Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr. Shashank Mishra' _publ_contact_author_address ;Universite Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne Cedex France. ; _publ_contact_author_email mishrashashank74@rediffmail.com _publ_contact_author_phone '(+33) 472445329' _publ_contact_author_fax '(+33) 472445399' loop_ _publ_author_name _publ_author_address E.Jeanneau ;Centre de Diffractometrie Henri Longchambon Universite Claude Bernard Lyon 1 Bat Raulin RdC 69622 Villeurbanne Cedex France. ; H.Chermette ;Universite Claude Bernard Lyon 1 Laboratoire de Chimie-Physique Theorique Bat 210 Dirac and CNRS UMR 5182 69622 Villeurbanne Cedex France. ; S.Daniele ;Universite Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne Cedex France ; L.G.Hubert-Pfalzgraf ;Universite Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne Cedex France ; 'Shashank Mishra' ;Universite Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne Cedex France. ; _publ_section_title # Title of paper - generally just the systematic or trivial name ; Crystal-to-crystal transformations in heterometallic yttrium(III)-copper(I) iodide derivatives in a confined solvent-free environment: Influence of solvated yttrium cations on the nuclearity and dimensionality of iodocuprate clusters ; _publ_contact_letter ; Dear Sir/ Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to Dalton Trans. Dr. Shashank Mishra ; data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 651249' _audit_creation_date 07-05-23 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.1838(2) _cell_length_b 9.8576(2) _cell_length_c 23.069(4) _cell_angle_alpha 90 _cell_angle_beta 117.643(1) _cell_angle_gamma 90 _cell_volume 2253.0(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1 ' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,-z+1/2 x,-y,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' 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' 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 = C2 H40 Cu4 I10 O3.25 S16 Y4 # Dc = 7.39 Fooo = 1396.00 Mu = 290.95 M = 2508.24 # Found Formula = C8 H24 Cu1 I2.50 O4 S4 Y0.50 # Dc = 2.17 FOOO = 1396.00 Mu = 60.40 M = 737.80 _chemical_formula_sum 'C16 H48 Cu2 I5 O8 S8 Y1' _chemical_formula_moiety 'C16 H48 O8 S8 Y, Cu2 I5' _chemical_compound_source ? _chemical_formula_weight 1475.61 _cell_measurement_reflns_used 9708 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.13 _exptl_crystal_density_diffrn 2.175 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 6.040 # Sheldrick geometric approximatio 0.58 0.62 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.62 # 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_type 'Nonius KappaCCD' _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 'SHELXS 86 (Sheldrick, 1986)' _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 17925 _reflns_number_total 5366 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 5366 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5375 _diffrn_reflns_theta_min 1.993 _diffrn_reflns_theta_max 27.876 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.876 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.90 _refine_diff_density_max 1.05 _refine_ls_number_reflns 3492 _refine_ls_number_restraints 0 _refine_ls_number_parameters 183 #_refine_ls_R_factor_ref 0.0287 _refine_ls_wR_factor_ref 0.0290 _refine_ls_goodness_of_fit_ref 1.0791 #_reflns_number_all 5350 _refine_ls_R_factor_all 0.0490 _refine_ls_wR_factor_all 0.0485 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3492 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_gt 0.0290 _refine_ls_shift/su_max 0.000433 # 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_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: 0.203 0.463E-01 0.300E-01 ; 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 I2 I 0.17151(3) -0.09758(3) -0.130079(16) 0.0297 1.0000 Uani . . . . . . I1 I 0.18368(4) 0.32783(4) -0.063460(19) 0.0373 1.0000 Uani . . . . . . Y1 Y 0.5000 0.40826(6) -0.2500 0.0171 1.0000 Uani S T . . . . I3 I 0.0000 0.0000 0.0000 0.0725 1.0000 Uani S . . . . . Cu1 Cu 0.12338(7) 0.08224(7) -0.06556(3) 0.0327 1.0000 Uani . . . . . . S3 S 0.30708(12) 0.13455(12) -0.23790(6) 0.0255 1.0000 Uani . . . . . . S1 S 0.78371(12) 0.62413(12) -0.17517(6) 0.0273 1.0000 Uani . . . . . . S2 S 0.54191(12) 0.62575(12) -0.12433(6) 0.0254 1.0000 Uani . . . . . . S4 S 0.38595(13) 0.21766(12) -0.39605(6) 0.0268 1.0000 Uani . . . . . . O1 O 0.7192(3) 0.4853(3) -0.18223(16) 0.0275 1.0000 Uani . . . . . . C4 C 0.4375(5) 0.5884(5) -0.0872(2) 0.0317 1.0000 Uani . . . . . . C1 C 0.8864(6) 0.6104(6) -0.2155(3) 0.0387 1.0000 Uani . . . . . . C3 C 0.5406(6) 0.8063(5) -0.1196(3) 0.0377 1.0000 Uani . . . . . . C2 C 0.9146(5) 0.6308(6) -0.0933(3) 0.0377 1.0000 Uani . . . . . . O4 O 0.4760(3) 0.3300(3) -0.35143(15) 0.0240 1.0000 Uani . . . . . . O2 O 0.4567(3) 0.5932(3) -0.19639(14) 0.0241 1.0000 Uani . . . . . . O3 O 0.3540(4) 0.2235(4) -0.27697(16) 0.0304 1.0000 Uani . . . . . . C8 C 0.4650(6) 0.1719(6) -0.4451(3) 0.0417 1.0000 Uani . . . . . . C5 C 0.1653(7) 0.2178(8) -0.2405(4) 0.0619 1.0000 Uani . . . . . . C7 C 0.2440(6) 0.3051(7) -0.4555(3) 0.0567 1.0000 Uani . . . . . . C6 C 0.2234(8) -0.0021(7) -0.2918(3) 0.0607 1.0000 Uani . . . . . . H11 