Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shashank Mishra' _publ_contact_author_address ; Institut du Rechearches sur la Catalyse 2 Avenue A. Einstein Villeurbanne 69626 FRANCE ; _publ_contact_author_email MISHRASHASHANK74@REDIFFMAIL.COM _publ_section_title ; Rare example of a polynuclear heterometallic yttrium(III)-copper(I) iodide cluster with a [Y6(?6-O)(?3-OH)8]8+ core structure showing single crystal-to-single crystal transformation ; loop_ _publ_author_name 'Shashank Mishra' 'Stephane Daniele' 'Liliane Hubert-Pfalzgraf' 'Erwann Jeanneau' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 670605' _audit_creation_date 07-10-03 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'scale in P 21/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.29910(100) _cell_length_b 19.29990(150) _cell_length_c 18.79500(119) _cell_angle_alpha 90.0000 _cell_angle_beta 91.0374(35) _cell_angle_gamma 90.0000 _cell_volume 5186.029(635) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Y -2.7962 3.5667 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' 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' _cell_formula_units_Z 2 # Given Formula = C36 H60 Cu1.50 I6 N12 O3.50 S6 Y1.50 # Dc = 2.43 Fooo = 3180.00 Mu = 61.40 M = 1899.45 # Found Formula = C16 H52 Cu1 I5 O13.50 S8 Y3 # Dc = 2.15 FOOO = 3180.00 Mu = 70.69 M = 1681.89 _chemical_formula_sum 'C32 H104 Cu2 I10 O27 S16 Y6' _chemical_formula_moiety ; C32 H104 O27 S16 Y6, Cu2 I4, 6(I) ; _chemical_compound_source ? _chemical_formula_weight 3363.83 _cell_measurement_reflns_used 51056 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 23.534 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3180 _exptl_absorpt_coefficient_mu 7.069 # Sheldrick geometric approximatio 0.75 0.79 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.79 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 13386 _reflns_number_total 7670 _diffrn_reflns_av_R_equivalents 0.041 # Number of reflections with Friedels Law is 7670 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7712 _diffrn_reflns_theta_min 2.091 _diffrn_reflns_theta_max 23.545 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.075 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.94 _refine_diff_density_max 2.57 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 3432 _refine_ls_number_restraints 174 _refine_ls_number_parameters 421 _oxford_refine_ls_R_factor_ref 0.0809 _refine_ls_wR_factor_ref 0.0864 _refine_ls_goodness_of_fit_ref 1.2006 _refine_ls_shift/su_max 0.000443 # The values computed from all data _oxford_reflns_number_all 7643 _refine_ls_R_factor_all 0.1456 _refine_ls_wR_factor_all 0.1139 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4045 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_gt 0.0901 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_special_details ; The atoms of some of the DMSO molecules showed physically incorrect displacement parameters. The anisotropic displacement parameters thus had to be restrained in order for the model to be reasonable. All the atoms of the same chemical species (S,C and O) were forced to have similar U~ij~ parameters. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _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: 1.64 1.43 1.19 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.0860(3) 0.01888(18) 0.98737(19) 0.1101 1.0000 Uani . . . . . . . I1 I 0.25743(19) 0.04298(13) 0.96689(12) 0.1330 1.0000 Uani . . . . . . . I2 I -0.03488(17) 0.01697(12) 0.88681(11) 0.1199 1.0000 Uani . . . . . . . I3 I 0.13538(13) -0.13140(12) 0.62374(10) 0.1111 1.0000 Uani . . . . . . . I4 I 0.18784(13) 0.19621(9) 0.62660(9) 0.0939 1.0000 Uani . . . . . . . I5 I 0.2344(2) 0.30725(19) 0.24649(19) 0.1698 1.0000 Uani . . . . . . . Y1 Y 0.52524(13) 0.12790(9) 0.49646(10) 0.0552 1.0000 Uani . . . . . . . Y2 Y 0.53580(13) -0.00800(10) 0.37092(10) 0.0545 1.0000 Uani . . . . . . . Y3 Y 0.33256(12) 0.01705(10) 0.47058(10) 0.0536 1.0000 Uani . . . . . . . S1 S 0.4347(7) 0.2998(4) 0.4996(6) 0.1283 1.0000 Uani . U . . . . . S2 S 0.6823(8) 0.2688(5) 0.5284(6) 0.1428 1.0000 Uani . U . . . . . S3 S 0.5936(5) 0.2220(3) 0.3350(3) 0.0893 1.0000 Uani . U . . . . . S4 S 0.6886(5) 0.0094(4) 0.2275(3) 0.0944 1.0000 Uani . U . . . . . S5 S 0.5828(7) -0.1535(5) 0.2478(5) 0.1310 1.0000 Uani . U . . . . . S6 S 0.4319(9) 0.0193(7) 0.1967(6) 0.1652 1.0000 Uani . U . . . . . S7 S 0.1249(8) -0.0874(6) 0.4058(6) 0.1478 1.0000 Uani . U . . . . . S8 S 0.1430(5) 0.1133(4) 0.4033(4) 0.0996 1.0000 Uani . U . . . . . O1 O 0.4451(15) 0.2273(9) 0.5273(11) 0.1146 1.0000 Uani . U . . . . . O2 O 0.6492(15) 0.1965(9) 0.5430(10) 0.1093 1.0000 Uani . U . . . . . O3 O 0.5547(13) 0.2085(8) 0.4057(9) 0.0959 1.0000 Uani . U . . . . . O4 O 0.6590(13) 0.0230(9) 0.3033(8) 0.1009 1.0000 Uani . U . . . . . O5 O 0.5423(14) -0.0976(10) 0.2884(9) 0.1065 1.0000 Uani . U . . . . . O6 O 0.4637(14) 0.0347(10) 0.2685(10) 0.1127 1.0000 Uani . U . . . . . O7 O 0.2107(12) -0.0401(10) 0.4120(9) 0.0976 1.0000 Uani . U . . . . . O8 O 0.2498(11) 0.1090(9) 0.4190(9) 0.0927 1.0000 Uani . U . . . . . O9 O 0.2001(9) 0.0324(7) 0.5495(7) 0.0687 1.0000 Uani . . . . . . . O10 O 0.3912(9) 0.0903(6) 0.5579(6) 0.0574 1.0000 Uani . . . . . . . O11 O 0.6369(8) 0.0641(6) 0.4401(6) 0.0538 1.0000 Uani . . . . . . . O12 O 0.4061(8) -0.0698(7) 0.4044(6) 0.0567 1.0000 Uani . . . . . . . O13 O 0.4372(9) 0.0821(6) 0.4028(7) 0.0575 1.0000 Uani . . . . . . . O14 O 0.5000 0.0000 0.5000 0.0462 1.0000 Uani S . . . . . . C1 C 0.339(3) 0.291(2) 0.446(2) 0.1602 1.0000 Uani . U . . . . . C2 C 0.373(3) 0.342(2) 0.559(2) 0.1572 1.0000 Uani . U . . . . . C3 C 0.650(3) 0.321(2) 0.597(2) 0.1593 1.0000 Uani . U . . . . . C4 C 0.793(3) 0.267(2) 0.547(2) 0.1652 1.0000 Uani . U . . . . . C5 C 0.505(3) 0.231(3) 0.273(2) 0.1652 1.0000 Uani . U . . . . . C6 C 0.674(3) 0.283(2) 0.342(2) 0.1579 1.0000 Uani . U . . . . . C7 C 0.803(3) -0.025(2) 0.243(2) 0.1469 1.0000 Uani . U . . . . . C8 C 0.717(3) 0.090(2) 0.196(2) 0.1418 1.0000 Uani . U . . . . . C9 C 0.536(3) -0.156(2) 0.1626(19) 0.1426 1.0000 Uani . U . . . . . C10 C 0.546(3) -0.233(2) 0.283(2) 0.1460 1.0000 Uani . U . . . . . C11 C 0.440(3) 