data_General _audit_creation_date 2012-02-06 _audit_creation_method 'by CrystalStructure 4.0' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Hiroki Akutsu' _publ_contact_author_email 'akutsu@sci.u-hyogo.ac.jp' _publ_contact_author_fax '+81-791-58-0164' _publ_contact_author_phone '+81-791-58-0164' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Crystals' _publ_requested_category 'FO' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. M.C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G.L. Cascarano, L. De Caro, C. Giacovazzo, G. Polidori, D. Siliqi, R. Spagna (2007) SIR2008 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_V111022a #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C46 H42 N2 O9 S34' _chemical_formula_moiety '4(C10 H8 S8), C6 H4 N2 O6 S2, 3(H2 O)' _chemical_formula_weight 1856.89 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' #------------------------------------------------------------------------------ _cell_length_a 6.742(3) _cell_length_b 15.518(7) _cell_length_c 18.034(7) _cell_angle_alpha 74.29(3) _cell_angle_beta 82.16(4) _cell_angle_gamma 80.36(3) _cell_volume 1782.2(14) _cell_formula_units_Z 1 _cell_measurement_reflns_used 4124 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 30.10 _cell_measurement_temperature 294 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.650 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.005 _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948.00 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_absorpt_correction_T_min 0.770 _exptl_absorpt_correction_T_max 0.995 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 294 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 13528 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measured_fraction_theta_full 0.947 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7764 _reflns_number_gt 3650 _reflns_threshold_expression F^2^>2.5\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.0565 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3129 _refine_ls_number_parameters 424 _refine_ls_goodness_of_fit_ref 1.1552 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: -0.212 -6.65 -2.39 -2.89 -1.09 ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.0001543 _refine_diff_density_min -0.48 _refine_diff_density_max 0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens S1 S 0.6575(3) 0.4681(2) 0.28936(14) 0.0576 1.0000 Uani . . . . . . S2 S 1.1681(4) 0.4890(2) 0.23012(13) 0.0537 1.0000 Uani . . . . . . S3 S 0.7546(3) 0.47974(19) 0.44028(12) 0.0491 1.0000 Uani . . . . . . S4 S 1.1860(3) 0.4979(2) 0.39084(13) 0.0522 1.0000 Uani . . . . . . S5 S 0.2931(4) 0.7245(2) 0.23658(15) 0.0690 1.0000 Uani . . . . . . S6 S 0.8155(4) 0.7253(2) 0.18545(13) 0.0563 1.0000 Uani . . . . . . S7 S 