# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Dr. Shashank Mishra' _publ_contact_author_address ;Universit\'e Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne C\'edex France. ; _publ_contact_author_email mishrashashank74@rediffmail.com _publ_contact_author_phone '(+33) 472445322' _publ_contact_author_fax '(+33) 472445399' loop_ _publ_author_name _publ_author_address 'Mishra, Shashank' ;Universit\'e Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne C\'edex France ; 'Jeanneau, Erwann' ;Centre de Diffractom\'etrie Henri Longchambon Universit\'e Claude Bernard Lyon 1 B\^at Raulin RdC 69622 Villeurbanne C\'edex France ; 'Ledoux, Gilles' ;Universit\'e Claude Bernard Lyon 1 Laboratoire de Physico des Materiaux Luminescent 10 rue A. M. Ampere 69622 Villeurbanne C\'edex France ; "Daniele, St\'ephane" ;Universit\'e Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne C\'edex France ; _publ_section_title # Title of paper - ; Solid state structural --- iodocuprate clusters ; _publ_contact_letter ; Dear Sir/ Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to the journal CrystEngComm Dr. Shashank Mishra ; data_complex1 _database_code_depnum_ccdc_archive 'CCDC 864815' #TrackingRef '- Combined CIFs_TbCuI-CEC-Jan 2012.cif' _audit_creation_date 11-02-02 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'scale in P 2/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.1937(5) _cell_length_b 9.8578(2) _cell_length_c 20.4580(9) _cell_angle_alpha 90 _cell_angle_beta 91.604(2) _cell_angle_gamma 90 _cell_volume 2256.56(15) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 2/n 1 ' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,-z+1/2 x+1/2,-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' 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' 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' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C8 H24 Cu1 I2.50 O4 S4 Tb0.50 # Dc = 2.27 Fooo = 1448.00 Mu = 63.05 M = 772.81 # Found Formula = C8 H24 Cu1 I2.50 O4 S4 Tb0.50 # Dc = 2.27 FOOO = 1448.00 Mu = 63.05 M = 772.81 _chemical_formula_sum 'C16 H48 Cu2 I5 O8 S8 Tb' _chemical_formula_moiety 'C16 H48 O8 S8 Tb, Cu2 I5' _chemical_compound_source ? _chemical_formula_weight 1545.63 _cell_measurement_reflns_used 3365 _cell_measurement_theta_min 0.679 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.286 _exptl_crystal_size_mid 0.326 _exptl_crystal_size_max 0.494 _exptl_crystal_density_diffrn 2.275 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 6.305 # Sheldrick geometric approximatio 0.13 0.16 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.10 _exptl_absorpt_correction_T_max 0.16 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 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 7700 _reflns_number_total 5038 _diffrn_reflns_av_R_equivalents 0.035 # Number of reflections without Friedels Law is 5038 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 5409 _diffrn_reflns_theta_min 1.992 _diffrn_reflns_theta_max 27.924 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 27.924 _diffrn_measured_fraction_theta_full 0.932 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 2.12 _oxford_diffrn_Wilson_scale 82.99 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.51 _refine_diff_density_max 2.94 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5023 _refine_ls_number_restraints 0 _refine_ls_number_parameters 183 _oxford_refine_ls_R_factor_ref 0.0669 _refine_ls_wR_factor_ref 0.1631 _refine_ls_goodness_of_fit_ref 0.9636 _refine_ls_shift/su_max 0.0004823 _refine_ls_shift/su_mean 0.0000242 # The values computed from all data _oxford_reflns_number_all 5023 _refine_ls_R_factor_all 0.0669 _refine_ls_wR_factor_all 0.1631 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3928 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_gt 0.1348 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # 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: 31.3 48.5 24.8 6.61 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Tb1 Tb 0.7500 0.40672(5) 0.7500 0.0183 1.0000 Uani S T . . . . O4 O 0.6307(5) 0.2190(6) 0.7778(3) 0.0315 1.0000 Uani . . . . . . S4 S 0.54421(17) 0.1312(2) 0.73823(9) 0.0260 1.0000 Uani . . . . . . C8 C 0.5147(12) -0.0056(12) 0.7904(6) 0.0610 1.0000 Uani . . . . . . C7 C 0.4055(10) 0.2136(15) 0.7407(7) 0.0651 1.0000 Uani . . . . . . O2 O 0.9028(5) 0.4836(6) 0.6816(3) 0.0280 1.0000 Uani . . . . . . S2 S 0.95961(17) 0.6234(2) 0.67397(10) 0.0282 