0.099(2) 0.158(2) 0.1564 1.0000 Uani . U . . . . . C12 C 0.317(3) 0.002(2) 0.202(2) 0.1576 1.0000 Uani . U . . . . . C13 C 0.069(3) -0.076(2) 0.322(2) 0.1525 1.0000 Uani . U . . . . . C14 C 0.035(3) -0.049(2) 0.452(2) 0.1467 1.0000 Uani . U . . . . . C15 C 0.128(3) 0.110(2) 0.3099(17) 0.1366 1.0000 Uani . U . . . . . C16 C 0.117(3) 0.1984(18) 0.4183(18) 0.1299 1.0000 Uani . U . . . . . H11 H 0.3568 0.2653 0.4027 0.1952 1.0000 Uiso R . . . . . . H12 H 0.3136 0.3379 0.4324 0.1952 1.0000 Uiso R . . . . . . H13 H 0.2892 0.2648 0.4718 0.1952 1.0000 Uiso R . . . . . . H21 H 0.4142 0.3552 0.6000 0.1914 1.0000 Uiso R . . . . . . H22 H 0.3453 0.3847 0.5366 0.1914 1.0000 Uiso R . . . . . . H23 H 0.3210 0.3116 0.5760 0.1914 1.0000 Uiso R . . . . . . H31 H 0.5805 0.3286 0.5945 0.1932 1.0000 Uiso R . . . . . . H32 H 0.6670 0.2984 0.6432 0.1932 1.0000 Uiso R . . . . . . H33 H 0.6827 0.3663 0.5931 0.1932 1.0000 Uiso R . . . . . . H41 H 0.8254 0.2376 0.5111 0.1998 1.0000 Uiso R . . . . . . H42 H 0.8033 0.2472 0.5955 0.1998 1.0000 Uiso R . . . . . . H43 H 0.8189 0.3152 0.5454 0.1998 1.0000 Uiso R . . . . . . H51 H 0.4623 0.1904 0.2749 0.2000 1.0000 Uiso R . . . . . . H52 H 0.4693 0.2744 0.2842 0.2000 1.0000 Uiso R . . . . . . H53 H 0.5315 0.2352 0.2243 0.2000 1.0000 Uiso R . . . . . . H61 H 0.7211 0.2694 0.3794 0.1914 1.0000 Uiso R . . . . . . H62 H 0.6436 0.3274 0.3552 0.1914 1.0000 Uiso R . . . . . . H63 H 0.7058 0.2882 0.2953 0.1914 1.0000 Uiso R . . . . . . H71 H 0.7975 -0.0735 0.2621 0.1779 1.0000 Uiso R . . . . . . H72 H 0.8377 0.0044 0.2776 0.1779 1.0000 Uiso R . . . . . . H73 H 0.8369 -0.0266 0.1968 0.1779 1.0000 Uiso R . . . . . . H81 H 0.6581 0.1165 0.1843 0.1720 1.0000 Uiso R . . . . . . H82 H 0.7546 0.1157 0.2321 0.1720 1.0000 Uiso R . . . . . . H83 H 0.7538 0.0847 0.1513 0.1720 1.0000 Uiso R . . . . . . H91 H 0.5527 -0.1130 0.1364 0.1731 1.0000 Uiso R . . . . . . H92 H 0.5610 -0.1974 0.1373 0.1731 1.0000 Uiso R . . . . . . H93 H 0.4659 -0.1598 0.1649 0.1731 1.0000 Uiso R . . . . . . H101 H 0.5690 -0.2367 0.3331 0.1773 1.0000 Uiso R . . . . . . H102 H 0.5709 -0.2717 0.2540 0.1773 1.0000 Uiso R . . . . . . H103 H 0.4758 -0.2342 0.2816 0.1773 1.0000 Uiso R . . . . . . H104 H 0.3491 0.1253 0.5799 0.0696 1.0000 Uiso R . . . . . . H111 H 0.5073 0.1125 0.1539 0.1897 1.0000 Uiso R . . . . . . H112 H 0.4073 0.1343 0.1879 0.1897 1.0000 Uiso R . . . . . . H113 H 0.4101 0.0984 0.1093 0.1897 1.0000 Uiso R . . . . . . H114 H 0.6901 0.0882 0.4168 0.0649 1.0000 Uiso R . . . . . . H121 H 0.3084 -0.0448 0.2241 0.1914 1.0000 Uiso R . . . . . . H122 H 0.2863 0.0378 0.2316 0.1914 1.0000 Uiso R . . . . . . H123 H 0.2891 0.0020 0.1530 0.1914 1.0000 Uiso R . . . . . . H124 H 0.3693 -0.0966 0.3680 0.0681 1.0000 Uiso R . . . . . . H131 H 0.1099 -0.0952 0.2836 0.1857 1.0000 Uiso R . . . . . . H132 H 0.0084 -0.1017 0.3216 0.1857 1.0000 Uiso R . . . . . . H133 H 0.0577 -0.0259 0.3132 0.1857 1.0000 Uiso R . . . . . . H134 H 0.4119 0.1139 0.3650 0.0693 1.0000 Uiso R . . . . . . H141 H 0.0507 -0.0492 0.5043 0.1788 1.0000 Uiso R . . . . . . H142 H -0.0242 -0.0763 0.4439 0.1788 1.0000 Uiso R . . . . . . H143 H 0.0251 -0.0005 0.4355 0.1788 1.0000 Uiso R . . . . . . H151 H 0.1406 0.0613 0.2933 0.1667 1.0000 Uiso R . . . . . . H152 H 0.1722 0.1424 0.2870 0.1667 1.0000 Uiso R . . . . . . H153 H 0.0621 0.1227 0.2965 0.1667 1.0000 Uiso R . . . . . . H161 H 0.1231 0.2081 0.4705 0.1590 1.0000 Uiso R . . . . . . H162 H 0.1621 0.2283 0.3920 0.1590 1.0000 Uiso R . . . . . . H163 H 0.0520 0.2086 0.4015 0.1590 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 Cu1 0.143(3) 0.092(2) 0.097(2) -0.0021(18) 0.042(2) 0.007(2) I1 0.156(2) 0.1359(19) 0.1083(15) -0.0218(13) 0.0462(14) -0.0163(15) I2 0.1436(17) 0.1211(16) 0.0965(13) 0.0186(11) 0.0421(12) 0.0149(13) I3 0.0885(12) 0.1357(17) 0.1097(14) 0.0117(12) 0.0143(10) -0.0436(11) I4 0.1105(13) 0.0884(11) 0.0839(11) -0.0095(9) 0.0353(10) 0.0070(9) I5 0.130(2) 0.192(3) 0.187(3) 0.050(2) 0.0230(19) -0.0261(19) Y3 0.0468(10) 0.0585(11) 0.0562(11) 0.0054(9) 0.0148(8) 0.0046(9) Y2 0.0524(11) 0.0592(12) 0.0527(11) 0.0028(9) 0.0206(8) 0.0010(9) Y1 0.0559(11) 0.0504(11) 0.0599(11) 0.0033(9) 0.0201(9) 0.0000(9) S1 0.139(6) 0.097(5) 0.150(6) -0.002(5) 0.047(5) -0.005(4) S2 0.168(6) 0.114(5) 0.146(6) 0.001(5) 0.015(5) -0.028(5) S3 0.108(4) 0.073(3) 0.089(4) 0.007(3) 0.035(3) -0.004(3) S4 0.104(4) 0.102(4) 0.080(3) -0.013(3) 0.051(3) -0.025(3) S5 0.156(6) 0.133(5) 0.105(5) -0.020(4) 0.041(4) 0.003(5) S6 0.175(6) 0.192(7) 0.129(6) -0.012(6) 0.012(5) 0.019(6) S7 0.135(6) 0.157(6) 0.151(6) 0.011(5) 0.006(5) 0.000(5) S8 0.073(4) 0.116(5) 0.110(5) 0.035(4) 0.016(3) 0.004(3) O1 0.144(11) 0.077(9) 0.123(10) 0.015(8) 0.031(9) 0.004(8) O2 0.141(9) 0.078(8) 0.110(8) 0.016(7) 0.018(8) -0.010(7) O3 0.125(8) 0.082(7) 0.081(7) 0.007(6) 0.033(7) -0.016(7) O4 0.122(8) 0.109(8) 0.073(7) -0.009(6) 0.043(6) -0.018(7) O5 0.128(8) 0.119(8) 0.074(7) -0.020(7) 0.025(7) -0.006(7) O6 0.120(8) 0.136(9) 0.082(8) -0.013(7) 0.010(7) 0.011(7) O7 0.081(7) 0.119(9) 0.093(8) -0.008(7) 0.012(6) 0.000(7) O8 0.071(8) 0.109(10) 0.099(9) 0.028(8) 0.014(7) 0.000(7) O9 0.055(7) 0.088(10) 0.064(8) 0.013(7) 0.022(6) 0.021(7) O10 0.063(7) 0.047(7) 0.063(8) -0.001(6) 0.021(6) -0.010(6) O11 0.038(6) 0.059(7) 0.064(8) 0.011(6) 0.013(5) -0.004(6) O12 0.058(7) 0.073(8) 0.039(7) 0.001(6) 0.001(6) 0.000(6) O13 0.059(7) 0.055(8) 0.058(8) 0.017(6) 0.003(6) 0.004(6) O14 0.061(10) 0.036(9) 0.043(9) 0.006(7) 0.020(8) -0.008(7) C1 0.147(17) 0.168(18) 0.167(17) 0.002(16) 0.018(16) -0.010(15) C2 0.148(15) 0.164(16) 0.160(15) 0.001(14) 0.021(14) -0.007(14) C3 0.152(15) 0.167(15) 0.160(14) 0.003(13) 0.012(13) -0.004(13) C4 0.161(14) 0.175(15) 0.160(14) 0.001(13) 0.008(12) -0.005(13) C5 0.163(14) 0.180(14) 0.152(13) 0.007(12) 0.008(12) -0.005(12) C6 0.159(13) 0.172(14) 0.143(13) 0.003(12) 0.011(12) -0.007(12) C7 0.149(13) 0.160(13) 0.131(12) -0.006(11) 0.013(11) -0.006(12) C8 0.140(13) 0.158(13) 0.128(12) -0.011(11) 0.014(11) -0.006(12) C9 0.137(12) 0.160(13) 0.131(12) -0.012(11) 0.019(11) -0.011(11) C10 0.139(13) 0.164(13) 0.136(12) -0.014(11) 0.017(11) -0.013(11) C11 0.148(13) 0.173(14) 0.149(13) -0.012(12) 0.014(11) -0.011(12) C12 0.149(13) 0.174(14) 0.151(13) -0.008(12) 0.017(12) -0.006(12) C13 0.141(13) 0.173(14) 0.144(13) -0.004(12) 0.014(11) -0.009(12) C14 0.137(13) 0.168(14) 0.135(13) 0.000(12) 0.019(11) -0.015(12) C15 0.131(14) 0.160(15) 0.120(13) 0.002(12) 0.025(12) -0.014(12) C16 0.123(15) 0.151(17) 0.116(14) 0.003(13) 0.027(13) -0.017(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0710(3) 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 Y3 . Y1 2_656 3.507(3) yes Y3 . Y2 2_656 3.499(3) yes Y3 . O11 2_656 2.331(12) yes Y3 . Y2 . 