0.3891(3) 0.7264(2) 0.38968(13) 0.0543 1.0000 Uani . . . . . . S8 S 0.8246(3) 0.72335(19) 0.34893(13) 0.0489 1.0000 Uani . . . . . . S9 S 0.4371(3) 0.74577(19) 0.55909(13) 0.0498 1.0000 Uani . . . . . . S10 S 0.8716(3) 0.74862(19) 0.51823(13) 0.0500 1.0000 Uani . . . . . . S11 S 0.4336(3) 0.7806(2) 0.71315(14) 0.0542 1.0000 Uani . . . . . . S12 S 0.9508(4) 0.7912(2) 0.65896(15) 0.0635 1.0000 Uani . . . . . . S13 S 0.5469(4) 0.9597(2) 0.23854(15) 0.0613 1.0000 Uani . . . . . . S14 S 1.0199(4) 0.9620(3) 0.29199(17) 0.0766 1.0000 Uani . . . . . . S15 S 0.3976(3) 0.9790(2) 0.39723(14) 0.0535 1.0000 Uani . . . . . . S16 S 0.7994(4) 0.9947(2) 0.43610(14) 0.0591 1.0000 Uani . . . . . . S17 S 1.0910(4) 0.71842(19) -0.04900(14) 0.0538 1.0000 Uani . . . . . . O1 O 1.2074(13) 0.7507(6) -0.1192(5) 0.1003 1.0000 Uani . . . . . . O2 O 1.1285(17) 0.7450(7) 0.0155(6) 0.1366 1.0000 Uani . . . . . . O3 O 0.8762(11) 0.7352(6) -0.0597(5) 0.0970 1.0000 Uani . . . . . . O4 O 1.071(6) 0.9296(15) 0.0215(12) 0.2768 0.5000 Uani . . . . . . O5 O 0.538(3) 0.8574(14) -0.0616(12) 0.1232 0.5000 Uani . . . . . . O6 O 0.366(6) 1.023(4) 0.039(2) 0.3742 0.5000 Uani . . . . . . N1 N 1.1381(11) 0.6033(6) -0.0267(5) 0.0598 1.0000 Uani . . . . . . C1 C 0.8150(15) 0.4311(8) 0.2120(6) 0.0641 1.0000 Uani . . . . . . C2 C 0.9757(14) 0.4873(8) 0.1731(5) 0.0630 1.0000 Uani . . . . . . C3 C 0.8398(12) 0.4788(7) 0.3442(4) 0.0433 1.0000 Uani . . . . . . C4 C 1.0363(12) 0.4881(6) 0.3213(4) 0.0354 1.0000 Uani . . . . . . C5 C 0.9874(13) 0.4961(7) 0.4647(5) 0.0435 1.0000 Uani . . . . . . C6 C 0.4389(17) 0.7047(11) 0.1517(6) 0.0935 1.0000 Uani . . . . . . C7 C 0.6135(15) 0.7545(10) 0.1238(6) 0.0792 1.0000 Uani . . . . . . C8 C 0.4798(13) 0.7218(7) 0.2957(5) 0.0448 1.0000 Uani . . . . . . C9 C 0.6815(13) 0.7243(7) 0.2748(5) 0.0485 1.0000 Uani . . . . . . C10 C 0.6206(13) 0.7302(6) 0.4179(5) 0.0407 1.0000 Uani . . . . . . C11 C 0.6406(12) 0.7395(6) 0.4906(5) 0.0397 1.0000 Uani . . . . . . C12 C 0.5727(12) 0.7675(6) 0.6254(5) 0.0406 1.0000 Uani . . . . . . C13 C 0.7718(13) 0.7706(7) 0.6068(5) 0.0460 1.0000 Uani . . . . . . C14 C 0.6356(14) 0.7542(8) 0.7749(5) 0.0580 1.0000 Uani . . . . . . C15 C 0.8037(13) 0.8085(7) 0.7464(5) 0.0544 1.0000 Uani . . . . . . C16 C 0.7568(18) 1.0091(11) 0.1779(6) 0.0975 1.0000 Uani . . . . . . C17 C 0.9527(18) 0.9685(12) 0.1994(6) 0.1073 1.0000 Uani . . . . . . C18 C 0.6031(13) 0.9671(6) 0.3289(5) 0.0438 1.0000 Uani . . . . . . C19 C 0.7866(13) 0.9736(6) 0.3452(5) 0.0493 1.0000 Uani . . . . . . C20 C 0.5420(13) 0.9947(6) 0.4644(5) 0.0457 1.0000 Uani . . . . . . C21 C 1.3154(14) 0.5600(8) -0.0148(5) 0.0556 1.0000 Uani . . . . . . C22 C 1.3262(15) 0.4610(7) 0.0021(6) 0.0602 1.0000 Uani . . . . . . C23 C 1.4983(14) 0.5980(7) -0.0161(5) 0.0507 1.0000 Uani . . . . . . H12 