1.0000 Uani . . . . . . C3 C 1.1016(8) 0.6098(10) 0.7136(5) 0.0373 1.0000 Uani . . . . . . C4 C 1.0081(8) 0.6303(11) 0.5921(4) 0.0377 1.0000 Uani . . . . . . O3 O 0.6705(5) 0.3266(5) 0.6478(2) 0.0247 1.0000 Uani . . . . . . S3 S 0.71580(18) 0.21522(19) 0.60305(9) 0.0275 1.0000 Uani . . . . . . C6 C 0.5874(9) 0.1714(11) 0.5545(5) 0.0427 1.0000 Uani . . . . . . C5 C 0.7969(12) 0.3025(12) 0.5441(6) 0.0592 1.0000 Uani . . . . . . O1 O 0.8485(5) 0.5945(5) 0.8042(3) 0.0258 1.0000 Uani . . . . . . S1 S 0.83429(17) 0.6261(2) 0.87585(9) 0.0262 1.0000 Uani . . . . . . C1 C 0.9768(8) 0.5868(9) 0.9127(4) 0.0347 1.0000 Uani . . . . . . C2 C 0.8420(9) 0.8065(9) 0.8809(5) 0.0404 1.0000 Uani . . . . . . I2 I 0.69849(5) 0.09809(5) 0.37003(3) 0.0308 1.0000 Uani . . . . . . Cu1 Cu 0.81103(10) -0.08189(11) 0.43441(5) 0.0339 1.0000 Uani . . . . . . I3 I 0.75243(5) -0.32737(6) 0.43652(3) 0.0385 1.0000 Uani . . . . . . I1 I 1.0000 0.0000 0.5000 0.0739 1.0000 Uani S . . . . . H51 H 0.8721 0.3309 0.5632 0.0940 1.0000 Uiso R . . . . . H52 H 0.7524 0.3811 0.5297 0.0940 1.0000 Uiso R . . . . . H53 H 0.8109 0.2434 0.5076 0.0941 1.0000 Uiso R . . . . . H61 H 0.5334 0.1201 0.5806 0.0641 1.0000 Uiso R . . . . . H62 H 0.5482 0.2521 0.5387 0.0641 1.0000 Uiso R . . . . . H63 H 0.6116 0.1173 0.5180 0.0639 1.0000 Uiso R . . . . . H71 H 0.4011 0.2818 0.7073 0.1049 1.0000 Uiso R . . . . . H72 H 0.3963 0.2554 0.7825 0.1050 1.0000 Uiso R . . . . . H73 H 0.3423 0.1493 0.7332 0.1050 1.0000 Uiso R . . . . . H81 H 0.5820 -0.0659 0.7919 0.0981 1.0000 Uiso R . . . . . H82 H 0.5018 0.0284 0.8337 0.0980 1.0000 Uiso R . . . . . H83 H 0.4452 -0.0536 0.7748 0.0980 1.0000 Uiso R . . . . . H41 H 0.9400 0.6392 0.5634 0.0581 1.0000 Uiso R . . . . . H42 H 1.0594 0.7067 0.5865 0.0582 1.0000 Uiso R . . . . . H43 H 1.0507 0.5490 0.5810 0.0580 1.0000 Uiso R . . . . . H31 H 1.0911 0.5923 0.7592 0.0571 1.0000 Uiso R . . . . . H32 H 1.1443 0.6934 0.7085 0.0570 1.0000 Uiso R . . . . . H33 H 1.1452 0.5366 0.6944 0.0570 1.0000 Uiso R . . . . . H11 H 0.9995 0.4953 0.9024 0.0511 1.0000 Uiso R . . . . . H12 H 0.9743 0.5961 0.9594 0.0511 1.0000 Uiso R . . . . . H13 H 1.0358 0.6477 0.8961 0.0512 1.0000 Uiso R . . . . . H21 H 0.7733 0.8450 0.8588 0.0591 1.0000 Uiso R . . . . . H22 H 0.8424 0.8335 0.9260 0.0592 1.0000 Uiso R . . . . . H23 H 0.9132 0.8384 0.8608 0.0589 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 Tb1 0.0169(2) 0.0186(2) 0.0195(2) 0.0000 0.00038(16) 0.0000 O4 0.030(3) 0.032(3) 0.032(3) 0.004(2) -0.001(2) -0.015(2) S4 0.0255(8) 0.0258(8) 0.0269(8) -0.0015(7) 0.0012(7) -0.0057(7) C8 0.074(8) 0.048(6) 0.059(7) 0.021(5) -0.025(6) -0.047(6) C7 0.043(6) 0.076(8) 0.075(8) -0.035(7) -0.019(5) 0.025(6) O2 0.025(3) 0.026(3) 0.033(3) 0.002(2) 0.008(2) -0.005(2) S2 0.0244(9) 0.0261(9) 0.0344(10) 0.0052(7) 0.0056(7) 0.0005(7) C3 0.024(4) 0.041(5) 0.047(5) 0.007(4) 0.001(4) -0.003(3) C4 0.028(4) 0.054(5) 0.032(4) 0.011(4) 0.007(3) -0.001(4) O3 0.031(3) 0.023(2) 0.019(2) -0.0054(19) -0.001(2) 0.002(2) S3 0.0351(10) 0.0236(9) 0.0239(8) -0.0035(7) -0.0014(7) 0.0028(7) C6 0.044(5) 0.051(6) 0.032(4) -0.008(4) -0.007(4) -0.001(4) C5 0.078(8) 0.049(6) 0.052(6) -0.009(5) 0.033(6) -0.018(6) O1 0.028(3) 0.027(3) 0.022(2) -0.002(2) 0.000(2) -0.007(2) S1 0.0258(9) 0.0266(9) 0.0260(8) -0.0016(7) -0.0009(7) -0.0044(7) C1 0.037(4) 0.033(4) 0.034(4) -0.002(3) -0.015(3) 0.001(3) C2 0.045(5) 0.026(4) 0.049(5) -0.005(4) -0.002(4) -0.001(4) I2 0.0286(3) 0.0291(3) 0.0343(3) 0.00011(19) -0.0046(2) 0.00042(18) Cu1 0.0368(6) 0.0308(5) 0.0340(5) 0.0010(4) 0.0014(4) 0.0023(4) I3 0.0381(3) 0.0296(3) 0.0476(3) 0.0044(2) -0.0024(2) -0.0011(2) I1 0.0781(8) 0.0458(6) 0.0941(9) -0.0039(6) -0.0632(7) 0.0024(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.11609(7) 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 Tb1 . O1 3_656 2.409(5) yes Tb1 . O3 3_656 2.383(5) yes Tb1 . O2 3_656 2.364(5) yes Tb1 . O4 3_656 2.360(5) yes Tb1 . O4 . 2.360(5) yes Tb1 . O2 . 2.364(5) yes Tb1 . O3 . 2.383(5) yes Tb1 . O1 . 2.409(5) yes O4 . S4 . 1.516(6) yes S4 . C8 . 1.757(10) yes S4 . C7 . 1.754(11) yes C8 . H81 . 0.960 no C8 . H82 . 0.961 no C8 . H83 . 0.958 no C7 . H71 . 0.958 no C7 . H72 . 0.957 no C7 . H73 . 0.960 no O2 . S2 . 1.527(6) yes S2 . C3 . 1.769(9) yes S2 . C4 . 1.777(9) yes C3 . H31 . 0.961 no C3 . H32 . 0.960 no C3 . H33 . 0.961 no C4 . H41 . 0.953 no C4 . H42 . 0.956 no C4 . H43 . 0.962 no O3 . S3 . 1.526(5) yes S3 . C6 . 1.777(10) yes S3 . C5 . 1.756(10) yes C6 . H61 . 