3.519(2) yes Y3 . Y1 . 3.515(3) yes Y3 . O13 . 2.346(11) yes Y3 . O12 . 2.347(12) yes Y3 . O9 . 2.445(11) yes Y3 . O10 . 2.312(12) yes Y3 . O7 . 2.323(18) yes Y3 . O14 . 2.469(2) yes Y3 . O8 . 2.334(16) yes Y2 . Y1 2_656 3.523(2) yes Y2 . O10 2_656 2.314(13) yes Y2 . Y1 . 3.533(3) yes Y2 . O11 . 2.376(12) yes Y2 . O13 . 2.324(12) yes Y2 . O12 . 2.302(12) yes Y2 . O4 . 2.271(15) yes Y2 . O14 . 2.4933(18) yes Y2 . O5 . 2.324(17) yes Y2 . O6 . 2.318(19) yes Y1 . O12 2_656 2.373(12) yes Y1 . O11 . 2.291(11) yes Y1 . O13 . 2.321(13) yes Y1 . O10 . 2.369(11) yes Y1 . O1 . 2.314(18) yes Y1 . O14 . 2.4957(19) yes Y1 . O3 . 2.351(15) yes Y1 . O2 . 2.37(2) yes I2 . Cu1 2_557 2.582(4) yes I2 . Cu1 . 2.539(5) yes I1 . Cu1 . 2.531(5) yes O11 . H114 . 1.000 no O13 . H134 . 1.000 no O12 . H124 . 1.000 no O10 . H104 . 1.000 no O4 . S4 . 1.518(16) yes O7 . S7 . 1.53(2) yes O1 . S1 . 1.499(19) yes Cu1 . Cu1 2_557 2.618(8) yes S3 . O3 . 1.474(16) yes S3 . C6 . 1.64(4) yes S3 . C5 . 1.71(4) yes S4 . C7 . 1.78(4) yes S4 . C8 . 1.72(4) yes S1 . C2 . 1.65(4) yes S1 . C1 . 1.69(4) yes S8 . O8 . 1.553(18) yes S8 . C16 . 1.71(3) yes S8 . C15 . 1.77(3) yes S5 . O5 . 1.449(19) yes S5 . C10 . 1.75(4) yes S5 . C9 . 1.73(4) yes S7 . C13 . 1.77(4) yes S7 . C14 . 1.74(4) yes S2 . O2 . 1.502(19) yes S2 . C4 . 1.61(4) yes S2 . C3 . 1.70(4) yes S6 . O6 . 1.45(2) yes S6 . C12 . 1.68(4) yes S6 . C11 . 1.71(4) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C15 . H151 . 1.000 no C15 . H152 . 1.000 no C15 . H153 . 1.000 no C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C14 . H143 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 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 Y1 2_656 Y3 . Y2 2_656 60.57(6) yes Y1 2_656 Y3 . O11 2_656 40.2(3) yes Y2 2_656 Y3 . O11 2_656 42.5(3) yes Y1 2_656 Y3 . Y2 . 60.18(5) yes Y2 2_656 Y3 . Y2 . 90.55(6) yes O11 2_656 Y3 . Y2 . 98.3(3) yes Y1 2_656 Y3 . Y1 . 90.61(6) yes Y2 2_656 Y3 . Y1 . 60.29(5) yes O11 2_656 Y3 . Y1 . 100.0(3) yes Y2 . Y3 . Y1 . 60.30(5) yes Y1 2_656 Y3 . O13 . 98.6(3) yes Y2 2_656 Y3 . O13 . 98.7(3) yes O11 2_656 Y3 . O13 . 129.6(4) yes Y2 . Y3 . O13 . 40.9(3) yes Y1 . Y3 . O13 . 40.9(3) yes Y1 2_656 Y3 . O12 . 42.3(3) yes Y2 2_656 Y3 . O12 . 100.2(3) yes O11 2_656 Y3 . O12 . 79.8(4) yes Y2 . Y3 . O12 . 40.3(3) yes Y1 . Y3 . O12 . 98.6(3) yes Y1 2_656 Y3 . O9 . 116.3(3) yes Y2 2_656 Y3 . O9 . 84.3(3) yes O11 2_656 Y3 . O9 . 77.4(4) yes Y2 . Y3 . O9 . 174.8(3) yes Y1 . Y3 . O9 . 117.1(4) yes Y1 2_656 Y3 . O10 . 99.3(3) yes Y2 2_656 Y3 . O10 . 40.9(3) yes O11 2_656 Y3 . O10 . 80.7(4) yes Y2 . Y3 . O10 . 99.7(3) yes Y1 . Y3 . O10 . 41.9(3) yes Y1 2_656 Y3 . O7 . 97.6(5) yes Y2 2_656 Y3 . O7 . 140.1(5) yes O11 2_656 Y3 . O7 . 98.7(5) yes Y2 . Y3 . O7 . 107.6(4) yes Y1 . Y3 . O7 . 159.1(4) yes Y1 2_656 Y3 . O14 . 45.37(5) yes Y2 2_656 Y3 . O14 . 45.44(4) yes O11 2_656 Y3 . O14 . 65.2(3) yes Y2 . Y3 . O14 . 45.11(5) yes Y1 . Y3 . O14 . 45.24(5) yes Y1 2_656 Y3 . O8 . 165.4(4) yes Y2 2_656 Y3 . O8 . 130.7(5) yes O11 2_656 Y3 . O8 . 153.8(5) yes Y2 . Y3 . O8 . 107.5(4) yes Y1 . Y3 . O8 . 89.1(4) yes O13 . Y3 . O12 . 78.3(4) yes O13 . Y3 . O9 . 140.6(4) yes O12 . Y3 . O9 . 140.2(4) yes O13 . Y3 . O10 . 80.3(4) yes O12 . Y3 . O10 . 130.7(4) yes O9 . Y3 . O10 . 76.7(4) yes O13 . Y3 . O7 . 118.5(5) yes O12 . Y3 . O7 . 75.5(5) yes O9 . Y3 . O7 . 76.2(5) yes O10 . Y3 . O7 . 152.4(5) yes O13 . Y3 . O14 . 64.4(3) yes O12 . Y3 . O14 . 65.3(3) yes O9 . Y3 . O14 . 129.7(3) yes O10 . Y3 . O14 . 65.5(3) yes O7 . Y3 . O14 . 139.3(4) yes O13 . Y3 . O8 . 72.0(5) yes O12 . Y3 . O8 . 123.4(5) yes O9 . Y3 . O8 . 76.5(5) yes O10 . Y3 . O8 . 90.3(6) yes O7 . Y3 . O8 . 78.1(7) yes O14 . Y3 . O8 . 132.6(4) yes Y1 2_656 Y2 . Y3 . 59.74(5) yes Y1 2_656 Y2 . Y3 2_656 60.08(6) yes Y3 . Y2 . Y3 2_656 89.45(7) yes Y1 2_656 Y2 . O10 2_656 41.8(3) yes Y3 . Y2 . O10 2_656 98.9(3) yes Y3 2_656 Y2 . O10 2_656 40.8(3) yes Y1 2_656 Y2 . Y1 . 90.06(6) yes Y3 . Y2 . Y1 . 59.79(5) yes Y3 2_656 Y2 . Y1 . 59.82(6) yes O10 2_656 Y2 . Y1 . 98.5(3) yes Y1 2_656 Y2 . O11 . 98.8(3) yes Y3 . Y2 . O11 . 97.4(3) yes Y3 2_656 Y2 . O11 . 41.5(3) yes O10 2_656 Y2 . O11 . 79.7(4) yes Y1 . Y2 . O11 . 39.9(3) yes Y1 2_656 Y2 . O13 . 98.6(3) yes Y3 . Y2 . O13 . 41.3(3) yes Y3 2_656 Y2 . O13 . 97.9(3) yes O10 2_656 Y2 . O13 . 129.4(4) yes Y1 . Y2 . O13 . 40.5(3) yes Y1 2_656 Y2 . O12 . 41.9(3) yes Y3 . Y2 . O12 . 41.3(3) yes Y3 2_656 Y2 . O12 . 99.5(3) yes O10 2_656 Y2 . O12 . 81.0(4) yes Y1 . Y2 . O12 . 99.1(3) yes Y1 2_656 Y2 . O4 . 140.7(5) yes Y3 . Y2 . O4 . 156.7(5) yes Y3 2_656 Y2 . O4 . 94.5(5) yes O10 2_656 Y2 . O4 . 99.1(6) yes Y1 . Y2 . O4 . 102.8(4) yes Y1 2_656 Y2 . O14 . 45.11(4) yes Y3 . Y2 . O14 . 44.56(4) yes Y3 2_656 Y2 . O14 . 44.89(5) yes O10 2_656 Y2 . O14 . 65.0(3) yes Y1 . Y2 . O14 . 44.94(4) yes Y1 2_656 Y2 . O5 . 89.8(4) yes Y3 . Y2 . O5 . 120.0(5) yes Y3 2_656 Y2 . O5 . 120.2(5) yes O10 2_656 Y2 . O5 . 81.5(6) yes Y1 . Y2 . O5 . 179.8(5) yes Y1 2_656 Y2 . O6 . 135.1(5) yes Y3 . Y2 . O6 . 91.9(5) yes Y3 2_656 Y2 . O6 . 161.6(5) yes O10 2_656 Y2 . O6 . 156.0(6) yes Y1 . Y2 . O6 . 105.5(5) yes O11 . Y2 . O13 . 77.7(4) yes O11 . Y2 . O12 . 129.7(4) yes O13 . Y2 . O12 . 79.7(4) yes O11 . Y2 . O4 . 71.4(5) yes O13 . Y2 . O4 . 115.3(6) yes O12 . Y2 . O4 . 157.9(5) yes O11 . Y2 . O14 . 64.2(3) yes O13 . Y2 . O14 . 64.3(3) yes O12 . Y2 . O14 . 65.5(3) yes O4 . Y2 . O14 . 134.7(5) yes O11 . Y2 . O5 . 140.3(6) yes O13 . Y2 . O5 . 139.4(6) yes O12 . Y2 . O5 . 80.7(5) yes O4 . Y2 . O5 . 77.4(6) yes O14 . Y2 . O5 . 134.9(4) yes O11 . Y2 . O6 . 120.2(6) yes O13 . Y2 . O6 . 71.6(5) yes O12 . Y2 . O6 . 93.6(6) yes O4 . Y2 . O6 . 77.3(7) yes O14 . Y2 . O6 . 