Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #==================================================================== # 1. SUBMISSION DETAILS #==================================================================== _publ_contact_author_name 'Dr. Shashank Mishra' _publ_contact_author_address ;Universit\'e Claude Bernard Lyon 1 IRC-UPR 5401 2 avenue A. Einstein 69626 Villeurbanne C\'edex France. ; _publ_contact_author_email mishrashashank74@rediffmail.com _publ_contact_author_phone '(+33) 472445329' _publ_contact_author_fax '(+33) 472445399' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to Dalton Trans. Dr. Shashank Mishra ; #======================================================= # 2. TITLE AND AUTHOR LIST #======================================================= _publ_section_title ; From discrete [Y(DMF)8][Cu4(\m3-I)2(\m-I)3I2] ion pairs to extended [Y(DMF)6(H2O)2][Cu7(\m4-I)3(\m3-I)2(\m-I)4(I)]1? and [Y(DMF)6(H2O)3][CuI7CuII2(\m3-I)8(\m-I)6] 2? arrays by H-bonding templating in a confined solvent-free environment ? ; loop_ _publ_author_name _publ_author_address 'Shashank Mishra' ;Universit\'e Claude Bernard Lyon 1 IRC-UPR 5401 2 avenue A. Einstein 69626 Villeurbanne C\'edex France ; L.G.Hubert-Pfalzgraf ;Universit\'e Claude Bernard Lyon 1 IRC-UPR 5401 2 avenue A. Einstein 69626 Villeurbanne C\'edex France ; E.Jeanneau ;Centre de Diffractom\'etrie Henri Longchambon Universit\'e Claude Bernard Lyon 1 B\^at Raulin RdC 69622 Villeurbanne C\'edex France. ; H.Chermette ;Universit\'e Claude Bernard Lyon 1 Laboratoire de Chimie-Physique Th\'eorique B\^at 210 Dirac and CNRS UMR 5182 69622 Villeurbanne C\'edex France. ; #======================================================= # 2. Structures of the three complexes #===================================================== data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 620033' _audit_creation_date 05-07-13 _audit_creation_method CRYSTALS_ver_12.82 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 17.386(5) _cell_length_b 11.819(5) _cell_length_c 26.162(5) _cell_angle_alpha 90 _cell_angle_beta 106.219(5) _cell_angle_gamma 90 _cell_volume 5162(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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' 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' 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 4 # Given Formula = C100 H70 Cu5 I5 N30 O30 Y5 # Dc = 4.59 Fooo = 3384.00 Mu = 107.56 M = 3568.62 # Found Formula = C24 H56 Cu4 I7 N8 O8 Y1 # Dc = 2.34 FOOO = 3384.00 Mu = 69.63 M = 1816.18 _chemical_formula_sum 'C24 H56 Cu4 I7 N8 O8 Y1' _chemical_formula_moiety 'C24 H56 N8 O8 Y1, Cu4 I7' _chemical_compound_source ? _chemical_formula_weight 1816.18 _cell_measurement_reflns_used 9057 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_min 0.151 _exptl_crystal_size_mid 0.273 _exptl_crystal_size_max 0.316 _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 6.963 # Sheldrick geometric approximatio 0.71 0.71 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.71 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement '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 'DIAMOND v3 (Brandenburg & Putz)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 19802 _reflns_number_total 11944 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections with Friedels Law is 11944 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12345 _diffrn_reflns_theta_min 1.220 _diffrn_reflns_theta_max 27.903 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.345 _diffrn_measured_fraction_theta_full 0.969 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -22 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _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 2.58 _refine_ls_number_reflns 8018 _refine_ls_number_restraints 12 _refine_ls_number_parameters 469 #_refine_ls_R_factor_ref 0.0495 _refine_ls_wR_factor_ref 0.0566 _refine_ls_goodness_of_fit_ref 1.0819 #_reflns_number_all 11909 _refine_ls_R_factor_all 0.0861 _refine_ls_wR_factor_all 0.0817 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 8018 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_gt 0.0566 _refine_ls_shift/su_max 0.001171 # 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 noref # 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: 1.15 0.526 0.794 ; _publ_section_exptl_refinement ; All non hydroen atoms were refined anisotropically. Hydrogen were placed geometrically and initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Brandenburg, K., & Putz, H. Diamond - Crystal and Molecular Structure Visualization Crystal Impact - GbR, Postfach 1251, D-53002 Bonn 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. Walker, N., and Stuart, (1983). D. Acta Cryst, A39, 158-166 Watkin D.J. (1994). Acta Cryst, A50, 411-437 ; 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 Cu1 Cu 0.18592(6) -0.40386(9) 0.78413(4) 0.0261 1.0000 Uani . . . . . . Cu2 Cu 0.14127(8) -0.41877(12) 0.67728(6) 0.0474 1.0000 Uani . . . . . . Cu3 Cu 0.11838(9) -0.24275(13) 0.62432(8) 0.0653 1.0000 Uani . . . . . . Cu4 Cu 0.25797(7) -0.15477(11) 0.63706(5) 0.0361 1.0000 Uani . . . . . . I1 I 0.26036(4) -0.39362(5) 0.88198(2) 0.0303 1.0000 Uani . . . . . . I2 I 0.15664(4) -0.59426(5) 0.73606(2) 0.0300 1.0000 Uani . . . . . . I3 I 0.14167(4) -0.21420(4) 0.73747(2) 0.0281 1.0000 Uani . . . . . . I4 I 0.00961(3) -0.39481(5) 0.59772(2) 0.0272 1.0000 Uani . . . . . . I5 I 0.26870(4) -0.37378(5) 0.64182(3) 0.0335 1.0000 Uani . . . . . . I6 I 0.13063(4) -0.06911(5) 0.57090(2) 0.0320 1.0000 Uani . . . . . . I7 I 0.36851(4) -0.01712(6) 0.67796(3) 0.0401 1.0000 Uani . . . . . . Y1 Y 0.30861(4) -0.58846(6) 0.42092(3) 0.0173 1.0000 Uani . . . . . . O1 O 0.2108(4) -0.5678(5) 0.3385(2) 0.0253 1.0000 Uani . . . . . . O2 O 0.3749(4) -0.4749(5) 0.3730(3) 0.0337 1.0000 Uani . . . . . . O3 O 0.3945(4) -0.4645(5) 0.4790(2) 0.0269 1.0000 Uani . . . . . . O4 O 0.2190(4) -0.4519(5) 0.4298(2) 0.0284 1.0000 Uani . . . . . . O5 O 0.3466(4) -0.7043(5) 0.3590(3) 0.0286 1.0000 Uani . . . . . . O6 O 0.4085(4) -0.7115(5) 0.4693(2) 0.0276 1.0000 Uani . . . . . . O7 O 0.2904(4) -0.6153(5) 0.5080(2) 0.0279 1.0000 Uani . . . . . . O8 O 0.2242(4) -0.7403(5) 0.4185(2) 0.0269 1.0000 Uani . . . . . . N1 N 0.1411(4) -0.5926(5) 0.2523(3) 0.0197 1.0000 Uani . . . . . . N2 N 0.4159(4) -0.3431(6) 0.3227(3) 0.0282 1.0000 Uani . . . . . . N3 N 0.4070(4) -0.3336(7) 0.5442(3) 0.0322 1.0000 Uani . . . . . . N4 N 0.1130(4) -0.3366(6) 0.4171(3) 0.0269 1.0000 Uani . . . . . . N5 N 0.3834(4) -0.8302(6) 0.3051(3) 0.0276 1.0000 Uani . . . . . . N6 N 0.4384(5) -0.8488(8) 0.5302(4) 0.0432 1.0000 Uani . . . . . . N7 N 0.2130(5) -0.6728(7) 0.5596(3) 0.0297 1.0000 Uani . . . . . . N8 N 0.1222(4) -0.8665(6) 0.3973(3) 0.0216 1.0000 Uani . . . . . . C1 C 0.2076(5) -0.5783(7) 0.2899(3) 0.0209 1.0000 Uani . . . . . . C2 C 0.1417(6) -0.5972(8) 0.1967(3) 0.0278 1.0000 Uani . . . . . . C3 C 0.0633(6) -0.5973(9) 0.2629(4) 0.0329 1.0000 Uani . . . . . . C4 C 0.3624(5) -0.3904(7) 0.3447(4) 0.0247 1.0000 Uani . . . . . . C5 C 0.3945(6) -0.2463(9) 0.2863(4) 0.0387 1.0000 Uani . U . . . . C6 C 0.4930(7) -0.3983(11) 0.3293(5) 0.0499 1.0000 Uani . U . . . . C7 