0.961 no C6 . H62 . 0.960 no C6 . H63 . 0.963 no C5 . H51 . 0.960 no C5 . H52 . 0.962 no C5 . H53 . 0.962 no O1 . S1 . 1.511(6) yes S1 . C1 . 1.787(9) yes S1 . C2 . 1.783(9) yes C1 . H11 . 0.962 no C1 . H12 . 0.963 no C1 . H13 . 0.962 no C2 . H21 . 0.959 no C2 . H22 . 0.961 no C2 . H23 . 0.961 no I2 . Cu1 . 2.5252(12) yes Cu1 . I3 . 2.5080(12) yes Cu1 . I1 . 2.6015(12) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 3_656 Tb1 . O3 3_656 144.40(18) yes O1 3_656 Tb1 . O2 3_656 72.35(19) yes O3 3_656 Tb1 . O2 3_656 81.13(19) yes O1 3_656 Tb1 . O4 3_656 138.25(19) yes O3 3_656 Tb1 . O4 3_656 75.63(19) yes O2 3_656 Tb1 . O4 3_656 144.8(2) yes O1 3_656 Tb1 . O4 . 117.3(2) yes O3 3_656 Tb1 . O4 . 74.27(19) yes O2 3_656 Tb1 . O4 . 71.7(2) yes O4 3_656 Tb1 . O4 . 76.8(3) yes O1 3_656 Tb1 . O2 . 79.08(19) yes O3 3_656 Tb1 . O2 . 111.50(19) yes O2 3_656 Tb1 . O2 . 142.6(3) yes O4 3_656 Tb1 . O2 . 71.7(2) yes O4 . Tb1 . O2 . 144.8(2) yes O1 3_656 Tb1 . O3 . 72.30(18) yes O3 3_656 Tb1 . O3 . 141.3(3) yes O2 3_656 Tb1 . O3 . 111.50(19) yes O4 3_656 Tb1 . O3 . 74.27(19) yes O4 . Tb1 . O3 . 75.63(19) yes O1 3_656 Tb1 . O1 . 79.6(3) yes O3 3_656 Tb1 . O1 . 72.30(18) yes O2 3_656 Tb1 . O1 . 79.08(19) yes O4 3_656 Tb1 . O1 . 117.3(2) yes O4 . Tb1 . O1 . 138.25(19) yes O2 . Tb1 . O3 . 81.13(19) yes O2 . Tb1 . O1 . 72.35(19) yes O3 . Tb1 . O1 . 144.40(18) yes Tb1 . O4 . S4 . 132.6(3) yes O4 . S4 . C8 . 104.0(4) yes O4 . S4 . C7 . 105.8(5) yes C8 . S4 . C7 . 99.0(8) yes S4 . C8 . H81 . 109.6 no S4 . C8 . H82 . 109.1 no H81 . C8 . H82 . 109.0 no S4 . C8 . H83 . 109.9 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.8 no S4 . C7 . H71 . 109.4 no S4 . C7 . H72 . 110.1 no H71 . C7 . H72 . 109.3 no S4 . C7 . H73 . 109.8 no H71 . C7 . H73 . 109.0 no H72 . C7 . H73 . 109.3 no Tb1 . O2 . S2 . 131.3(3) yes O2 . S2 . C3 . 104.8(4) yes O2 . S2 . C4 . 105.7(4) yes C3 . S2 . C4 . 98.1(4) yes S2 . C3 . H31 . 109.1 no S2 . C3 . H32 . 109.2 no H31 . C3 . H32 . 109.5 no S2 . C3 . H33 . 109.3 no H31 . C3 . H33 . 109.8 no H32 . C3 . H33 . 109.9 no S2 . C4 . H41 . 108.9 no S2 . C4 . H42 . 110.1 no H41 . C4 . H42 . 109.0 no S2 . C4 . H43 . 110.8 no H41 . C4 . H43 . 109.0 no H42 . C4 . H43 . 108.9 no Tb1 . O3 . S3 . 130.0(3) yes O3 . S3 . C6 . 103.5(4) yes O3 . S3 . C5 . 104.3(4) yes C6 . S3 . C5 . 99.2(6) yes S3 . C6 . H61 . 109.2 no S3 . C6 . H62 . 109.9 no H61 . C6 . H62 . 109.5 no S3 . C6 . H63 . 109.1 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no S3 . C5 . H51 . 109.1 no S3 . C5 . H52 . 109.4 no H51 . C5 . H52 . 109.3 no S3 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.4 no H52 . C5 . H53 . 110.1 no Tb1 . O1 . S1 . 123.1(3) yes O1 . S1 . C1 . 104.3(4) yes O1 . S1 . C2 . 104.8(4) yes C1 . S1 . C2 . 98.7(5) yes S1 . C1 . H11 . 110.5 no S1 . C1 . H12 . 110.4 no H11 . C1 . H12 . 108.8 no S1 . C1 . H13 . 109.3 no H11 . C1 . H13 . 108.6 no H12 . C1 . H13 . 109.3 no S1 . C2 . H21 . 109.3 no S1 . C2 . H22 . 109.4 no H21 . C2 . H22 . 109.0 no S1 . C2 . H23 . 109.9 no H21 . C2 . H23 . 109.4 no H22 . C2 . H23 . 109.8 no I2 . Cu1 . I3 . 124.06(5) yes I2 . Cu1 . I1 . 115.95(4) yes I3 . Cu1 . I1 . 119.99(5) yes Cu1 2_756 I1 . Cu1 . 179.996 yes _iucr_refine_instruction_details_constraints ; # # Punched on 02/02/11 at 13:59:25 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) H ( 73,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S) RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 02/02/11 at 13:59:25 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 864816' #TrackingRef '- Combined CIFs_TbCuI-CEC-Jan 2012.cif' _audit_creation_date 11-02-02 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'scale in P -1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.00230(20) _cell_length_b 12.94800(20) _cell_length_c 17.05820(29) _cell_angle_alpha 79.5186(11) _cell_angle_beta 73.0295(11) _cell_angle_gamma 73.5139(10) _cell_volume 2215.657(67) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 '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 = C20 H20 Cu4 I9 N8 O4 Tb1 # Dc = 2.99 Fooo = 1252.00 Mu = 97.69 M = 1991.68 # Found Formula = C24 H56 Cu1 I4 N8 O8 Tb1 # Dc = 1.97 FOOO = 1252.00 Mu = 48.95 M = 1314.85 _chemical_formula_sum 'C24 H56 Cu1 I4 N8 O8 Tb1' _chemical_formula_moiety 'C24 H56 N8 O8 Tb, Cu I3, I' _chemical_compound_source ? _chemical_formula_weight 1314.85 _cell_measurement_reflns_used 26873 _cell_measurement_theta_min 0.679 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.220 _exptl_crystal_size_mid 0.256 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 4.895 # Sheldrick geometric approximatio 0.13 0.16 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.2856 _exptl_absorpt_correction_T_max 0.3406 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 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 19410 _reflns_number_total 10429 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections without Friedels Law is 10429 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 10519 _diffrn_reflns_theta_min 1.255 _diffrn_reflns_theta_max 27.826 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.600 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.32 _refine_diff_density_max 1.08 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 10392 _refine_ls_number_restraints 0 _refine_ls_number_parameters 416 _oxford_refine_ls_R_factor_ref 0.0387 _refine_ls_wR_factor_ref 0.0748 _refine_ls_goodness_of_fit_ref 0.9046 _refine_ls_shift/su_max 0.0015852 _refine_ls_shift/su_mean 0.0000247 # The values computed from all data _oxford_reflns_number_all 10392 _refine_ls_R_factor_all 0.0387 _refine_ls_wR_factor_all 0.0748 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8802 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_gt 0.0625 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # 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: 7.42 9.48 3.18 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.7862(5) 0.3147(4) 0.3158(3) 0.0306 1.0000 Uani . . . . . . C2 C 0.6633(6) 0.4206(5) 0.4292(4) 0.0476 1.0000 Uani . . . . . . C3 C 0.5574(6) 0.3964(6) 0.3252(4) 0.0477 1.0000 Uani . . . . . . C4 C 0.9055(5) 0.4072(4) 0.1275(3) 0.0276 1.0000 Uani . . . . . . C5 C 0.9846(5) 0.3416(5) -0.0051(3) 0.0371 1.0000 Uani . . . . . . C6 C 0.7961(5) 0.5036(5) 0.0226(3) 0.0368 1.0000 Uani . . . . . . C7 C 1.0460(5) 0.4518(4) 0.3543(3) 0.0285 1.0000 Uani . . . . . . C8 C 1.0042(5) 0.6319(4) 0.3950(4) 0.0349 1.0000 Uani . . . . . . C9 C 1.1944(6) 0.4853(5) 0.4214(4) 0.0382 1.0000 Uani . . . . . . C10 C 1.3047(5) 0.4173(4) 0.1617(3) 0.0265 1.0000 Uani . . . . . . C11 C 1.2046(5) 0.6105(4) 0.1667(3) 0.0324 1.0000 Uani . . . . . . C12 C 1.4463(5) 0.5415(4) 0.1289(4) 0.0368 1.0000 Uani . . . . . . C13 C 1.4101(5) 0.1665(4) 0.2931(3) 0.0254 1.0000 Uani . . . . . . C14 C 1.5274(7) -0.0002(4) 0.2383(4) 0.0472 1.0000 Uani . . . . . . C15 C 1.6098(6) 0.0728(5) 0.3321(4) 0.0428 1.0000 Uani . . . . . . C16 C 1.0741(5) 0.1294(4) 0.4451(3) 0.0274 1.0000 Uani . . . . . . C17 C 1.0647(6) 0.0760(5) 0.5898(3) 0.0385 1.0000 Uani . . . . . . C18 C 1.2393(6) -0.0254(5) 0.4812(4) 0.0424 1.0000 Uani . . . . . . C19 C 0.9800(5) 0.0753(4) 0.1868(3) 0.0245 1.0000 Uani . . . . . . C20 C 0.9716(7) -0.0620(5) 0.1105(4) 0.0489 1.0000 Uani . . . . . . C21 C 1.1286(7) -0.1002(5) 0.1967(5) 0.0558 1.0000 Uani . . . . . . C22 C 1.3289(5) 0.1762(4) 0.0688(3) 0.0272 1.0000 Uani . . . . . . C23 C 1.4804(6) 0.1528(5) -0.0662(3) 0.0374 1.0000 Uani . . . . . . C24 C 1.2763(5) 0.0905(4) -0.0281(3) 0.0331 1.0000 Uani . . . . . . N1 N 0.6742(4) 0.3724(3) 0.3559(3) 0.0274 1.0000 Uani . . . . . . N2 N 0.8989(4) 0.4196(3) 0.0510(2) 0.0248 1.0000 Uani . . . . . . N3 N 1.0779(4) 0.5196(3) 0.3897(3) 0.0266 1.0000 Uani . . . . . . N4 N 1.3177(4) 0.5173(3) 0.1536(3) 0.0269 1.0000 Uani . . . . . . N5 N 1.5085(4) 0.0825(3) 0.2906(2) 0.0240 1.0000 Uani . . . . . . N6 N 1.1223(4) 0.0616(3) 0.5025(3) 0.0291 1.0000 Uani . . . . . . N7 N 1.0257(4) -0.0230(3) 0.1648(3) 0.0299 1.0000 Uani . . . . . . N8 N 1.3603(4) 0.1411(3) -0.0039(2) 0.0249 1.0000 Uani . . . . . . O1 O 0.8913(3) 0.2962(3) 0.3350(2) 0.0385 1.0000 Uani . . . . . . O2 O 0.9847(4) 0.3326(3) 0.1569(2) 0.0371 1.0000 Uani . . . . . . O3 O 1.1091(4) 0.3563(3) 0.3466(2) 0.0306 1.0000 Uani . . . . . . O4 O 1.1981(4) 0.3929(3) 0.1771(2) 0.0306 1.0000 Uani . . . . . . O5 O 1.3280(3) 0.1840(3) 0.2519(2) 0.0318 1.0000 Uani . . . . . . O6 O 1.1188(4) 0.1238(3) 0.3706(2) 0.0309 1.0000 Uani . . . . . . O7 O 1.0153(4) 0.1093(3) 0.2378(2) 0.0308 1.0000 Uani . . . . . . O8 O 1.2266(3) 0.1691(3) 0.1221(2) 0.0328 1.0000 Uani . . . . . . Tb1 Tb 1.109669(19) 0.243745(16) 0.250159(12) 0.0177 1.0000 Uani . . . . . . I4 I 0.67494(3) 0.22939(3) 0.08416(2) 0.0309 1.0000 Uani . . . . . . I3 I 0.38774(3) 0.22097(3) 0.52910(2) 0.0334 1.0000 Uani . . . . . . I1 I 0.21771(4) 0.32521(3) 0.77308(2) 0.0407 1.0000 Uani . . . . . . I2 I 0.64387(3) 0.26516(3) 0.67493(2) 0.0357 1.0000 Uani . . . . . . Cu1 