133.6(4) yes O5 . Y2 . O6 . 74.5(7) yes Y2 . Y1 . Y2 2_656 89.94(6) yes Y2 . Y1 . Y3 . 59.91(5) yes Y2 2_656 Y1 . Y3 . 59.63(6) yes Y2 . Y1 . Y3 2_656 59.61(6) yes Y2 2_656 Y1 . Y3 2_656 60.08(5) yes Y3 . Y1 . Y3 2_656 89.39(7) yes Y2 . Y1 . O12 2_656 98.7(3) yes Y2 2_656 Y1 . O12 2_656 40.3(3) yes Y3 . Y1 . O12 2_656 97.6(3) yes Y3 2_656 Y1 . O12 2_656 41.7(3) yes Y2 . Y1 . O11 . 41.7(3) yes Y2 2_656 Y1 . O11 . 99.1(3) yes Y3 . Y1 . O11 . 99.2(3) yes Y3 2_656 Y1 . O11 . 41.1(3) yes O12 2_656 Y1 . O11 . 80.0(4) yes Y2 . Y1 . O13 . 40.5(3) yes Y2 2_656 Y1 . O13 . 98.5(3) yes Y3 . Y1 . O13 . 41.4(3) yes Y3 2_656 Y1 . O13 . 97.8(3) yes O12 2_656 Y1 . O13 . 128.8(4) yes Y2 . Y1 . O10 . 98.2(3) yes Y2 2_656 Y1 . O10 . 40.6(3) yes Y3 . Y1 . O10 . 40.7(3) yes Y3 2_656 Y1 . O10 . 98.1(3) yes O12 2_656 Y1 . O10 . 78.4(4) yes Y2 . Y1 . O1 . 144.1(6) yes Y2 2_656 Y1 . O1 . 103.7(5) yes Y3 . Y1 . O1 . 98.5(5) yes Y3 2_656 Y1 . O1 . 154.9(5) yes O12 2_656 Y1 . O1 . 113.3(6) yes Y2 . Y1 . O14 . 44.89(4) yes Y2 2_656 Y1 . O14 . 45.06(4) yes Y3 . Y1 . O14 . 44.63(5) yes Y3 2_656 Y1 . O14 . 44.76(5) yes O12 2_656 Y1 . O14 . 64.5(3) yes Y2 . Y1 . O3 . 89.8(4) yes Y2 2_656 Y1 . O3 . 176.0(5) yes Y3 . Y1 . O3 . 116.9(5) yes Y3 2_656 Y1 . O3 . 123.0(4) yes O12 2_656 Y1 . O3 . 143.6(6) yes Y2 . Y1 . O2 . 128.4(5) yes Y2 2_656 Y1 . O2 . 107.4(4) yes Y3 . Y1 . O2 . 166.2(4) yes Y3 2_656 Y1 . O2 . 87.3(5) yes O12 2_656 Y1 . O2 . 71.2(5) yes O11 . Y1 . O13 . 79.5(4) yes O11 . Y1 . O10 . 129.6(4) yes O13 . Y1 . O10 . 79.6(4) yes O11 . Y1 . O1 . 156.1(5) yes O13 . Y1 . O1 . 104.0(6) yes O10 . Y1 . O1 . 73.9(5) yes O11 . Y1 . O14 . 65.3(3) yes O13 . Y1 . O14 . 64.3(3) yes O10 . Y1 . O14 . 64.2(3) yes O1 . Y1 . O14 . 137.8(5) yes O11 . Y1 . O3 . 83.4(5) yes O13 . Y1 . O3 . 78.7(5) yes O10 . Y1 . O3 . 135.5(6) yes O1 . Y1 . O3 . 74.3(6) yes O14 . Y1 . O3 . 134.5(4) yes O11 . Y1 . O2 . 87.0(6) yes O13 . Y1 . O2 . 152.3(5) yes O10 . Y1 . O2 . 126.7(5) yes O1 . Y1 . O2 . 79.3(7) yes O14 . Y1 . O2 . 130.6(5) yes O3 . Y1 . O2 . 75.8(6) yes Cu1 2_557 I2 . Cu1 . 61.48(16) yes Y2 . O11 . Y3 2_656 96.0(4) yes Y2 . O11 . Y1 . 98.4(4) yes Y3 2_656 O11 . Y1 . 98.7(4) yes Y2 . O11 . H114 . 119.5 no Y3 2_656 O11 . H114 . 119.6 no Y1 . O11 . H114 . 119.6 no Y3 . O13 . Y2 . 97.8(4) yes Y3 . O13 . Y1 . 97.7(5) yes Y2 . O13 . Y1 . 99.0(5) yes Y3 . O13 . H134 . 119.2 no Y2 . O13 . H134 . 119.3 no Y1 . O13 . H134 . 119.2 no Y1 2_656 O12 . Y3 . 96.0(4) yes Y1 2_656 O12 . Y2 . 97.8(5) yes Y3 . O12 . Y2 . 98.4(5) yes Y1 2_656 O12 . H124 . 119.8 no Y3 . O12 . H124 . 119.9 no Y2 . O12 . H124 . 119.9 no Y1 . O10 . Y2 2_656 97.6(5) yes Y1 . O10 . Y3 . 97.3(4) yes Y2 2_656 O10 . Y3 . 98.3(4) yes Y1 . O10 . H104 . 119.6 no Y2 2_656 O10 . H104 . 119.5 no Y3 . O10 . H104 . 119.6 no Y2 . O4 . S4 . 135.5(11) yes Y3 . O7 . S7 . 155.8(11) yes Y1 . O1 . S1 . 137.1(11) yes I2 2_557 Cu1 . I2 . 118.52(16) yes I2 2_557 Cu1 . I1 . 118.67(19) yes I2 . Cu1 . I1 . 122.54(15) yes I2 2_557 Cu1 . Cu1 2_557 58.43(14) yes I2 . Cu1 . Cu1 2_557 60.08(18) yes I1 . Cu1 . Cu1 2_557 174.1(3) yes O3 . S3 . C6 . 109.3(17) yes O3 . S3 . C5 . 110.2(17) yes C6 . S3 . C5 . 119(2) yes O4 . S4 . C7 . 100.6(16) yes O4 . S4 . C8 . 104.1(14) yes C7 . S4 . C8 . 100.3(20) yes O1 . S1 . C2 . 106.0(17) yes O1 . S1 . C1 . 100.9(17) yes C2 . S1 . C1 . 90(2) yes O8 . S8 . C16 . 103.5(15) yes O8 . S8 . C15 . 106.8(14) yes C16 . S8 . C15 . 100.4(18) yes Y1 . O14 . Y1 2_656 179.995 yes Y1 . O14 . Y2 . 90.17(6) yes Y1 2_656 O14 . Y2 . 89.83(6) yes Y1 . O14 . Y2 2_656 89.83(6) yes Y1 2_656 O14 . Y2 2_656 90.17(6) yes Y2 . O14 . Y2 2_656 179.995 yes Y1 . O14 . Y3 . 90.13(7) yes Y1 2_656 O14 . Y3 . 89.87(7) yes Y2 . O14 . Y3 . 90.33(7) yes Y2 2_656 O14 . Y3 . 89.67(7) yes Y1 . O14 . Y3 2_656 89.87(7) yes Y1 2_656 O14 . Y3 2_656 90.13(7) yes Y2 . O14 . Y3 2_656 89.67(7) yes Y2 2_656 O14 . Y3 2_656 90.33(7) yes Y3 . O14 . Y3 2_656 179.995 yes O5 . S5 . C10 . 109.0(15) yes O5 . S5 . C9 . 110.9(17) yes C10 . S5 . C9 . 102.0(19) yes O7 . S7 . C13 . 110.0(16) yes O7 . S7 . C14 . 108.1(16) yes C13 . S7 . C14 . 94.1(20) yes O2 . S2 . C4 . 105(2) yes O2 . S2 . C3 . 108.6(17) yes C4 . S2 . C3 . 98(2) yes Y1 . O3 . S3 . 147.9(10) yes Y3 . O8 . S8 . 127.5(9) yes Y2 . O5 . S5 . 157.9(13) yes Y1 . O2 . S2 . 133.6(13) yes O6 . S6 . C12 . 106.0(18) yes O6 . S6 . C11 . 101.0(18) yes C12 . S6 . C11 . 106(2) yes Y2 . O6 . S6 . 146.0(13) yes S4 . C7 . H71 . 109.6 no S4 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no S4 . C7 . H73 . 109.3 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no S4 . C8 . H81 . 109.7 no S4 . C8 . H82 . 109.6 no H81 . C8 . H82 . 109.5 no S4 . C8 . H83 . 109.1 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no S5 . C10 . H101 . 109.2 no S5 . C10 . H102 . 110.0 no H101 . C10 . H102 . 109.5 no S5 . C10 . H103 . 109.2 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no S1 . C2 . H21 . 109.1 no S1 . C2 . H22 . 109.5 no H21 . C2 . H22 . 109.5 no S1 . C2 . H23 . 109.7 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no S8 . C16 . H161 . 109.1 no S8 . C16 . H162 . 109.4 no H161 . C16 . H162 . 109.5 no S8 . C16 . H163 . 109.9 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no S8 . C15 . H151 . 109.1 no S8 . C15 . H152 . 109.5 no H151 . C15 . H152 . 109.5 no S8 . C15 . H153 . 109.8 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no S1 . C1 . H11 . 108.2 no S1 . C1 . H12 . 110.4 no H11 . C1 . H12 . 109.5 no S1 . C1 . H13 . 109.8 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no S7 . C13 . H131 . 109.9 no S7 . C13 . H132 . 108.9 no H131 . C13 . H132 . 109.5 no S7 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no S5 . C9 . H91 . 109.7 no S5 . C9 . H92 . 109.0 no H91 . C9 . H92 . 109.5 no S5 . C9 . H93 . 109.7 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no S6 . C12 . H121 . 109.9 no S6 . C12 . H122 . 109.7 no H121 . C12 . H122 . 109.5 no S6 . C12 . H123 . 108.8 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no S2 . C4 . H41 . 109.4 no S2 . C4 . H42 . 109.3 no H41 . C4 . H42 . 109.5 no S2 . C4 . H43 . 109.7 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no S7 . C14 . H141 . 109.4 no S7 . C14 . H142 . 