 C4 116.6(11) . . ? C8 C2 C1 123.3(11) . . ? C8 C2 C7 116.2(12) . . ? C1 C2 C7 120.5(9) . . ? C10 C3 C1 121.2(10) . . ? C10 C3 C9 116.4(11) . . ? C1 C3 C9 122.5(13) . . ? C5 C4 C11 120.9(9) . . ? C5 C4 C1 125.0(10) . . ? C11 C4 C1 114.2(9) . . ? C6 C5 C4 132.0(10) . . ? C6 C5 C12 114.5(10) . . ? C4 C5 C12 113.5(11) . . ? C5 C6 C14 123.9(11) . . ? C5 C6 C13 118.5(10) . . ? C14 C6 C13 117.2(11) . . ? N1 C7 C2 178.0(16) . . ? N2 C8 C2 171.5(19) . . ? N3 C9 C3 174.2(19) . . ? N4 C10 C3 177.1(13) . . ? N5 C11 C4 177.8(13) . . ? N6 C12 C5 179.8(14) . . ? N7 C13 C6 176.1(23) . . ? N8 C14 C6 174.7(15) . . ? C62 C61 C65 98.9(21) . . ? C61 C62 C63 119.0(29) . . ? C64 C63 C62 85.8(28) . . ? C63 C64 C65 100.6(27) . . ? C61 C65 C64 108.4(29) . . ? C75 C71 C72 90.4(29) . . ? C73 C72 C71 95.8(26) . . ? C74 C73 C72 103.9(22) . . ? C73 C74 C75 106.7(28) . . ? C71 C75 C74 77.7(30) . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S23 S58 3.474(6) . 1_455 ? S24 S37 3.503(6) . 1_554 ? S26 S31 3.554(6) . 1_554 ? S26 S35 3.442(6) . 1_554 ? S27 S58 3.373(6) . 1_455 ? S28 S37 3.519(7) . 1_554 ? S35 N6 3.252(14) . 1_556 ? S36 S45 3.462(6) . . ? S38 S43 3.449(6) . . ? S38 S47 3.305(6) . . ? S46 S55 3.509(7) . 1_554 ? S48 N3 3.053(15) . 1_564 ? S48 S57 3.410(7) . 1_554 ? H27A N5 2.6736 . . ? H28A N6 2.5334 . . ? H30A N4 2.6095 . 1_565 ? H30B N2 2.6091 . 1_464 ? H37A N7 2.5227 . 1_464 ? H37B N5 2.6441 . . ? H47A N1 2.7358 . . ? H59B N3 2.6289 . 1_565 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_ET2 #------------------------------------------------------------------------------ _chemical_name_common ? _chemical_formula_moiety '2(C10 H8 S8 1+),2(C10 H8 S8), C14 N8 2-, 2(C4 H8 O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H48 N8 O2 S32' _chemical_formula_weight 1963.23 _chemical_melting_point ? _chemical_compound_source 'Local laboratory' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.365(7) _cell_length_b 21.369(9) _cell_length_c 12.961(5) _cell_angle_alpha 99.92(3) _cell_angle_beta 105.22(5) _cell_angle_gamma 77.02(5) _cell_volume 3972(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 1.639 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'flotation in mixture of CHCl3 and CCl4' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC-5' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7660 _diffrn_reflns_av_R_equivalents 0.0102 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 20.50 _reflns_number_total 7109 _reflns_number_observed 3806 _reflns_observed_criterion >sigma(F) #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku MSC/AFC diffractometer software' _computing_cell_refinement 'Rigaku MSC/AFC diffractometer software' _computing_data_reduction ? _computing_structure_solution 'SIR-92 for Crystan6.3.3 (MacScience, 1995)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _computing_publication_material ? #------------------------------------------------------------------------------ _refine_special_details ; Refinement on F^2^ using reflections with F^2^ > 2.0 sigma(F^2^). Weighted R-factors wR and goodnesses of fit S are based on F^2^, conventional R-factors R are based on F. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4946 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1423 _refine_ls_R_factor_obs 0.0603 _refine_ls_wR_factor_all 1.1870 _refine_ls_wR_factor_obs 0.1764 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.195 _refine_ls_restrained_S_all 5.508 _refine_ls_restrained_S_obs 1.195 _refine_ls_shift/esd_max 0.073 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 0.411 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.096 #------------------------------------------------------------------------------ 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S21 S 0.1399(2) 0.66253(14) 0.5494(2) 0.0434(9) Uani 1 d . . S22 S 0.1536(2) 0.66207(14) 0.3284(2) 0.0398(9) Uani 1 d . . S23 S 0.1323(2) 0.50932(14) 0.4993(2) 0.0447(9) Uani 1 d . . S24 S 0.1426(2) 0.51098(14) 0.2776(2) 0.0419(9) Uani 1 d . . S25 S 0.1196(2) 0.80362(14) 0.6066(2) 0.0507(9) Uani 1 d . . S26 S 0.1415(2) 0.80254(14) 0.3440(2) 0.0480(9) Uani 1 d . . S27 S 0.0902(2) 0.3796(2) 0.4659(2) 0.0536(10) Uani 1 d . . S28 S 0.1061(2) 0.3793(2) 0.2017(2) 0.0523(10) Uani 1 d . . C21 C 0.1437(7) 0.6183(5) 0.4223(7) 0.025(3) Uani 1 d . . C22 C 0.1383(7) 0.5545(5) 0.4038(8) 0.031(3) Uani 1 d . . C23 C 0.1348(7) 0.7376(5) 0.5092(9) 0.035(3) Uani 1 d . . C24 C 0.1424(7) 0.7369(5) 0.4078(8) 0.035(3) Uani 1 d . . C25 C 0.1105(7) 0.4396(5) 0.4098(8) 0.029(3) Uani 1 d . . C26 C 0.1176(7) 0.4410(5) 0.3085(8) 0.034(3) Uani 1 d . . C271 C 0.1389(26) 0.8698(10) 0.5377(18) 0.041(11) Uiso 0.52(6) d P 1 C272 C 0.0821(32) 0.8656(13) 0.5307(22) 0.057(13) Uiso 0.48(6) d P 2 C28 C 0.0962(13) 0.8657(6) 0.4292(12) 0.101(6) Uani 1 d . . C29 C 0.0737(10) 0.3193(6) 0.3560(10) 0.069(4) Uani 1 d . . C30 C 0.1287(9) 0.3120(6) 0.2757(10) 0.060(4) Uani 1 d . . H27A H 0.1157 0.9113 0.5726 0.050 Uiso 0.52 calc P 1 H27B H 0.2036 0.8666 0.5460 0.050 Uiso 0.52 calc P 1 H28A H 0.0960 0.9054 0.4040 0.050 Uiso 0.52 calc P 1 H28B H 0.0333 0.8631 0.4222 0.050 Uiso 0.52 calc P 1 H27C H 0.0168 0.8763 0.5228 0.050 Uiso 0.48 calc P 2 H27D H 0.1062 0.9017 0.5747 0.050 Uiso 0.48 calc P 2 H28C H 0.1334 0.8977 0.4387 0.050 Uiso 0.48 calc P 2 H28D H 0.0371 0.8834 0.3872 0.050 Uiso 0.48 calc P 2 H29A H 0.0856 0.2787 0.3838 0.050 Uiso 1 calc . . H29B H 0.0100 0.3275 0.3192 0.050 Uiso 1 calc . . H30A H 0.1178 0.2743 0.2257 0.050 Uiso 1 calc . . H30B H 0.1925 0.3046 0.3119 0.050 Uiso 1 calc . . S31 S 0.3839(2) 0.63172(14) 0.7769(2) 0.0420(9) Uani 1 d . . S32 S 0.3958(2) 0.62972(14) 0.5550(2) 0.0416(9) Uani 1 d . . S33 S 0.3727(2) 0.47931(14) 0.7301(2) 0.0413(9) Uani 1 d . . S34 S 0.3907(2) 0.47734(14) 0.5097(2) 0.0424(9) Uani 1 d . . S35 S 0.3704(2) 0.77218(14) 0.8349(2) 0.0460(9) Uani 1 d . . S36 S 0.3833(2) 0.77124(14) 0.5678(2) 0.0434(9) Uani 1 d . . S37 S 0.3487(2) 0.34502(14) 0.7035(2) 0.0477(9) Uani 1 d . . S38 S 0.3727(2) 0.34178(14) 0.4410(2) 0.0489(9) Uani 1 d . . C31 C 0.3869(7) 0.5872(5) 0.6527(7) 0.027(3) Uani 1 d . . C32 C 0.3825(7) 0.5229(5) 0.6331(8) 0.030(3) Uani 1 d . . C33 C 0.3793(7) 0.7059(5) 0.7359(8) 0.033(3) Uani 1 d . . C34 C 0.3846(7) 0.7059(5) 0.6336(8) 0.034(3) Uani 1 d . . C35 C 0.3650(7) 0.4073(5) 0.6450(8) 0.036(3) Uani 1 d . . C36 C 0.3743(7) 0.4068(5) 0.5432(8) 0.034(3) Uani 1 d . . C37 C 0.3596(8) 0.8390(5) 0.7642(8) 0.046(3) Uani 1 d . . C38 C 0.4186(8) 0.8264(6) 0.6854(9) 0.050(3) Uani 1 d . . C39 