C 0.4286(6) -0.4281(9) 0.5245(5) 0.0385 1.0000 Uani . . . . . . C8 C 0.4572(6) -0.2976(12) 0.5978(5) 0.0502 1.0000 Uani . . . . . . C9 C 0.3433(9) -0.2664(12) 0.5163(6) 0.0609 1.0000 Uani . . . . . . C10 C 0.1636(5) -0.3947(7) 0.3993(3) 0.0229 1.0000 Uani . . . . . . C11 C 0.1138(7) -0.3358(11) 0.4731(5) 0.0508 1.0000 Uani . . . . . . C12 C 0.0488(6) -0.2744(8) 0.3790(5) 0.0373 1.0000 Uani . . . . . . C13 C 0.3520(5) -0.8013(8) 0.3437(4) 0.0270 1.0000 Uani . . . . . . C14 C 0.4113(9) -0.7466(11) 0.2758(5) 0.0564 1.0000 Uani . . . . . . C15 C 0.3873(7) -0.9483(10) 0.2891(6) 0.0541 1.0000 Uani . . . . . . C16 C 0.4514(8) -0.7490(12) 0.5105(6) 0.0570 1.0000 Uani . . . . . . C17 C 0.4935(9) -0.8820(14) 0.5804(7) 0.0689 1.0000 Uani . U . . . . C18 C 0.3641(10) -0.9075(15) 0.5109(7) 0.0774 1.0000 Uani . U . . . . C19 C 0.2241(5) -0.6246(8) 0.5170(3) 0.0234 1.0000 Uani . . . . . . C20 C 0.2792(7) -0.7134(12) 0.6026(5) 0.0497 1.0000 Uani . . . . . . C21 C 0.1334(6) -0.6794(11) 0.5685(4) 0.0404 1.0000 Uani . . . . . . C22 C 0.1692(5) -0.7893(7) 0.3854(3) 0.0218 1.0000 Uani . . . . . . C23 C 0.1315(7) -0.9030(9) 0.4514(4) 0.0422 1.0000 Uani . . . . . . C24 C 0.0578(5) -0.9197(8) 0.3570(4) 0.0340 1.0000 Uani . . . . . . H11 H 0.2552 -0.5739 0.2801 0.0242 1.0000 Uiso . . . . . . H21 H 0.1216 -0.6686 0.1815 0.0450 1.0000 Uiso . . . . . . H22 H 0.1954 -0.5867 0.1946 0.0449 1.0000 Uiso . . . . . . H23 H 0.1081 -0.5374 0.1774 0.0449 1.0000 Uiso . . . . . . H31 H 0.0370 -0.6665 0.2491 0.0520 1.0000 Uiso . . . . . . H32 H 0.0699 -0.5938 0.3005 0.0520 1.0000 Uiso . . . . . . H33 H 0.0312 -0.5342 0.2461 0.0521 1.0000 Uiso . . . . . . H41 H 0.3125 -0.3562 0.3377 0.0329 1.0000 Uiso . . . . . . H51 H 0.4337 -0.1879 0.2975 0.0650 1.0000 Uiso . . . . . . H52 H 0.3427 -0.2185 0.2868 0.0650 1.0000 Uiso . . . . . . H53 H 0.3928 -0.2700 0.2509 0.0649 1.0000 Uiso . . . . . . H61 H 0.5353 -0.3478 0.3466 0.0859 1.0000 Uiso . . . . . . H62 H 0.4959 -0.4651 0.3508 0.0861 1.0000 Uiso . . . . . . H63 H 0.4991 -0.4190 0.2954 0.0860 1.0000 Uiso . . . . . . H71 H 0.4715 -0.4699 0.5458 0.0529 1.0000 Uiso . . . . . . H81 H 0.4789 -0.2235 0.5956 0.0759 1.0000 Uiso . . . . . . H82 H 0.4248 -0.2961 0.6223 0.0760 1.0000 Uiso . . . . . . H83 H 0.5005 -0.3512 0.6102 0.0760 1.0000 Uiso . . . . . . H91 H 0.3600 -0.1880 0.5213 0.0958 1.0000 Uiso . . . . . . H92 H 0.2981 -0.2783 0.5297 0.0961 1.0000 Uiso . . . . . . H93 H 0.3302 -0.2854 0.4791 0.0961 1.0000 Uiso . . . . . . H101 H 0.1583 -0.3940 0.3628 0.0270 1.0000 Uiso . . . . . . H111 H 0.1198 -0.2594 0.4859 0.0770 1.0000 Uiso . . . . . . H112 H 0.0648 -0.3667 0.4766 0.0770 1.0000 Uiso . . . . . . H113 H 0.1580 -0.3804 0.4934 0.0769 1.0000 Uiso . . . . . . H121 H 0.0484 -0.1969 0.3900 0.0569 1.0000 Uiso . . . . . . H122 H -0.0020 -0.3085 0.3773 0.0569 1.0000 Uiso . . . . . . H123 H 0.0579 -0.2771 0.3443 0.0571 1.0000 Uiso . . . . . . H131 H 0.3325 -0.8596 0.3606 0.0350 1.0000 Uiso . . . . . . H141 H 0.4659 -0.7618 0.2765 0.0869 1.0000 Uiso . . . . . . H142 H 0.4084 -0.6731 0.2912 0.0869 1.0000 Uiso . . . . . . H143 H 0.3783 -0.7466 0.2396 0.0870 1.0000 Uiso . . . . . . H151 H 0.4418 -0.9686 0.2922 0.0819 1.0000 Uiso . . . . . . H152 H 0.3666 -0.9962 0.3120 0.0820 1.0000 Uiso . . . . . . H153 H 0.3559 -0.9582 0.2531 0.0820 1.0000 Uiso . . . . . . H161 H 0.4959 -0.7065 0.5296 0.0971 1.0000 Uiso . . . . . . H171 H 0.5163 -0.9536 0.5764 0.1020 1.0000 Uiso . . . . . . H172 H 0.5349 -0.8239 0.5891 0.1020 1.0000 Uiso . . . . . . H173 H 0.4658 -0.8841 0.6074 0.1020 1.0000 Uiso . . . . . . H181 H 0.3776 -0.9873 0.5070 0.1181 1.0000 Uiso . . . . . . H182 H 0.3334 -0.9020 0.5357 0.1181 1.0000 Uiso . . . . . . H183 H 0.3361 -0.8774 0.4767 0.1181 1.0000 Uiso . . . . . . H191 H 0.1794 -0.5969 0.4914 0.0311 1.0000 Uiso . . . . . . H201 H 0.2764 -0.6806 0.6354 0.0840 1.0000 Uiso . . . . . . H202 H 0.2755 -0.7941 0.6047 0.0840 1.0000 Uiso . . . . . . H203 H 0.3288 -0.6935 0.5959 0.0839 1.0000 Uiso . . . . . . H211 H 0.1226 -0.7566 0.5759 0.0600 1.0000 Uiso . . . . . . H212 H 0.0934 -0.6542 0.5374 0.0599 1.0000 Uiso . . . . . . H213 H 0.1319 -0.6328 0.5984 0.0600 1.0000 Uiso . . . . . . H221 H 0.1604 -0.7702 0.3496 0.0270 1.0000 Uiso . . . . . . H231 H 0.0907 -0.8694 0.4643 0.0620 1.0000 Uiso . . . . . . H232 H 0.1277 -0.9836 0.4525 0.0622 1.0000 Uiso . . . . . . H233 H 0.1833 -0.8795 0.4734 0.0620 1.0000 Uiso . . . . . . H241 H 0.0087 -0.9131 0.3668 0.0511 1.0000 Uiso . . . . . . H242 H 0.0701 -0.9981 0.3542 0.0509 1.0000 Uiso . . . . . . H243 H 0.0517 -0.8836 0.3235 0.0509 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0267(5) 0.0230(5) 0.0280(5) -0.0006(4) 0.0065(4) -0.0013(4) Cu2 0.0409(7) 0.0484(8) 0.0425(8) 0.0240(6) -0.0057(6) -0.0105(6) Cu3 0.0375(8) 0.0420(8) 0.0985(13) 0.0384(8) -0.0106(8) -0.0135(6) Cu4 0.0339(6) 0.0340(6) 0.0425(7) -0.0032(5) 0.0142(5) -0.0034(5) I1 0.0358(3) 0.0283(3) 0.0247(3) -0.0012(2) 0.0047(2) -0.0037(2) I2 0.0446(3) 0.0188(2) 0.0239(3) 0.0009(2) 0.0051(2) -0.0033(2) I3 0.0366(3) 0.0190(2) 0.0255(3) -0.0020(2) 0.0032(2) 0.0033(2) I5 0.0356(3) 0.0294(3) 0.0407(3) 0.0002(2) 0.0194(3) -0.0008(2) I4 0.0264(3) 0.0271(3) 0.0251(3) -0.0012(2) 0.0020(2) -0.0034(2) I6 0.0480(4) 0.0273(3) 0.0210(3) 0.0025(2) 0.0102(2) -0.0018(2) I7 0.0319(3) 0.0310(3) 0.0552(4) 0.0039(3) 0.0084(3) -0.0050(3) Y1 0.0157(3) 0.0192(3) 0.0174(3) 0.0007(3) 0.0050(3) -0.0007(3) O3 0.025(3) 0.025(3) 0.030(3) -0.007(2) 0.006(3) -0.007(2) O4 0.030(3) 0.024(3) 0.027(3) -0.008(2) 0.001(3) 0.006(2) O7 0.027(3) 0.041(4) 0.019(3) 0.000(2) 0.011(2) -0.005(3) O8 0.025(3) 0.030(3) 0.025(3) 0.004(2) 0.005(2) -0.011(2) O1 0.026(3) 0.036(3) 0.014(3) 0.005(2) 0.006(2) 0.002(3) O5 0.032(3) 0.027(3) 0.028(3) -0.006(2) 0.010(3) 0.000(3) O6 0.024(3) 0.030(3) 0.026(3) 0.006(2) 0.003(3) 0.008(2) O2 0.046(4) 0.025(3) 0.032(4) 0.007(3) 0.014(3) -0.013(3) N3 0.014(3) 0.036(4) 0.045(5) -0.013(4) 0.004(3) -0.012(3) N4 0.019(3) 0.019(3) 0.042(4) -0.007(3) 0.006(3) -0.001(3) N7 0.030(4) 0.034(4) 0.029(4) -0.002(3) 0.013(3) -0.001(3) N8 0.017(3) 0.026(3) 0.021(3) 0.002(3) 0.003(3) -0.001(3) N1 0.023(3) 0.010(3) 0.025(3) 0.006(2) 0.004(3) 0.004(2) N5 0.027(4) 0.027(4) 0.028(4) -0.011(3) 0.007(3) 0.004(3) N2 0.028(4) 0.032(4) 0.030(4) 0.006(3) 0.016(3) -0.006(3) C7 0.028(5) 0.034(5) 0.050(6) -0.002(4) 0.006(4) -0.005(4) C9 0.063(8) 0.060(8) 0.061(9) 0.006(7) 0.019(7) 0.016(7) C8 0.030(5) 0.079(9) 0.041(6) -0.024(6) 0.008(5) -0.012(5) C10 0.018(4) 0.027(4) 0.024(4) -0.002(3) 0.008(3) -0.003(3) C12 0.024(4) 0.034(5) 0.054(7) 0.015(4) 0.012(4) 0.010(4) C11 0.046(6) 0.068(8) 0.046(6) -0.014(6) 0.025(5) 0.030(6) C19 0.021(4) 0.038(5) 0.011(3) -0.002(3) 0.004(3) 0.008(3) C20 0.037(6) 0.077(8) 0.040(6) 0.024(6) 0.018(5) 0.015(6) C21 0.023(5) 0.072(7) 0.030(5) 0.000(5) 0.012(4) 0.001(5) C22 0.025(4) 0.025(4) 0.014(4) 0.003(3) 0.003(3) -0.002(3) C24 0.020(4) 0.039(5) 0.040(5) -0.006(4) 0.005(4) -0.002(4) C23 0.054(6) 0.046(6) 0.027(5) 0.005(4) 0.012(5) -0.016(5) C1 0.024(4) 0.020(4) 0.018(4) 0.000(3) 0.005(3) -0.005(3) C2 0.034(5) 0.032(4) 0.015(4) -0.004(3) 0.004(3) 0.002(4) C3 0.030(5) 0.046(5) 0.023(4) 0.004(4) 0.007(4) -0.007(4) C13 0.018(4) 0.033(5) 0.031(5) 0.006(4) 0.010(3) 0.002(3) C15 0.037(6) 0.039(6) 0.091(10) -0.038(6) 0.026(6) 0.001(5) C14 0.082(9) 0.050(7) 0.051(7) 0.010(6) 0.042(7) 0.008(6) C16 0.043(7) 0.068(8) 0.064(9) -0.001(7) 0.020(6) -0.009(6) C17 0.047(6) 0.090(8) 0.065(7) 0.010(6) 0.009(6) 0.002(6) C18 0.067(7) 0.086(8) 0.071(8) 0.011(7) 0.005(6) -0.007(7) C4 0.029(4) 0.020(4) 0.029(4) -0.012(3) 0.015(4) -0.007(3) C5 0.039(5) 0.045(5) 0.040(5) 0.015(4) 0.025(4) 0.010(4) C6 0.032(5) 0.070(7) 0.054(6) 0.025(5) 0.022(5) 0.003(5) N6 0.030(4) 0.053(5) 0.039(5) 0.028(4) -0.004(4) -0.003(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 Cu1 . Cu2 . 