109.3 no H141 . C14 . H142 . 109.5 no S7 . C14 . H143 . 109.8 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no S2 . C3 . H31 . 109.8 no S2 . C3 . H32 . 109.5 no H31 . C3 . H32 . 109.5 no S2 . C3 . H33 . 109.1 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no S6 . C11 . H111 . 109.3 no S6 . C11 . H112 . 109.2 no H111 . C11 . H112 . 109.5 no S6 . C11 . H113 . 109.8 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no S3 . C6 . H61 . 109.6 no S3 . C6 . H62 . 109.1 no H61 . C6 . H62 . 109.5 no S3 . C6 . H63 . 109.7 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no S3 . C5 . H51 . 109.8 no S3 . C5 . H52 . 108.6 no H51 . C5 . H52 . 109.5 no S3 . C5 . H53 . 110.1 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 670606' _audit_creation_date 07-10-12 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'import in C 2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 23.93380(40) _cell_length_b 18.24150(40) _cell_length_c 23.86040(40) _cell_angle_alpha 90.0000 _cell_angle_beta 110.4417(11) _cell_angle_gamma 90.0000 _cell_volume 9761.184(322) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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' 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' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Y -2.7962 3.5667 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C60 H140 Br1 Cl1 Cu5 I12.50 N1 O20 S20 Y2.50 # Dc = 2.77 Fooo = 6544.00 Mu = 74.14 M = 2039.37 # Found Formula = C28 H100 Cu2 I12 O27 S14 Y6 # Dc = 2.38 FOOO = 6544.00 Mu = 80.94 M = 1750.69 _chemical_formula_sum 'C28 H100 Cu2 I12 O27 S14 Y6' _chemical_formula_moiety ; C28 H100 O27 S14 Y6, 2(Cu I3), I3, 3(I) ; _chemical_compound_source ? _chemical_formula_weight 3501.39 _cell_measurement_reflns_used 70453 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'reddish yellow' _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 2.381 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 6544 _exptl_absorpt_coefficient_mu 8.094 # Sheldrick geometric approximatio 0.27 0.33 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.20 _exptl_absorpt_correction_T_max 0.33 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11273 _reflns_number_total 10964 _diffrn_reflns_av_R_equivalents 0.037 # Number of reflections with Friedels Law is 10964 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12465 _diffrn_reflns_theta_min 1.438 _diffrn_reflns_theta_max 28.569 _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 25.141 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -32 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.35 _refine_diff_density_max 3.46 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5335 _refine_ls_number_restraints 24 _refine_ls_number_parameters 405 _oxford_refine_ls_R_factor_ref 0.0497 _refine_ls_wR_factor_ref 0.0610 _refine_ls_goodness_of_fit_ref 1.0864 _refine_ls_shift/su_max 0.000640 # The values computed from all data _oxford_reflns_number_all 10931 _refine_ls_R_factor_all 0.1043 _refine_ls_wR_factor_all 0.1005 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6290 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_gt 0.0663 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_special_details ; The atoms of one of the DMSO molecules showed physically incorrect displacement parameters. Its anisotropic displacement parameters thus had to be restrained in order for the model to be reasonable. They were restrained to be similar to a those of a neighbouring DMSO molecule. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _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: 1.53 0.202 0.958 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.58590(7) 0.83432(9) 0.61032(7) 0.0445 1.0000 Uani . . . . . . . I1 I 0.59288(4) 0.85734(5) 0.71928(4) 0.0476 1.0000 Uani . . . . . . . I2 I 0.49298(3) 0.89668(5) 0.53840(4) 0.0423 1.0000 Uani . . . . . . . I3 I 0.65343(4) 0.76494(6) 0.56974(4) 0.0545 1.0000 Uani . . . . . . . I4 I 0.33928(4) 0.46932(5) 0.21334(4) 0.0422 1.0000 Uani . . . . . . . I5 I 0.5000 0.5000 0.5000 0.0643 1.0000 Uani S . . . . . . I6 I 0.5000 0.77637(13) 0.2500 0.1820 1.0000 Uani S T . . . . . I7 I 0.38354(16) 0.77600(13) 0.17032(15) 0.2064 1.0000 Uani . . . . . . . Y1 Y 0.29939(5) 0.75595(6) 0.42315(5) 0.0294 1.0000 Uani . . . . . . . Y2 Y 0.23473(5) 0.61411(6) 0.48219(5) 0.0300 1.0000 Uani . . . . . . . Y3 Y 0.15400(4) 0.77235(6) 0.42180(5) 0.0295 1.0000 Uani . . . . . . . S1 S 0.43155(15) 0.72090(19) 0.38762(17) 0.0491 1.0000 Uani . . . . . . . S2 S 0.34218(14) 0.91698(18) 0.34774(15) 0.0443 1.0000 Uani . . . . . . . S3 S 0.28913(13) 0.74012(19) 0.27244(13) 0.0411 1.0000 Uani . . . . . . . S4 S 0.28822(14) 0.53311(17) 0.37035(14) 0.0406 1.0000 Uani . . . . . . . S5 S 0.13355(15) 0.47293(18) 0.40410(17) 0.0474 1.0000 Uani . U . . . . . S6 S 0.2861(3) 0.4325(3) 0.5590(4) 0.1157 1.0000 Uani . U . . . . . S7 S 0.02103(15) 0.8642(2) 0.34452(15) 0.0507 1.0000 Uani . . . . . . . O1 O 0.3871(4) 0.7052(5) 0.4178(4) 0.0521 1.0000 Uani . . . . . . . O2 O 0.3391(4) 0.8495(5) 0.3820(5) 0.0546 1.0000 Uani . . . . . . . O3 O 0.2665(4) 0.7221(5) 0.3223(4) 0.0504 1.0000 Uani . . . . . . . O4 O 0.2653(4) 0.5323(5) 0.4220(4) 0.0508 1.0000 Uani . . . . . . . O5 O 0.1499(4) 0.5460(5) 0.4356(4) 0.0517 1.0000 Uani . U . . . . . O6 O 0.2593(5) 0.5057(5) 0.5363(5) 0.0649 1.0000 Uani . U . . . . . O7 O 0.0789(4) 0.8577(5) 0.3995(4) 0.0491 1.0000 Uani . . . . . . . O8 O 0.0700(4) 0.6951(5) 0.3673(4) 0.0453 1.0000 Uani . . . . . . . O9 O 0.1280(4) 0.7926(5) 0.3154(3) 0.0405 1.0000 Uani . . . . . . . O10 O 0.1519(3) 0.6809(4) 0.4896(3) 0.0322 1.0000 Uani . . . . . . . O11 O 0.2109(3) 0.6843(4) 0.3968(3) 0.0336 1.0000 Uani . . . . . . . O12 O 0.2703(3) 0.6506(4) 0.5832(3) 0.0319 1.0000 Uani . . . . . . . O13 O 0.3291(3) 0.6581(4) 0.4915(3) 0.0335 1.0000 Uani . . . . . . . O14 O 0.2500 0.7500 0.5000 0.0283 1.0000 Uani S . . . . . . C1 C 0.5024(7) 0.7175(10) 0.4453(8) 0.0695 1.0000 Uani . . . . . . . C2 C 0.4364(6) 0.6372(8) 0.3522(6) 0.0544 1.0000 Uani . . . . . . . C3 C 0.3431(7) 0.9930(8) 0.3952(7) 0.0597 1.0000 Uani . . . . . . . C4 C 0.4175(6) 0.9223(8) 0.3517(7) 0.0570 1.0000 Uani . . . . . . . C5 C 