Cu 0.42200(6) 0.27210(5) 0.65580(4) 0.0284 1.0000 Uani . . . . . . H11 H 0.7855 0.2849 0.2697 0.0352 1.0000 Uiso R . . . . . H21 H 0.5929 0.4007 0.4724 0.0709 1.0000 Uiso R . . . . . H22 H 0.6447 0.4980 0.4188 0.0711 1.0000 Uiso R . . . . . H23 H 0.7433 0.3940 0.4468 0.0710 1.0000 Uiso R . . . . . H31 H 0.4900 0.3697 0.3669 0.0680 1.0000 Uiso R . . . . . H32 H 0.5281 0.4739 0.3133 0.0679 1.0000 Uiso R . . . . . H33 H 0.5779 0.3622 0.2757 0.0679 1.0000 Uiso R . . . . . H41 H 0.8461 0.4582 0.1622 0.0328 1.0000 Uiso R . . . . . H51 H 1.0136 0.3788 -0.0586 0.0579 1.0000 Uiso R . . . . . H52 H 1.0598 0.3019 0.0149 0.0579 1.0000 Uiso R . . . . . H53 H 0.9381 0.2914 -0.0098 0.0579 1.0000 Uiso R . . . . . H61 H 0.8322 0.5426 -0.0284 0.0520 1.0000 Uiso R . . . . . H62 H 0.7527 0.5538 0.0629 0.0517 1.0000 Uiso R . . . . . H63 H 0.7339 0.4714 0.0132 0.0518 1.0000 Uiso R . . . . . H71 H 0.9710 0.4777 0.3346 0.0331 1.0000 Uiso R . . . . . H81 H 1.0610 0.6799 0.3700 0.0529 1.0000 Uiso R . . . . . H82 H 0.9358 0.6478 0.3669 0.0529 1.0000 Uiso R . . . . . H83 H 0.9659 0.6433 0.4517 0.0530 1.0000 Uiso R . . . . . H91 H 1.1717 0.5022 0.4771 0.0603 1.0000 Uiso R . . . . . H92 H 1.2584 0.5228 0.3880 0.0600 1.0000 Uiso R . . . . . H93 H 1.2300 0.4087 0.4202 0.0599 1.0000 Uiso R . . . . . H101 H 1.3812 0.3621 0.1547 0.0293 1.0000 Uiso R . . . . . H111 H 1.2107 0.6600 0.1177 0.0491 1.0000 Uiso R . . . . . H112 H 1.2047 0.6458 0.2111 0.0488 1.0000 Uiso R . . . . . H113 H 1.1251 0.5865 0.1798 0.0487 1.0000 Uiso R . . . . . H121 H 1.4536 0.5805 0.1699 0.0555 1.0000 Uiso R . . . . . H122 H 1.5139 0.4748 0.1237 0.0556 1.0000 Uiso R . . . . . H123 H 1.4560 0.5853 0.0765 0.0557 1.0000 Uiso R . . . . . H131 H 1.4002 0.2173 0.3279 0.0296 1.0000 Uiso R . . . . . H141 H 1.5706 -0.0684 0.2618 0.0663 1.0000 Uiso R . . . . . H142 H 1.5794 0.0173 0.1844 0.0665 1.0000 Uiso R . . . . . H143 H 1.4444 -0.0050 0.2341 0.0663 1.0000 Uiso R . . . . . H151 H 1.6261 0.0024 0.3618 0.0632 1.0000 Uiso R . . . . . H152 H 1.6879 0.0825 0.2913 0.0629 1.0000 Uiso R . . . . . H153 H 1.5812 0.1274 0.3698 0.0631 1.0000 Uiso R . . . . . H161 H 1.0000 0.1872 0.4630 0.0320 1.0000 Uiso R . . . . . H171 H 1.0534 0.0076 0.6194 0.0578 1.0000 Uiso R . . . . . H172 H 1.1225 0.1008 0.6099 0.0579 1.0000 Uiso R . . . . . H173 H 0.9814 0.1276 0.5968 0.0581 1.0000 Uiso R . . . . . H181 H 1.2281 -0.0897 0.5170 0.0628 1.0000 Uiso R . . . . . H182 H 1.3128 -0.0054 0.4877 0.0631 1.0000 Uiso R . . . . . H183 H 1.2556 -0.0384 0.4250 0.0631 1.0000 Uiso R . . . . . H191 H 0.9173 0.1226 0.1621 0.0303 1.0000 Uiso R . . . . . H201 H 1.0410 -0.0887 0.0647 0.0838 1.0000 Uiso R . . . . . H202 H 0.9064 -0.0038 0.0911 0.0839 1.0000 Uiso R . . . . . H203 H 0.9325 -0.1196 0.1402 0.0837 1.0000 Uiso R . . . . . H211 H 1.2009 -0.1251 0.1511 0.0820 1.0000 Uiso R . . . . . H212 H 1.1570 -0.0658 0.2312 0.0822 1.0000 Uiso R . . . . . H213 H 1.0959 -0.1606 0.2279 0.0820 1.0000 Uiso R . . . . . H221 H 1.3885 0.2080 0.0801 0.0340 1.0000 Uiso R . . . . . H231 H 1.5177 0.0906 -0.0977 0.0578 1.0000 Uiso R . . . . . H232 H 1.5447 0.1607 -0.0400 0.0579 1.0000 Uiso R . . . . . H233 H 1.4600 0.2174 -0.1035 0.0581 1.0000 Uiso R . . . . . H241 H 1.2569 0.1289 -0.0783 0.0527 1.0000 Uiso R . . . . . H242 H 1.3189 0.0161 -0.0357 0.0531 1.0000 Uiso R . . . . . H243 H 1.1966 0.0948 0.0142 0.0531 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 C1 0.023(2) 0.035(3) 0.032(2) -0.010(2) -0.0002(19) -0.007(2) C2 0.043(3) 0.049(4) 0.046(3) -0.022(3) 0.003(3) -0.009(3) C3 0.025(3) 0.053(4) 0.057(4) 0.005(3) -0.012(3) -0.003(3) C4 0.030(2) 0.028(2) 0.026(2) 0.0054(18) -0.0106(19) -0.0103(19) C5 0.031(3) 0.046(3) 0.037(3) -0.013(2) -0.006(2) -0.011(2) C6 0.034(3) 0.043(3) 0.034(3) 0.014(2) -0.020(2) -0.011(2) C7 0.030(2) 0.030(2) 0.026(2) -0.0057(19) -0.0065(19) -0.0069(19) C8 0.033(3) 0.025(2) 0.047(3) -0.011(2) -0.011(2) -0.003(2) C9 0.035(3) 0.033(3) 0.053(3) -0.006(2) -0.019(3) -0.009(2) C10 0.033(2) 0.020(2) 0.024(2) -0.0003(17) -0.0053(18) -0.0053(18) C11 0.037(3) 0.022(2) 0.035(3) -0.0033(19) -0.012(2) 0.000(2) C12 0.031(3) 0.032(3) 0.051(3) -0.006(2) -0.005(2) -0.018(2) C13 0.024(2) 0.025(2) 0.025(2) -0.0045(17) -0.0055(17) -0.0033(18) C14 0.062(4) 0.022(3) 0.052(4) -0.011(2) -0.014(3) 0.001(3) C15 0.029(3) 0.050(3) 0.045(3) -0.002(3) -0.018(2) 0.003(2) C16 0.033(2) 0.021(2) 0.026(2) 0.0003(17) -0.0069(19) -0.0067(18) C17 0.051(3) 0.039(3) 0.026(2) -0.006(2) -0.004(2) -0.015(3) C18 0.044(3) 0.038(3) 