2.6899(19) yes Cu1 . I1 . 2.5283(13) yes Cu1 . I2 . 2.5586(15) yes Cu1 . I3 . 2.5657(15) yes Cu2 . Cu3 . 2.469(2) yes Cu2 . I2 . 2.5513(15) yes Cu2 . I3 . 2.8842(19) yes Cu2 . I5 . 2.6832(17) yes Cu2 . I4 . 2.6441(15) yes Cu3 . Cu4 . 2.575(2) yes Cu3 . I3 . 2.893(2) yes Cu3 . I5 . 2.961(2) yes Cu3 . I4 . 2.5603(16) yes Cu3 . I6 . 2.5252(17) yes Cu4 . I5 . 2.5957(18) yes Cu4 . I6 . 2.6042(15) yes Cu4 . I7 . 2.5174(15) yes Y1 . O3 . 2.327(6) yes Y1 . O4 . 2.299(6) yes Y1 . O7 . 2.408(6) yes Y1 . O8 . 2.308(6) yes Y1 . O1 . 2.356(6) yes Y1 . O5 . 2.353(6) yes Y1 . O6 . 2.347(6) yes Y1 . O2 . 2.348(6) yes O3 . C7 . 1.250(12) yes O4 . C10 . 1.262(10) yes O7 . C19 . 1.244(10) yes O8 . C22 . 1.239(10) yes O1 . C1 . 1.263(9) yes O5 . C13 . 1.226(11) yes O6 . C16 . 1.209(15) yes O2 . C4 . 1.226(11) yes N3 . C7 . 1.328(13) yes N3 . C9 . 1.391(15) yes N3 . C8 . 1.492(13) yes N4 . C10 . 1.300(11) yes N4 . C12 . 1.470(12) yes N4 . C11 . 1.461(14) yes N7 . C19 . 1.314(11) yes N7 . C20 . 1.447(13) yes N7 . C21 . 1.469(12) yes N8 . C22 . 1.318(10) yes N8 . C24 . 1.449(11) yes N8 . C23 . 1.445(12) yes N1 . C1 . 1.303(10) yes N1 . C2 . 1.457(10) yes N1 . C3 . 1.457(11) yes N5 . C13 . 1.321(11) yes N5 . C15 . 1.464(12) yes N5 . C14 . 1.417(14) yes N2 . C4 . 1.344(10) yes N2 . C5 . 1.469(12) yes N2 . C6 . 1.456(13) yes C7 . H71 . 0.937 no C9 . H91 . 0.969 no C9 . H92 . 0.957 no C9 . H93 . 0.962 no C8 . H81 . 0.962 no C8 . H82 . 0.964 no C8 . H83 . 0.968 no C10 . H101 . 0.932 no C12 . H121 . 0.960 no C12 . H122 . 0.960 no C12 . H123 . 0.966 no C11 . H111 . 0.960 no C11 . H112 . 0.953 no C11 . H113 . 0.961 no C19 . H191 . 0.932 no C20 . H201 . 0.956 no C20 . H202 . 0.958 no C20 . H203 . 0.956 no C21 . H211 . 0.962 no C21 . H212 . 0.959 no C21 . H213 . 0.962 no C22 . H221 . 0.933 no C24 . H241 . 0.962 no C24 . H242 . 0.958 no C24 . H243 . 0.953 no C23 . H231 . 0.953 no C23 . H232 . 0.957 no C23 . H233 . 0.964 no C1 . H11 . 0.934 no C2 . H21 . 0.956 no C2 . H22 . 0.959 no C2 . H23 . 0.965 no C3 . H31 . 0.957 no C3 . H32 . 0.957 no C3 . H33 . 0.962 no C13 . H131 . 0.932 no C15 . H151 . 0.959 no C15 . H152 . 0.964 no C15 . H153 . 0.956 no C14 . H141 . 0.961 no C14 . H142 . 0.964 no C14 . H143 . 0.960 no C16 . N6 . 1.331(16) yes C16 . H161 . 0.941 no C17 . N6 . 1.447(17) yes C17 . H171 . 0.953 no C17 . H172 . 0.975 no C17 . H173 . 0.960 no C18 . N6 . 1.428(18) yes C18 . H181 . 0.983 no C18 . H182 . 0.951 no C18 . H183 . 0.960 no C4 . H41 . 0.928 no C5 . H51 . 0.957 no C5 . H52 . 0.962 no C5 . H53 . 0.960 no C6 . H61 . 0.957 no C6 . H62 . 0.961 no C6 . H63 . 0.955 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 Cu2 . Cu1 . I1 . 166.62(6) yes Cu2 . Cu1 . I2 . 58.10(4) yes I1 . Cu1 . I2 . 121.00(5) yes Cu2 . Cu1 . I3 . 66.52(4) yes I1 . Cu1 . I3 . 116.14(4) yes I2 . Cu1 . I3 . 122.86(5) yes Cu1 . Cu2 . Cu3 . 118.84(8) yes Cu1 . Cu2 . I2 . 58.37(4) yes Cu3 . Cu2 . I2 . 175.17(9) yes Cu1 . Cu2 . I3 . 54.68(4) yes Cu3 . Cu2 . I3 . 64.88(7) yes I2 . Cu2 . I3 . 111.63(6) yes Cu1 . Cu2 . I5 . 108.66(5) yes Cu3 . Cu2 . I5 . 70.02(6) yes I2 . Cu2 . I5 . 114.33(6) yes I3 . Cu2 . I5 . 98.41(5) yes Cu1 . Cu2 . I4 . 138.26(7) yes Cu3 . Cu2 . I4 . 59.98(5) yes I2 . Cu2 . I4 . 118.91(6) yes I3 . Cu2 . I4 . 102.09(6) yes I5 . Cu2 . I4 . 108.88(5) yes Cu2 . Cu3 . Cu4 . 105.62(7) yes Cu2 . Cu3 . I3 . 64.51(6) yes Cu4 . Cu3 . I3 . 87.88(6) yes Cu2 . Cu3 . I5 . 58.38(5) yes Cu4 . Cu3 . I5 . 55.39(5) yes I3 . Cu3 . I5 . 92.15(5) yes Cu2 . Cu3 . I4 . 63.40(5) yes Cu4 . Cu3 . I4 . 156.42(10) yes I3 . Cu3 . I4 . 103.98(6) yes I5 . Cu3 . I4 . 103.17(6) yes Cu2 . Cu3 . I6 . 165.91(9) yes Cu4 . Cu3 . I6 . 61.40(5) yes I3 . Cu3 . I6 . 117.53(7) yes I5 . Cu3 . I6 . 107.66(7) yes I4 . Cu3 . I6 . 126.16(7) yes Cu3 . Cu4 . I5 . 69.88(6) yes Cu3 . Cu4 . I6 . 58.36(5) yes I5 . Cu4 . I6 . 117.13(5) yes Cu3 . Cu4 . I7 . 153.64(8) yes I5 . Cu4 . I7 . 126.01(6) yes I6 . Cu4 . I7 . 115.96(6) yes Cu1 . I2 . Cu2 . 63.53(5) yes Cu3 . I3 . Cu2 . 50.61(4) yes Cu3 . I3 . Cu1 . 108.82(4) yes Cu2 . I3 . Cu1 . 58.80(4) yes Cu3 . I5 . Cu2 . 51.60(5) yes Cu3 . I5 . Cu4 . 54.73(5) yes Cu2 . I5 . Cu4 . 99.15(6) yes Cu2 . I4 . Cu3 . 56.63(5) yes Cu4 . I6 . Cu3 . 60.24(5) yes O3 . Y1 . O4 . 79.7(2) yes O3 . Y1 . O7 . 72.2(2) yes O4 . Y1 . O7 . 74.1(2) yes O3 . Y1 . O8 . 142.6(2) yes O4 . Y1 . O8 . 96.0(2) yes O7 . Y1 . O8 . 70.9(2) yes O3 . Y1 . O1 . 134.4(2) yes O4 . Y1 . O1 . 71.5(2) yes O7 . Y1 . O1 . 128.9(2) yes O8 . Y1 . O1 . 76.4(2) yes O3 . Y1 . O5 . 124.3(2) yes O4 . Y1 . O5 . 143.8(2) yes O7 . Y1 . O5 . 135.4(2) yes O8 . Y1 . O5 . 80.0(2) yes O1 . Y1 . O5 . 72.5(2) yes O3 . Y1 . O6 . 78.2(2) yes O4 . Y1 . O6 . 143.2(2) yes O7 . Y1 . O6 . 71.4(2) yes O8 . Y1 . O6 . 84.4(2) yes O1 . Y1 . O6 . 142.6(2) yes O3 . Y1 . O2 . 70.6(2) yes O4 . Y1 . O2 . 95.7(2) yes O7 . Y1 . O2 . 142.7(2) yes O8 . Y1 . O2 . 146.4(2) yes O1 . Y1 . O2 . 77.8(2) yes O5 . Y1 . O6 . 72.7(2) yes O5 . Y1 . O2 . 72.0(2) yes O6 . Y1 . O2 . 104.1(2) yes Y1 . O3 . C7 . 152.4(6) yes Y1 . O4 . C10 . 137.0(5) yes Y1 . O7 . C19 . 124.3(5) yes Y1 . O8 . C22 . 138.0(5) yes Y1 . O1 . C1 . 136.7(5) yes Y1 . O5 . C13 . 146.1(6) yes Y1 . O6 . C16 . 152.5(8) yes Y1 . O2 . C4 . 139.3(6) yes C7 . N3 . C9 . 123.1(10) yes C7 . N3 . C8 . 116.7(9) yes C9 . N3 . C8 . 120.1(10) yes C10 . N4 . C12 . 118.9(8) yes C10 . N4 . C11 . 123.1(8) yes C12 . N4 . C11 . 117.9(8) yes C19 . N7 . C20 . 122.0(8) yes C19 . N7 . C21 . 121.7(8) yes C20 . N7 . C21 . 116.1(8) yes C22 . N8 . C24 . 122.2(7) yes C22 . N8 . C23 . 122.0(7) yes C24 . N8 . C23 . 115.8(8) yes C1 . N1 . C2 . 120.5(7) yes C1 . N1 . C3 . 122.4(7) yes C2 . N1 . C3 . 117.0(7) yes C13 . N5 . C15 . 121.8(9) yes C13 . N5 . C14 . 120.7(8) yes C15 . N5 . C14 . 117.4(9) yes C4 . N2 . C5 . 121.3(8) yes C4 . N2 . C6 . 119.1(8) yes C5 . N2 . C6 . 119.0(7) yes N3 . C7 . O3 . 123.2(9) yes N3 . C7 . H71 . 118.5 no O3 . C7 . H71 . 118.3 no N3 . C9 . H91 . 108.1 no N3 . C9 . H92 . 109.8 no H91 . C9 . H92 . 109.7 no N3 . C9 . H93 . 109.1 no H91 . C9 . H93 . 109.6 no H92 . C9 . H93 . 110.5 no N3 . C8 . H81 . 109.8 no N3 . C8 . H82 . 109.4 no H81 . C8 . H82 . 109.6 no N3 . C8 . H83 . 108.9 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.6 no N4 . C10 . O4 . 121.9(8) yes N4 . C10 . H101 . 118.6 no O4 . C10 . H101 . 119.5 no N4 . C12 . H121 . 110.0 no N4 . C12 . H122 . 109.7 no H121 . C12 . H122 . 109.4 no N4 . C12 . H123 . 109.1 no H121 . C12 . H123 . 109.3 no H122 . C12 . H123 . 109.3 no N4 . C11 . H111 . 109.0 no N4 . C11 . H112 . 109.6 no H111 . C11 . H112 . 109.9 no N4 . C11 . H113 . 109.4 no H111 . C11 . H113 . 109.3 no H112 . C11 . H113 . 