C 0.3261(8) 0.2861(5) 0.5898(9) 0.048(3) Uani 1 d . . C40 C 0.3889(8) 0.2748(6) 0.5141(9) 0.054(4) Uani 1 d . . H37A H 0.2966 0.8507 0.7265 0.050 Uiso 1 calc . . H37B H 0.3749 0.8753 0.8155 0.050 Uiso 1 calc . . H38A H 0.4804 0.8092 0.7212 0.050 Uiso 1 calc . . H38B H 0.4190 0.8668 0.6628 0.050 Uiso 1 calc . . H39A H 0.3297 0.2457 0.6153 0.050 Uiso 1 calc . . H39B H 0.2642 0.2989 0.5499 0.050 Uiso 1 calc . . H40A H 0.3784 0.2371 0.4640 0.050 Uiso 1 calc . . H40B H 0.4515 0.2665 0.5547 0.050 Uiso 1 calc . . S41 S 0.6242(2) 0.59583(14) 1.0161(2) 0.0461(9) Uani 1 d . . S42 S 0.6448(2) 0.59348(14) 0.7967(2) 0.0459(9) Uani 1 d . . S43 S 0.6119(2) 0.44402(14) 0.9664(2) 0.0416(9) Uani 1 d . . S44 S 0.6320(2) 0.44226(13) 0.7474(2) 0.0410(9) Uani 1 d . . S45 S 0.6279(2) 0.73479(14) 1.0802(2) 0.0466(9) Uani 1 d . . S46 S 0.6536(2) 0.73118(15) 0.8174(2) 0.0492(9) Uani 1 d . . S47 S 0.6038(2) 0.30665(14) 0.9452(2) 0.0463(9) Uani 1 d . . S48 S 0.6263(2) 0.30491(14) 0.6824(2) 0.0459(9) Uani 1 d . . C41 C 0.6308(7) 0.5504(5) 0.8920(8) 0.038(3) Uani 1 d . . C42 C 0.6261(7) 0.4860(5) 0.8718(8) 0.035(3) Uani 1 d . . C43 C 0.6349(7) 0.6686(5) 0.9820(8) 0.037(3) Uani 1 d . . C44 C 0.6428(7) 0.6679(5) 0.8790(8) 0.033(3) Uani 1 d . . C45 C 0.6138(7) 0.3699(5) 0.8844(8) 0.028(3) Uani 1 d . . C46 C 0.6224(7) 0.3702(5) 0.7834(8) 0.032(3) Uani 1 d . . C47 C 0.6030(8) 0.8016(5) 1.0009(9) 0.051(3) Uani 1 d . . C48 C 0.6697(8) 0.7938(6) 0.9300(9) 0.052(4) Uani 1 d . . C49 C 0.5843(9) 0.2455(6) 0.8316(10) 0.062(4) Uani 1 d . . C50 C 0.6406(9) 0.2383(6) 0.7541(9) 0.058(4) Uani 1 d . . H47A H 0.5418 0.8045 0.9566 0.050 Uiso 1 calc . . H47B H 0.6057 0.8412 1.0485 0.050 Uiso 1 calc . . H48A H 0.7312 0.7838 0.9729 0.050 Uiso 1 calc . . H48B H 0.6630 0.8341 0.9030 0.050 Uiso 1 calc . . H49A H 0.5943 0.2046 0.8584 0.050 Uiso 1 calc . . H49B H 0.5209 0.2550 0.7942 0.050 Uiso 1 calc . . H50A H 0.6283 0.2014 0.7025 0.050 Uiso 1 calc . . H50B H 0.7039 0.2286 0.7917 0.050 Uiso 1 calc . . S51 S 0.8771(2) 0.56592(14) 1.2530(2) 0.0457(9) Uani 1 d . . S52 S 0.8864(2) 0.56521(14) 1.0305(2) 0.0434(9) Uani 1 d . . S53 S 0.8495(2) 0.41715(14) 1.1982(2) 0.0404(9) Uani 1 d . . S54 S 0.8704(2) 0.41558(15) 0.9798(2) 0.0423(9) Uani 1 d . . S55 S 0.8886(2) 0.70322(15) 1.3202(2) 0.0527(10) Uani 1 d . . S56 S 0.9001(2) 0.70168(14) 1.0520(2) 0.0469(9) Uani 1 d . . S57 S 0.8402(2) 0.28053(15) 1.1771(2) 0.0513(10) Uani 1 d . . S58 S 0.8616(2) 0.27715(15) 0.9154(2) 0.0449(9) Uani 1 d . . C51 C 0.8750(7) 0.5221(5) 1.1246(8) 0.033(3) Uani 1 d . . C52 C 0.8652(7) 0.4588(5) 1.1041(8) 0.035(3) Uani 1 d . . C53 C 0.8860(7) 0.6393(5) 1.2174(9) 0.038(3) Uani 1 d . . C54 C 0.8905(7) 0.6399(5) 1.1156(9) 0.034(3) Uani 1 d . . C55 C 0.8508(7) 0.3432(5) 1.1153(8) 0.033(3) Uani 1 d . . C56 C 0.8582(7) 0.3431(5) 1.0145(8) 0.035(3) Uani 1 d . . C57 C 0.8653(9) 0.7693(6) 1.2433(10) 0.061(4) Uani 1 d . . C58 C 0.9184(9) 0.7646(6) 1.1629(10) 0.061(4) Uani 1 d . . C59 C 0.8493(9) 0.2116(5) 1.0744(10) 0.055(4) Uani 1 d . . C60 C 0.9061(8) 0.2145(5) 0.9978(9) 0.051(3) Uani 1 d . . H57A H 0.8014 0.7756 1.2071 0.050 Uiso 1 calc . . H57B H 0.8745 0.8075 1.2928 0.050 Uiso 1 calc . . H58A H 0.9825 0.7575 1.1983 0.050 Uiso 1 calc . . H58B H 0.9038 0.8053 1.1346 0.050 Uiso 1 calc . . H59A H 0.8752 0.1733 1.1094 0.050 Uiso 1 calc . . H59B H 0.7886 0.2075 1.0335 0.050 Uiso 1 calc . . H60A H 0.9122 0.1740 0.9525 0.050 Uiso 1 calc . . H60B H 0.9666 0.2196 1.0386 0.050 Uiso 1 calc . . N1 N 0.3415(8) -0.1004(5) 0.4482(8) 0.067(3) Uani 1 d . . N2 N 0.1162(10) 0.0367(7) 0.5533(11) 0.108(5) Uani 1 d . . N3 N 0.1412(9) 0.1804(6) 0.4962(10) 0.090(4) Uani 1 d . . N4 N 0.1217(9) 0.1564(6) 0.1520(10) 0.095(5) Uani 1 d . . N5 N 0.2060(8) -0.1053(6) 0.1618(9) 0.081(4) Uani 1 d . . N6 N 0.3685(8) 0.1345(6) 0.3143(9) 0.073(4) Uani 1 d . . N7 N 0.4814(10) 0.0626(6) 0.0934(10) 0.099(5) Uani 1 d . . N8 N 0.3632(11) -0.1116(7) 0.0219(10) 0.112(5) Uani 1 d . . C1 C 0.2127(7) 0.0384(5) 0.3309(8) 0.033(3) Uani 1 d . . C2 C 0.2208(8) 0.0014(6) 0.4154(9) 0.046(3) Uani 1 d . . C3 C 0.1682(7) 0.1018(5) 0.3261(9) 0.044(3) Uani 1 d . . C4 C 0.2564(8) 0.0034(5) 0.2433(8) 0.038(3) Uani 1 d . . C5 C 0.3191(8) 0.0287(5) 0.2090(8) 0.041(3) Uani 1 d . . C6 C 0.3686(10) 0.0017(6) 0.1287(9) 0.058(4) Uani 1 d . . C7 C 0.2877(9) -0.0556(7) 0.4337(9) 0.044(3) Uani 1 d . . C8 C 0.1628(11) 0.0233(7) 0.4930(13) 0.078(4) Uani 1 d . . C9 C 0.1511(8) 0.1455(6) 0.4232(10) 0.053(4) Uani 1 d . . C10 C 0.1427(9) 0.1300(6) 0.2269(11) 0.061(4) Uani 1 d . . C11 C 0.2307(8) -0.0579(6) 0.1964(9) 0.048(3) Uani 1 d . . C12 C 0.3446(9) 0.0870(7) 0.2706(10) 0.053(4) Uani 1 d . . C13 C 0.4341(12) 0.0344(7) 0.1098(11) 0.071(4) Uani 1 d . . C14 C 0.3618(10) -0.0612(7) 0.0689(10) 0.063(4) Uani 1 d . . C61 C 0.6048(16) -0.1444(8) 0.2717(15) 0.098(7) Uani 1 d . . C62 C 0.6499(21) -0.1034(14) 0.2752(21) 0.198(13) Uani 1 d . . C63 C 0.6117(17) -0.0390(10) 0.3211(20) 0.149(8) Uani 1 d . . C64 C 0.5567(15) -0.0602(17) 0.3881(18) 0.180(12) Uani 1 d . . C65 C 0.5421(19) -0.1238(14) 0.3318(24) 0.174(10) Uani 1 d . . C71 C 0.0593(32) 0.0584(20) 0.8249(32) 0.246(20) Uani 1 d . . C72 C 0.1514(25) 0.0436(20) 0.8658(35) 0.221(14) Uani 1 d . . C73 C 0.1583(24) -0.0324(17) 0.8277(23) 0.211(15) Uani 1 d . . C74 C 0.0744(31) -0.0419(19) 0.7924(21) 0.235(21) Uani 1 d . . C75 C 0.0676(45) 0.0151(34) 0.8954(39) 0.373(32) Uani 1 d . . #------------------------------------------------------------------------------ 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 S21 0.058(2) 0.045(2) 0.031(2) -0.0050(15) 0.018(2) -0.016(2) S22 0.056(2) 0.036(2) 0.033(2) -0.0037(14) 0.021(2) -0.014(2) S23 0.067(2) 0.041(2) 0.029(2) -0.0025(14) 0.018(2) -0.013(2) S24 0.066(2) 0.037(2) 0.028(2) -0.0028(14) 0.021(2) -0.013(2) S25 0.068(2) 0.044(2) 0.039(2) -0.012(2) 0.019(2) -0.013(2) S26 0.067(2) 0.038(2) 0.040(2) 0.0016(15) 0.015(2) -0.012(2) S27 0.078(3) 0.050(2) 0.044(2) 0.008(2) 0.027(2) -0.017(2) S28 0.083(3) 0.047(2) 0.031(2) -0.005(2) 0.017(2) -0.022(2) C21 0.029(7) 0.022(7) 0.027(6) -0.007(5) 0.012(5) -0.011(5) C22 0.035(7) 0.037(7) 0.026(6) -0.005(5) 0.014(5) -0.017(6) C23 0.031(8) 0.033(7) 0.034(7) -0.006(6) 0.003(6) -0.005(6) C24 0.038(8) 0.034(7) 0.032(7) -0.006(5) 0.010(6) -0.009(6) C25 0.031(7) 0.027(7) 0.026(7) -0.004(5) 0.009(5) -0.004(5) C26 0.024(7) 0.042(7) 0.033(7) 0.003(6) 0.007(6) -0.001(5) C28 0.174(17) 0.055(10) 0.091(12) 0.029(8) 0.074(13) 0.010(10) C29 0.090(11) 0.079(10) 0.045(9) 0.011(7) 0.003(8) -0.041(9) C30 0.073(10) 0.060(9) 0.060(9) -0.022(7) 