H 0.8774 0.3696 0.2323 0.1376 1.0000 Uiso R . . . . . H11 H 0.7290 0.4300 0.1734 0.0467 1.0000 Uiso R . . . . . H22 H 0.9126 0.5489 0.1535 0.1241 1.0000 Uiso R . . . . . H21 H 1.0388 0.4654 0.1288 0.1003 1.0000 Uiso R . . . . . H42 H 1.1757 0.9459 -0.0033 0.3198 0.5000 Uiso R . . . . . H41 H 1.0657 0.8775 0.0209 0.3198 0.5000 Uiso R . . . . . H51 H 0.6615 0.8540 -0.0714 0.1272 0.5000 Uiso R . . . . . H52 H 0.4885 0.9107 -0.0706 0.2939 0.5000 Uiso R . . . . . H62 H 0.4872 0.6405 0.1616 0.2714 1.0000 Uiso R . . . . . H61 H 0.3508 0.7195 0.1105 0.1592 1.0000 Uiso R . . . . . H641 H 0.4614 1.0315 0.0056 0.4103 0.5000 Uiso R . . . . . H63 H 0.3583 0.9686 0.0537 0.4103 0.5000 Uiso R . . . . . H72 H 0.5659 0.8186 0.1158 0.2950 1.0000 Uiso R . . . . . H71 H 0.6675 0.7443 0.0737 0.1392 1.0000 Uiso R . . . . . H142 H 0.5799 0.7645 0.8248 0.0818 1.0000 Uiso R . . . . . H141 H 0.6875 0.6905 0.7832 0.0809 1.0000 Uiso R . . . . . H151 H 0.8944 0.7945 0.7867 0.0562 1.0000 Uiso R . . . . . H152 H 0.7505 0.8721 0.7376 0.0876 1.0000 Uiso R . . . . . H162 H 0.7512 1.0002 0.1271 0.0508 1.0000 Uiso R . . . . . H161 H 0.7370 1.0738 0.1724 0.3467 1.0000 Uiso R . . . . . H172 H 1.0432 1.0060 0.1632 0.1782 1.0000 Uiso R . . . . . H171 H 0.9848 0.9087 0.1903 0.3091 1.0000 Uiso R . . . . . H221 H 1.2078 0.4368 0.0041 0.0655 1.0000 Uiso R . . . . . H231 H 1.4966 0.6601 -0.0256 0.1340 1.0000 Uiso R . . . . . 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 S1 0.0407(12) 0.100(2) 0.0406(14) -0.0291(14) -0.0060(10) -0.0130(13) S2 0.0445(12) 0.088(2) 0.0352(13) -0.0268(13) 0.0046(10) -0.0146(13) S3 0.0389(12) 0.0802(19) 0.0331(12) -0.0213(12) 0.0003(9) -0.0135(12) S4 0.0372(12) 0.090(2) 0.0346(13) -0.0233(13) 0.0006(9) -0.0149(13) S5 0.0461(14) 0.127(3) 0.0446(15) -0.0371(16) -0.0069(11) -0.0160(16) S6 0.0469(13) 0.089(2) 0.0363(13) -0.0233(13) 0.0021(10) -0.0122(13) S7 0.0373(12) 0.090(2) 0.0397(13) -0.0237(13) -0.0003(9) -0.0118(13) S8 0.0372(11) 0.0758(18) 0.0358(12) -0.0188(12) -0.0032(9) -0.0066(12) S9 0.0376(11) 0.0839(19) 0.0346(12) -0.0248(12) -0.0010(9) -0.0126(12) S10 0.0332(11) 0.082(2) 0.0394(13) -0.0248(13) -0.0028(9) -0.0065(12) S11 0.0434(12) 0.086(2) 0.0422(13) -0.0301(13) 0.0020(10) -0.0158(13) S12 0.0433(13) 0.108(2) 0.0525(15) -0.0347(16) -0.0036(11) -0.0255(15) S13 0.0602(15) 0.083(2) 0.0492(15) -0.0285(14) -0.0062(12) -0.0147(15) S14 0.0456(14) 0.128(3) 0.0662(19) -0.0427(19) 0.0035(13) -0.0177(17) S15 0.0413(13) 0.0757(19) 0.0466(14) -0.0189(13) -0.0048(10) -0.0107(12) S16 0.0450(13) 0.091(2) 0.0476(14) -0.0226(14) -0.0012(11) -0.0198(14) S17 0.0429(13) 0.0727(19) 0.0433(13) -0.0124(13) -0.0041(10) -0.0046(12) O1 0.094(6) 0.094(7) 0.077(6) 0.009(5) 0.038(5) -0.001(5) O2 0.174(11) 0.128(9) 0.129(9) -0.074(7) -0.096(8) 0.055(8) O3 0.047(4) 