0.040(3) -0.007(2) -0.016(3) 0.008(2) C19 0.027(2) 0.026(2) 0.023(2) -0.0001(17) -0.0073(17) -0.0102(18) C20 0.070(4) 0.041(3) 0.049(4) -0.017(3) -0.020(3) -0.022(3) C21 0.063(4) 0.035(3) 0.066(4) -0.005(3) -0.035(4) 0.013(3) C22 0.031(2) 0.029(2) 0.026(2) -0.0090(18) -0.0117(19) -0.0062(19) C23 0.038(3) 0.045(3) 0.027(2) -0.009(2) 0.004(2) -0.015(2) C24 0.037(3) 0.038(3) 0.031(3) -0.015(2) -0.005(2) -0.016(2) N1 0.0182(18) 0.028(2) 0.030(2) -0.0030(16) 0.0003(15) -0.0030(15) N2 0.0229(19) 0.027(2) 0.0263(19) 0.0063(15) -0.0114(15) -0.0100(15) N3 0.027(2) 0.0230(19) 0.032(2) -0.0055(16) -0.0070(16) -0.0073(16) N4 0.025(2) 0.0232(19) 0.032(2) -0.0019(16) -0.0078(16) -0.0044(16) N5 0.0226(18) 0.0214(18) 0.0216(18) 0.0010(14) -0.0051(15) 0.0020(15) N6 0.035(2) 0.029(2) 0.0241(19) 0.0008(16) -0.0103(17) -0.0098(18) N7 0.036(2) 0.025(2) 0.031(2) -0.0066(17) -0.0123(18) -0.0063(17) N8 0.0260(19) 0.030(2) 0.0196(18) -0.0082(15) -0.0044(15) -0.0059(16) O1 0.0197(17) 0.054(2) 0.039(2) -0.0173(18) -0.0020(15) -0.0019(16) O2 0.0325(19) 0.042(2) 0.040(2) 0.0092(17) -0.0210(17) -0.0109(17) O3 0.038(2) 0.0242(17) 0.0316(18) -0.0090(14) -0.0111(15) -0.0046(14) O4 0.0314(18) 0.0268(17) 0.0361(19) 0.0012(14) -0.0083(15) -0.0140(14) O5 0.0214(16) 0.038(2) 0.0330(18) 0.0006(15) -0.0100(14) -0.0029(14) O6 0.044(2) 0.0249(17) 0.0233(16) 0.0031(13) -0.0119(15) -0.0082(15) O7 0.045(2) 0.0285(18) 0.0268(17) 0.0000(14) -0.0114(15) -0.0209(16) O8 0.0288(18) 0.044(2) 0.0250(17) -0.0150(15) -0.0008(14) -0.0069(16) Tb1 0.01876(10) 0.01753(10) 0.01762(10) -0.00259(7) -0.00599(7) -0.00395(7) I4 0.02418(15) 0.02593(16) 0.04270(19) -0.00058(13) -0.00886(13) -0.00786(12) I3 0.03557(18) 0.03647(18) 0.02879(16) -0.00678(13) -0.01133(13) -0.00449(14) I1 0.03701(19) 0.0446(2) 0.02885(17) -0.00828(14) -0.00229(14) 0.00444(15) I2 0.03349(18) 0.03547(18) 0.0446(2) -0.00207(14) -0.01702(15) -0.01274(14) Cu1 0.0290(3) 0.0261(3) 0.0300(3) -0.0027(2) -0.0087(2) -0.0055(2) _refine_ls_extinction_coef 64(2) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.14606(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 C1 . N1 . 1.310(6) yes C1 . O1 . 1.239(6) yes C1 . H11 . 0.940 no C2 . N1 . 1.457(7) yes C2 . H21 . 0.959 no C2 . H22 . 0.958 no C2 . H23 . 0.963 no C3 . N1 . 1.459(7) yes C3 . H31 . 0.961 no C3 . H32 . 0.965 no C3 . H33 . 0.963 no C4 . N2 . 1.307(6) yes C4 . O2 . 1.242(6) yes C4 . H41 . 0.941 no C5 . N2 . 1.453(7) yes C5 . H51 . 0.962 no C5 . H52 . 0.962 no C5 . H53 . 0.960 no C6 . N2 . 1.458(6) yes C6 . H61 . 0.960 no C6 . H62 . 0.959 no C6 . H63 . 0.957 no C7 . N3 . 1.325(6) yes C7 . O3 . 1.243(6) yes C7 . H71 . 0.932 no C8 . N3 . 1.455(6) yes C8 . H81 . 0.962 no C8 . H82 . 0.961 no C8 . H83 . 0.956 no C9 . N3 . 1.457(7) yes C9 . H91 . 0.959 no C9 . H92 . 0.957 no C9 . H93 . 0.959 no C10 . N4 . 1.321(6) yes C10 . O4 . 1.243(6) yes C10 . H101 . 0.930 no C11 . N4 . 1.462(6) yes C11 . H111 . 0.954 no C11 . H112 . 0.953 no C11 . H113 . 0.962 no C12 . N4 . 1.460(6) yes C12 . H121 . 0.967 no C12 . H122 . 0.965 no C12 . H123 . 0.963 no C13 . N5 . 1.296(6) yes C13 . O5 . 1.248(6) yes C13 . H131 . 0.927 no C14 . N5 . 1.448(7) yes C14 . H141 . 0.954 no C14 . H142 . 0.956 no C14 . H143 . 0.957 no C15 . N5 . 1.452(7) yes C15 . H151 . 0.956 no C15 . H152 . 0.958 no C15 . H153 . 0.966 no C16 . N6 . 1.319(6) yes C16 . O6 . 1.229(6) yes C16 . H161 . 0.953 no C17 . N6 . 1.461(6) yes C17 . H171 . 0.958 no C17 . H172 . 0.953 no C17 . H173 . 0.958 no C18 . N6 . 1.453(7) yes C18 . H181 . 0.954 no C18 . H182 . 0.957 no C18 . H183 . 0.959 no C19 . N7 . 1.309(6) yes C19 . O7 . 1.239(6) yes C19 . H191 . 0.929 no C20 . N7 . 1.459(7) yes C20 . H201 . 0.956 no C20 . H202 . 0.966 no C20 . H203 . 0.958 no C21 . N7 . 1.449(7) yes C21 . H211 . 0.962 no C21 . H212 . 0.961 no C21 . H213 . 0.958 no C22 . N8 . 1.316(6) yes C22 . O8 . 1.238(6) yes C22 . H221 . 0.944 no C23 . N8 . 1.460(6) yes C23 . H231 . 0.975 no C23 . H232 . 0.976 no C23 . H233 . 0.969 no C24 . N8 . 1.455(6) yes C24 . H241 . 0.958 no C24 . H242 . 0.958 no C24 . H243 . 0.954 no O1 . Tb1 . 2.394(4) yes O2 . Tb1 . 2.337(4) yes O3 . Tb1 . 2.386(3) yes O4 . Tb1 . 2.390(3) yes O5 . Tb1 . 2.313(4) yes O6 . Tb1 . 2.348(3) yes O7 . Tb1 . 2.333(3) yes O8 . Tb1 . 2.404(3) yes I3 . Cu1 . 2.5276(9) yes I1 . Cu1 . 2.5545(10) yes I2 . Cu1 . 2.5305(13) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . C1 . O1 . 124.7(5) yes N1 . C1 . H11 . 116.8 no O1 . C1 . H11 . 118.5 no N1 . C2 . H21 . 