H 0.8312 0.5985 -0.2614 0.0550 1.0000 Uiso R . . . . . H12 H 0.9395 0.6916 -0.2081 0.0549 1.0000 Uiso R . . . . . H13 H 0.9459 0.5338 -0.1975 0.0550 1.0000 Uiso R . . . . . H21 H 0.8756 0.6302 -0.0640 0.0550 1.0000 Uiso R . . . . . H22 H 0.9653 0.7128 -0.0865 0.0551 1.0000 Uiso R . . . . . H23 H 0.9738 0.5540 -0.0837 0.0549 1.0000 Uiso R . . . . . H31 H 0.5843 0.8437 -0.1431 0.0554 1.0000 Uiso R . . . . . H32 H 0.5887 0.8323 -0.0740 0.0549 1.0000 Uiso R . . . . . H33 H 0.4482 0.8377 -0.1386 0.0549 1.0000 Uiso R . . . . . H41 H 0.4046 0.4971 -0.0977 0.0410 1.0000 Uiso R . . . . . H42 H 0.4883 0.5996 -0.0411 0.0413 1.0000 Uiso R . . . . . H43 H 0.3618 0.6495 -0.1041 0.0407 1.0000 Uiso R . . . . . H81 H 0.5470 0.1218 -0.4184 0.0630 1.0000 Uiso R . . . . . H82 H 0.4860 0.2532 -0.4615 0.0633 1.0000 Uiso R . . . . . H83 H 0.4029 0.1174 -0.4816 0.0630 1.0000 Uiso R . . . . . H71 H 0.1910 0.3376 -0.4356 0.0848 1.0000 Uiso R . . . . . H72 H 0.2756 0.3797 -0.4721 0.0848 1.0000 Uiso R . . . . . H73 H 0.1916 0.2433 -0.4904 0.0848 1.0000 Uiso R . . . . . H61 H 0.2905 -0.0589 -0.2942 0.0851 1.0000 Uiso R . . . . . H62 H 0.1643 0.0326 -0.3342 0.0850 1.0000 Uiso R . . . . . H63 H 0.1721 -0.0531 -0.2758 0.0850 1.0000 Uiso R . . . . . H51 H 0.1931 0.2987 -0.2142 0.0790 1.0000 Uiso R . . . . . H52 H 0.1037 0.2407 -0.2855 0.0790 1.0000 Uiso R . . . . . H53 H 0.1207 0.1581 -0.2237 0.0791 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 I2 0.03292(17) 0.02977(16) 0.03088(16) -0.00010(13) 0.01870(14) 0.00087(14) I1 0.0416(2) 0.03007(17) 0.0448(2) -0.00494(15) 0.02405(17) -0.00345(16) Y1 0.0153(3) 0.0206(3) 0.0155(3) 0.0000 0.0071(2) 0.0000 I3 0.1364(7) 0.0453(3) 0.0911(5) 0.0043(3) 0.0995(6) 0.0058(4) Cu1 0.0347(3) 0.0315(3) 0.0298(3) -0.0008(3) 0.0131(3) 0.0012(3) S3 0.0257(6) 0.0272(6) 0.0240(6) 0.0021(4) 0.0118(5) -0.0034(5) S1 0.0203(6) 0.0281(6) 0.0316(6) -0.0043(5) 0.0105(5) -0.0028(5) S2 0.0270(6) 0.0269(6) 0.0225(6) -0.0029(4) 0.0117(5) 0.0038(5) S4 0.0326(6) 0.0258(6) 0.0206(5) -0.0032(5) 0.0112(5) -0.0063(5) O1 0.0231(17) 0.0285(17) 0.0291(18) -0.0015(14) 0.0105(15) -0.0050(14) C4 0.041(3) 0.035(3) 0.030(2) -0.002(2) 0.025(2) 0.001(2) C1 0.035(3) 0.047(3) 0.045(3) -0.001(3) 0.028(3) -0.008(3) C3 0.051(4) 0.024(3) 0.043(3) -0.003(2) 0.026(3) 0.000(2) C2 0.025(3) 0.053(3) 0.031(3) -0.011(2) 0.009(2) -0.006(2) O4 0.0254(17) 0.0235(16) 0.0221(16) -0.0027(13) 0.0102(14) -0.0034(14) O2 0.0249(17) 0.0272(16) 0.0175(15) -0.0020(13) 0.0077(13) 0.0032(14) O3 0.0334(19) 0.0347(18) 0.0240(17) -0.0019(15) 0.0140(15) -0.0133(16) C8 0.052(4) 0.048(3) 0.030(3) -0.013(3) 0.023(3) -0.005(3) C5 0.066(5) 0.072(5) 0.076(5) 0.036(4) 0.057(4) 0.033(4) C7 0.037(3) 0.049(4) 0.045(4) -0.014(3) -0.015(3) 0.009(3) C6 0.089(5) 0.057(4) 0.048(4) -0.026(3) 0.042(4) -0.051(4) _refine_ls_extinction_method None 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 . 2.5280(10) yes I1 . Cu1 . 2.5076(14) yes Y1 . O2 3_654 2.376(3) yes Y1 . O4 3_654 2.358(3) yes Y1 . O1 3_654 2.340(3) yes Y1 . O3 3_654 2.330(3) yes Y1 . O1 . 2.340(3) yes Y1 . O4 . 2.358(3) yes Y1 . O2 . 2.376(3) yes Y1 . O3 . 2.330(3) yes I3 . Cu1 2_555 2.6049(9) yes I3 . Cu1 . 2.6049(9) yes S3 . O3 . 1.515(3) yes S3 . C5 . 1.762(6) yes S3 . C6 . 1.777(6) yes S1 . O1 . 1.520(3) yes S1 . C1 . 1.786(5) yes S1 . C2 . 1.775(5) yes S2 . C4 . 1.777(5) yes S2 . C3 . 1.784(5) yes S2 . O2 . 1.518(3) yes S4 . O4 . 1.529(3) yes S4 . C8 . 1.787(5) yes S4 . C7 . 1.767(6) yes C4 . H41 . 0.960 no C4 . H42 . 0.952 no C4 . H43 . 0.961 no C1 . H11 . 0.954 no C1 . H12 . 0.965 no C1 . H13 . 0.964 no C3 . H31 . 0.958 no C3 . H32 . 0.966 no C3 . H33 . 0.967 no C2 . H21 . 0.958 no C2 . H22 . 0.958 no C2 . H23 . 0.962 no C8 . H81 . 0.970 no C8 . H82 . 0.961 no C8 . H83 . 0.968 no C5 . H51 . 0.962 no C5 . H52 . 0.969 no C5 . H53 . 0.961 no C7 . H71 . 0.957 no C7 . H72 . 0.969 no C7 . H73 . 0.962 no C6 . H61 . 0.958 no C6 . H62 . 0.955 no C6 . H63 . 0.957 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 O2 3_654 Y1 . O4 3_654 144.18(11) yes O2 3_654 Y1 . O1 3_654 78.84(11) yes O4 3_654 Y1 . O1 3_654 111.79(11) yes O2 3_654 Y1 . O3 3_654 116.88(12) yes O4 3_654 Y1 . O3 3_654 74.69(11) yes O1 3_654 Y1 . O3 3_654 145.03(12) yes O2 3_654 Y1 . O1 . 72.25(11) yes O4 3_654 Y1 . O1 . 80.87(11) yes O1 3_654 Y1 . O1 . 142.10(17) yes O3 3_654 Y1 . O1 . 71.85(13) yes O2 3_654 Y1 . O4 . 72.03(11) yes O4 3_654 Y1 . O4 . 141.79(16) yes O1 3_654 Y1 . O4 . 80.87(12) yes O3 3_654 Y1 . O4 . 75.66(11) yes O1 . Y1 . O4 . 111.79(12) yes O2 3_654 Y1 . O2 . 79.76(16) yes O4 3_654 Y1 . O2 . 72.03(11) yes O1 3_654 Y1 . O2 . 72.25(11) yes O3 3_654 Y1 . O2 . 138.41(11) yes O1 . Y1 . O2 . 78.84(12) yes O2 3_654 Y1 . O3 . 138.41(11) yes O4 3_654 Y1 . O3 . 75.66(12) yes O1 3_654 Y1 . O3 . 71.85(12) yes O3 3_654 Y1 . O3 . 77.13(19) yes O1 . Y1 . O3 . 145.03(12) yes O4 . Y1 . O2 . 144.18(11) yes O4 . Y1 . O3 . 74.69(11) yes O2 . Y1 . O3 . 116.88(12) yes Cu1 2_555 I3 . Cu1 . 179.996 yes I3 . Cu1 . I2 . 116.00(3) yes I3 . Cu1 . I1 . 119.96(3) yes I2 . Cu1 . I1 . 124.02(4) yes O3 . S3 . C5 . 105.4(3) yes O3 . S3 . C6 . 103.7(2) yes C5 . S3 . C6 . 99.0(4) yes O1 . S1 . C1 . 105.3(2) yes O1 . S1 . C2 . 105.3(2) yes C1 . S1 . C2 . 98.3(3) yes C4 . S2 . C3 . 98.7(3) yes C4 . S2 . O2 . 105.3(2) yes C3 . S2 . O2 . 