0.110(7) 0.118(7) -0.004(6) -0.010(4) -0.005(5) O4 0.66(7) 0.076(16) 0.065(14) -0.038(12) 0.10(3) -0.05(3) O5 0.111(15) 0.119(17) 0.128(17) -0.022(14) -0.046(13) 0.030(13) O6 0.29(5) 0.55(8) 0.22(4) 0.20(5) -0.16(4) -0.24(6) N1 0.041(4) 0.085(7) 0.057(5) -0.018(5) -0.002(4) -0.018(4) C1 0.068(7) 0.091(9) 0.048(6) -0.039(6) 0.000(5) -0.021(6) C2 0.054(6) 0.107(9) 0.035(5) -0.029(6) 0.001(4) -0.017(6) C3 0.041(5) 0.068(7) 0.025(4) -0.020(4) 0.000(3) -0.010(5) C4 0.038(4) 0.045(5) 0.028(4) -0.015(4) -0.003(3) -0.009(4) C5 0.037(4) 0.060(6) 0.037(5) -0.018(4) -0.002(4) -0.006(4) C6 0.072(7) 0.186(15) 0.038(6) -0.048(8) -0.009(5) -0.025(9) C7 0.055(6) 0.152(12) 0.031(5) -0.021(6) -0.001(4) -0.021(7) C8 0.048(5) 0.061(6) 0.025(4) -0.009(4) -0.002(4) -0.008(5) C9 0.043(5) 0.068(7) 0.033(5) -0.008(4) -0.002(4) -0.013(5) C10 0.047(5) 0.051(6) 0.029(4) -0.014(4) -0.002(4) -0.015(4) C11 0.031(4) 0.041(5) 0.044(5) -0.008(4) -0.007(4) -0.001(4) C12 0.038(4) 0.046(6) 0.041(5) -0.017(4) 0.002(4) -0.010(4) C13 0.041(5) 0.062(7) 0.035(5) -0.010(4) -0.007(4) -0.007(5) C14 0.058(6) 0.078(8) 0.044(6) -0.019(5) -0.003(5) -0.023(6) C15 0.049(5) 0.078(8) 0.043(5) -0.027(5) -0.017(4) 0.003(5) C16 0.070(8) 0.174(15) 0.041(6) -0.015(8) -0.007(5) -0.012(9) C17 0.073(8) 0.215(18) 0.035(6) -0.037(8) 0.011(6) -0.028(10) C18 0.051(5) 0.043(6) 0.039(5) -0.009(4) -0.006(4) -0.012(4) C19 0.045(5) 0.049(6) 0.057(6) -0.018(5) 0.002(4) -0.012(4) C20 0.045(5) 0.046(6) 0.051(5) -0.016(5) -0.006(4) -0.011(4) C21 0.043(5) 0.088(9) 0.044(5) -0.025(5) 0.004(4) -0.023(5) C22 0.049(6) 0.071(8) 0.070(7) -0.027(6) -0.002(5) -0.023(6) C23 0.054(6) 0.053(6) 0.048(6) -0.013(5) -0.009(4) -0.010(5) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; 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 S1 . C1 . 1.797(9) yes S1 . C3 . 1.734(8) yes S2 . C2 . 1.770(9) yes S2 . C4 . 1.758(8) yes S3 . C3 . 1.753(8) yes S3 . C5 . 1.762(9) yes S4 . C4 . 1.764(8) yes S4 . C5 . 1.753(8) yes S5 . C6 . 1.774(11) yes S5 . C8 . 1.746(9) yes S6 . C7 . 1.797(10) yes S6 . C9 . 1.733(9) yes S7 . C8 . 1.737(8) yes S7 . C10 . 1.722(8) yes S8 . C9 . 1.748(9) yes S8 . C10 . 1.734(8) yes S9 . C11 . 1.724(8) yes S9 . C12 . 1.732(9) yes S10 . C11 . 1.737(8) yes S10 . C13 . 1.746(9) yes S11 . C12 . 1.769(8) yes S11 . C14 . 1.801(10) yes S12 . C13 . 1.745(9) yes S12 . C15 . 1.804(9) yes S13 . C16 . 1.810(12) yes S13 . C18 . 1.760(9) yes S14 . C17 . 1.761(11) yes S14 . C19 . 1.736(9) yes S15 . C18 . 1.744(9) yes S15 . C20 . 1.742(9) yes S16 . C19 . 1.773(10) yes S16 . C20 . 1.741(9) yes S17 . O1 . 1.409(7) yes S17 . O2 . 1.401(9) yes S17 . O3 . 1.457(7) yes S17 . N1 . 1.705(10) yes O4 . H42 . 0.820 no O4 . H41 . 0.820 no O5 . H51 . 0.820 no O5 . H52 . 0.820 no O6 . H641 . 0.820 no O6 . H63 . 0.820 no N1 . C21 . 