0.039(8) -0.033(8) S31 0.065(2) 0.039(2) 0.024(2) -0.0029(14) 0.016(2) -0.012(2) S32 0.058(2) 0.041(2) 0.029(2) -0.0035(14) 0.020(2) -0.009(2) S33 0.063(2) 0.039(2) 0.023(2) -0.0029(14) 0.017(2) -0.010(2) S34 0.065(2) 0.043(2) 0.022(2) -0.0043(14) 0.017(2) -0.015(2) S35 0.071(3) 0.045(2) 0.030(2) -0.0076(15) 0.025(2) -0.020(2) S36 0.068(2) 0.038(2) 0.029(2) 0.0004(14) 0.018(2) -0.015(2) S37 0.071(2) 0.042(2) 0.038(2) 0.0032(15) 0.025(2) -0.012(2) S38 0.076(3) 0.043(2) 0.031(2) -0.0101(15) 0.018(2) -0.021(2) C31 0.028(7) 0.030(7) 0.021(6) 0.007(5) 0.003(5) -0.005(5) C32 0.028(7) 0.027(7) 0.036(7) 0.000(5) 0.008(6) -0.009(5) C33 0.028(7) 0.050(7) 0.022(7) -0.014(5) 0.015(5) -0.011(6) C34 0.042(8) 0.033(7) 0.029(7) -0.011(5) 0.020(6) -0.010(6) C35 0.016(7) 0.047(8) 0.040(8) 0.002(6) 0.009(6) 0.005(6) C36 0.036(8) 0.044(7) 0.024(7) 0.002(6) 0.016(6) -0.003(6) C37 0.051(8) 0.056(8) 0.028(7) -0.012(6) 0.010(6) -0.014(7) C38 0.061(9) 0.058(8) 0.036(7) 0.010(6) -0.002(7) -0.033(7) C39 0.050(9) 0.036(7) 0.058(8) 0.013(6) 0.005(7) -0.011(6) C40 0.056(9) 0.060(9) 0.052(8) 0.005(7) 0.015(7) -0.020(7) S41 0.069(3) 0.043(2) 0.032(2) -0.0039(15) 0.023(2) -0.014(2) S42 0.066(2) 0.043(2) 0.031(2) -0.0016(15) 0.020(2) -0.010(2) S43 0.060(2) 0.039(2) 0.028(2) -0.0011(14) 0.016(2) -0.010(2) S44 0.065(2) 0.037(2) 0.026(2) -0.0001(14) 0.020(2) -0.012(2) S45 0.066(2) 0.044(2) 0.034(2) -0.0107(15) 0.023(2) -0.018(2) S46 0.068(2) 0.045(2) 0.042(2) 0.001(2) 0.028(2) -0.012(2) S47 0.069(2) 0.042(2) 0.034(2) 0.0026(15) 0.022(2) -0.013(2) S48 0.070(3) 0.044(2) 0.032(2) -0.0094(15) 0.025(2) -0.023(2) C41 0.028(7) 0.048(8) 0.037(7) -0.002(6) 0.014(6) -0.004(6) C42 0.038(8) 0.043(8) 0.020(6) -0.009(6) 0.010(6) -0.007(6) C43 0.029(8) 0.059(8) 0.027(7) -0.009(6) 0.012(6) -0.020(6) C44 0.028(7) 0.037(7) 0.031(7) -0.006(5) 0.005(6) -0.009(6) C45 0.033(7) 0.027(6) 0.018(6) -0.005(5) 0.003(5) -0.003(5) C46 0.038(8) 0.037(7) 0.022(7) 0.000(5) 0.012(6) -0.005(6) C47 0.053(9) 0.038(8) 0.055(8) -0.007(6) 0.014(7) -0.002(6) C48 0.055(9) 0.063(9) 0.033(7) 0.004(6) 0.003(7) -0.014(7) C49 0.064(10) 0.058(9) 0.066(9) -0.010(7) 0.025(8) -0.016(7) C50 0.076(10) 0.066(9) 0.036(7) -0.020(6) 0.033(7) -0.018(8) S51 0.069(2) 0.040(2) 0.031(2) -0.0006(15) 0.018(2) -0.011(2) S52 0.068(2) 0.039(2) 0.026(2) 0.0005(14) 0.014(2) -0.014(2) S53 0.059(2) 0.038(2) 0.025(2) 0.0020(14) 0.018(2) -0.003(2) S54 0.053(2) 0.055(2) 0.022(2) -0.0015(15) 0.014(2) -0.013(2) S55 0.081(3) 0.048(2) 0.035(2) -0.012(2) 0.026(2) -0.022(2) S56 0.062(2) 0.044(2) 0.041(2) -0.004(2) 0.022(2) -0.020(2) S57 0.079(3) 0.045(2) 0.039(2) 0.000(2) 0.020(2) -0.026(2) S58 0.051(2) 0.054(2) 0.030(2) -0.012(2) 0.013(2) -0.020(2) C51 0.037(8) 0.036(7) 0.021(6) 0.000(5) 0.006(5) -0.001(6) C52 0.030(7) 0.042(8) 0.034(7) 0.001(6) 0.012(6) -0.007(6) C53 0.030(8) 0.049(8) 0.038(8) 0.002(6) 0.015(6) -0.006(6) C54 0.029(7) 0.036(7) 0.039(7) -0.005(6) 0.018(6) -0.006(6) C55 0.034(8) 0.040(7) 0.020(7) -0.008(5) 0.005(6) -0.008(6) C56 0.021(7) 0.058(8) 0.027(7) -0.003(6) 0.003(6) -0.016(6) C57 0.077(10) 0.045(8) 0.067(9) -0.009(7) 0.032(8) -0.018(7) C58 0.087(11) 0.047(8) 0.054(9) -0.003(7) 0.028(8) -0.017(8) C59 0.068(10) 0.040(8) 0.065(9) 0.004(7) 0.029(8) -0.012(7) C60 0.057(9) 0.034(7) 