105.0(2) yes O4 . S4 . C8 . 104.2(2) yes O4 . S4 . C7 . 104.1(2) yes C8 . S4 . C7 . 99.3(3) yes Y1 . O1 . S1 . 131.5(2) yes S2 . C4 . H41 . 109.5 no S2 . C4 . H42 . 109.2 no H41 . C4 . H42 . 110.5 no S2 . C4 . H43 . 109.1 no H41 . C4 . H43 . 108.8 no H42 . C4 . H43 . 109.7 no S1 . C1 . H11 . 110.3 no S1 . C1 . H12 . 109.7 no H11 . C1 . H12 . 109.0 no S1 . C1 . H13 . 108.6 no H11 . C1 . H13 . 110.1 no H12 . C1 . H13 . 109.2 no S2 . C3 . H31 . 109.1 no S2 . C3 . H32 . 108.4 no H31 . C3 . H32 . 109.9 no S2 . C3 . H33 . 109.2 no H31 . C3 . H33 . 109.9 no H32 . C3 . H33 . 110.3 no S1 . C2 . H21 . 109.2 no S1 . C2 . H22 . 109.7 no H21 . C2 . H22 . 108.7 no S1 . C2 . H23 . 110.8 no H21 . C2 . H23 . 108.9 no H22 . C2 . H23 . 109.5 no Y1 . O4 . S4 . 129.91(18) yes Y1 . O2 . S2 . 123.78(18) yes Y1 . O3 . S3 . 133.38(19) yes S4 . C8 . H81 . 109.1 no S4 . C8 . H82 . 108.8 no H81 . C8 . H82 . 110.1 no S4 . C8 . H83 . 109.0 no H81 . C8 . H83 . 110.7 no H82 . C8 . H83 . 109.2 no S3 . C5 . H51 . 110.0 no S3 . C5 . H52 . 109.0 no H51 . C5 . H52 . 110.1 no S3 . C5 . H53 . 109.2 no H51 . C5 . H53 . 109.3 no H52 . C5 . H53 . 109.2 no S4 . C7 . H71 . 109.0 no S4 . C7 . H72 . 108.5 no H71 . C7 . H72 . 110.8 no S4 . C7 . H73 . 108.6 no H71 . C7 . H73 . 109.9 no H72 . C7 . H73 . 109.9 no S3 . C6 . H61 . 108.1 no S3 . C6 . H62 . 109.6 no H61 . C6 . H62 . 109.9 no S3 . C6 . H63 . 110.1 no H61 . C6 . H63 . 109.9 no H62 . C6 . H63 . 109.2 no #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 651250' _audit_creation_date 07-05-25 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.91460(20) _cell_length_b 11.70160(20) _cell_length_c 37.89470(70) _cell_angle_alpha 90.0000 _cell_angle_beta 96.5889(9) _cell_angle_gamma 90.0000 _cell_volume 4367.379(141) _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' 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' _cell_formula_units_Z 4 # Given Formula = C30 H75 Cu1.50 I6 N3 O12 S9 Y1.50 # Dc = 2.96 Fooo = 2448.00 Mu = 74.39 M = 1948.64 # Found Formula = C18 H50 Cu1 I4 N2 O8 S6 Y1 # Dc = 1.94 FOOO = 2448.00 Mu = 49.57 M = 1275.07 _chemical_formula_sum 'C18 H50 Cu1 I4 N2 O8 S6 Y1' _chemical_formula_moiety 'C18 H50 N2 O8 S6 Y, Cu I3, I' _chemical_compound_source ? _chemical_formula_weight 1275.07 _cell_measurement_reflns_used 4587 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 20.389 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.41 _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 4.957 # Sheldrick geometric approximatio 0.41 0.45 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.45 # 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_type 'Nonius KappaCCD' _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 43392 _reflns_number_total 8865 _diffrn_reflns_av_R_equivalents 0.067 # Number of reflections with Friedels Law is 8865 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10529 _diffrn_reflns_theta_min 1.082 _diffrn_reflns_theta_max 28.180 _diffrn_measured_fraction_theta_max 0.825 _diffrn_reflns_theta_full 25.080 _diffrn_measured_fraction_theta_full 0.900 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 49 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -3.11 _refine_diff_density_max 2.65 _refine_ls_number_reflns 3531 _refine_ls_number_restraints 50 _refine_ls_number_parameters 361 #_refine_ls_R_factor_ref 0.0531 _refine_ls_wR_factor_ref 0.0758 _refine_ls_goodness_of_fit_ref 1.1436 #_reflns_number_all 8832 _refine_ls_R_factor_all 0.1459 _refine_ls_wR_factor_all 0.0929 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3531 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_gt 0.0758 _refine_ls_shift/su_max 0.000828 # 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_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: 2.39 0.677 2.00 ; 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 I1 I -0.72867(15) 0.71273(11) 0.11293(3) 0.0526 1.0000 Uani . . . . . . I2 I -0.35745(12) 0.76692(12) 0.18685(4) 0.0528 1.0000 Uani . . . . . . Y1 Y -0.20017(16) 0.29347(14) 0.11980(4) 0.0336 1.0000 Uani . . . . . . Cu1 Cu -0.6073(2) 0.80646(18) 0.16900(6) 0.0401 1.0000 Uani . . . . . . I4 I -0.7295(3) 0.1888(2) 0.00569(5) 0.1129 1.0000 Uani . . . . . . S8 S -0.1285(4) 0.1924(4) 0.20749(9) 0.0330 1.0000 Uani . . . . . . S6 S 0.0172(5) 0.0543(4) 0.11347(12) 0.0471 1.0000 Uani . . . . . . S3 S -0.2841(8) 0.5444(6) 0.07186(16) 0.0804 1.0000 Uani . U . . . . S4 S 0.0942(6) 0.3344(5) 0.07924(14) 0.0578 1.0000 Uani . . . . . . S7 S -0.4181(6) 0.0615(6) 0.11396(18) 0.0747 1.0000 Uani . . . . . . S5 S -0.2380(8) 0.1876(6) 0.03167(17) 0.0830 1.0000 Uani D U . . . . O3 O -0.2987(16) 0.4631(10) 0.1034(3) 0.0596 1.0000 Uani . . . . . . O2 O -0.3741(11) 0.3161(11) 0.1579(3) 0.0429 1.0000 Uani . . . . . . O7 O -0.3824(14) 0.1778(12) 0.1000(3) 0.0584 1.0000 Uani . . . . . . N2 N -0.5380(13) 0.3908(13) 0.1877(4) 0.0448 1.0000 Uani . . . . . . O1 O -0.1165(13) 0.4163(10) 0.1666(3) 0.0458 1.0000 Uani . . . . . . O6 O -0.1017(16) 0.1311(11) 0.0990(3) 0.0572 1.0000 Uani . . . . . . O5 O -0.2185(14) 0.2988(11) 0.0561(3) 0.0519 1.0000 Uani . . . . . . O4 O 0.0063(13) 0.3690(13) 0.1075(3) 0.0567 1.0000 Uani . . . . . . C3 C -0.0943(17) 0.5336(16) 0.2299(4) 0.0408 1.0000 Uani . . . . . . C5 C -0.629(2) 0.483(2) 0.1923(6) 0.0636 1.0000 