109.7 no N7 . C19 . O7 . 124.2(8) yes N7 . C19 . H191 . 118.1 no O7 . C19 . H191 . 117.8 no N7 . C20 . H201 . 109.6 no N7 . C20 . H202 . 109.0 no H201 . C20 . H202 . 109.2 no N7 . C20 . H203 . 109.8 no H201 . C20 . H203 . 109.8 no H202 . C20 . H203 . 109.5 no N7 . C21 . H211 . 109.1 no N7 . C21 . H212 . 109.9 no H211 . C21 . H212 . 109.2 no N7 . C21 . H213 . 109.8 no H211 . C21 . H213 . 109.2 no H212 . C21 . H213 . 109.6 no N8 . C22 . O8 . 124.6(7) yes N8 . C22 . H221 . 117.6 no O8 . C22 . H221 . 117.8 no N8 . C24 . H241 . 109.6 no N8 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.4 no N8 . C24 . H243 . 109.8 no H241 . C24 . H243 . 109.3 no H242 . C24 . H243 . 109.4 no N8 . C23 . H231 . 109.4 no N8 . C23 . H232 . 109.7 no H231 . C23 . H232 . 109.8 no N8 . C23 . H233 . 109.2 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.2 no N1 . C1 . O1 . 123.6(8) yes N1 . C1 . H11 . 117.7 no O1 . C1 . H11 . 118.7 no N1 . C2 . H21 . 110.2 no N1 . C2 . H22 . 109.4 no H21 . C2 . H22 . 109.7 no N1 . C2 . H23 . 109.0 no H21 . C2 . H23 . 109.3 no H22 . C2 . H23 . 109.3 no N1 . C3 . H31 . 109.4 no N1 . C3 . H32 . 110.1 no H31 . C3 . H32 . 109.5 no N1 . C3 . H33 . 109.6 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 108.8 no N5 . C13 . O5 . 125.2(8) yes N5 . C13 . H131 . 117.1 no O5 . C13 . H131 . 117.7 no N5 . C15 . H151 . 109.8 no N5 . C15 . H152 . 109.1 no H151 . C15 . H152 . 109.3 no N5 . C15 . H153 . 109.9 no H151 . C15 . H153 . 109.4 no H152 . C15 . H153 . 109.3 no N5 . C14 . H141 . 110.2 no N5 . C14 . H142 . 109.7 no H141 . C14 . H142 . 109.0 no N5 . C14 . H143 . 109.4 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.1 no O6 . C16 . N6 . 122.7(12) yes O6 . C16 . H161 . 119.3 no N6 . C16 . H161 . 118.0 no N6 . C17 . H171 . 109.4 no N6 . C17 . H172 . 106.2 no H171 . C17 . H172 . 110.3 no N6 . C17 . H173 . 109.5 no H171 . C17 . H173 . 111.6 no H172 . C17 . H173 . 109.7 no N6 . C18 . H181 . 106.6 no N6 . C18 . H182 . 110.5 no H181 . C18 . H182 . 109.3 no N6 . C18 . H183 . 108.9 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 111.9 no N2 . C4 . O2 . 124.7(8) yes N2 . C4 . H41 . 117.2 no O2 . C4 . H41 . 118.1 no N2 . C5 . H51 . 109.4 no N2 . C5 . H52 . 109.1 no H51 . C5 . H52 . 109.9 no N2 . C5 . H53 . 109.4 no H51 . C5 . H53 . 109.4 no H52 . C5 . H53 . 109.7 no N2 . C6 . H61 . 109.7 no N2 . C6 . H62 . 109.5 no H61 . C6 . H62 . 109.1 no N2 . C6 . H63 . 110.0 no H61 . C6 . H63 . 109.2 no H62 . C6 . H63 . 109.3 no C17 . N6 . C18 . 119.6(11) yes C17 . N6 . C16 . 116.8(11) yes C18 . N6 . C16 . 121.9(11) yes #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 620034' _audit_creation_date 06-04-07 _audit_creation_method CRYSTALS_ver_12.83 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.761(5) _cell_length_b 13.862(5) _cell_length_c 21.330(5) _cell_angle_alpha 90 _cell_angle_beta 114.768(5) _cell_angle_gamma 90 _cell_volume 5305(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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' 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' 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' 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' 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' Ca 0.2262 0.3064 8.6266 10.4421 7.3873 0.6599 1.5899 85.7484 1.0211 178.4370 1.3751 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C30 H70 Ca10 Cu10 I10 N10 O10 Y10 # Dc = 4.91 Fooo = 4112.00 Mu = 215.56 M = 3925.30 # Found Formula = C18 H42 Cu7 I10 N6 O8 Y1 # Dc = 2.85 FOOO = 4112.00 Mu = 96.86 M = 2273.34 _chemical_formula_sum 'C18 H42 Cu7 I10 N6 O8 Y1' _chemical_formula_moiety 'C18 H42 Cu7 I10 N6 O8 Y1' _chemical_compound_source ? _chemical_formula_weight 2273.34 _cell_measurement_reflns_used 8847 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_min 0.151 _exptl_crystal_size_mid 0.273 _exptl_crystal_size_max 0.316 _exptl_crystal_density_diffrn 2.846 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 9.686 # Sheldrick geometric approximatio 0.62 0.62 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.52 _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_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement '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 'DIAMOND v3 (Brandenburg & Putz)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 14017 _reflns_number_total 13472 _diffrn_reflns_av_R_equivalents 0.096 # Number of reflections with Friedels Law is 13472 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 13598 _diffrn_reflns_theta_min 1.135 _diffrn_reflns_theta_max 28.695 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.834 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -26 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.97 _refine_diff_density_max 13.75 _refine_ls_number_reflns 4625 _refine_ls_number_restraints 204 _refine_ls_number_parameters 451 #_refine_ls_R_factor_ref 0.0973 _refine_ls_wR_factor_ref 0.0969 _refine_ls_goodness_of_fit_ref 1.1134 #_reflns_number_all 13430 _refine_ls_R_factor_all 0.2045 _refine_ls_wR_factor_all 0.1597 # 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 4625 _refine_ls_R_factor_gt 0.0973 _refine_ls_wR_factor_gt 0.0969 _refine_ls_shift/su_max 0.026141 # 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 noref # 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: 3.14 -0.453E-01 2.13 0.221 -0.695E-01 ; _publ_section_exptl_refinement ; All non hydroen atoms were refined anisotropically. Hydrogen were placed geometrically and initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Brandenburg, K., & Putz, H. Diamond - Crystal and Molecular Structure Visualization Crystal Impact - GbR, Postfach 1251, D-53002 Bonn 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. Walker, N., and Stuart, (1983). D. Acta Cryst, A39, 158-166 Watkin D.J. (1994). Acta Cryst, A50, 411-437 ; 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 Cu1 Cu 0.8942(3) 0.8503(4) 0.8066(3) 0.0978 1.0000 Uani . . . . . . Cu2 Cu 0.7218(3) 0.9308(3) 0.8563(2) 0.0676 1.0000 Uani . . . . . . Cu3 Cu 0.6781(2) 0.9377(4) 0.7121(2) 0.0696 1.0000 Uani . . . . . . Cu4 Cu 0.5619(3) 0.8865(4) 0.8297(2) 0.0720 1.0000 Uani . . . . . . Cu5 Cu 0.5188(2) 0.8851(3) 0.6838(2) 0.0680 1.0000 Uani . . . . . . Cu6 Cu 0.6050(3) 1.0989(4) 0.8414(3) 0.0807 1.0000 Uani . . . . . . Cu7 Cu 0.5656(3) 1.1044(4) 0.6928(2) 0.0750 1.0000 Uani . . . . . . I1 I 1.00624(15) 0.7553(2) 0.81217(16) 0.0872 1.0000 Uani . . . . . . I2 I 0.85943(12) 0.86801(17) 0.91007(11) 0.0606 1.0000 Uani . . . . . . I3 I 0.79270(15) 0.8899(3) 0.68759(13) 0.0885 1.0000 Uani . . . . . . I4 I 0.63865(10) 0.79002(14) 0.77231(10) 0.0478 1.0000 Uani . . . . . . I5 I 0.66412(12) 0.97041(15) 0.94522(10) 0.0519 1.0000 Uani . . . . . . I6 I 0.71109(11) 1.10246(14) 0.78996(10) 0.0469 1.0000 Uani . . . . . . I7 I 0.56272(11) 0.97982(15) 0.59813(9) 0.0504 1.0000 Uani . . . . . . I8 I 0.40806(11) 0.77006(15) 0.61583(10) 0.0550 1.0000 Uani . . . . . . I9 I 0.47865(10) 1.02970(14) 0.74823(9) 0.0449 1.0000 Uani . . . . . . I10 I 0.52305(12) 1.27268(15) 0.63730(10) 0.0546 1.0000 Uani . . . . . . Y1 Y 0.20589(16) 0.5292(2) 0.20668(14) 0.0437 1.0000 Uani . . . . . . O1 O 0.1709(13) 0.3607(16) 