0.050(8) -0.020(6) 0.015(7) -0.004(6) N1 0.075(9) 0.054(8) 0.061(7) 0.013(6) 0.011(7) 0.006(7) N2 0.131(13) 0.107(11) 0.111(12) 0.003(9) 0.089(11) -0.007(9) N3 0.128(12) 0.055(8) 0.074(9) -0.018(7) 0.029(8) 0.000(7) N4 0.124(12) 0.066(9) 0.061(9) 0.017(7) -0.020(8) 0.010(8) N5 0.096(10) 0.068(9) 0.081(9) -0.019(7) 0.022(7) -0.039(8) N6 0.092(10) 0.070(9) 0.074(8) -0.013(7) 0.046(7) -0.036(7) N7 0.147(13) 0.063(9) 0.123(12) 0.006(8) 0.097(11) -0.020(9) N8 0.174(15) 0.104(12) 0.077(10) -0.039(8) 0.075(10) -0.047(11) C1 0.041(8) 0.029(7) 0.030(7) 0.009(6) 0.000(6) -0.011(6) C2 0.043(9) 0.056(9) 0.038(7) -0.026(7) 0.021(7) -0.015(7) C3 0.041(8) 0.027(7) 0.059(9) 0.005(6) 0.006(7) -0.004(6) C4 0.041(8) 0.041(8) 0.033(7) 0.005(6) 0.008(6) -0.008(6) C5 0.056(9) 0.045(8) 0.017(6) -0.006(6) 0.006(6) -0.008(7) C6 0.096(12) 0.039(8) 0.038(8) -0.015(6) 0.029(8) -0.009(8) C7 0.032(9) 0.059(9) 0.039(8) -0.001(7) 0.003(6) -0.014(8) C8 0.073(12) 0.078(11) 0.076(11) 0.011(9) 0.005(10) -0.014(9) C9 0.057(10) 0.042(8) 0.050(9) -0.009(7) 0.007(7) -0.006(7) C10 0.059(10) 0.049(9) 0.055(10) -0.007(8) 0.006(8) 0.011(7) C11 0.060(10) 0.044(9) 0.041(8) 0.002(7) 0.017(7) -0.007(7) C12 0.063(10) 0.062(10) 0.039(8) -0.005(7) 0.024(7) -0.017(8) C13 0.111(14) 0.059(10) 0.065(10) 0.002(8) 0.054(10) -0.025(10) C14 0.089(11) 0.065(10) 0.046(9) 0.008(8) 0.036(8) -0.010(9) C61 0.144(20) 0.044(11) 0.086(13) -0.039(10) 0.032(13) -0.009(11) C62 0.256(34) 0.117(22) 0.190(25) -0.097(20) 0.078(23) -0.028(22) C63 0.152(22) 0.105(18) 0.147(20) -0.005(15) -0.038(16) -0.037(16) C64 0.112(18) 0.269(35) 0.148(21) -0.062(22) 0.078(16) -0.020(20) C65 0.186(28) 0.148(23) 0.167(25) -0.024(19) -0.015(20) -0.086(21) C71 0.190(33) 0.284(45) 0.246(38) 0.159(34) 0.058(32) 0.098(32) C72 0.164(30) 0.210(38) 0.272(42) -0.010(29) 0.033(30) -0.054(29) C73 0.220(33) 0.156(27) 0.162(25) -0.017(20) 0.018(24) 0.100(24) C74 0.369(47) 0.285(42) 0.087(17) -0.047(21) -0.012(25) -0.267(41) C75 0.362(65) 0.584(98) 0.231(46) 0.123(54) 0.205(46) 0.008(67) #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S21 C23 1.749(11) . ? S21 C21 1.760(9) . ? S22 C21 1.713(10) . ? S22 C24 1.745(10) . ? S23 C22 1.727(10) . ? S23 C25 1.761(10) . ? S24 C22 1.746(10) . ? S24 C26 1.757(11) . ? S25 C272 1.69(3) . ? S25 C23 1.742(10) . ? S25 C271 1.91(3) . ? S26 C28 1.731(14) . ? S26 C24 1.743(11) . ? S27 C25 1.701(10) . ? S27 C29 1.754(13) . ? S28 C26 1.743(11) . ? S28 C30 1.784(13) . ? C21 C22 1.361(13) . ? C23 C24 1.347(13) . ? C25 C26 1.352(13) . ? C271 C28 1.38(3) . ? C272 C28 1.39(3) . ? C29 C30 1.47(2) . ? S31 C31 1.729(10) . ? S31 C33 1.739(11) . ? S32 C31 1.730(10) . ? S32 C34 1.765(10) . ? S33 C35 1.740(11) . ? S33 C32 1.742(10) . ? S34 C36 1.725(11) . ? S34 C32 1.743(10) . ? S35 C33 1.746(10) . ? S35 C37 1.782(12) . ? S36 C34 1.751(11) . ? S36 C38 1.800(11) . ? S37 C35 1.734(11) . ? S37 C39 1.780(12) . ? S38 C36 1.746(10) . ? S38 C40 1.787(12) . ? C31 C32 1.368(13) . ? C33 C34 1.349(13) . ? C35 C36 1.362(13) . ? C37 C38 1.489(15) . ? C39 C40 1.50(2) . ? S41 C43 1.741(11) . ? S41 C41 1.745(11) . ? S42 C41 1.743(11) . ? S42 C44 1.754(10) . ? S43 C42 1.722(11) . ? S43 C45 1.748(9) . ? S44 C42 1.732(10) . ? S44 C46 1.732(10) . ? S45 C43 1.736(10) . ? S45 C47 1.814(12) . ? S46 