1.284(12) yes C1 . C2 . 1.485(13) yes C1 . H12 . 0.970 no C1 . H11 . 0.970 no C2 . H22 . 0.970 no C2 . H21 . 0.970 no C3 . C4 . 1.352(11) yes C5 . C5 2_766 1.347(16) yes C6 . C7 . 1.473(15) yes C6 . H62 . 0.970 no C6 . H61 . 0.970 no C7 . H72 . 0.970 no C7 . H71 . 0.970 no C8 . C9 . 1.365(11) yes C10 . C11 . 1.383(11) yes C12 . C13 . 1.344(11) yes C14 . C15 . 1.478(12) yes C14 . H142 . 0.970 no C14 . H141 . 0.970 no C15 . H151 . 0.970 no C15 . H152 . 0.970 no C16 . C17 . 1.422(16) yes C16 . H162 . 0.970 no C16 . H161 . 0.970 no C17 . H172 . 0.970 no C17 . H171 . 0.970 no C18 . C19 . 1.336(12) yes C20 . C20 2_676 1.372(17) yes C21 . C22 . 1.474(15) yes C21 . C23 . 1.448(12) yes C22 . C23 2_865 1.377(13) yes C22 . H221 . 0.930 no C23 . H231 . 0.930 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 C1 . S1 . C3 . 100.5(4) yes C2 . S2 . C4 . 103.1(4) yes C3 . S3 . C5 . 95.6(4) yes C4 . S4 . C5 . 95.1(4) yes C6 . S5 . C8 . 102.0(5) yes C7 . S6 . C9 . 101.0(4) yes C8 . S7 . C10 . 95.4(4) yes C9 . S8 . C10 . 95.8(4) yes C11 . S9 . C12 . 95.2(4) yes C11 . S10 . C13 . 95.1(4) yes C12 . S11 . C14 . 99.9(4) yes C13 . S12 . C15 . 103.0(4) yes C16 . S13 . C18 . 99.4(5) yes C17 . S14 . C19 . 102.6(5) yes C18 . S15 . C20 . 94.5(4) yes C19 . S16 . C20 . 94.7(4) yes O1 . S17 . O2 . 116.9(7) yes O1 . S17 . O3 . 111.0(5) yes O2 . S17 . O3 . 111.5(6) yes O1 . S17 . N1 . 107.2(5) yes O2 . S17 . N1 . 106.9(5) yes O3 . S17 . N1 . 102.1(5) yes H42 . O4 . H41 . 109.5 no H51 . O5 . H52 . 109.5 no H641 . O6 . H63 . 109.5 no S17 . N1 . C21 . 122.3(7) yes S1 . C1 . C2 . 115.6(7) yes S1 . C1 . H12 . 108.3 no C2 . C1 . H12 . 108.8 no S1 . C1 . H11 . 108.2 no C2 . C1 . H11 . 108.2 no H12 . C1 . H11 . 107.5 no C1 . C2 . S2 . 116.4(7) yes C1 . C2 . H22 . 108.4 no S2 . C2 . H22 . 108.4 no C1 . C2 . H21 . 107.9 no S2 . C2 . H21 . 108.1 no H22 . C2 . H21 . 107.3 no S3 . C3 . S1 . 115.1(5) yes S3 . C3 . C4 . 116.9(6) yes S1 . C3 . C4 . 127.9(6) yes S4 . C4 . S2 . 114.3(4) yes S4 . C4 . C3 . 117.5(6) yes S2 . C4 . C3 . 128.2(6) yes S3 . C5 . S4 . 114.7(4) yes S3 . C5 . C5 2_766 122.7(9) yes S4 . C5 . C5 2_766 122.5(9) yes S5 . C6 . C7 . 116.5(9) yes S5 . C6 . H62 . 107.8 no C7 . C6 . H62 . 108.4 no S5 . C6 . H61 . 108.4 no C7 . C6 . H61 . 108.1 no H62 . C6 . H61 . 107.3 no C6 . C7 . S6 . 115.9(8) yes C6 . C7 . H72 . 108.4 no S6 . C7 . H72 . 108.6 no C6 . C7 . H71 . 107.9 no S6 . C7 . H71 . 108.3 no H72 . C7 . H71 . 107.3 no S5 . C8 . S7 . 114.5(5) yes S5 . C8 . C9 . 127.6(6) yes S7 . C8 . C9 . 117.7(6) yes S8 . C9 . S6 . 115.8(5) yes S8 . C9 . C8 . 115.3(6) yes S6 . C9 . C8 . 128.9(7) yes S8 . C10 . S7 . 115.5(5) yes S8 . C10 . C11 . 122.7(6) yes S7 . C10 . C11 . 121.8(6) yes S10 . C11 . S9 . 115.4(5) yes S10 . C11 . C10 . 122.2(6) yes S9 . C11 . C10 . 122.4(6) yes S11 . C12 . S9 . 