0.2693(7) 0.6626(7) 0.2247(6) 0.0522 1.0000 Uani . . . . . . . C6 C 0.2358(7) 0.8028(8) 0.2270(6) 0.0611 1.0000 Uani . . . . . . . C7 C 0.2288(6) 0.4993(9) 0.3085(6) 0.0546 1.0000 Uani . . . . . . . C8 C 0.3361(7) 0.4571(10) 0.3827(7) 0.0708 1.0000 Uani . . . . . . . C9 C 0.0688(8) 0.4923(10) 0.3404(8) 0.0750 1.0000 Uani . U . . . . . C10 C 0.0980(8) 0.4228(10) 0.4456(8) 0.0702 1.0000 Uani . U . . . . . C11 C 0.2642(9) 0.3680(11) 0.5049(10) 0.0934 1.0000 Uani . U . . . . . C12 C 0.3583(10) 0.4484(13) 0.5607(10) 0.1009 1.0000 Uani . U . . . . . C13 C 0.0097(6) 0.9603(8) 0.3349(7) 0.0551 1.0000 Uani . . . . . . . C14 C -0.0368(6) 0.8438(8) 0.3715(7) 0.0563 1.0000 Uani . . . . . . . H11 H 0.5051 0.7554 0.4740 0.1040 1.0000 Uiso R . . . . . . H12 H 0.5330 0.7243 0.4284 0.1040 1.0000 Uiso R . . . . . . H13 H 0.5073 0.6705 0.4647 0.1040 1.0000 Uiso R . . . . . . H17 H 0.0626 0.6746 0.3944 0.0690 1.0000 Uiso R . . . . . . H19 H 0.2792 0.6220 0.6114 0.0471 1.0000 Uiso R . . . . . . H21 H 0.3985 0.6257 0.3226 0.0821 1.0000 Uiso R . . . . . . H22 H 0.4657 0.6419 0.3334 0.0821 1.0000 Uiso R . . . . . . H23 H 0.4479 0.5989 0.3816 0.0820 1.0000 Uiso R . . . . . . H31 H 0.3046 0.9980 0.3991 0.0899 1.0000 Uiso R . . . . . . H32 H 0.3525 1.0368 0.3781 0.0901 1.0000 Uiso R . . . . . . H33 H 0.3727 0.9849 0.4340 0.0900 1.0000 Uiso R . . . . . . H35 H 0.1230 0.6547 0.4734 0.0489 1.0000 Uiso R . . . . . . H38 H 0.3553 0.6305 0.4898 0.0510 1.0000 Uiso R . . . . . . H41 H 0.4254 0.8836 0.3280 0.0869 1.0000 Uiso R . . . . . . H42 H 0.4243 0.9688 0.3365 0.0870 1.0000 Uiso R . . . . . . H43 H 0.4437 0.9171 0.3926 0.0871 1.0000 Uiso R . . . . . . H50 H 0.2039 0.6718 0.3621 0.0509 1.0000 Uiso R . . . . . . H51 H 0.2906 0.6207 0.2458 0.0810 1.0000 Uiso R . . . . . . H52 H 0.2799 0.6713 0.1900 0.0810 1.0000 Uiso R . . . . . . H53 H 0.2272 0.6538 0.2128 0.0810 1.0000 Uiso R . . . . . . H55 H 0.1356 0.8306 0.3009 0.0600 1.0000 Uiso R . . . . . . H61 H 0.2366 0.8474 0.2488 0.0910 1.0000 Uiso R . . . . . . H62 H 0.2448 0.8135 0.1917 0.0910 1.0000 Uiso R . . . . . . H63 H 0.1969 0.7811 0.2157 0.0910 1.0000 Uiso R . . . . . . H67 H 0.0425 0.6902 0.3353 0.0691 1.0000 Uiso R . . . . . . H71 H 0.1963 0.5335 0.2980 0.0840 1.0000 Uiso R . . . . . . H72 H 0.2160 0.4532 0.3189 0.0840 1.0000 Uiso R . . . . . . H73 H 0.2420 0.4927 0.2753 0.0841 1.0000 Uiso R . . . . . . H81 H 0.3722 0.4674 0.4155 0.1040 1.0000 Uiso R . . . . . . H82 H 0.3168 0.4151 0.3920 0.1040 1.0000 Uiso R . . . . . . H83 H 0.3452 0.4476 0.3472 0.1040 1.0000 Uiso R . . . . . . H91 H 0.0803 0.5199 0.3120 0.1100 1.0000 Uiso R . . . . . . H92 H 0.0412 0.5207 0.3525 0.1100 1.0000 Uiso R . . . . . . H93 H 0.0501 0.4474 0.3224 0.1100 1.0000 Uiso R . . . . . . H101 H 0.1263 0.4126 0.4847 0.1090 1.0000 Uiso R . . . . . . H102 H 0.0657 0.4513 0.4493 0.1090 1.0000 Uiso R . . . . . . H103 H 0.0828 0.3778 0.4252 0.1090 1.0000 Uiso R . . . . . . H111 H 0.2218 0.3602 0.4934 0.1351 1.0000 Uiso R . . . . . . H112 H 0.2852 0.3230 0.5203 0.1351 1.0000 Uiso R . . . . . . H113 H 0.2735 0.3842 0.4707 0.1351 1.0000 Uiso R . . . . . . H121 H 0.3785 0.4807 0.5934 0.1470 1.0000 Uiso R . . . . . . H122 H 0.3795 0.4023 0.5662 0.1469 1.0000 Uiso R . . . . . . H123 H 0.3569 0.4705 0.5237 0.1471 1.0000 Uiso R . . . . . . H124 H 0.1304 0.7695 0.2869 0.0601 1.0000 Uiso R . . . . . . H131 H 0.0407 0.9813 0.3229 0.0810 1.0000 Uiso R . . . . . . H132 H -0.0283 0.9697 0.3044 0.0811 1.0000 Uiso R . . . . . . H133 H 0.0107 0.9823 0.3719 0.0810 1.0000 Uiso R . . . . . . H141 H -0.0339 0.7934 0.3841 0.0869 1.0000 Uiso R . . . . . . H142 H -0.0747 0.8516 0.3403 0.0870 1.0000 Uiso R . . . . . . H143 H -0.0338 0.8752 0.4049 0.0870 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 Cu1 0.0403(8) 0.0481(9) 0.0451(9) 0.0033(7) 0.0149(7) -0.0019(7) I1 0.0542(5) 0.0481(5) 0.0407(5) 0.0047(4) 0.0169(4) 0.0043(4) I2 0.0332(4) 0.0474(5) 0.0463(5) 0.0059(4) 0.0140(3) -0.0024(3) I3 0.0458(5) 0.0761(6) 0.0427(5) 0.0074(4) 0.0167(4) 0.0124(4) I4 0.0434(4) 0.0431(5) 0.0424(5) -0.0051(4) 0.0178(4) 0.0021(3) I5 0.0858(10) 0.0621(9) 0.0404(7) -0.0027(6) 0.0161(7) -0.0142(7) I6 0.320(5) 0.0787(15) 0.270(4) 0.0000 0.258(4) 0.0000 I7 0.313(4) 0.1303(17) 0.289(3) 0.0610(19) 0.246(3) 0.0015(19) Y1 0.0284(5) 0.0342(6) 0.0269(5) -0.0011(5) 0.0115(4) -0.0028(4) Y2 0.0274(5) 0.0344(6) 0.0290(6) -0.0017(5) 0.0108(4) -0.0015(4) Y3 0.0278(5) 0.0343(6) 0.0271(6) -0.0007(5) 0.0103(4) -0.0028(4) S1 0.0466(18) 0.0474(19) 0.061(2) 0.0055(16) 0.0282(16) 0.0048(14) S2 0.0405(16) 0.0469(18) 0.0468(18) 0.0047(15) 0.0169(14) -0.0056(14) S3 0.0392(15) 0.0548(19) 0.0308(15) -0.0010(14) 0.0142(12) -0.0019(14) S4 0.0433(16) 0.0422(17) 0.0403(17) -0.0040(14) 0.0199(14) -0.0024(14) S5 0.0455(17) 0.0396(17) 0.064(2) -0.0084(15) 0.0271(16) -0.0096(14) S6 0.093(4) 0.076(3) 0.153(5) -0.002(3) 0.012(4) 0.001(3) S7 0.0392(17) 0.066(2) 0.0408(18) -0.0128(16) 0.0060(14) 0.0128(15) O1 0.050(5) 0.061(6) 0.059(6) 0.018(5) 0.036(5) 0.015(4) O2 0.068(6) 0.036(5) 0.075(7) 0.002(4) 0.043(5) -0.007(4) O3 0.053(5) 0.071(6) 0.034(5) -0.017(4) 0.025(4) -0.019(5) O4 0.057(5) 0.055(5) 0.049(5) -0.019(4) 0.030(4) -0.012(4) O5 0.048(5) 0.037(4) 0.073(6) -0.014(4) 0.025(4) -0.007(4) O6 0.090(6) 0.037(5) 0.056(5) 0.000(4) 0.012(5) 0.019(4) O7 0.038(5) 0.063(6) 0.041(5) -0.008(4) 0.007(4) 0.015(4) O8 0.039(5) 0.061(6) 0.036(5) 0.002(4) 0.014(4) -0.012(4) O9 0.052(5) 0.044(5) 0.025(4) 0.004(4) 0.014(4) -0.005(4) O10 0.030(4) 0.039(4) 0.028(4) -0.001(3) 0.012(3) -0.003(3) O11 0.034(4) 0.041(4) 0.028(4) -0.009(3) 0.014(3) -0.010(3) O12 0.031(4) 0.037(4) 0.026(4) 0.003(3) 0.009(3) -0.005(3) O13 0.031(4) 0.038(4) 0.032(4) -0.002(3) 0.011(3) 0.000(3) O14 0.028(5) 0.032(6) 0.027(5) 0.000(4) 0.012(4) 0.001(4) C1 0.055(9) 0.072(11) 0.079(11) -0.013(9) 0.021(8) 0.002(8) C2 0.053(8) 0.066(9) 0.046(8) -0.002(7) 0.019(7) 0.014(7) C3 0.058(9) 0.052(8) 0.070(10) -0.010(8) 0.024(8) -0.010(7) C4 0.053(8) 0.053(9) 0.069(10) 0.002(7) 0.025(7) -0.008(7) C5 0.067(9) 0.042(7) 0.053(8) -0.003(6) 0.027(7) 0.012(6) C6 0.083(11) 0.053(9) 0.044(8) -0.003(7) 0.018(8) 0.008(8) C7 0.049(8) 0.071(9) 0.044(8) -0.003(7) 0.016(6) 0.015(7) C8 0.069(10) 0.087(12) 0.051(9) -0.014(8) 0.015(8) 0.038(9) C9 0.073(9) 0.071(9) 0.077(10) -0.001(8) 0.021(8) -0.009(7) C10 0.080(10) 0.071(9) 0.069(9) 0.019(8) 0.038(8) -0.003(8) C11 0.086(10) 0.080(10) 0.105(11) -0.008(9) 0.022(9) -0.008(8) C12 0.104(11) 0.096(11) 0.095(11) 0.010(9) 0.025(9) 0.007(9) C13 0.057(8) 0.053(8) 0.052(9) 0.005(7) 0.015(7) 0.011(7) C14 0.051(8) 0.056(9) 0.065(9) 0.000(7) 0.024(7) -0.006(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.06835(13) 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 I2 . Cu1 . 