Uani . U . . . . N1 N -0.0247(12) 0.5644(13) 0.1991(3) 0.0362 1.0000 Uani . . . . . . C16 C -0.441(4) -0.022(3) 0.0756(9) 0.1242 1.0000 Uani . U . . . . C1 C -0.0436(16) 0.5027(15) 0.1709(4) 0.0325 1.0000 Uani . . . . . . C2 C 0.0585(17) 0.6636(17) 0.2014(5) 0.0492 1.0000 Uani . . . . . . C13 C -0.0552(18) -0.0673(17) 0.1297(4) 0.0470 1.0000 Uani . . . . . . C18 C -0.1253(17) 0.0464(14) 0.2245(5) 0.0373 1.0000 Uani . . . . . . C14 C 0.062(3) -0.007(2) 0.0739(5) 0.0709 1.0000 Uani . . . . . . C4 C -0.4465(18) 0.3988(17) 0.1646(5) 0.0460 1.0000 Uani . . . . . . I3 I -0.74094(11) 0.94102(11) 0.20479(3) 0.0424 1.0000 Uani . . . . . . C17 C 0.0414(15) 0.2293(15) 0.2232(4) 0.0370 1.0000 Uani . . . . . . C6 C -0.556(2) 0.287(2) 0.2067(6) 0.0729 1.0000 Uani . U . . . . C9 C 0.086(3) 0.452(3) 0.0488(7) 0.0939 1.0000 Uani . . . . . . O8 O -0.1312(11) 0.1746(10) 0.1678(2) 0.0358 1.0000 Uani . . . . . . C10 C 0.259(4) 0.360(3) 0.0984(9) 0.1284 1.0000 Uani . U . . . . C15 C -0.580(4) 0.078(3) 0.1169(10) 0.1297 1.0000 Uani . U . . . . C7 C -0.451(4) 0.564(3) 0.0501(9) 0.1289 1.0000 Uani . U . . . . C8 C -0.259(4) 0.679(3) 0.0895(10) 0.1306 1.0000 Uani . U . . . . C11 C -0.109(4) 0.195(3) 0.0054(9) 0.1315 1.0000 Uani D U . . . . C12 C -0.373(3) 0.201(3) 0.0021(8) 0.1406 1.0000 Uani D U . . . . H31 H -0.0666 0.5885 0.2496 0.0651 1.0000 Uiso R . . . . . H32 H -0.1946 0.5385 0.2231 0.0651 1.0000 Uiso R . . . . . H33 H -0.0696 0.4541 0.2379 0.0651 1.0000 Uiso R . . . . . H51 H -0.6906 0.4589 0.2101 0.0998 1.0000 Uiso R . . . . . H52 H -0.5762 0.5517 0.2013 0.0998 1.0000 Uiso R . . . . . H53 H -0.6848 0.5017 0.1693 0.0998 1.0000 Uiso R . . . . . H11 H 0.0032 0.5285 0.1503 0.0621 1.0000 Uiso R . . . . . H21 H 0.1000 0.6719 0.1787 0.0696 1.0000 Uiso R . . . . . H22 H -0.0009 0.7311 0.2046 0.0696 1.0000 Uiso R . . . . . H23 H 0.1320 0.6593 0.2218 0.0696 1.0000 Uiso R . . . . . H41 H -0.4329 0.4743 0.1533 0.0652 1.0000 Uiso R . . . . . H61 H -0.4872 0.2294 0.2009 0.1081 1.0000 Uiso R . . . . . H62 H -0.5442 0.3023 0.2329 0.1081 1.0000 Uiso R . . . . . H63 H -0.6494 0.2560 0.1996 0.1081 1.0000 Uiso R . . . . . H151 H -0.5936 0.1246 0.1383 0.1867 1.0000 Uiso R . . . . . H152 H -0.6205 0.0007 0.1190 0.1867 1.0000 Uiso R . . . . . H153 H -0.6244 0.1171 0.0951 0.1867 1.0000 Uiso R . . . . . H161 H -0.3494 -0.0401 0.0687 0.1842 1.0000 Uiso R . . . . . H162 H -0.4903 -0.0941 0.0799 0.1842 1.0000 Uiso R . . . . . H163 H -0.4942 0.0224 0.0561 0.1842 1.0000 Uiso R . . . . . H121 H -0.4559 0.1991 0.0150 0.2025 1.0000 Uiso R . . . . . H122 H -0.3672 0.2770 -0.0097 0.2025 1.0000 Uiso R . . . . . H123 H -0.3800 0.1393 -0.0163 0.2025 1.0000 Uiso R . . . . . H111 H -0.0185 0.1834 0.0198 0.1847 1.0000 Uiso R . . . . . H112 H -0.1103 0.2713 -0.0064 0.1847 1.0000 Uiso R . . . . . H113 H -0.1231 0.1336 -0.0130 0.1847 1.0000 Uiso R . . . . . H131 H -0.0902 -0.0483 0.1527 0.0692 1.0000 Uiso R . . . . . H132 H 0.0143 -0.1293 0.1337 0.0692 1.0000 Uiso R . . . . . H133 H -0.1320 -0.0938 0.1122 0.0692 1.0000 Uiso R . . . . . H141 H 0.1079 0.0518 0.0604 0.1124 1.0000 Uiso R . . . . . H142 H 0.1260 -0.0720 0.0802 0.1124 1.0000 Uiso R . . . . . H143 H -0.0203 -0.0364 0.0588 0.1124 1.0000 Uiso R . . . . . H91 H -0.0052 0.4533 0.0347 0.1871 1.0000 Uiso R . . . . . H92 H 0.1014 0.5261 0.0621 0.1871 1.0000 Uiso R . . . . . H93 H 0.1579 0.4429 0.0324 0.1871 1.0000 Uiso R . . . . . H101 H 0.2845 0.3013 0.1172 0.0829 1.0000 Uiso R . . . . . H102 H 0.2649 0.4378 0.1093 0.0829 1.0000 Uiso R . . . . . H103 H 0.3214 0.3546 0.0797 0.0829 1.0000 Uiso R . . . . . H81 H -0.1662 0.6799 0.1031 0.1878 1.0000 Uiso R . . . . . H82 H -0.3279 0.6982 0.1059 0.1878 1.0000 Uiso R . . . . . H83 H -0.2635 0.7358 0.0698 0.1878 1.0000 Uiso R . . . . . H71 H -0.4787 0.4883 0.0390 0.1881 1.0000 Uiso R . . . . . H72 H -0.5163 0.5855 0.0672 0.1881 1.0000 Uiso R . . . . . H73 H -0.4519 0.6232 0.0312 0.1881 1.0000 Uiso R . . . . . H171 H 0.0592 0.3096 0.2160 0.0642 1.0000 Uiso R . . . . . H172 H 0.0564 0.2228 0.2497 0.0642 1.0000 Uiso R . . . . . H173 H 0.1045 0.1763 0.2124 0.0642 1.0000 Uiso R . . . . . H181 H -0.2159 0.0096 0.2184 0.0666 1.0000 Uiso R . . . . . H182 H -0.1026 0.0482 0.2509 0.0666 1.0000 Uiso R . . . . . H183 H -0.0545 0.0016 0.2137 0.0666 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 I1 0.0700(8) 0.0412(7) 0.0456(6) -0.0045(6) 0.0021(6) 0.0002(6) I2 0.0327(5) 0.0591(9) 0.0686(8) 0.0034(7) 0.0152(5) 0.0062(6) Y1 0.0417(9) 0.0290(9) 0.0295(7) 0.0020(7) 0.0025(6) -0.0067(7) Cu1 0.0377(11) 0.0391(13) 0.0450(11) 0.0023(10) 0.0119(9) 0.0014(10) I4 0.1452(19) 0.137(2) 0.0676(10) 0.0277(12) 0.0591(11) 0.0283(15) S8 0.0289(18) 0.046(3) 0.0240(16) -0.0028(17) 0.0045(14) 0.0042(18) S6 0.066(3) 0.035(2) 0.041(2) 0.000(2) 0.011(2) -0.004(2) S3 0.117(4) 0.070(3) 0.054(2) 0.002(2) 0.012(2) -0.001(3) S4 0.059(3) 0.068(4) 0.050(3) -0.020(3) 0.020(2) -0.023(3) S7 0.069(4) 0.064(4) 0.089(4) 0.004(3) 0.002(3) -0.026(3) S5 0.119(4) 0.073(3) 0.058(2) 0.001(2) 0.011(2) -0.001(3) O3 0.106(11) 0.037(8) 0.039(7) 0.021(6) 0.022(7) 0.007(7) O2 0.033(6) 0.047(8) 0.051(7) 0.004(6) 0.012(5) 0.008(6) O7 0.064(9) 0.058(9) 0.051(7) 0.004(6) -0.004(6) -0.040(7) N2 0.029(7) 0.052(10) 0.050(9) 0.012(7) -0.009(6) 0.019(7) O1 0.062(8) 0.043(7) 0.032(6) -0.002(6) 0.001(5) -0.017(6) O6 