108.4 no N1 . C2 . H22 . 110.9 no H21 . C2 . H22 . 108.9 no N1 . C2 . H23 . 110.4 no H21 . C2 . H23 . 108.9 no H22 . C2 . H23 . 109.4 no N1 . C3 . H31 . 108.9 no N1 . C3 . H32 . 108.9 no H31 . C3 . H32 . 109.7 no N1 . C3 . H33 . 109.6 no H31 . C3 . H33 . 110.0 no H32 . C3 . H33 . 109.7 no N2 . C4 . O2 . 124.1(5) yes N2 . C4 . H41 . 117.4 no O2 . C4 . H41 . 118.5 no N2 . C5 . H51 . 109.6 no N2 . C5 . H52 . 110.4 no H51 . C5 . H52 . 109.1 no N2 . C5 . H53 . 109.7 no H51 . C5 . H53 . 109.1 no H52 . C5 . H53 . 108.8 no N2 . C6 . H61 . 110.8 no N2 . C6 . H62 . 109.9 no H61 . C6 . H62 . 108.6 no N2 . C6 . H63 . 109.9 no H61 . C6 . H63 . 107.9 no H62 . C6 . H63 . 109.7 no N3 . C7 . O3 . 123.9(5) yes N3 . C7 . H71 . 117.3 no O3 . C7 . H71 . 118.8 no N3 . C8 . H81 . 110.4 no N3 . C8 . H82 . 110.1 no H81 . C8 . H82 . 108.8 no N3 . C8 . H83 . 109.0 no H81 . C8 . H83 . 109.4 no H82 . C8 . H83 . 109.1 no N3 . C9 . H91 . 109.6 no N3 . C9 . H92 . 109.2 no H91 . C9 . H92 . 109.3 no N3 . C9 . H93 . 110.2 no H91 . C9 . H93 . 109.1 no H92 . C9 . H93 . 109.6 no N4 . C10 . O4 . 124.5(5) yes N4 . C10 . H101 . 116.9 no O4 . C10 . H101 . 118.6 no N4 . C11 . H111 . 108.8 no N4 . C11 . H112 . 109.6 no H111 . C11 . H112 . 109.0 no N4 . C11 . H113 . 109.7 no H111 . C11 . H113 . 110.3 no H112 . C11 . H113 . 109.4 no N4 . C12 . H121 . 109.3 no N4 . C12 . H122 . 109.6 no H121 . C12 . H122 . 110.1 no N4 . C12 . H123 . 109.3 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.0 no N5 . C13 . O5 . 124.6(5) yes N5 . C13 . H131 . 117.6 no O5 . C13 . H131 . 117.7 no N5 . C14 . H141 . 109.2 no N5 . C14 . H142 . 110.0 no H141 . C14 . H142 . 109.6 no N5 . C14 . H143 . 109.9 no H141 . C14 . H143 . 109.0 no H142 . C14 . H143 . 109.0 no N5 . C15 . H151 . 108.9 no N5 . C15 . H152 . 108.5 no H151 . C15 . H152 . 109.9 no N5 . C15 . H153 . 109.6 no H151 . C15 . H153 . 109.7 no H152 . C15 . H153 . 110.1 no N6 . C16 . O6 . 124.6(5) yes N6 . C16 . H161 . 117.3 no O6 . C16 . H161 . 118.1 no N6 . C17 . H171 . 108.7 no N6 . C17 . H172 . 109.1 no H171 . C17 . H172 . 109.6 no N6 . C17 . H173 . 110.1 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.8 no N6 . C18 . H181 . 109.6 no N6 . C18 . H182 . 109.3 no H181 . C18 . H182 . 108.9 no N6 . C18 . H183 . 110.1 no H181 . C18 . H183 . 109.9 no H182 . C18 . H183 . 109.0 no N7 . C19 . O7 . 124.3(5) yes N7 . C19 . H191 . 117.5 no O7 . C19 . H191 . 118.2 no N7 . C20 . H201 . 108.9 no N7 . C20 . H202 . 110.1 no H201 . C20 . H202 . 109.7 no N7 . C20 . H203 . 109.2 no H201 . C20 . H203 . 109.2 no H202 . C20 . H203 . 109.6 no N7 . C21 . H211 . 108.7 no N7 . C21 . H212 . 109.4 no H211 . C21 . H212 . 109.8 no N7 . C21 . H213 . 109.3 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 110.2 no N8 . C22 . O8 . 123.3(4) yes N8 . C22 . H221 . 117.3 no O8 . C22 . H221 . 119.4 no N8 . C23 . H231 . 111.1 no N8 . C23 . H232 . 110.1 no H231 . C23 . H232 . 109.4 no N8 . C23 . H233 . 108.8 no H231 . C23 . H233 . 108.8 no H232 . C23 . H233 . 108.6 no N8 . C24 . H241 . 109.0 no N8 . C24 . H242 . 110.3 no H241 . C24 . H242 . 110.0 no N8 . C24 . H243 . 108.8 no H241 . C24 . H243 . 109.1 no H242 . C24 . H243 . 109.7 no C3 . N1 . C2 . 117.6(5) yes C3 . N1 . C1 . 120.8(5) yes C2 . N1 . C1 . 121.5(5) yes C6 . N2 . C5 . 118.3(4) yes C6 . N2 . C4 . 121.1(5) yes C5 . N2 . C4 . 120.2(4) yes C9 . N3 . C8 . 117.1(4) yes C9 . N3 . C7 . 120.5(4) yes C8 . N3 . C7 . 122.3(4) yes C11 . N4 . C12 . 116.1(4) yes C11 . N4 . C10 . 122.1(4) yes C12 . N4 . C10 . 121.8(4) yes C15 . N5 . C14 . 117.7(5) yes C15 . N5 . C13 . 122.1(4) yes C14 . N5 . C13 . 119.9(5) yes C17 . N6 . C18 . 117.7(4) yes C17 . N6 . C16 . 120.9(5) yes C18 . N6 . C16 . 121.2(4) yes C20 . N7 . C21 . 116.7(5) yes C20 . N7 . C19 . 122.0(5) yes C21 . N7 . C19 . 121.3(5) yes C23 . N8 . C24 . 115.9(4) yes C23 . N8 . C22 . 122.0(4) yes C24 . N8 . C22 . 122.2(4) yes C1 . O1 . Tb1 . 128.4(3) yes C4 . O2 . Tb1 . 156.7(4) yes C7 . O3 . Tb1 . 127.4(3) yes C10 . O4 . Tb1 . 136.2(3) yes C13 . O5 . Tb1 . 146.8(3) yes C16 . O6 . Tb1 . 136.1(3) yes C19 . O7 . Tb1 . 141.3(3) yes C22 . O8 . Tb1 . 135.8(3) yes O8 . Tb1 . O1 . 140.64(13) yes O8 . Tb1 . O4 . 80.90(13) yes O1 . Tb1 . O4 . 113.92(14) yes O8 . Tb1 . O3 . 145.40(13) yes O1 . Tb1 . O3 . 71.41(14) yes O4 . Tb1 . O3 . 70.80(13) yes O8 . Tb1 . O6 . 116.16(13) yes O1 . Tb1 . O6 . 77.64(14) yes O4 . Tb1 . O6 . 138.67(13) yes O3 . Tb1 . O6 . 76.74(13) yes O8 . Tb1 . O2 . 74.59(14) yes O1 . Tb1 . O2 . 75.78(14) yes O4 . Tb1 . O2 . 