0.1881(11) 0.0612 1.0000 Uani . . . . . . O2 O 0.3167(11) 0.6214(14) 0.2283(11) 0.0553 1.0000 Uani . . . . . . O3 O 0.3061(10) 0.4645(14) 0.2970(9) 0.0498 1.0000 Uani D . . . . . O4 O 0.1584(12) 0.4724(15) 0.2821(10) 0.0836 1.0000 Uani D . . . . . O5 O 0.2452(7) 0.4563(15) 0.1300(8) 0.0539 1.0000 Uani D . . . . . O6 O 0.0806(13) 0.5412(19) 0.1402(7) 0.0782 1.0000 Uani D . . . . . O7 O 0.1838(9) 0.6481(12) 0.1189(9) 0.0642 1.0000 Uani D . . . . . O8 O 0.1946(9) 0.6578(14) 0.2660(11) 0.0560 1.0000 Uani D . . . . . N1 N 0.3812(13) 0.3771(17) 0.3893(11) 0.0587 1.0000 Uani D U . . . . N2 N 0.0961(13) 0.4375(15) 0.3489(9) 0.0640 1.0000 Uani D U . . . . N3 N 0.2996(9) 0.4182(18) 0.0584(9) 0.0580 1.0000 Uani D U . . . . N4 N -0.0460(14) 0.528(2) 0.0887(8) 0.0656 1.0000 Uani D U . . . . N5 N 0.1356(11) 0.7796(15) 0.0512(9) 0.0626 1.0000 Uani D U . . . . N6 N 0.2567(10) 0.7424(17) 0.3669(12) 0.0595 1.0000 Uani D U . . . . C1 C 0.3197(17) 0.389(2) 0.3322(14) 0.0687 1.0000 Uani D U . . . . C2 C 0.393(3) 0.282(3) 0.429(2) 0.1083 1.0000 Uani D U . . . . C3 C 0.442(2) 0.449(3) 0.420(2) 0.1088 1.0000 Uani D U . . . . C4 C 0.1069(16) 0.488(2) 0.3006(12) 0.0694 1.0000 Uani D U . . . . C5 C 0.038(2) 0.453(3) 0.3695(17) 0.1121 1.0000 Uani D U . . . . C6 C 0.146(2) 0.357(2) 0.3850(16) 0.1079 1.0000 Uani D U . . . . C7 C 0.2876(11) 0.477(2) 0.1001(11) 0.0638 1.0000 Uani D U . . . . C8 C 0.2661(16) 0.322(3) 0.0409(17) 0.1055 1.0000 Uani D U . . . . C9 C 0.3505(14) 0.459(3) 0.0299(17) 0.1104 1.0000 Uani D U . . . . C10 C 0.0240(17) 0.491(3) 0.1118(9) 0.0747 1.0000 Uani D U . . . . C11 C -0.106(3) 0.457(3) 0.0567(11) 0.1166 1.0000 Uani D U . . . . C12 C -0.063(3) 0.633(3) 0.0943(12) 0.1146 1.0000 Uani D U . . . . C13 C 0.1350(15) 0.7136(19) 0.1018(12) 0.0703 1.0000 Uani D U . . . . C14 C 0.0776(18) 0.857(2) 0.0326(17) 0.1062 1.0000 Uani D U . . . . C15 C 0.1869(18) 0.779(3) 0.0171(15) 0.0967 1.0000 Uani D U . . . . C16 C 0.2087(13) 0.737(2) 0.2988(16) 0.0686 1.0000 Uani D U . . . . C17 C 0.2941(15) 0.656(3) 0.404(2) 0.0885 1.0000 Uani D U . . . . C18 C 0.2695(15) 0.838(3) 0.3995(19) 0.0791 1.0000 Uani D U . . . . H11 H 0.2820 0.3345 0.3165 0.0901 1.0000 Uiso . . . . . . H21 H 0.4413 0.2869 0.4702 0.1338 1.0000 Uiso . . . . . . H22 H 0.3512 0.2748 0.4431 0.1338 1.0000 Uiso . . . . . . H23 H 0.3932 0.2300 0.3981 0.1338 1.0000 Uiso . . . . . . H31 H 0.4823 0.4224 0.4644 0.1370 1.0000 Uiso . . . . . . H32 H 0.4221 0.5098 0.4328 0.1370 1.0000 Uiso . . . . . . H33 H 0.4642 0.4654 0.3878 0.1370 1.0000 Uiso . . . . . . H41 H 0.0742 0.5405 0.2782 0.0887 1.0000 Uiso . . . . . . H51 H 0.0471 0.4012 0.4111 0.1409 1.0000 Uiso . . . . . . H52 H 0.0431 0.5162 0.3933 0.1409 1.0000 Uiso . . . . . . H53 H -0.0097 0.4401 0.3349 0.1409 1.0000 Uiso . . . . . . H61 H 0.1341 0.3271 0.4199 0.1377 1.0000 Uiso . . . . . . H62 H 0.2008 0.3831 0.4086 0.1377 1.0000 Uiso . . . . . . H63 H 0.1467 0.3082 0.3500 0.1377 1.0000 Uiso . . . . . . H71 H 0.3122 0.5404 0.1092 0.0833 1.0000 Uiso . . . . . . H81 H 0.2842 0.2904 0.0075 0.1336 1.0000 Uiso . . . . . . H82 H 0.2827 0.2821 0.0833 0.1336 1.0000 Uiso . . . . . . H83 H 0.2113 0.3274 0.0183 0.1336 1.0000 Uiso . . . . . . H91 H 0.3574 0.4102 -0.0017 0.1368 1.0000 Uiso . . . . . . H92 H 0.3998 0.4736 0.0686 0.1368 1.0000 Uiso . . . . . . H93 H 0.3285 0.5190 0.0036 0.1368 1.0000 Uiso . . . . . . H101 H 0.0289 0.4191 0.1063 0.0901 1.0000 Uiso . . . . . . H111 H -0.1572 0.5034 0.0417 0.1403 1.0000 Uiso . . . . . . H112 H -0.1100 0.4134 0.0894 0.1403 1.0000 Uiso . . . . . . H113 H -0.1089 0.4331 0.0144 0.1403 1.0000 Uiso . . . . . . H121 H -0.1137 0.6455 0.0747 0.1385 1.0000 Uiso . . . . . . H122 H -0.0364 0.6516 0.1449 0.1385 1.0000 Uiso . . . . . . H123 H -0.0354 0.6711 0.0698 0.1385 1.0000 Uiso . . . . . . H131 H 0.0981 0.7182 0.1210 0.0885 1.0000 Uiso . . . . . . H141 H 0.0800 0.8963 -0.0045 0.1308 1.0000 Uiso . . . . . . H142 H 0.0831 0.8920 0.0732 0.1308 1.0000 Uiso . . . . . . H143 H 0.0261 0.8216 0.0127 0.1308 1.0000 Uiso . . . . . . H151 H 0.1762 0.8300 -0.0163 0.1217 1.0000 Uiso . . . . . . H152 H 0.2399 0.7839 0.0541 0.1217 1.0000 Uiso . . . . . . H153 H 0.1834 0.7131 -0.0064 0.1217 1.0000 Uiso . . . . . . H161 H 0.1831 0.7973 0.2742 0.0878 1.0000 Uiso . . . . . . H171 H 0.3278 0.6748 0.4545 0.1123 1.0000 Uiso . . . . . . H172 H 0.3257 0.6275 0.3836 0.1123 1.0000 Uiso . . . . . . H173 H 0.2571 0.6083 0.4057 0.1123 1.0000 Uiso . . . . . . H181 H 0.3064 0.8326 0.4499 0.1017 1.0000 Uiso . . . . . . H182 H 0.2909 0.8836 0.3762 0.1017 1.0000 Uiso . . . . . . H183 H 0.2221 0.8660 0.3983 0.1017 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.096(4) 0.091(4) 0.093(4) -0.006(3) 0.026(3) 0.014(3) Cu2 0.068(3) 0.072(3) 0.061(3) -0.001(2) 0.026(2) 0.002(2) Cu3 0.064(3) 0.083(3) 0.059(2) 0.000(2) 0.023(2) 0.006(2) Cu4 0.076(3) 0.077(3) 0.073(3) 0.002(2) 0.040(2) 0.000(2) Cu5 0.058(2) 0.077(3) 0.063(3) -0.002(2) 0.019(2) -0.001(2) Cu6 0.084(3) 0.070(3) 0.081(3) -0.010(3) 0.028(3) 0.000(3) Cu7 0.093(3) 0.068(3) 0.070(3) 0.002(2) 0.040(3) 0.002(2) I1 0.0648(16) 0.0845(19) 0.106(2) 0.0050(16) 0.0301(14) 0.0065(14) I2 0.0540(12) 0.0685(15) 0.0533(12) 0.0019(10) 0.0166(10) 0.0026(11) I3 0.0735(17) 0.140(3) 0.0588(14) 0.0138(15) 0.0340(13) 0.0404(17) I4 0.0469(11) 0.0446(11) 0.0489(11) -0.0007(9) 0.0171(9) 0.0039(9) I5 0.0604(12) 0.0497(12) 0.0479(11) -0.0015(9) 0.0249(9) -0.0022(10) I6 0.0470(11) 0.0443(11) 0.0495(11) -0.0004(9) 0.0202(9) -0.0025(9) I7 0.0507(11) 0.0577(12) 0.0441(10) 0.0006(9) 0.0212(9) 0.0056(10) I8 0.0514(12) 0.0478(12) 0.0565(12) 0.0037(9) 0.0135(10) -0.0007(10) I9 0.0443(11) 0.0425(11) 0.0500(10) 0.0012(9) 0.0217(9) -0.0012(9) I10 0.0625(13) 0.0470(12) 0.0555(12) 0.0032(9) 0.0259(10) 0.0070(10) Y1 0.0448(16) 0.0420(16) 0.0483(15) 0.0025(14) 0.0235(13) -0.0006(14) O1 0.082(15) 0.055(13) 0.067(14) -0.012(11) 0.051(13) -0.015(12) O2 0.042(11) 0.045(12) 0.067(13) 0.008(10) 0.011(10) 0.000(10) O3 0.055(12) 0.049(12) 0.056(12) 0.013(10) 0.033(10) 0.022(10) O4 0.11(2) 0.064(16) 0.11(2) 0.015(15) 0.073(18) 0.004(15) O5 0.039(11) 0.070(14) 0.057(12) 0.002(11) 0.025(10) -0.005(10) O6 0.056(14) 0.085(18) 0.080(17) 0.009(14) 0.016(13) -0.014(14) O7 0.048(12) 0.053(13) 0.088(16) 0.020(12) 0.026(12) 0.018(11) O8 0.049(12) 0.049(13) 0.085(15) -0.010(11) 0.043(11) 0.005(10) N1 0.065(9) 0.055(9) 0.069(9) 0.007(8) 0.041(8) 0.007(8) N2 0.070(9) 0.065(10) 0.072(9) 0.009(8) 0.043(8) 0.004(8) N3 0.058(9) 0.064(10) 0.069(9) 0.008(8) 0.042(8) 0.003(8) N4 0.056(9) 0.064(10) 0.079(10) 0.011(9) 0.031(8) 0.000(8) N5 0.059(9) 0.060(10) 0.073(10) 0.012(8) 0.031(8) 0.006(8) N6 0.063(9) 0.055(9) 0.070(9) 0.007(8) 0.037(8) 0.006(8) C1 0.073(10) 0.068(10) 0.074(10) -0.007(9) 0.040(9) -0.010(9) C2 0.141(19) 0.090(17) 0.094(17) 0.022(15) 0.050(15) 0.001(16) C3 0.140(18) 0.096(16) 0.094(15) 0.020(13) 0.053(14) 0.000(14) C4 0.072(11) 0.067(11) 0.076(11) 0.002(9) 0.037(10) -0.012(9) C5 0.140(16) 0.100(15) 0.099(14) 0.017(12) 0.054(13) -0.001(13) C6 0.132(16) 0.099(14) 0.098(14) 0.016(12) 0.053(13) -0.005(13) C7 0.065(11) 0.060(11) 0.074(11) 0.005(10) 0.036(10) -0.017(10) C8 0.124(15) 0.098(14) 0.097(13) 0.012(12) 0.049(12) -0.010(13) C9 0.121(14) 0.103(14) 0.103(13) 0.008(12) 0.043(12) -0.015(13) C10 0.069(11) 0.063(11) 0.085(11) 0.006(10) 0.025(10) -0.013(10) C11 0.118(14) 0.109(14) 0.109(13) 0.006(12) 0.034(12) -0.016(12) C12 0.114(14) 0.109(14) 0.107(13) 0.003(12) 0.033(12) -0.011(12) C13 0.067(11) 0.060(11) 0.083(11) -0.004(10) 0.031(10) -0.013(10) C14 0.105(13) 0.104(13) 0.102(13) 0.001(12) 0.036(11) -0.007(12) C15 0.098(12) 0.097(13) 0.093(12) -0.003(11) 0.039(11) -0.006(11) C16 0.068(11) 0.064(11) 0.079(11) -0.011(10) 0.035(9) -0.011(9) C17 0.093(12) 0.090(12) 0.085(11) -0.009(11) 0.039(10) -0.005(11) C18 0.087(11) 0.079(11) 0.077(11) -0.009(10) 0.040(10) -0.008(10) _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 I9 . Cu5 . 