C44 1.744(11) . ? S46 C48 1.807(11) . ? S47 C45 1.730(10) . ? S47 C49 1.802(12) . ? S48 C46 1.743(10) . ? S48 C50 1.774(13) . ? C41 C42 1.370(14) . ? C43 C44 1.369(13) . ? C45 C46 1.350(13) . ? C47 C48 1.51(2) . ? C49 C50 1.46(2) . ? S51 C53 1.752(11) . ? S51 C51 1.759(10) . ? S52 C51 1.714(11) . ? S52 C54 1.781(10) . ? S53 C52 1.722(11) . ? S53 C55 1.750(10) . ? S54 C52 1.726(10) . ? S54 C56 1.746(11) . ? S55 C53 1.736(11) . ? S55 C57 1.785(13) . ? S56 C54 1.724(11) . ? S56 C58 1.801(12) . ? S57 C55 1.731(11) . ? S57 C59 1.813(12) . ? S58 C56 1.736(11) . ? S58 C60 1.760(12) . ? C51 C52 1.367(14) . ? C53 C54 1.341(13) . ? C55 C56 1.342(13) . ? C57 C58 1.46(2) . ? C59 C60 1.50(2) . ? N1 C7 1.122(14) . ? N2 C8 1.15(2) . ? N3 C9 1.120(13) . ? N4 C10 1.144(15) . ? N5 C11 1.140(14) . ? N6 C12 1.160(14) . ? N7 C13 1.12(2) . ? N8 C14 1.14(2) . ? C1 C3 1.377(13) . ? C1 C2 1.422(14) . ? C1 C4 1.477(14) . ? C2 C7 1.42(2) . ? C2 C8 1.47(2) . ? C3 C10 1.44(2) . ? C3 C9 1.48(2) . ? C4 C5 1.399(14) . ? C4 C11 1.44(2) . ? C5 C6 1.416(15) . ? C5 C12 1.43(2) . ? C6 C13 1.44(2) . ? C6 C14 1.44(2) . ? C61 C62 1.22(3) . ? C61 C65 1.35(3) . ? C62 C63 1.46(3) . ? C63 C64 1.54(3) . ? C64 C65 1.46(3) . ? C71 C72 1.36(4) . ? C71 C75 1.37(5) . ? C72 C73 1.60(4) . ? C73 C74 1.30(4) . ? C74 C75 1.65(6) . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 S21 C21 95.2(5) . . ? C21 S22 C24 95.9(5) . . ? C22 S23 C25 96.4(5) . . ? C22 S24 C26 94.5(5) . . ? C272 S25 C23 101.6(10) . . ? C23 S25 C271 100.0(8) . . ? C28 S26 C24 100.4(6) . . ? C25 S27 C29 102.4(5) . . ? C26 S28 C30 99.4(5) . . ? C22 C21 S22 124.6(8) . . ? C22 C21 S21 120.7(8) . . ? S22 C21 S21 114.7(6) . . ? C21 C22 S23 124.9(8) . . ? C21 C22 S24 120.3(8) . . ? S23 C22 S24 114.8(6) . . ? C24 C23 S25 128.7(8) . . ? C24 C23 S21 116.3(8) . . ? S25 C23 S21 115.0(6) . . ? C23 C24 S26 127.8(8) . . ? C23 C24 S22 117.3(8) . . ? S26 C24 S22 114.9(6) . . ? C26 C25 S27 130.2(8) . . ? C26 C25 S23 114.6(8) . . ? S27 C25 S23 115.1(6) . . ? C25 C26 S28 126.8(9) . . ? C25 C26 S24 118.6(8) . . ? S28 C26 S24 114.6(6) . . ? C28 C271 S25 112.4(19) . . ? C28 C272 S25 126.3(21) . . ? C271 C28 S26 118.0(14) . . ? C272 C28 S26 129.7(14) . . ? C30 C29 S27 118.0(9) . . ? C29 C30 S28 115.1(9) . . ? C31 S31 C33 95.6(5) . . ? C31 S32 C34 95.3(5) . . ? C35 S33 C32 95.5(5) . . ? C36 S34 C32 95.6(5) . . ? C33 S35 C37 103.0(5) . . ? C34 S36 C38 97.9(5) . . ? C35 S37 C39 101.6(5) . . ? C36 S38 C40 102.1(5) . . ? C32 C31 S31 122.3(8) . . ? C32 C31 S32 122.3(8) . . ? S31 C31 S32 115.3(6) . . ? C31 C32 S33 123.1(8) . . ? C31 C32 S34 122.2(8) . . ? S33 C32 S34 114.7(6) . . ? C34 C33 S31 117.3(8) . . ? C34 C33 S35 127.6(9) . . ? S31 C33 S35 115.0(6) . . ? C33 C34 S36 128.9(8) . . ? C33 C34 S32 116.1(8) . . ? S36 C34 S32 115.0(6) . . ? C36 C35 S37 128.8(9) . . ? C36 C35 S33 116.4(8) . . ? S37 C35 S33 114.7(6) . . ? C35 C36 S34 117.5(8) . . ? C35 C36 S38 127.1(9) . . ? S34 C36 S38 115.3(6) . . ? C38 C37 S35 114.0(8) . . ? C37 C38 S36 114.6(8) . . ? C40 C39 S37 115.9(8) . . ? C39 C40 S38 112.9(8) . . ? C43 S41 C41 96.5(5) . . ? C41 S42 C44 95.8(5) . . ? C42 S43 C45 95.4(5) . . ? C42 S44 C46 94.7(5) . . ? C43 S45 C47 101.6(5) . . ? C44 S46 C48 101.7(5) . . ? C45 S47 C49 101.6(5) . . ? C46 S48 