0.113(12) 0.034(7) 0.027(6) 0.002(5) 0.019(6) 0.023(8) O5 0.081(9) 0.043(7) 0.033(6) 0.002(6) 0.014(6) 0.003(7) O4 0.051(8) 0.076(10) 0.046(7) -0.025(7) 0.021(6) -0.022(7) C3 0.039(9) 0.046(11) 0.039(9) -0.002(8) 0.012(7) -0.005(8) C5 0.062(11) 0.076(12) 0.059(10) 0.032(9) 0.030(8) 0.033(9) N1 0.024(6) 0.045(8) 0.040(7) 0.007(7) 0.006(5) -0.007(6) C16 0.160(16) 0.106(14) 0.105(12) -0.024(11) 0.006(12) -0.004(12) C1 0.035(8) 0.043(10) 0.021(7) -0.005(7) 0.008(6) -0.012(8) C2 0.034(9) 0.055(12) 0.061(12) -0.01(1) 0.015(8) -0.012(9) C13 0.044(10) 0.058(12) 0.040(9) 0.001(9) 0.008(8) -0.009(9) C18 0.044(9) 0.027(9) 0.043(9) 0.019(7) 0.017(7) 0.008(8) C14 0.107(19) 0.063(15) 0.045(11) 0.003(11) 0.018(12) 0.026(14) C4 0.041(10) 0.046(12) 0.048(10) 0.012(9) -0.005(8) -0.008(9) I3 0.0305(5) 0.0503(7) 0.0460(6) -0.0045(6) 0.0029(4) 0.0079(5) C17 0.026(7) 0.038(10) 0.047(9) -0.013(8) 0.009(7) -0.007(7) C6 0.075(11) 0.080(12) 0.072(10) 0.031(10) 0.041(9) 0.035(10) C9 0.10(2) 0.12(3) 0.064(15) 0.020(16) 0.019(14) 0.007(18) O8 0.046(6) 0.043(7) 0.018(4) -0.001(5) 0.003(4) 0.008(5) C10 0.168(14) 0.110(11) 0.105(10) -0.001(8) 0.006(9) -0.002(10) C15 0.167(16) 0.112(14) 0.108(12) 0.000(11) 0.005(12) 0.010(13) C7 0.168(14) 0.111(12) 0.105(11) 0.003(9) 0.005(10) -0.001(10) C8 0.173(14) 0.110(12) 0.107(11) 0.000(9) 0.006(10) -0.004(10) C11 0.173(16) 0.116(14) 0.105(12) -0.009(11) 0.014(12) 0.000(12) C12 0.182(16) 0.118(14) 0.118(13) 0.006(12) 0.002(12) 0.001(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1230(4) 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 I1 . Cu1 . 2.565(2) yes I2 . Cu1 . 2.535(3) yes Y1 . O3 . 2.268(12) yes Y1 . O2 . 2.388(12) yes Y1 . O7 . 2.313(11) yes Y1 . O1 . 2.358(11) yes Y1 . O6 . 2.315(12) yes Y1 . O5 . 2.401(11) yes Y1 . O4 . 2.325(12) yes Y1 . O8 . 2.329(10) yes Cu1 . I3 . 2.547(2) yes S8 . C18 . 1.825(15) yes S8 . C17 . 1.774(15) yes S8 . O8 . 1.516(10) yes S6 . O6 . 1.533(14) yes S6 . C13 . 1.738(18) yes S6 . C14 . 1.77(2) yes S3 . O3 . 1.547(13) yes S3 . C7 . 1.78(4) yes S3 . C8 . 1.71(3) yes S4 . O4 . 1.513(13) yes S4 . C9 . 1.80(3) yes S4 . C10 . 1.73(3) yes S7 . O7 . 1.517(13) yes S7 . C16 . 1.74(3) yes S7 . C15 . 1.63(4) yes S5 . O5 . 1.595(14) yes S5 . C11 . 1.71(4) yes S5 . C12 . 1.65(3) yes O2 . C4 . 1.25(2) yes N2 . C5 . 1.43(2) yes N2 . C4 . 1.33(2) yes N2 . C6 . 1.44(3) yes O1 . C1 . 1.243(19) yes C3 . N1 . 1.47(2) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no N1 . C1 . 1.29(2) yes N1 . C2 . 1.42(2) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C1 . H11 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C14 . H143 . 1.000 no C4 . H41 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C15 . H151 . 1.000 no C15 . H152 . 1.000 no C15 . H153 . 1.000 no 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 C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 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 O3 . Y1 . O2 . 75.6(5) yes O3 . Y1 . O7 . 97.3(5) yes O2 . Y1 . O7 . 70.7(5) yes O3 . Y1 . O1 . 77.1(5) yes O2 . Y1 . O1 . 72.2(4) yes O7 . Y1 . O1 . 142.7(5) yes O3 . Y1 . O6 . 144.1(4) yes O2 . Y1 . O6 . 131.2(5) yes O7 . Y1 . O6 . 75.7(6) yes O1 . Y1 . O6 . 129.1(5) yes O3 . Y1 . O5 . 73.8(4) yes O2 . Y1 . O5 . 129.0(4) yes O7 . Y1 . O5 . 73.9(5) yes O1 . Y1 . O5 . 136.0(4) yes O6 . Y1 . O5 . 70.4(4) yes O3 . Y1 . O4 . 88.5(5) yes O2 . Y1 . O4 . 142.4(4) yes O7 . Y1 . O4 . 146.2(5) yes O1 . Y1 . O4 . 71.1(4) yes O6 . Y1 . O4 . 80.1(5) yes O3 . Y1 . O8 . 144.7(4) yes O2 . Y1 . O8 . 76.2(4) yes O7 . Y1 . O8 . 93.0(4) yes O1 . Y1 . O8 . 74.4(4) yes O6 . Y1 . O8 . 71.2(4) yes O5 . Y1 . O4 . 75.9(5) yes O5 . Y1 . O8 . 141.5(4) yes O4 . Y1 . O8 . 101.3(5) yes I1 . Cu1 . I2 . 119.62(10) yes I1 . Cu1 . I3 . 118.84(9) yes I2 . Cu1 . I3 . 121.53(9) yes C18 . S8 . C17 . 97.6(8) yes C18 . S8 . O8 . 102.7(7) yes C17 . S8 . O8 . 105.9(7) yes O6 . S6 . C13 . 106.0(9) yes O6 . S6 . C14 . 101.1(9) yes C13 . S6 . C14 . 97.0(10) yes O3 . S3 . C7 . 105.7(14) yes O3 . S3 . C8 . 106.5(14) yes C7 . S3 . C8 . 98.7(18) yes O4 . S4 . C9 . 105.3(11) yes O4 . S4 . C10 . 104.3(14) yes C9 . S4 . C10 . 96.1(15) yes O7 . S7 . C16 . 102.9(14) yes O7 . S7 . C15 . 100.8(14) yes C16 . S7 . C15 . 95.0(18) yes O5 . S5 . C11 . 104.3(13) yes O5 . S5 . C12 . 110.5(14) yes C11 . S5 . C12 . 101.9(9) yes S3 . O3 . Y1 . 132.5(9) yes Y1 . O2 . C4 . 132.9(12) yes Y1 . O7 . S7 . 128.1(8) yes C5 . N2 . C4 . 121.0(16) yes C5 . N2 . C6 . 117.4(16) yes C4 . N2 . C6 . 121.5(16) yes Y1 . O1 . C1 . 138.0(10) yes Y1 . O6 . S6 . 134.2(7) yes Y1 . O5 . S5 . 123.5(7) yes Y1 . O4 . S4 . 129.2(7) yes N1 . C3 . H31 . 108.8 no N1 . C3 . H32 . 109.1 no H31 . C3 . H32 . 109.5 no N1 . C3 . H33 . 110.5 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no N2 . C5 . H51 . 108.3 no N2 . C5 . H52 . 109.4 no H51 . C5 . H52 . 109.5 no N2 . C5 . H53 . 110.7 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no C3 . N1 . C1 . 119.1(14) yes C3 . N1 . C2 . 118.4(14) yes C1 . N1 . C2 . 122.5(15) yes S7 . C16 . H161 . 107.6 no S7 . C16 . H162 . 111.0 no H161 . C16 . H162 . 109.5 no S7 . C16 . H163 . 109.8 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no N1 . C1 . O1 . 126.3(15) yes N1 . C1 . H11 . 116.3 no O1 . C1 . H11 . 117.3 no N1 . C2 . H21 . 108.7 no N1 . C2 . H22 . 