2.5534(18) yes I3 . Cu1 . 2.4994(19) yes I1 . Cu1 . 2.5815(19) yes Y2 . Y1 4_566 3.5613(16) yes Y2 . Y3 4_566 3.5174(16) yes Y2 . Y3 . 3.4934(17) yes Y2 . Y1 . 3.5503(16) yes Y2 . O14 . 2.5211(13) yes Y2 . O11 . 2.304(8) yes Y2 . O13 . 2.333(7) yes Y2 . O4 . 2.358(8) yes Y2 . O5 . 2.309(9) yes Y2 . O10 . 2.386(7) yes Y2 . O12 . 2.356(7) yes Y2 . O6 . 2.323(10) yes Y3 . O13 4_566 2.338(7) yes Y3 . O12 4_566 2.329(7) yes Y3 . O14 . 2.4356(11) yes Y3 . O11 . 2.317(8) yes Y3 . O7 . 2.296(8) yes Y3 . O10 . 2.338(7) yes Y3 . O9 . 2.423(8) yes Y3 . O8 . 2.427(8) yes Y1 . O12 4_566 2.352(8) yes Y1 . O10 4_566 2.307(7) yes Y1 . O14 . 2.5076(11) yes Y1 . O11 . 2.379(7) yes Y1 . O13 . 2.354(8) yes Y1 . O1 . 2.339(8) yes Y1 . O2 . 2.331(9) yes Y1 . O3 . 2.339(8) yes O11 . H50 . 0.817 no O13 . H38 . 0.817 no S4 . O4 . 1.515(9) yes S4 . C7 . 1.764(14) yes S4 . C8 . 1.758(14) yes C7 . H71 . 0.959 no C7 . H72 . 0.958 no C7 . H73 . 0.959 no S1 . O1 . 1.505(9) yes S1 . C2 . 1.770(14) yes S1 . C1 . 1.773(16) yes C2 . H21 . 0.958 no C2 . H22 . 0.958 no C2 . H23 . 0.961 no S2 . O2 . 1.494(9) yes S2 . C4 . 1.775(14) yes S2 . C3 . 1.785(15) yes C4 . H41 . 0.963 no C4 . H42 . 0.960 no C4 . H43 . 0.963 no C3 . H31 . 0.963 no C3 . H32 . 0.960 no C3 . H33 . 0.960 no S3 . O3 . 1.507(9) yes S3 . C5 . 1.774(14) yes S3 . C6 . 1.774(15) yes C5 . H51 . 0.958 no C5 . H52 . 0.960 no C5 . H53 . 0.960 no C6 . H61 . 0.963 no C6 . H62 . 0.960 no C6 . H63 . 0.959 no S5 . O5 . 1.514(9) yes S5 . C9 . 1.787(17) yes S5 . C10 . 1.770(15) yes C9 . H91 . 0.959 no C9 . H92 . 0.959 no C9 . H93 . 0.959 no C10 . H101 . 0.960 no C10 . H102 . 0.960 no C10 . H103 . 0.960 no S7 . O7 . 1.544(9) yes S7 . C14 . 1.759(14) yes S7 . C13 . 1.776(14) yes C14 . H141 . 0.963 no C14 . H142 . 0.962 no C14 . H143 . 0.964 no C13 . H131 . 0.962 no C13 . H132 . 0.960 no C13 . H133 . 0.962 no O10 . H35 . 0.818 no O12 . H19 . 0.818 no O6 . S6 . 1.499(11) yes S6 . C12 . 1.74(2) yes S6 . C11 . 1.69(2) yes O9 . H55 . 0.822 no O9 . H124 . 0.819 no O8 . H17 . 0.819 no O8 . H67 . 0.820 no C1 . H11 . 0.959 no C1 . H12 . 0.960 no C1 . H13 . 0.962 no C8 . H81 . 0.960 no C8 . H82 . 0.959 no C8 . H83 . 0.961 no C12 . H121 . 0.962 no C12 . H122 . 0.967 no C12 . H123 . 0.960 no C11 . H111 . 0.966 no C11 . H112 . 0.966 no C11 . H113 . 0.965 no I6 . I7 5_655 2.772(4) yes I6 . I7 . 2.772(4) yes 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 Y1 4_566 Y2 . Y3 4_566 58.92(3) yes Y1 4_566 Y2 . Y3 . 59.66(3) yes Y3 4_566 Y2 . Y3 . 88.02(4) yes Y1 4_566 Y2 . Y1 . 89.69(4) yes Y3 4_566 Y2 . Y1 . 59.55(3) yes Y3 . Y2 . Y1 . 59.24(3) yes Y1 4_566 Y2 . O14 . 44.76(3) yes Y3 4_566 Y2 . O14 . 43.82(3) yes Y3 . Y2 . O14 . 44.20(3) yes Y1 . Y2 . O14 . 44.93(3) yes Y1 4_566 Y2 . O11 . 98.67(19) yes Y3 4_566 Y2 . O11 . 98.39(18) yes Y3 . Y2 . O11 . 41.02(19) yes Y1 . Y2 . O11 . 41.49(17) yes O14 . Y2 . O11 . 65.11(18) yes Y1 4_566 Y2 . O13 . 97.98(19) yes Y3 4_566 Y2 . O13 . 41.20(18) yes Y3 . Y2 . O13 . 97.58(19) yes Y1 . Y2 . O13 . 40.99(18) yes O14 . Y2 . O13 . 64.31(19) yes Y1 4_566 Y2 . O4 . 175.3(2) yes Y3 4_566 Y2 . O4 . 116.4(2) yes Y3 . Y2 . O4 . 121.1(2) yes Y1 . Y2 . O4 . 87.1(2) yes O14 . Y2 . O4 . 131.9(2) yes Y1 4_566 Y2 . O5 . 107.8(2) yes Y3 4_566 Y2 . O5 . 165.8(2) yes Y3 . Y2 . O5 . 88.9(2) yes Y1 . Y2 . O5 . 129.4(3) yes O14 . Y2 . O5 . 131.5(2) yes Y1 4_566 Y2 . O10 . 39.83(18) yes Y3 4_566 Y2 . O10 . 96.33(18) yes Y3 . Y2 . O10 . 41.79(18) yes Y1 . Y2 . O10 . 98.39(18) yes O14 . Y2 . O10 . 63.92(18) yes Y1 4_566 Y2 . O12 . 40.81(18) yes Y3 4_566 Y2 . O12 . 41.06(17) yes Y3 . Y2 . O12 . 97.95(19) yes Y1 . Y2 . O12 . 98.52(18) yes O14 . Y2 . O12 . 64.52(18) yes Y1 4_566 Y2 . O6 . 106.5(3) yes Y3 4_566 Y2 . O6 . 98.8(3) yes Y3 . Y2 . O6 . 158.3(3) yes Y1 . Y2 . O6 . 141.3(3) yes O14 . Y2 . O6 . 138.6(3) yes O11 . Y2 . O13 . 79.9(3) yes O11 . Y2 . O4 . 81.2(3) yes O13 . Y2 . O4 . 77.3(3) yes O11 . Y2 . O5 . 88.3(3) yes O13 . Y2 . O5 . 153.0(3) yes O4 . Y2 . O5 . 76.9(3) yes O11 . Y2 . O10 . 80.1(3) yes O13 . Y2 . O10 . 128.2(3) yes O4 . Y2 . O10 . 144.2(3) yes O5 . Y2 . O10 . 72.3(3) yes O11 . Y2 . O12 . 129.6(3) yes O13 . Y2 . O12 . 79.2(3) yes O4 . Y2 . O12 . 136.4(3) yes O5 . Y2 . O12 . 126.0(3) yes O10 . Y2 . O12 . 78.0(3) yes O11 . Y2 . O6 . 154.3(3) yes O13 . Y2 . O6 . 101.1(3) yes O4 . Y2 . O6 . 74.2(4) yes O5 . Y2 . O6 . 79.5(4) yes O10 . Y2 . O6 . 116.7(3) yes O12 . Y2 . O6 . 75.0(3) yes Y2 4_566 Y3 . Y2 . 91.98(4) yes Y2 4_566 Y3 . O13 4_566 41.08(18) yes Y2 . Y3 . O13 4_566 100.58(19) yes Y2 4_566 Y3 . O12 4_566 41.64(18) yes Y2 . Y3 . O12 4_566 101.07(19) yes O13 4_566 Y3 . O12 4_566 79.7(3) yes Y2 4_566 Y3 . O14 . 45.79(3) yes Y2 . Y3 . O14 . 46.19(3) yes O13 4_566 Y3 . O14 . 65.63(18) yes O12 4_566 Y3 . O14 . 66.30(18) yes Y2 4_566 Y3 . O11 . 101.37(18) yes Y2 . Y3 . O11 . 40.75(19) yes O13 4_566 Y3 . O11 . 132.0(3) yes O12 4_566 Y3 . O11 . 82.4(3) yes O14 . Y3 . O11 . 66.36(18) yes Y2 4_566 Y3 . O7 . 96.0(2) yes Y2 . Y3 . O7 . 158.7(2) yes O13 4_566 Y3 . O7 . 73.6(3) yes O12 4_566 Y3 . O7 . 98.0(3) yes O14 . Y3 . O7 . 138.1(2) yes Y2 4_566 Y3 . O10 . 99.45(18) yes Y2 . Y3 . O10 . 42.85(18) yes O13 4_566 Y3 . O10 . 79.3(3) yes O12 4_566 Y3 . O10 . 132.2(3) yes O14 . Y3 . O10 . 65.96(18) yes Y2 4_566 Y3 . O9 . 116.85(19) yes Y2 . Y3 . O9 . 117.5(2) yes O13 4_566 Y3 . O9 . 138.3(3) yes O12 4_566 Y3 . O9 . 76.9(3) yes O14 . Y3 . O9 . 131.1(2) yes Y2 4_566 Y3 . O8 . 171.1(2) yes Y2 . Y3 . O8 . 88.6(2) yes O13 4_566 Y3 . O8 . 130.1(3) yes O12 4_566 Y3 . O8 . 146.7(3) yes O14 . Y3 . O8 . 134.1(2) yes O11 . Y3 . O7 . 153.4(3) yes O11 . Y3 . O10 . 80.8(3) yes O7 . Y3 . O10 . 116.1(3) yes O11 . Y3 . O9 . 78.1(3) yes O7 . Y3 . O9 . 