C50 102.3(5) . . ? C42 C41 S42 123.0(8) . . ? C42 C41 S41 122.5(9) . . ? S42 C41 S41 114.5(6) . . ? C41 C42 S43 122.6(8) . . ? C41 C42 S44 121.5(9) . . ? S43 C42 S44 115.9(6) . . ? C44 C43 S45 127.5(9) . . ? C44 C43 S41 116.2(8) . . ? S45 C43 S41 116.2(6) . . ? C43 C44 S46 128.7(8) . . ? C43 C44 S42 116.9(8) . . ? S46 C44 S42 114.4(6) . . ? C46 C45 S47 129.4(8) . . ? C46 C45 S43 115.9(8) . . ? S47 C45 S43 114.7(5) . . ? C45 C46 S44 118.0(8) . . ? C45 C46 S48 127.3(8) . . ? S44 C46 S48 114.7(6) . . ? C48 C47 S45 112.2(8) . . ? C47 C48 S46 113.5(8) . . ? C50 C49 S47 116.4(9) . . ? C49 C50 S48 117.3(9) . . ? C53 S51 C51 95.8(5) . . ? C51 S52 C54 96.4(5) . . ? C52 S53 C55 95.1(5) . . ? C52 S54 C56 94.9(5) . . ? C53 S55 C57 100.0(5) . . ? C54 S56 C58 101.6(5) . . ? C55 S57 C59 103.0(5) . . ? C56 S58 C60 99.4(5) . . ? C52 C51 S52 124.0(8) . . ? C52 C51 S51 121.4(8) . . ? S52 C51 S51 114.6(6) . . ? C51 C52 S53 123.4(8) . . ? C51 C52 S54 120.5(8) . . ? S53 C52 S54 116.1(6) . . ? C54 C53 S55 127.6(9) . . ? C54 C53 S51 117.3(8) . . ? S55 C53 S51 115.2(6) . . ? C53 C54 S56 130.6(9) . . ? C53 C54 S52 115.9(8) . . ? S56 C54 S52 113.5(6) . . ? C56 C55 S57 129.5(8) . . ? C56 C55 S53 116.7(8) . . ? S57 C55 S53 113.9(6) . . ? C55 C56 S58 126.6(9) . . ? C55 C56 S54 117.2(8) . . ? S58 C56 S54 116.1(6) . . ? C58 C57 S55 117.9(9) . . ? C57 C58 S56 115.4(9) . . ? C60 C59 S57 115.5(8) . . ? C59 C60 S58 114.7(8) . . ? C3 C1 C2 125.2(10) . . ? C3 C1 C4 120.1(10) . . ? C2 C1 C4 114.7(9) . . ? C7 C2 C1 122.9(10) . . ? C7 C2 C8 116.3(11) . . ? C1 C2 C8 120.7(11) . . ? C1 C3 C10 121.0(10) . . ? C1 C3 C9 122.1(11) . . ? C10 C3 C9 116.6(10) . . ? C5 C4 C11 122.6(10) . . ? C5 C4 C1 121.5(9) . . ? C11 C4 C1 115.9(10) . . ? C4 C5 C6 129.3(11) . . ? C4 C5 C12 115.9(10) . . ? C6 C5 C12 114.4(11) . . ? C5 C6 C13 120.4(11) . . ? C5 C6 C14 122.4(12) . . ? C13 C6 C14 117.0(11) . . ? N1 C7 C2 179.2(14) . . ? N2 C8 C2 175.8(16) . . ? N3 C9 C3 176.5(14) . . ? N4 C10 C3 175.4(14) . . ? N5 C11 C4 176.0(13) . . ? N6 C12 C5 174.7(13) . . ? N7 C13 C6 176.2(17) . . ? N8 C14 C6 174.9(17) . . ? C62 C61 C65 112.2(20) . . ? C61 C62 C63 113.9(27) . . ? C62 C63 C64 97.5(20) . . ? C65 C64 C63 102.6(18) . . ? C61 C65 C64 107.0(21) . . ? C72 C71 C75 76.7(29) . . ? C71 C72 C73 94.4(30) . . ? C74 C73 C72 106.2(27) . . ? C73 C74 C75 76.9(24) . . ? C71 C75 C74 86.5(31) . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S21 S57 3.500(4) . . ? S22 S58 3.552(4) . 2_666 ? S25 S57 3.436(4) . 2_667 ? S26 S58 3.491(4) . 2_666 ? S27 S55 3.447(5) . 2_667 ? S27 S51 3.567(5) . 2_667 ? S28 S52 3.455(4) . 2_666 ? S28 S56 3.429(4) . 2_666 ? S31 S47 3.588(4) . 2_667 ? S32 S48 3.499(4) . 2_666 ? S35 N8 3.162(14) . 2_566 ? S35 S47 3.447(4) . 2_667 ? S36 N1 3.239(11) . 2_565 ? S36 S48 3.350(4) . 2_666 ? S37 S41 3.583(4) . 2_667 ? S37 S45 3.426(4) . 2_667 ? S38 S46 3.404(4) . 2_666 ? S38 S42 3.513(4) . 2_666 ? S55 N3 3.175(13) . 2_667 ? H27A N2 2.735 . 1_565 ? H27C N2 2.543 . 2_566 ? H29A N3 2.618 . . ? H30A N4 2.529 . . ? H37B N8 2.691 . 1_566 ? H37B N7 2.726 . 2_666 ? H40A N6 2.668 . . ? H49A N8 2.595 . 2_656 ? H50A N1 2.695 . 2_656 ? H60A N5 2.584 . 2_656 ? H60B N4 2.658 . 1_656 ? #------------------------------------------------------------------------------ #===END