107.9 no H21 . C2 . H22 . 109.5 no N1 . C2 . H23 . 111.8 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no S6 . C13 . H131 . 109.0 no S6 . C13 . H132 . 110.0 no H131 . C13 . H132 . 109.5 no S6 . C13 . H133 . 109.4 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no S8 . C18 . H181 . 110.0 no S8 . C18 . H182 . 109.1 no H181 . C18 . H182 . 109.5 no S8 . C18 . H183 . 109.3 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no S6 . C14 . H141 . 109.0 no S6 . C14 . H142 . 108.5 no H141 . C14 . H142 . 109.5 no S6 . C14 . H143 . 110.8 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N2 . C4 . O2 . 122.0(17) yes N2 . C4 . H41 . 118.7 no O2 . C4 . H41 . 119.2 no S8 . C17 . H171 . 109.2 no S8 . C17 . H172 . 110.2 no H171 . C17 . H172 . 109.5 no S8 . C17 . H173 . 109.1 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no N2 . C6 . H61 . 109.3 no N2 . C6 . H62 . 109.6 no H61 . C6 . H62 . 109.5 no N2 . C6 . H63 . 109.6 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no S4 . C9 . H91 . 108.7 no S4 . C9 . H92 . 110.3 no H91 . C9 . H92 . 109.5 no S4 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no Y1 . O8 . S8 . 131.5(6) yes S4 . C10 . H101 . 109.5 no S4 . C10 . H102 . 110.0 no H101 . C10 . H102 . 109.5 no S4 . C10 . H103 . 108.9 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no S7 . C15 . H151 . 110.4 no S7 . C15 . H152 . 107.8 no H151 . C15 . H152 . 109.5 no S7 . C15 . H153 . 110.2 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no S3 . C7 . H71 . 106.2 no S3 . C7 . H72 . 111.6 no H71 . C7 . H72 . 109.5 no S3 . C7 . H73 . 110.6 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no S3 . C8 . H81 . 107.3 no S3 . C8 . H82 . 111.9 no H81 . C8 . H82 . 109.5 no S3 . C8 . H83 . 109.2 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no S5 . C11 . H111 . 111.0 no S5 . C11 . H112 . 109.2 no H111 . C11 . H112 . 109.5 no S5 . C11 . H113 . 108.2 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no S5 . C12 . H121 . 108.2 no S5 . C12 . H122 . 107.4 no H121 . C12 . H122 . 109.5 no S5 . C12 . H123 . 112.7 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 651251' _audit_creation_date 07-05-25 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.533(3) _cell_length_b 11.655(4) _cell_length_c 17.053(2) _cell_angle_alpha 85.871(2) _cell_angle_beta 82.713(2) _cell_angle_gamma 84.847(2) _cell_volume 1868.3(9) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' _cell_formula_units_Z 2 # Given Formula = C12 H30 Cu1 I4 O8 S6 Y1 # Dc = 2.05 Fooo = 1096.00 Mu = 57.82 M = 1154.83 # Found Formula = C12 H36 Cu1 I4 O8 S6 Y1 # Dc = 2.06 FOOO = 1096.00 Mu = 57.82 M = 1160.88 _chemical_formula_sum 'C12 H36 Cu1 I4 O8 S6 Y1' _chemical_formula_moiety 'C12 H36 O8 S6 Y, Cu I3, I' _chemical_compound_source ? _chemical_formula_weight 1160.88 _cell_measurement_reflns_used 8249 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.41 _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 5.782 # Sheldrick geometric approximatio 0.35 0.39 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.22 _exptl_absorpt_correction_T_max 0.39 # 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_type 'Nonius KappaCCD' _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 32008 _reflns_number_total 8928 _diffrn_reflns_av_R_equivalents 0.069 # Number of reflections with Friedels Law is 8928 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8934 _diffrn_reflns_theta_min 1.206 _diffrn_reflns_theta_max 27.898 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.898 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.80 _refine_diff_density_max 3.90 _refine_ls_number_reflns 4963 _refine_ls_number_restraints 63 _refine_ls_number_parameters 289 #_refine_ls_R_factor_ref 0.0606 _refine_ls_wR_factor_ref 0.0741 _refine_ls_goodness_of_fit_ref 1.2056 #_reflns_number_all 8899 _refine_ls_R_factor_all 0.1049 _refine_ls_wR_factor_all 0.1035 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4963 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_gt 0.0741 _refine_ls_shift/su_max 0.000482 # 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_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: 2.40 0.860 1.84 ; 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 I1 I -0.87470(11) 0.55985(8) 0.82843(5) 0.0467 1.0000 Uani . . . . . . I4 I -0.69597(9) 0.28623(7) 0.56002(6) 0.0448 1.0000 Uani . . . . . . I3 I -0.55261(10) 0.77724(9) 0.88899(5) 0.0467 1.0000 Uani . . . . . . I2 I -0.77017(12) 0.86771(7) 0.67835(5) 0.0491 1.0000 Uani . . . . . . Y1 Y -0.16928(10) 0.24080(8) 0.71844(6) 0.0210 1.0000 Uani D . . . . . Cu1 Cu -0.73460(16) 0.73600(12) 0.80140(9) 0.0339 1.0000 Uani . . . . . . S5 S -0.3843(3) 0.5011(2) 0.73359(15) 0.0293 1.0000 Uani . . . . . . S6 S -0.1440(3) 0.3821(2) 0.52914(15) 0.0253 1.0000 Uani . . . . . . S2 S -0.2372(3) -0.0071(3) 0.83951(19) 0.0379 1.0000 Uani . . . . . . S4 S -0.2167(3) 0.3196(3) 0.91567(16) 0.0362 1.0000 Uani . . . . . . S3 S -0.5428(5) 0.2545(5) 0.7883(3) 0.0680 1.0000 Uani . U . . . . S1 S -0.2650(7) 0.0489(5) 0.5872(3) 0.0902 1.0000 Uani D U . . . . O5 O -0.3025(8) 0.4084(7) 0.6841(4) 0.0317 1.0000 Uani . . . . . . O4 O -0.1564(9) 0.3427(7) 0.8283(4) 0.0346 1.0000 Uani . . . . . . O2 O -0.1355(9) 0.0867(8) 0.8154(5) 0.0406 1.0000 Uani . . . . . . O6 