115.9(5) yes S11 . C12 . C13 . 126.3(7) yes S9 . C12 . C13 . 117.8(6) yes S10 . C13 . S12 . 113.9(5) yes S10 . C13 . C12 . 116.2(6) yes S12 . C13 . C12 . 129.8(7) yes S11 . C14 . C15 . 115.0(7) yes S11 . C14 . H142 . 108.2 no C15 . C14 . H142 . 107.4 no S11 . C14 . H141 . 108.8 no C15 . C14 . H141 . 109.6 no H142 . C14 . H141 . 107.5 no C14 . C15 . S12 . 115.9(7) yes C14 . C15 . H151 . 108.1 no S12 . C15 . H151 . 107.9 no C14 . C15 . H152 . 109.2 no S12 . C15 . H152 . 108.2 no H151 . C15 . H152 . 107.3 no S13 . C16 . C17 . 115.9(10) yes S13 . C16 . H162 . 106.0 no C17 . C16 . H162 . 105.6 no S13 . C16 . H161 . 109.7 no C17 . C16 . H161 . 111.9 no H162 . C16 . H161 . 107.1 no C16 . C17 . S14 . 120.5(9) yes C16 . C17 . H172 . 104.1 no S14 . C17 . H172 . 105.6 no C16 . C17 . H171 . 110.9 no S14 . C17 . H171 . 108.1 no H172 . C17 . H171 . 106.6 no S13 . C18 . S15 . 116.4(5) yes S13 . C18 . C19 . 124.5(7) yes S15 . C18 . C19 . 118.7(7) yes S16 . C19 . S14 . 113.7(5) yes S16 . C19 . C18 . 116.1(7) yes S14 . C19 . C18 . 130.2(8) yes S15 . C20 . S16 . 116.0(5) yes S15 . C20 . C20 2_676 122.0(9) yes S16 . C20 . C20 2_676 122.1(9) yes N1 . C21 . C22 . 114.2(9) yes N1 . C21 . C23 . 127.1(10) yes C22 . C21 . C23 . 118.7(9) yes C21 . C22 . C23 2_865 123.7(9) yes C21 . C22 . H221 . 118.4 no C23 2_865 C22 . H221 . 117.9 no C21 . C23 . C22 2_865 117.7(9) yes C21 . C23 . H231 . 121.0 no C22 2_865 C23 . H231 . 121.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O4 . H42 . O6 1_655 121.9(13) 0.820 2.214 2.738(14) yes O4 . H41 . O2 . 165.7(12) 0.820 2.054 2.856(14) yes O5 . H51 . O3 . 127.8(7) 0.820 2.125 2.706(14) yes C6 . H61 . O2 1_455 175.6(5) 0.970 2.338 3.306(14) yes O6 . H641 . O6 2_675 140(3) 0.820 1.579 2.270(14) yes C14 . H142 . O1 1_456 123.6(3) 0.970 2.597 3.237(14) yes C22 . H221 . N1 2_765 167.2(3) 0.930 2.466 3.380(14) yes _iucr_refine_instruction_details_constraints ; # # Punched on 16/02/12 at 18:44:05 # #LIST 12 BLOCK SCALE X'S, U'S RIDE O ( 4,X'S) H ( 42,X'S) H ( 41,X'S) RIDE O ( 5,X'S) H ( 51,X'S) H ( 52,X'S) RIDE O ( 6,X'S) H ( 641,X'S) H ( 63,X'S) RIDE C ( 1,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 22,X'S) H ( 21,X'S) RIDE C ( 6,X'S) H ( 62,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 14,X'S) H ( 142,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) RIDE C ( 16,X'S) H ( 162,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 172,X'S) H ( 171,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 16/02/12 at 18:44:05 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE) END ; #============================================================================== # 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 #==============================================================================