2.729(5) yes I9 . Cu4 . 2.696(5) yes I9 . Cu7 . 2.668(5) yes I9 . Cu6 . 2.635(5) yes I5 . Cu4 . 2.708(5) yes I5 . Cu2 . 2.648(5) yes I5 . Cu6 . 2.697(6) yes Cu5 . Cu4 . 2.860(6) yes Cu5 . Cu3 . 3.035(6) yes Cu5 . I7 . 2.673(5) yes Cu5 . I4 . 2.676(5) yes Cu5 . I8 . 2.603(5) yes Cu4 . I10 3_646 2.608(5) yes Cu4 . Cu2 . 3.030(7) yes Cu4 . Cu6 . 3.045(7) yes Cu4 . I4 . 2.672(5) yes Cu2 . Cu3 . 2.826(6) yes Cu2 . Cu6 . 3.201(7) yes Cu2 . I6 . 2.731(5) yes Cu2 . I4 . 2.693(5) yes Cu2 . I2 . 2.618(5) yes Cu3 . Cu7 . 3.112(7) yes Cu3 . I6 . 2.737(5) yes Cu3 . I7 . 2.609(5) yes Cu3 . I4 . 2.699(5) yes Cu3 . I3 . 2.614(5) yes Cu7 . Cu6 . 2.930(7) yes Cu7 . I6 . 2.751(5) yes Cu7 . I7 . 2.640(5) yes Cu7 . I10 . 2.592(5) yes Cu6 . I8 3_656 2.593(5) yes Cu6 . I6 . 2.744(6) yes I2 . Cu1 . 2.583(7) yes I3 . Cu1 . 2.550(6) yes Y1 . O5 . 2.32(2) yes Y1 . O2 . 2.41(2) yes Y1 . O1 . 2.42(2) yes Y1 . O3 . 2.289(19) yes Y1 . O8 . 2.249(19) yes Y1 . O4 . 2.31(2) yes Y1 . O7 . 2.39(2) yes Y1 . O6 . 2.29(2) yes I1 . Cu1 . 2.536(6) yes O5 . C7 . 1.28(3) yes O3 . C1 . 1.25(3) yes O8 . C16 . 1.27(3) yes O4 . C4 . 1.25(3) yes O7 . C13 . 1.26(3) yes O6 . C10 . 1.24(3) yes N1 . C1 . 1.32(3) yes N1 . C2 . 1.53(4) yes N1 . C3 . 1.49(4) yes N3 . C7 . 1.30(3) yes N3 . C8 . 1.46(4) yes N3 . C9 . 1.49(4) yes N5 . C13 . 1.42(3) yes N5 . C15 . 1.48(4) yes N5 . C14 . 1.49(4) yes N6 . C16 . 1.36(3) yes N6 . C18 . 1.47(4) yes N6 . C17 . 1.46(4) yes N4 . C10 . 1.36(3) yes N4 . C12 . 1.51(4) yes N4 . C11 . 1.47(4) yes C7 . H71 . 0.986 no C1 . H11 . 1.012 no C8 . H81 . 1.020 no C8 . H82 . 0.994 no C8 . H83 . 0.987 no C16 . H161 . 1.005 no C13 . H131 . 0.977 no C10 . H101 . 1.010 no C15 . H151 . 0.967 no C15 . H152 . 1.016 no C15 . H153 . 1.026 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 0.999 no C2 . H21 . 0.992 no C2 . H22 . 0.991 no C2 . H23 . 0.979 no C18 . H181 . 1.018 no C18 . H182 . 1.005 no C18 . H183 . 1.006 no C3 . H31 . 1.022 no C3 . H32 . 1.013 no C3 . H33 . 0.982 no C17 . H171 . 1.030 no C17 . H172 . 0.984 no C17 . H173 . 0.991 no C14 . H141 . 0.982 no C14 . H142 . 0.961 no C14 . H143 . 1.042 no C12 . H121 . 0.930 no C12 . H122 . 1.015 no C12 . H123 . 1.036 no C11 . H111 . 1.126 no C11 . H112 . 0.952 no C11 . H113 . 0.941 no N2 . C4 . 1.33(3) yes N2 . C6 . 1.47(4) yes N2 . C5 . 1.41(4) yes C4 . H41 . 0.958 no C6 . H61 . 0.963 no C6 . H62 . 1.051 no C6 . H63 . 1.014 no C5 . H51 . 1.095 no C5 . H52 . 0.997 no C5 . H53 . 0.939 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 Cu5 . I9 . Cu4 . 63.64(14) yes Cu5 . I9 . Cu7 . 71.65(15) yes Cu4 . I9 . Cu7 . 103.79(16) yes Cu5 . I9 . Cu6 . 105.28(16) yes Cu4 . I9 . Cu6 . 69.65(16) yes Cu7 . I9 . Cu6 . 67.08(16) yes Cu4 . I5 . Cu2 . 68.88(14) yes Cu4 . I5 . Cu6 . 68.58(15) yes Cu2 . I5 . Cu6 . 73.58(16) yes I9 . Cu5 . Cu4 . 57.62(14) yes I9 . Cu5 . Cu3 . 102.68(17) yes Cu4 . Cu5 . Cu3 . 88.30(17) yes I9 . Cu5 . I7 . 103.28(17) yes Cu4 . Cu5 . I7 . 134.9(2) yes Cu3 . Cu5 . I7 . 53.95(12) yes I9 . Cu5 . I4 . 111.39(16) yes Cu4 . Cu5 . I4 . 57.59(13) yes Cu3 . Cu5 . I4 . 55.97(13) yes I7 . Cu5 . I4 . 106.22(16) yes I9 . Cu5 . I8 . 112.11(17) yes Cu4 . Cu5 . I8 . 114.08(19) yes Cu3 . Cu5 . I8 . 144.9(2) yes I7 . Cu5 . I8 . 110.97(17) yes I4 . Cu5 . I8 . 112.35(18) yes Cu5 . Cu4 . I5 . 139.6(2) yes Cu5 . Cu4 . I9 . 58.74(14) yes I5 . Cu4 . I9 . 106.95(18) yes Cu5 . Cu4 . I10 3_646 110.94(19) yes I5 . Cu4 . I10 3_646 109.45(17) yes I9 . Cu4 . I10 3_646 109.34(18) yes Cu5 . Cu4 . Cu2 . 91.00(17) yes I5 . Cu4 . Cu2 . 54.63(13) yes I9 . Cu4 . Cu2 . 106.20(18) yes I10 3_646 Cu4 . Cu2 . 144.2(2) yes Cu5 . Cu4 . Cu6 . 92.40(19) yes I5 . Cu4 . Cu6 . 55.54(14) yes I9 . Cu4 . Cu6 . 54.23(14) yes I10 3_646 Cu4 . Cu6 . 138.8(2) yes Cu2 . Cu4 . Cu6 . 63.61(16) yes Cu5 . Cu4 . I4 . 57.74(13) yes I5 . Cu4 . I4 . 106.38(17) yes I9 . Cu4 . I4 . 112.58(17) yes I10 3_646 Cu4 . I4 . 111.95(19) yes Cu2 . Cu4 . I4 . 55.94(13) yes Cu6 . Cu4 . I4 . 109.22(19) yes Cu4 . Cu2 . I5 . 56.49(13) yes Cu4 . Cu2 . Cu3 . 89.05(18) yes I5 . Cu2 . Cu3 . 138.2(2) yes Cu4 . Cu2 . Cu6 . 58.43(15) yes I5 . Cu2 . Cu6 . 53.91(13) yes Cu3 . Cu2 . Cu6 . 89.33(18) yes Cu4 . Cu2 . I6 . 103.34(17) yes I5 . Cu2 . I6 . 103.12(17) yes Cu3 . Cu2 . I6 . 58.99(14) yes Cu6 . Cu2 . I6 . 54.41(14) yes Cu4 . Cu2 . I4 . 55.29(13) yes I5 . Cu2 . I4 . 107.51(17) yes Cu3 . Cu2 . I4 . 58.50(14) yes Cu6 . Cu2 . I4 . 104.33(17) yes I6 . Cu2 . I4 . 113.17(16) yes Cu4 . Cu2 . I2 . 145.6(2) yes I5 . Cu2 . I2 . 115.79(17) yes Cu3 . Cu2 . I2 . 106.02(18) yes Cu6 . Cu2 . I2 . 149.2(2) yes I6 . Cu2 . I2 . 110.96(18) yes I4 . Cu2 . I2 . 106.45(17) yes Cu5 . Cu3 . Cu2 . 91.56(18) yes Cu5 . Cu3 . Cu7 . 61.84(16) yes Cu2 . Cu3 . Cu7 . 92.57(18) yes Cu5 . Cu3 . I6 . 106.54(17) yes Cu2 . Cu3 . I6 . 58.78(14) yes Cu7 . Cu3 . I6 . 55.67(13) yes Cu5 . Cu3 . I7 . 55.93(13) yes Cu2 . Cu3 . I7 . 140.5(2) yes Cu7 . Cu3 . I7 . 54.10(13) yes I6 . Cu3 . I7 . 105.76(17) yes Cu5 . Cu3 . I4 . 55.27(13) yes Cu2 . Cu3 . I4 . 58.29(14) yes Cu7 . Cu3 . I4 . 107.05(18) yes I6 . Cu3 . I4 . 112.79(16) yes I7 . Cu3 . I4 . 107.42(17) yes Cu5 . Cu3 . I3 . 144.3(2) yes Cu2 . Cu3 . I3 . 108.28(18) yes Cu7 . Cu3 . I3 . 142.4(2) yes I6 . Cu3 . I3 . 109.07(19) yes I7 . Cu3 . I3 . 111.23(17) yes I4 . Cu3 . I3 . 110.49(19) yes Cu3 . Cu7 . I9 . 102.14(18) yes Cu3 . Cu7 . Cu6 . 89.21(18) yes I9 . Cu7 . Cu6 . 55.93(14) yes Cu3 . Cu7 . I6 . 55.24(13) yes I9 . Cu7 . I6 . 109.06(17) yes Cu6 . Cu7 . I6 . 57.66(14) yes Cu3 . Cu7 . I7 . 53.18(13) yes I9 . Cu7 . I7 . 105.89(18) yes Cu6 . Cu7 . I7 . 136.2(2) yes I6 . Cu7 . I7 . 104.50(18) yes Cu3 . Cu7 . I10 . 143.7(2) yes I9 . Cu7 . I10 . 113.95(19) yes Cu6 . Cu7 . I10 . 114.0(2) yes I6 . Cu7 . I10 . 112.91(19) yes I7 . Cu7 . I10 . 109.88(17) yes Cu2 . Cu6 . Cu4 . 57.96(15) yes Cu2 . Cu6 . Cu7 . 88.86(18) yes Cu4 . Cu6 . Cu7 . 89.87(18) yes Cu2 . Cu6 . I5 . 52.51(13) yes Cu4 . Cu6 . I5 . 55.89(14) yes Cu7 . Cu6 . I5 . 137.1(2) yes Cu2 . Cu6 . I9 . 103.06(18) yes Cu4 . Cu6 . I9 . 56.11(14) yes Cu7 . Cu6 . I9 . 57.00(14) yes I5 . Cu6 . I9 . 109.06(19) yes Cu2 . Cu6 . I8 3_656 143.6(2) yes Cu4 . Cu6 . I8 3_656 148.0(2) yes Cu7 . Cu6 . I8 3_656 109.6(2) yes I5 . Cu6 . I8 3_656 112.83(19) yes I9 . Cu6 . I8 3_656 113.3(2) yes Cu2 . Cu6 . I6 . 54.03(13) yes Cu4 . Cu6 . I6 . 102.62(18) yes Cu7 . Cu6 . I6 . 57.90(15) yes I5 . Cu6 . I6 . 101.50(18) yes I9 . Cu6 . I6 . 110.25(18) yes I8 3_656 Cu6 . I6 . 109.2(2) yes Cu7 . I6 . Cu6 . 64.44(15) yes Cu7 . I6 . Cu3 . 69.09(15) yes Cu6 . I6 . Cu3 . 101.52(15) yes Cu7 . I6 . Cu2 . 