O -0.1232(8) 0.2704(6) 0.5806(4) 0.0246 1.0000 Uani . . . . . . O7 O 0.0153(8) 0.3732(7) 0.6950(5) 0.0321 1.0000 Uani . . . . . . O3 O -0.3925(9) 0.2250(8) 0.7960(5) 0.0384 1.0000 Uani D . . . . . O1 O -0.2668(10) 0.0930(8) 0.6684(5) 0.0450 1.0000 Uani D . . . . . O8 O 0.0493(9) 0.1342(7) 0.6799(6) 0.0454 1.0000 Uani D . . . . . C11 C -0.3123(13) 0.3790(10) 0.4964(7) 0.0334 1.0000 Uani . . . . . . C6 C -0.625(2) 0.272(2) 0.8922(14) 0.0871 1.0000 Uani . U . . . . C10 C -0.2691(19) 0.6119(12) 0.7282(10) 0.0559 1.0000 Uani . . . . . . C12 C -0.0347(13) 0.3547(12) 0.4379(7) 0.0388 1.0000 Uani . . . . . . C7 C -0.0657(15) 0.2827(12) 0.9656(7) 0.0435 1.0000 Uani . . . . . . C8 C -0.2680(16) 0.4594(12) 0.9491(7) 0.0438 1.0000 Uani . . . . . . C9 C -0.5066(15) 0.5664(13) 0.6688(9) 0.0465 1.0000 Uani . . . . . . C5 C -0.613(3) 0.133(2) 0.7669(17) 0.0988 1.0000 Uani . U . . . . C4 C -0.289(2) 0.007(2) 0.9421(13) 0.0812 1.0000 Uani . U . . . . C3 C -0.128(3) -0.139(2) 0.8451(16) 0.0968 1.0000 Uani . U . . . . H81 H -0.3403 0.4962 0.9194 0.0669 1.0000 Uiso R . . . . . H82 H -0.3043 0.4534 1.0042 0.0669 1.0000 Uiso R . . . . . H83 H -0.1877 0.5047 0.9418 0.0670 1.0000 Uiso R . . . . . H71 H -0.0174 0.2121 0.9471 0.0640 1.0000 Uiso R . . . . . H72 H -0.0938 0.2719 1.0215 0.0640 1.0000 Uiso R . . . . . H73 H -0.0021 0.3432 0.9557 0.0640 1.0000 Uiso R . . . . . H31 H -0.0784 -0.1542 0.7937 0.1510 1.0000 Uiso R . . . . . H32 H -0.0606 -0.1317 0.8814 0.1510 1.0000 Uiso R . . . . . H33 H -0.1853 -0.2015 0.8639 0.1510 1.0000 Uiso R . . . . . H41 H -0.3335 0.0832 0.9509 0.1061 1.0000 Uiso R . . . . . H42 H -0.2075 -0.0054 0.9700 0.1060 1.0000 Uiso R . . . . . H43 H -0.3552 -0.0490 0.9617 0.1059 1.0000 Uiso R . . . . . H121 H 0.0630 0.3404 0.4471 0.0580 1.0000 Uiso R . . . . . H122 H -0.0433 0.4196 0.4002 0.0579 1.0000 Uiso R . . . . . H123 H -0.0639 0.2875 0.4166 0.0579 1.0000 Uiso R . . . . . H111 H -0.3847 0.3859 0.5407 0.0530 1.0000 Uiso R . . . . . H112 H -0.3262 0.4418 0.4578 0.0530 1.0000 Uiso R . . . . . H113 H -0.3156 0.3069 0.4731 0.0530 1.0000 Uiso R . . . . . H101 H -0.1887 0.5842 0.7552 0.0829 1.0000 Uiso R . . . . . H102 H -0.3171 0.6783 0.7531 0.0830 1.0000 Uiso R . . . . . H103 H -0.2373 0.6325 0.6737 0.0831 1.0000 Uiso R . . . . . H91 H -0.5727 0.5120 0.6609 0.0670 1.0000 Uiso R . . . . . H92 H -0.5573 0.6335 0.6915 0.0670 1.0000 Uiso R . . . . . H93 H -0.4552 0.5887 0.6189 0.0668 1.0000 Uiso R . . . . . H61 H -0.5900 0.3380 0.9112 0.1230 1.0000 Uiso R . . . . . H62 H -0.5995 0.2041 0.9246 0.1230 1.0000 Uiso R . . . . . H63 H -0.7262 0.2822 0.8936 0.1230 1.0000 Uiso R . . . . . H51 H -0.6118 0.1337 0.7104 0.1490 1.0000 Uiso R . . . . . H52 H -0.5561 0.0658 0.7848 0.1490 1.0000 Uiso R . . . . . H53 H -0.7086 0.1310 0.7923 0.1490 1.0000 Uiso R . . . . . C1 C -0.118(2) -0.019(2) 0.5564(14) 0.1063 1.0000 Uani D U . . . . C2 C -0.382(3) -0.055(2) 0.5988(14) 0.1076 1.0000 Uani D U . . . . H11 H -0.0436 0.0372 0.5469 0.1250 1.0000 Uiso R . . . . . H12 H -0.0909 -0.0810 0.5966 0.1250 1.0000 Uiso R . . . . . H13 H -0.1274 -0.0542 0.5057 0.1250 1.0000 Uiso R . . . . . H21 H -0.4790 -0.0223 0.6191 0.1286 1.0000 Uiso R . . . . . H22 H -0.3480 -0.1163 0.6379 0.1286 1.0000 Uiso R . . . . . H23 H -0.3844 -0.0895 0.5470 0.1286 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 I1 0.0599(6) 0.0466(5) 0.0381(4) -0.0036(3) -0.0075(4) -0.0259(4) I4 0.0295(4) 0.0400(4) 0.0629(5) -0.0063(4) 0.0085(3) -0.0086(3) I3 0.0414(5) 0.0658(6) 0.0359(4) -0.0051(4) -0.0031(3) -0.0211(4) I2 0.0709(6) 0.0276(4) 0.0471(5) -0.0019(3) -0.0150(4) 0.0167(4) Y1 0.0203(4) 0.0198(4) 0.0226(4) 0.0036(3) -0.0053(3) 0.0005(3) Cu1 0.0333(7) 0.0310(7) 0.0369(7) -0.0031(6) -0.0032(6) -0.0006(6) S5 0.0297(13) 0.0296(13) 0.0249(12) 0.0037(10) 0.0003(10) 0.0084(10) S6 0.0277(12) 0.0232(12) 0.0255(11) 0.0060(9) -0.0081(9) -0.0040(10) S2 0.0372(15) 0.0327(15) 0.0416(15) 0.0110(12) -0.0045(12) -0.0031(12) S4 0.0437(16) 0.0434(16) 0.0227(12) -0.0010(11) -0.0022(11) -0.0145(13) S3 0.053(2) 0.085(3) 0.066(2) 0.002(2) -0.0057(19) -0.014(2) S1 0.108(4) 0.096(3) 0.071(3) -0.045(2) 0.028(3) -0.055(3) O5 0.032(4) 0.033(4) 0.028(4) 0.000(3) -0.012(3) 0.018(3) O4 0.046(5) 0.036(4) 0.024(4) -0.004(3) -0.005(3) -0.014(4) O2 0.030(4) 0.047(5) 0.043(5) 0.022(4) -0.006(3) -0.007(4) O6 0.023(3) 0.020(3) 0.028(3) 0.006(3) -0.005(3) 0.008(3) O7 0.031(4) 0.035(4) 0.031(4) -0.004(3) 0.001(3) -0.011(3) O3 0.026(4) 0.044(5) 0.045(5) -0.009(4) -0.003(3) -0.001(3) O1 0.060(6) 0.038(5) 0.040(5) -0.009(4) 0.008(4) -0.029(4) O8 0.032(5) 0.032(4) 0.064(6) 0.013(4) 0.009(4) 0.013(4) C11 0.033(6) 0.031(6) 0.039(6) 0.000(5) -0.017(5) 0.000(5) C6 0.054(8) 0.116(10) 0.092(9) -0.026(8) 0.001(7) -0.013(8) C10 0.070(10) 0.034(7) 0.060(9) -0.013(6) 0.013(8) -0.012(7) C12 0.032(6) 0.051(7) 0.033(6) 0.009(5) -0.001(5) -0.008(5) C7 0.051(8) 0.046(7) 0.032(6) 0.005(5) -0.017(5) 0.017(6) C8 0.060(8) 0.047(7) 0.024(5) -0.003(5) -0.003(5) -0.007(6) C9 0.035(7) 0.049(8) 0.052(8) -0.001(6) -0.005(6) 0.016(6) C5 0.067(8) 0.115(10) 0.114(10) -0.019(9) -0.005(8) -0.008(8) C4 0.072(9) 0.094(10) 0.076(9) -0.015(8) 0.015(8) -0.027(8) C3 0.071(7) 0.111(9) 0.106(8) -0.019(7) 0.008(6) -0.010(6) C1 0.078(8) 0.119(10) 0.119(10) -0.022(9) 0.002(8) -0.003(8) C2 0.084(8) 0.127(10) 0.113(10) -0.033(9) 0.001(8) -0.013(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2184(6) 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 I1 . Cu1 . 