76.1(3) yes O10 . Y3 . O9 . 140.8(3) yes O11 . Y3 . O8 . 84.8(3) yes O7 . Y3 . O8 . 80.5(3) yes O10 . Y3 . O8 . 75.1(3) yes O9 . Y3 . O8 . 70.5(3) yes Y2 4_566 Y1 . Y2 . 90.31(4) yes Y2 4_566 Y1 . O12 4_566 40.90(17) yes Y2 . Y1 . O12 4_566 99.01(18) yes Y2 4_566 Y1 . O10 4_566 41.48(18) yes Y2 . Y1 . O10 4_566 99.16(18) yes O12 4_566 Y1 . O10 4_566 79.6(3) yes Y2 4_566 Y1 . O14 . 45.06(3) yes Y2 . Y1 . O14 . 45.24(3) yes O12 4_566 Y1 . O14 . 64.79(18) yes O10 4_566 Y1 . O14 . 65.21(18) yes Y2 4_566 Y1 . O11 . 98.86(18) yes Y2 . Y1 . O11 . 39.92(19) yes O12 4_566 Y1 . O11 . 80.6(3) yes O10 4_566 Y1 . O11 . 129.5(3) yes O14 . Y1 . O11 . 64.31(18) yes Y2 4_566 Y1 . O13 . 98.38(19) yes Y2 . Y1 . O13 . 40.53(18) yes O12 4_566 Y1 . O13 . 129.0(3) yes O10 4_566 Y1 . O13 . 79.6(3) yes O14 . Y1 . O13 . 64.24(18) yes Y2 4_566 Y1 . O1 . 135.1(3) yes Y2 . Y1 . O1 . 104.9(2) yes O12 4_566 Y1 . O1 . 155.9(3) yes O10 4_566 Y1 . O1 . 93.8(3) yes O14 . Y1 . O1 . 133.2(2) yes Y2 4_566 Y1 . O2 . 89.8(2) yes Y2 . Y1 . O2 . 178.3(3) yes O12 4_566 Y1 . O2 . 80.0(3) yes O10 4_566 Y1 . O2 . 82.1(3) yes O14 . Y1 . O2 . 134.8(2) yes Y2 4_566 Y1 . O3 . 139.4(2) yes Y2 . Y1 . O3 . 100.3(2) yes O12 4_566 Y1 . O3 . 98.5(3) yes O10 4_566 Y1 . O3 . 160.5(3) yes O14 . Y1 . O3 . 131.7(2) yes O11 . Y1 . O13 . 78.0(3) yes O11 . Y1 . O1 . 120.0(3) yes O13 . Y1 . O1 . 71.3(3) yes O11 . Y1 . O2 . 138.4(3) yes O13 . Y1 . O2 . 141.1(3) yes O1 . Y1 . O2 . 76.2(3) yes O11 . Y1 . O3 . 68.5(3) yes O13 . Y1 . O3 . 115.1(3) yes O1 . Y1 . O3 . 79.9(3) yes O2 . Y1 . O3 . 78.5(3) yes Y2 . O14 . Y2 4_566 179.995 yes Y2 . O14 . Y1 4_566 90.18(4) yes Y2 4_566 O14 . Y1 4_566 89.82(4) yes Y2 . O14 . Y1 . 89.82(4) yes Y2 4_566 O14 . Y1 . 90.18(4) yes Y1 4_566 O14 . Y1 . 179.995 yes Y2 . O14 . Y3 4_566 90.39(4) yes Y2 4_566 O14 . Y3 4_566 89.61(4) yes Y1 4_566 O14 . Y3 4_566 89.54(4) yes Y1 . O14 . Y3 4_566 90.46(4) yes Y2 . O14 . Y3 . 89.61(4) yes Y2 4_566 O14 . Y3 . 90.39(4) yes Y1 4_566 O14 . Y3 . 90.46(4) yes Y1 . O14 . Y3 . 89.54(4) yes Y3 4_566 O14 . Y3 . 179.995 yes Y1 . O11 . Y3 . 95.7(3) yes Y1 . O11 . Y2 . 98.6(3) yes Y3 . O11 . Y2 . 98.2(3) yes Y1 . O11 . H50 . 105.6 no Y3 . O11 . H50 . 121.6 no Y2 . O11 . H50 . 129.9 no Y1 . O13 . Y3 4_566 96.8(3) yes Y1 . O13 . Y2 . 98.5(3) yes Y3 4_566 O13 . Y2 . 97.7(3) yes Y1 . O13 . H38 . 119.0 no Y3 4_566 O13 . H38 . 118.7 no Y2 . O13 . H38 . 121.2 no I1 . Cu1 . I2 . 109.83(6) yes I1 . Cu1 . I3 . 130.53(7) yes I2 . Cu1 . I3 . 119.65(7) yes O4 . S4 . C7 . 105.2(6) yes O4 . S4 . C8 . 104.9(7) yes C7 . S4 . C8 . 98.7(7) yes Y2 . O4 . S4 . 140.1(6) yes S4 . C7 . H71 . 109.6 no S4 . C7 . H72 . 109.1 no H71 . C7 . H72 . 109.5 no S4 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.7 no H72 . C7 . H73 . 109.4 no O1 . S1 . C2 . 103.9(7) yes O1 . S1 . C1 . 105.4(7) yes C2 . S1 . C1 . 97.8(7) yes Y1 . O1 . S1 . 138.5(5) yes S1 . C2 . H21 . 109.8 no S1 . C2 . H22 . 109.1 no H21 . C2 . H22 . 109.5 no S1 . C2 . H23 . 109.1 no H21 . C2 . H23 . 109.6 no H22 . C2 . H23 . 109.7 no O2 . S2 . C4 . 105.1(6) yes O2 . S2 . C3 . 106.5(7) yes C4 . S2 . C3 . 97.8(7) yes Y1 . O2 . S2 . 160.0(6) yes S2 . C4 . H41 . 109.4 no S2 . C4 . H42 . 109.4 no H41 . C4 . H42 . 109.3 no S2 . C4 . H43 . 109.8 no H41 . C4 . H43 . 109.4 no H42 . C4 . H43 . 109.5 no S2 . C3 . H31 . 109.6 no S2 . C3 . H32 . 109.3 no H31 . C3 . H32 . 109.7 no S2 . C3 . H33 . 109.5 no H31 . C3 . H33 . 109.3 no H32 . C3 . H33 . 109.5 no O3 . S3 . C5 . 104.1(6) yes O3 . S3 . C6 . 104.1(7) yes C5 . S3 . C6 . 98.5(7) yes Y1 . O3 . S3 . 132.1(5) yes S3 . C5 . H51 . 108.9 no S3 . C5 . H52 . 109.1 no H51 . C5 . H52 . 109.4 no S3 . C5 . H53 . 110.0 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.8 no S3 . C6 . H61 . 109.8 no S3 . C6 . H62 . 109.6 no H61 . C6 . H62 . 109.5 no S3 . C6 . H63 . 109.0 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.4 no O5 . S5 . C9 . 104.2(7) yes O5 . S5 . C10 . 105.5(7) yes C9 . S5 . C10 . 97.7(8) yes Y2 . O5 . S5 . 138.1(5) yes S5 . C9 . H91 . 109.0 no S5 . C9 . H92 . 109.6 no H91 . C9 . H92 . 109.1 no S5 . C9 . H93 . 109.9 no H91 . C9 . H93 . 109.6 no H92 . C9 . H93 . 109.5 no S5 . C10 . H101 . 109.2 no S5 . C10 . H102 . 109.3 no H101 . C10 . H102 . 109.6 no S5 . C10 . H103 . 109.1 no H101 . C10 . H103 . 109.9 no H102 . C10 . H103 . 109.7 no O7 . S7 . C14 . 105.1(6) yes O7 . S7 . C13 . 103.7(6) yes C14 . S7 . C13 . 98.7(7) yes S7 . O7 . Y3 . 130.3(5) yes S7 . C14 . H141 . 109.6 no S7 . C14 . H142 . 109.6 no H141 . C14 . H142 . 109.3 no S7 . C14 . H143 . 109.6 no H141 . C14 . H143 . 109.4 no H142 . C14 . H143 . 109.3 no S7 . C13 . H131 . 109.4 no S7 . C13 . H132 . 109.6 no H131 . C13 . H132 . 109.1 no S7 . C13 . H133 . 109.8 no H131 . C13 . H133 . 109.3 no H132 . C13 . H133 . 109.5 no Y2 . O10 . Y3 . 95.4(3) yes Y2 . O10 . Y1 4_566 98.7(3) yes Y3 . O10 . Y1 4_566 98.1(3) yes Y2 . O10 . H35 . 104.7 no Y3 . O10 . H35 . 107.9 no Y1 4_566 O10 . H35 . 142.8 no Y2 . O12 . Y1 4_566 98.3(3) yes Y2 . O12 . Y3 4_566 97.3(3) yes Y1 4_566 O12 . Y3 4_566 96.1(3) yes Y2 . O12 . H19 . 123.8 no Y1 4_566 O12 . H19 . 119.5 no Y3 4_566 O12 . H19 . 116.3 no Y2 . O6 . S6 . 162.4(8) yes O6 . S6 . C12 . 99.1(10) yes O6 . S6 . C11 . 111.4(9) yes C12 . S6 . C11 . 100.0(12) yes Y3 . O9 . H55 . 123.8 no Y3 . O9 . H124 . 136.4 no H55 . O9 . H124 . 89.7 no Y3 . O8 . H17 . 102.1 no Y3 . O8 . H67 . 143.8 no H17 . O8 . H67 . 111.1 no S1 . C1 . H11 . 109.6 no S1 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.7 no S1 . C1 . H13 . 109.1 no H11 . C1 . H13 . 109.6 no H12 . C1 . H13 . 109.5 no S4 . C8 . H81 . 109.3 no S4 . C8 . H82 . 109.3 no H81 . C8 . H82 . 109.7 no S4 . C8 . H83 . 109.3 no H81 . C8 . H83 . 109.7 no H82 . C8 . H83 . 109.5 no S6 . C12 . H121 . 109.4 no S6 . C12 . H122 . 109.2 no H121 . C12 . H122 . 109.5 no S6 . C12 . H123 . 109.4 no H121 . C12 . H123 . 109.6 no H122 . C12 . H123 . 109.8 no S6 . C11 . H111 . 109.6 no S6 . C11 . H112 . 108.7 no H111 . C11 . H112 . 109.6 no S6 . C11 . H113 . 109.4 no H111 . C11 . H113 . 109.6 no H112 . C11 . H113 . 110.0 no I7 5_655 I6 . I7 . 179.72(14) yes 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 C3 . H31 . O6 4_566 150 0.96 2.52 3.39(2) yes #===END