103.20(15) yes Cu6 . I6 . Cu2 . 71.56(15) yes Cu3 . I6 . Cu2 . 62.23(14) yes Cu5 . I7 . Cu7 . 72.96(15) yes Cu5 . I7 . Cu3 . 70.12(14) yes Cu7 . I7 . Cu3 . 72.72(16) yes Cu3 . I4 . Cu2 . 63.22(14) yes Cu3 . I4 . Cu5 . 68.75(14) yes Cu2 . I4 . Cu5 . 103.03(15) yes Cu3 . I4 . Cu4 . 99.81(16) yes Cu2 . I4 . Cu4 . 68.77(15) yes Cu5 . I4 . Cu4 . 64.67(15) yes Cu5 . I8 . Cu6 3_646 123.28(17) yes Cu2 . I2 . Cu1 . 104.85(17) yes Cu4 3_656 I10 . Cu7 . 122.93(16) yes Cu3 . I3 . Cu1 . 103.95(19) yes O5 . Y1 . O2 . 79.6(7) yes O5 . Y1 . O1 . 67.7(7) yes O2 . Y1 . O1 . 135.9(7) yes O5 . Y1 . O3 . 89.7(3) yes O2 . Y1 . O3 . 69.5(7) yes O1 . Y1 . O3 . 81.2(8) yes O5 . Y1 . O8 . 152.1(6) yes O2 . Y1 . O8 . 76.6(6) yes O1 . Y1 . O8 . 140.1(6) yes O3 . Y1 . O8 . 95.3(7) yes O5 . Y1 . O4 . 134.1(7) yes O2 . Y1 . O4 . 130.4(6) yes O1 . Y1 . O4 . 67.3(6) yes O3 . Y1 . O4 . 75.0(7) yes O8 . Y1 . O4 . 73.4(6) yes O5 . Y1 . O7 . 75.7(6) yes O2 . Y1 . O7 . 68.7(6) yes O1 . Y1 . O7 . 126.2(6) yes O3 . Y1 . O7 . 137.6(6) yes O8 . Y1 . O7 . 82.3(6) yes O5 . Y1 . O6 . 101.0(6) yes O2 . Y1 . O6 . 137.9(7) yes O1 . Y1 . O6 . 78.9(9) yes O3 . Y1 . O6 . 151.7(6) yes O8 . Y1 . O6 . 87.4(8) yes O4 . Y1 . O7 . 141.7(8) yes O4 . Y1 . O6 . 78.8(6) yes O7 . Y1 . O6 . 70.7(6) yes I2 . Cu1 . I3 . 116.8(2) yes I2 . Cu1 . I1 . 123.3(2) yes I3 . Cu1 . I1 . 117.7(2) yes Y1 . O5 . C7 . 138(2) yes Y1 . O3 . C1 . 137(2) yes Y1 . O8 . C16 . 160.9(9) yes Y1 . O4 . C4 . 141(2) yes Y1 . O7 . C13 . 126(2) yes Y1 . O6 . C10 . 142(2) yes C1 . N1 . C2 . 119(3) yes C1 . N1 . C3 . 126(3) yes C2 . N1 . C3 . 115(3) yes C7 . N3 . C8 . 123(3) yes C7 . N3 . C9 . 113(3) yes C8 . N3 . C9 . 123(3) yes C13 . N5 . C15 . 127(3) yes C13 . N5 . C14 . 114(3) yes C15 . N5 . C14 . 119(3) yes C16 . N6 . C18 . 117(3) yes C16 . N6 . C17 . 120(3) yes C18 . N6 . C17 . 122(3) yes C10 . N4 . C12 . 124(3) yes C10 . N4 . C11 . 114(3) yes C12 . N4 . C11 . 121(3) yes N3 . C7 . O5 . 123(3) yes N3 . C7 . H71 . 118.6 no O5 . C7 . H71 . 118.1 no N1 . C1 . O3 . 123(3) yes N1 . C1 . H11 . 118.7 no O3 . C1 . H11 . 118.7 no N3 . C8 . H81 . 108.6 no N3 . C8 . H82 . 109.6 no H81 . C8 . H82 . 108.4 no N3 . C8 . H83 . 110.3 no H81 . C8 . H83 . 108.9 no H82 . C8 . H83 . 111.0 no N6 . C16 . O8 . 122(3) yes N6 . C16 . H161 . 118.8 no O8 . C16 . H161 . 119.2 no N5 . C13 . O7 . 116(3) yes N5 . C13 . H131 . 121.5 no O7 . C13 . H131 . 122.6 no N4 . C10 . O6 . 122(3) yes N4 . C10 . H101 . 117.7 no O6 . C10 . H101 . 120.0 no N5 . C15 . H151 . 111.9 no N5 . C15 . H152 . 108.3 no H151 . C15 . H152 . 110.9 no N5 . C15 . H153 . 109.3 no H151 . C15 . H153 . 110.1 no H152 . C15 . H153 . 106.2 no N3 . C9 . H91 . 109.2 no N3 . C9 . H92 . 109.4 no H91 . C9 . H92 . 109.5 no N3 . C9 . H93 . 109.6 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N1 . C2 . H21 . 107.1 no N1 . C2 . H22 . 107.5 no H21 . C2 . H22 . 110.8 no N1 . C2 . H23 . 107.4 no H21 . C2 . H23 . 111.8 no H22 . C2 . H23 . 111.9 no N6 . C18 . H181 . 110.2 no N6 . C18 . H182 . 111.1 no H181 . C18 . H182 . 107.7 no N6 . C18 . H183 . 111.4 no H181 . C18 . H183 . 107.6 no H182 . C18 . H183 . 108.6 no N1 . C3 . H31 . 109.6 no N1 . C3 . H32 . 110.2 no H31 . C3 . H32 . 106.7 no N1 . C3 . H33 . 111.3 no H31 . C3 . H33 . 109.1 no H32 . C3 . H33 . 109.9 no N6 . C17 . H171 . 108.3 no N6 . C17 . H172 . 110.5 no H171 . C17 . H172 . 108.3 no N6 . C17 . H173 . 110.4 no H171 . C17 . H173 . 107.7 no H172 . C17 . H173 . 111.5 no N5 . C14 . H141 . 108.9 no N5 . C14 . H142 . 110.0 no H141 . C14 . H142 . 114.4 no N5 . C14 . H143 . 106.6 no H141 . C14 . H143 . 107.5 no H142 . C14 . H143 . 109.1 no N4 . C12 . H121 . 111.7 no N4 . C12 . H122 . 106.9 no H121 . C12 . H122 . 114.2 no N4 . C12 . H123 . 105.6 no H121 . C12 . H123 . 112.3 no H122 . C12 . H123 . 105.6 no N4 . C11 . H111 . 101.7 no N4 . C11 . H112 . 112.7 no H111 . C11 . H112 . 103.3 no N4 . C11 . H113 . 113.2 no H111 . C11 . H113 . 104.0 no H112 . C11 . H113 . 119.3 no C4 . N2 . C6 . 121(3) yes C4 . N2 . C5 . 125(3) yes C6 . N2 . C5 . 114(3) yes N2 . C4 . O4 . 124(3) yes N2 . C4 . H41 . 119.4 no O4 . C4 . H41 . 116.1 no N2 . C6 . H61 . 114.0 no N2 . C6 . H62 . 108.7 no H61 . C6 . H62 . 108.2 no N2 . C6 . H63 . 109.5 no H61 . C6 . H63 . 111.4 no H62 . C6 . H63 . 104.5 no N2 . C5 . H51 . 105.9 no N2 . C5 . H52 . 111.6 no H51 . C5 . H52 . 102.5 no N2 . C5 . H53 . 114.0 no H51 . C5 . H53 . 106.6 no H52 . C5 . H53 . 115.0 no #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 620035' _audit_creation_date 05-07-13 _audit_creation_method CRYSTALS_ver_12.82 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.7471(14) _cell_length_b 13.7471(14) _cell_length_c 60.040(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 9826.4(16) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 c ' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/3,y+2/3,z+2/3 -x+1/3,-y+2/3,-z+2/3 x+2/3,y+1/3,z+1/3 -x+2/3,-y+1/3,-z+1/3 -y,x-y,z y,-x+y,-z -y+1/3,x-y+2/3,z+2/3 y+1/3,-x+y+2/3,-z+2/3 -y+2/3,x-y+1/3,z+1/3 y+2/3,-x+y+1/3,-z+1/3 -x+y,-x,z x-y,x,-z -x+y+1/3,-x+2/3,z+2/3 x-y+1/3,x+2/3,-z+2/3 -x+y+2/3,-x+1/3,z+1/3 x-y+2/3,x+1/3,-z+1/3 -x+y,y,z+1/2 x-y,-y,-z+1/2 -x+y+1/3,y+2/3,z+7/6 x-y+1/3,-y+2/3,-z+7/6 -x+y+2/3,y+1/3,z+5/6 x-y+2/3,-y+1/3,-z+5/6 x,x-y,z+1/2 -x,-x+y,-z+1/2 x+1/3,x-y+2/3,z+7/6 -x+1/3,-x+y+2/3,-z+7/6 x+2/3,x-y+1/3,z+5/6 -x+2/3,-x+y+1/3,-z+5/6 -y,-x,z+1/2 y,x,-z+1/2 -y+1/3,-x+2/3,z+7/6 y+1/3,x+2/3,-z+7/6 -y+2/3,-x+1/3,z+5/6 y+2/3,x+1/3,-z+5/6 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' 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' 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' 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' 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 6 # Given Formula = C10 H15 Cu1.00 I1.00 N0.38 O8 Y1.00 # Dc = 2.41 Fooo = 7836.00 Mu = 73.03 M = 395.75 # Found Formula = C4.15 H9.69 Cu2.08 I3.23 N1.38 O2.08 Y0.23 # Dc = 2.96 FOOO = 7836.00 Mu = 103.67 M = 487.34 _chemical_formula_sum 'C18 H42 Cu9 I14 N6 O9 Y' _chemical_formula_moiety 'C18 H42 N6 O9 Y, Cu9 I14' _chemical_compound_source ? _chemical_formula_weight 2924.04 _cell_measurement_reflns_used 10299 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'light brown' _exptl_crystal_size_min 0.151 _exptl_crystal_size_mid 0.273 _exptl_crystal_size_max 0.316 _exptl_crystal_density_diffrn 2.965 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 7836 _exptl_absorpt_coefficient_mu 10.367 # Sheldrick geometric approximatio 0.60 0.60 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5955 _exptl_absorpt_correction_T_max 0.5955 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement '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 'DIAMOND v3 (Brandenburg & Putz)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 24339 _reflns_number_total 2589 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 2589 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2619 _diffrn_reflns_theta_min 1.840 _diffrn_reflns_theta_max 27.948 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.153 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 78 _reflns_limit_h_min -15 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 78 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.68 _refine_diff_density_max 5.92 _refine_ls_number_reflns 1447 _refine_ls_number_restraints 0 _refine_ls_number_parameters 88 #_refine_ls_R_factor_ref 0.0890 _refine_ls_wR_factor_ref 0.0763 _refine_ls_goodness_of_fit_ref 1.0663 #_reflns_number_all 2581 _refine_ls_R_factor_all 0.1407 _refine_ls_wR_factor_all 0.0839 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 1447 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_gt 0.0763 _refine_ls_shift/su_max 0.000329 # 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 noref # 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: 1.75 1.41 1.41 ; _publ_section_exptl_refinement ; All non hydroen atoms were refined anisotropically. Hydrogen were placed geometrically and initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. ; _publ_section_exptl_prep ; ? ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and 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. 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. ; 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 Cu1 Cu 0.45955(17) 0.68700(18) 0.06318(4) 0.0610 1.0000 Uani . . . . . . Cu2 Cu 0.6667 0.8193(2) 0.0833 0.0619 1.0000 Uani S T . . . . I1 I 0.3333 0.6667 0.02802(3) 0.0569 1.0000 Uani S T . . . . I2 I 0.49608(9) 0.86332(10) 0.08891(2) 0.0636 1.0000 Uani . . . . . . I3 I 0.64788(9) 0.70801(10) 0.046880(17) 0.0588 1.0000 Uani . . . . . . Y1 Y 0.6667 1.3333 0.0833 0.0525 1.0000 Uani S T . . . . O1w O 0.6667 1.5169(18) 0.0833 0.1034 1.0000 Uani S T . . . . O2 O 0.7941(14) 1.4454(13) 0.1109(3) 0.0890 1.0000 Uani . . . . . . N1 N 0.8998(15) 1.5730(13) 0.1366(3) 0.0716 1.0000 Uani . . . . . . C1 C 0.828(2) 1.532(2) 0.1190(4) 0.0945 1.0000 Uani . . . . . . C3 C 0.965(3) 1.6899(19) 0.1439(4) 0.0995 1.0000 Uani . . . . . . C2 C 0.931(2) 1.496(2) 0.1477(4) 0.0993 1.0000 Uani . . . . . . H11 H 0.8121 1.5828 0.1121 0.1200 1.0000 Uiso . . . . . . H21 H 0.8689 1.4303 0.1520 0.1530 1.0000 Uiso . . . . . . H22 H 0.9771 1.5347 0.1614 0.1530 1.0000 Uiso . . . . . . H23 H 0.9808 1.4837 0.1384 0.1530 1.0000 Uiso . . . . . . H31 H 0.9337 1.6932 0.1575 0.1420 1.0000 Uiso . . . . . . H33 H 0.9592 1.7315 0.1326 0.1420 1.0000 Uiso . . . . . . H32 H 1.0409 1.7046 0.1459 0.1420 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0504(11) 0.0548(11) 0.0787(13) -0.0037(9) -0.0012(9) 0.0270(9) Cu2 0.0683(17) 0.0561(11) 0.0653(17) -0.0058(7) -0.0116(14) 0.0341(9) I1 0.0525(6) 0.0525(6) 0.0657(11) 0.0000 0.0000 0.0263(3) I2 0.0456(6) 0.0537(6) 0.0948(8) -0.0203(5) -0.0098(5) 0.0274(5) I3 0.0530(6) 0.0715(7) 0.0575(6) -0.0111(5) -0.0041(4) 0.0353(5) Y1 0.0437(10) 0.0437(10) 0.070(2) 0.0000 0.0000 0.0218(5) O1w 0.14(2) 0.087(10) 0.103(17) -0.006(7) -0.011(15) 0.068(10) O2 0.097(10) 0.066(8) 0.089(10) -0.030(8) 0.009(8) 0.030(8) N1 0.093(11) 0.063(9) 0.068(9) -0.002(7) 0.012(8) 0.045(9) C1 0.12(2) 0.094(17) 0.083(15) 0.007(14) -0.005(14) 0.063(16) C3 0.14(2) 0.065(12) 0.079(13) -0.002(10) -0.031(14) 0.039(14) C2 0.118(19) 0.101(17) 0.078(14) -0.019(12) -0.045(13) 0.055(14) _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 Cu1 . Cu1 7_665 2.795(3) yes Cu1 . Cu1 13_565 2.795(3) yes Cu1 . I2 13_565 2.672(2) yes Cu1 . Cu2 . 2.775(2) yes Cu1 . I1 . 2.657(3) yes Cu1 . I2 . 2.701(2) yes Cu1 . I3 . 2.645(2) yes Cu2 . I2 28_654 2.720(2) yes Cu2 . I3 28_654 2.6080(18) yes Cu2 . I2 . 2.720(2) yes Cu2 . I3 . 2.6080(18) yes Y1 . O1w 13_575 2.52(2) yes Y1 . O1w 7_775 2.52(2) yes Y1 . O2 13_575 2.342(15) yes Y1 . O2 7_775 2.342(15) yes Y1 . O2 28_654 2.342(15) yes Y1 . O2 34_454 2.342(15) yes Y1 . O2 22_674 2.342(15) yes Y1 . O1w . 2.52(2) yes Y1 . O2 . 2.342(15) yes O2 . C1 . 1.14(3) yes N1 . C1 . 1.36(3) yes N1 . C3 . 1.46(3) yes N1 . C2 . 1.49(3) yes C1 . H11 . 0.931 no C3 . H31 . 0.939 no C3 . H33 . 0.915 no C3 . H32 . 0.966 no C2 . H21 . 0.918 no C2 . H22 . 1.011 no C2 . H23 . 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 Cu1 7_665 Cu1 . Cu1 13_565 60.000(9) yes Cu1 7_665 Cu1 . I2 13_565 107.08(7) yes Cu1 13_565 Cu1 . I2 13_565 59.18(8) yes Cu1 7_665 Cu1 . Cu2 . 116.34(12) yes Cu1 13_565 Cu1 . Cu2 . 154.15(5) yes I2 13_565 Cu1 . Cu2 . 102.34(9) yes Cu1 7_665 Cu1 . I1 . 58.27(4) yes Cu1 13_565 Cu1 . I1 . 58.27(4) yes I2 13_565 Cu1 . I1 . 112.50(8) yes Cu2 . Cu1 . I1 . 144.83(10) yes Cu1 7_665 Cu1 . I2 . 58.14(8) yes Cu1 13_565 Cu1 . I2 . 106.25(7) yes I2 13_565 Cu1 . I2 . 107.60(10) yes Cu2 . Cu1 . I2 . 59.55(7) yes I1 . Cu1 . I2 . 111.55(8) yes Cu1 7_665 Cu1 . I3 . 145.71(10) yes Cu1 13_565 Cu1 . I3 . 141.35(11) yes I2 13_565 Cu1 . I3 . 107.14(8) yes Cu2 . Cu1 . I3 . 57.47(6) yes I1 . Cu1 . I3 . 105.63(9) yes I2 . Cu1 . I3 . 112.40(8) yes I2 28_654 Cu2 . Cu1 28_654 58.88(5) yes I2 28_654 Cu2 . Cu1 . 134.65(9) yes Cu1 28_654 Cu2 . Cu1 . 163.64(14) yes I2 28_654 Cu2 . I3 28_654 112.98(4) yes Cu1 28_654 Cu2 . I3 28_654 58.77(5) yes Cu1 . Cu2 . I3 28_654 111.45(8) yes I2 28_654 Cu2 . I2 . 98.35(11) yes Cu1 28_654 Cu2 . I2 . 134.65(9) yes Cu1 . Cu2 . I2 . 58.88(5) yes I3 28_654 Cu2 . I2 . 108.16(4) yes I2 28_654 Cu2 . I3 . 108.16(4) yes Cu1 28_654 Cu2 . I3 . 111.45(8) yes Cu1 . Cu2 . I3 . 58.77(5) yes I3 28_654 Cu2 . I3 . 115.05(12) yes I2 . Cu2 . I3 . 112.98(4) yes Cu1 7_665 I1 . Cu1 13_565 63.46(9) yes Cu1 7_665 I1 . Cu1 . 63.46(9) yes Cu1 13_565 I1 . Cu1 . 63.46(9) yes Cu2 . I2 . Cu1 . 61.57(6) yes Cu2 . I2 . Cu1 7_665 122.72(7) yes Cu1 . I2 . Cu1 7_665 62.69(9) yes Cu1 . I3 . Cu2 . 63.77(5) yes O1w 13_575 Y1 . O1w 7_775 120.000(5) yes O1w 13_575 Y1 . O2 13_575 73.5(4) yes O1w 7_775 Y1 . O2 13_575 65.2(4) yes O1w 13_575 Y1 . O2 7_775 134.7(4) yes O1w 7_775 Y1 . O2 7_775 73.5(4) yes O2 13_575 Y1 . O2 7_775 75.5(6) yes O1w 13_575 Y1 . O2 28_654 134.7(4) yes O1w 7_775 Y1 . O2 28_654 65.2(4) yes O2 13_575 Y1 . O2 28_654 130.5(8) yes O2 7_775 Y1 . O2 28_654 90.7(8) yes O1w 13_575 Y1 . O2 34_454 73.5(4) yes O1w 7_775 Y1 . O2 34_454 134.7(4) yes O2 13_575 Y1 . O2 34_454 147.0(9) yes O2 7_775 Y1 . O2 34_454 130.5(8) yes O2 28_654 Y1 . O2 34_454 75.5(6) yes O1w 13_575 Y1 . O2 22_674 65.2(4) yes O1w 7_775 Y1 . O2 22_674 73.5(4) yes O2 13_575 Y1 . O2 22_674 90.7(8) yes O2 7_775 Y1 . O2 22_674 147.0(9) yes O2 28_654 Y1 . O2 22_674 75.5(6) yes O1w 13_575 Y1 . O1w . 120.000(5) yes O1w 7_775 Y1 . O1w . 120.000(10) yes O2 13_575 Y1 . O1w . 134.7(4) yes O2 7_775 Y1 . O1w . 65.2(4) yes O2 28_654 Y1 . O1w . 73.5(4) yes O1w 13_575 Y1 . O2 . 65.2(4) yes O1w 7_775 Y1 . O2 . 134.7(4) yes O2 13_575 Y1 . O2 . 75.5(6) yes O2 7_775 Y1 . O2 . 75.5(6) yes O2 28_654 Y1 . O2 . 147.0(9) yes O2 34_454 Y1 . O2 22_674 75.5(6) yes O2 34_454 Y1 . O1w . 65.2(4) yes O2 22_674 Y1 . O1w . 134.7(4) yes O2 34_454 Y1 . O2 . 90.7(8) yes O2 22_674 Y1 . O2 . 130.5(8) yes O1w . Y1 . O2 . 73.5(4) yes Y1 . O2 . C1 . 139.9(18) yes C1 . N1 . C3 . 127.5(18) yes C1 . N1 . C2 . 117.3(18) yes C3 . N1 . C2 . 114.4(18) yes N1 . C1 . O2 . 127(2) yes N1 . C1 . H11 . 115.2 no O2 . C1 . H11 . 117.8 no N1 . C3 . H31 . 105.6 no N1 . C3 . H33 . 105.7 no H31 . C3 . H33 . 115.3 no N1 . C3 . H32 . 105.9 no H31 . C3 . H32 . 110.6 no H33 . C3 . H32 . 112.9 no N1 . C2 . H21 . 111.2 no N1 . C2 . H22 . 108.2 no H21 . C2 . H22 . 108.6 no N1 . C2 . H23 . 110.3 no H21 . C2 . H23 . 113.1 no H22 . C2 . H23 . 105.3 no