2.5320(18) yes I3 . Cu1 . 2.5264(18) yes I2 . Cu1 . 2.5490(18) yes Y1 . S2 . 3.488(3) yes Y1 . O5 . 2.313(7) yes Y1 . O4 . 2.311(7) yes Y1 . O2 . 2.381(8) yes Y1 . O6 . 2.343(7) yes Y1 . O7 . 2.420(7) yes Y1 . O3 . 2.373(8) yes Y1 . O1 . 2.294(8) yes Y1 . O8 . 2.371(8) yes S5 . O5 . 1.517(8) yes S5 . C10 . 1.759(15) yes S5 . C9 . 1.790(14) yes S6 . O6 . 1.528(7) yes S6 . C11 . 1.769(11) yes S6 . C12 . 1.792(12) yes S2 . O2 . 1.526(9) yes S2 . C4 . 1.77(2) yes S2 . C3 . 1.78(3) yes S4 . O4 . 1.541(8) yes S4 . C7 . 1.768(13) yes S4 . C8 . 1.772(14) yes S3 . O3 . 1.463(10) yes S3 . C6 . 1.86(2) yes S3 . C5 . 1.70(3) yes S1 . O1 . 1.508(9) yes S1 . C1 . 1.59(2) yes S1 . C2 . 1.70(2) yes C11 . H111 . 0.959 no C11 . H112 . 0.960 no C11 . H113 . 0.960 no C6 . H61 . 0.961 no C6 . H62 . 0.959 no C6 . H63 . 0.961 no C10 . H101 . 0.962 no C10 . H102 . 0.960 no C10 . H103 . 0.960 no C12 . H121 . 0.962 no C12 . H122 . 0.961 no C12 . H123 . 0.963 no C7 . H71 . 0.961 no C7 . H72 . 0.959 no C7 . H73 . 0.962 no C8 . H81 . 0.960 no C8 . H82 . 0.960 no C8 . H83 . 0.958 no C9 . H91 . 0.961 no C9 . H92 . 0.961 no C9 . H93 . 0.957 no C5 . H51 . 0.962 no C5 . H52 . 0.961 no C5 . H53 . 0.963 no C4 . H41 . 0.961 no C4 . H42 . 0.958 no C4 . H43 . 0.962 no C3 . H31 . 0.961 no C3 . H32 . 0.960 no C3 . H33 . 0.962 no C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 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 S2 . Y1 . O5 . 134.8(2) yes S2 . Y1 . O4 . 90.6(2) yes O5 . Y1 . O4 . 80.8(3) yes S2 . Y1 . O2 . 21.0(2) yes O5 . Y1 . O2 . 146.8(3) yes O4 . Y1 . O2 . 79.3(3) yes S2 . Y1 . O6 . 131.56(18) yes O5 . Y1 . O6 . 73.6(3) yes O4 . Y1 . O6 . 137.3(3) yes O2 . Y1 . O6 . 137.1(3) yes S2 . Y1 . O7 . 136.9(2) yes O5 . Y1 . O7 . 80.1(3) yes O4 . Y1 . O7 . 68.1(3) yes O2 . Y1 . O7 . 115.9(3) yes O6 . Y1 . O7 . 74.2(3) yes S2 . Y1 . O3 . 59.2(2) yes O5 . Y1 . O3 . 75.7(3) yes O4 . Y1 . O3 . 75.5(3) yes O2 . Y1 . O3 . 73.7(3) yes O6 . Y1 . O3 . 127.8(3) yes S2 . Y1 . O1 . 60.8(2) yes O5 . Y1 . O1 . 106.3(3) yes O4 . Y1 . O1 . 146.5(3) yes O2 . Y1 . O1 . 77.7(3) yes O6 . Y1 . O1 . 74.8(3) yes S2 . Y1 . O8 . 83.3(2) yes O5 . Y1 . O8 . 141.2(3) yes O4 . Y1 . O8 . 111.2(3) yes O2 . Y1 . O8 . 71.5(3) yes O6 . Y1 . O8 . 73.5(3) yes O7 . Y1 . O3 . 138.9(3) yes O7 . Y1 . O1 . 144.9(3) yes O3 . Y1 . O1 . 74.7(3) yes O7 . Y1 . O8 . 71.6(3) yes O3 . Y1 . O8 . 142.3(3) yes O1 . Y1 . O8 . 84.1(4) yes I2 . Cu1 . I1 . 118.61(7) yes I2 . Cu1 . I3 . 119.73(7) yes I1 . Cu1 . I3 . 121.58(7) yes O5 . S5 . C10 . 104.7(6) yes O5 . S5 . C9 . 102.3(6) yes C10 . S5 . C9 . 99.2(8) yes O6 . S6 . C11 . 105.4(5) yes O6 . S6 . C12 . 104.1(5) yes C11 . S6 . C12 . 98.9(6) yes Y1 . S2 . O2 . 34.0(3) yes Y1 . S2 . C4 . 118.6(8) yes O2 . S2 . C4 . 104.5(8) yes Y1 . S2 . C3 . 127.7(8) yes O2 . S2 . C3 . 105.6(9) yes C4 . S2 . C3 . 98.9(13) yes O4 . S4 . C7 . 104.7(6) yes O4 . S4 . C8 . 103.7(5) yes C7 . S4 . C8 . 100.2(7) yes O3 . S3 . C6 . 103.5(9) yes O3 . S3 . C5 . 107.7(10) yes C6 . S3 . C5 . 101.3(12) yes O1 . S1 . C1 . 113.1(8) yes O1 . S1 . C2 . 105.6(7) yes C1 . S1 . C2 . 103.4(8) yes Y1 . O5 . S5 . 131.9(4) yes Y1 . O4 . S4 . 130.5(4) yes Y1 . O2 . S2 . 125.1(5) yes Y1 . O6 . S6 . 128.7(4) yes Y1 . O3 . S3 . 138.4(6) yes Y1 . O1 . S1 . 135.2(5) yes S6 . C11 . H111 . 109.3 no S6 . C11 . H112 . 109.4 no H111 . C11 . H112 . 109.9 no S6 . C11 . H113 . 108.6 no H111 . C11 . H113 . 109.7 no H112 . C11 . H113 . 109.9 no S3 . C6 . H61 . 108.5 no S3 . C6 . H62 . 109.6 no H61 . C6 . H62 . 109.7 no S3 . C6 . H63 . 109.4 no H61 . C6 . H63 . 109.9 no H62 . C6 . H63 . 109.6 no S5 . C10 . H101 . 108.5 no S5 . C10 . H102 . 110.0 no H101 . C10 . H102 . 109.5 no S5 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.7 no S6 . C12 . H121 . 109.9 no S6 . C12 . H122 . 110.7 no H121 . C12 . H122 . 109.0 no S6 . C12 . H123 . 109.0 no H121 . C12 . H123 . 108.9 no H122 . C12 . H123 . 109.2 no S4 . C7 . H71 . 109.8 no S4 . C7 . H72 . 110.1 no H71 . C7 . H72 . 108.5 no S4 . C7 . H73 . 109.8 no H71 . C7 . H73 . 109.2 no H72 . C7 . H73 . 109.4 no S4 . C8 . H81 . 109.5 no S4 . C8 . H82 . 109.5 no H81 . C8 . H82 . 109.3 no S4 . C8 . H83 . 109.8 no H81 . C8 . H83 . 109.2 no H82 . C8 . H83 . 109.5 no S5 . C9 . H91 . 109.6 no S5 . C9 . H92 . 109.9 no H91 . C9 . H92 . 109.5 no S5 . C9 . H93 . 109.2 no H91 . C9 . H93 . 109.3 no H92 . C9 . H93 . 109.4 no S3 . C5 . H51 . 108.0 no S3 . C5 . H52 . 109.8 no H51 . C5 . H52 . 109.6 no S3 . C5 . H53 . 110.0 no H51 . C5 . H53 . 109.6 no H52 . C5 . H53 . 109.7 no S2 . C4 . H41 . 110.1 no S2 . C4 . H42 . 109.7 no H41 . C4 . H42 . 109.2 no S2 . C4 . H43 . 109.5 no H41 . C4 . H43 . 109.2 no H42 . C4 . H43 . 109.2 no S2 . C3 . H31 . 110.0 no S2 . C3 . H32 . 108.4 no H31 . C3 . H32 . 109.4 no S2 . C3 . H33 . 110.0 no H31 . C3 . H33 . 109.7 no H32 . C3 . H33 . 109.4 no S1 . C1 . H11 . 108.4 no S1 . C1 . H12 . 110.6 no H11 . C1 . H12 . 109.5 no S1 . C1 . H13 . 109.4 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no S1 . C2 . H21 . 110.7 no S1 . C2 . H22 . 107.8 no H21 . C2 . H22 . 109.5 no S1 . C2 . H23 . 109.9 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no