72.70(13) yes O3 . Tb1 . O2 . 113.66(14) yes O6 . Tb1 . O2 . 145.97(13) yes O8 . Tb1 . O7 . 71.62(13) yes O1 . Tb1 . O7 . 77.39(14) yes O4 . Tb1 . O7 . 144.18(12) yes O3 . Tb1 . O7 . 141.92(13) yes O6 . Tb1 . O7 . 75.69(13) yes O8 . Tb1 . O5 . 73.16(13) yes O1 . Tb1 . O5 . 143.82(13) yes O4 . Tb1 . O5 . 77.15(13) yes O3 . Tb1 . O5 . 81.31(13) yes O6 . Tb1 . O5 . 73.22(13) yes O2 . Tb1 . O7 . 78.07(13) yes O2 . Tb1 . O5 . 138.59(13) yes O7 . Tb1 . O5 . 114.65(14) yes I1 . Cu1 . I2 . 119.09(4) yes I1 . Cu1 . I3 . 116.65(4) yes I2 . Cu1 . I3 . 124.20(3) yes _iucr_refine_instruction_details_constraints ; # # Punched on 02/02/11 at 13:51:03 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 02/02/11 at 13:51:03 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 864817' #TrackingRef '- Combined CIFs_TbCuI-CEC-Jan 2012.cif' _audit_creation_date 11-01-31 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'smr265b in P -1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.8626(5) _cell_length_b 11.9515(5) _cell_length_c 18.3798(8) _cell_angle_alpha 86.195(3) _cell_angle_beta 87.561(3) _cell_angle_gamma 87.005(3) _cell_volume 2375.80(18) _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' 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' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C36 H45 Cu3 I7.50 O12 S12 Tb1.50 # Dc = 3.40 Fooo = 1368.00 Mu = 89.93 M = 2435.35 # Found Formula = C18 H54 Cu1 I4 O9 S9 Tb1 # Dc = 2.00 FOOO = 1368.00 Mu = 49.52 M = 1433.30 _chemical_formula_sum 'C18 H54 Cu1 I4 O9 S9 Tb1' _chemical_formula_moiety 'C16 H48 O8 S8 Tb, C2 H6 O S, Cu I3, I ' _chemical_compound_source ? _chemical_formula_weight 1433.30 _cell_measurement_reflns_used 25304 _cell_measurement_theta_min 3.3931 _cell_measurement_theta_max 29.5017 _cell_measurement_temperature 110 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.353 _exptl_crystal_size_mid 0.448 _exptl_crystal_size_max 0.594 _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 4.952 # Sheldrick geometric approximatio 0.11 0.17 _exptl_absorpt_correction_T_min 0.177 _exptl_absorpt_correction_T_max 0.292 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.4685 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _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 110 _diffrn_reflns_number 39872 _reflns_number_total 11729 _diffrn_reflns_av_R_equivalents 0.061 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 11729 # Theoretical number of reflections is about 26643 _diffrn_reflns_theta_min 3.400 _diffrn_reflns_theta_max 29.565 _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 26.313 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -3.03 _refine_diff_density_max 3.10 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 11729 _refine_ls_number_restraints 298 _refine_ls_number_parameters 524 _oxford_refine_ls_R_factor_ref 0.0596 _refine_ls_wR_factor_ref 0.1110 _refine_ls_goodness_of_fit_ref 1.0253 _refine_ls_shift/su_max 0.0026053 _refine_ls_shift/su_mean 0.0000747 # The values computed from all data _oxford_reflns_number_all 11729 _refine_ls_R_factor_all 0.0596 _refine_ls_wR_factor_all 0.1110 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10236 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_gt 0.1004 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # 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: 0.148E+04 0.226E+04 0.119E+04 332. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2006). Gemini User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.9752(8) 1.0172(7) 0.5854(4) 0.0303 1.0000 Uani . U . . . . C2 C 1.0952(9) 1.0011(8) 0.7118(5) 0.0377 1.0000 Uani . U . . . . C3 C 0.7575(8) 0.7996(7) 0.5275(4) 0.0323 1.0000 Uani . U . . . . C4 C 0.8161(10) 0.5773(7) 0.5514(5) 0.0403 1.0000 Uani . U . . . . C5 C 1.1228(9) 0.6194(8) 0.7451(6) 0.0440 1.0000 Uani . U . . . . C6 C 1.0010(9) 0.4850(7) 0.8422(5) 0.0382 1.0000 Uani . U . . . . C7 C 0.8622(9) 0.6671(9) 0.9957(5) 0.0451 1.0000 Uani . U . . . . C8 C 0.6151(8) 0.6488(8) 0.9982(5) 0.0349 1.0000 Uani . U . . . . C9 C 0.4523(19) 0.510(2) 0.8188(12) 0.0339 0.5150 Uani . U . 1 5 . C10 C 0.667(2) 0.4556(16) 0.7529(12) 0.0369 0.5150 Uani D U . 1 5 . C11 C 0.439(3) 0.939(2) 0.9376(13) 0.0427 0.5000 Uani . U . 1 4 . C12 C 0.326(3) 0.876(2) 0.8224(18) 0.0437 0.5000 Uani . U . 1 4 . C13 C 0.4629(16) 1.0480(14) 0.6339(10) 0.0424 0.5800 Uani . U . 1 2 . C14 C 0.6716(16) 1.1595(15) 0.6304(10) 0.0457 0.5800 Uani . U . 1 2 . C15 C 0.672(2) 1.1661(19) 0.8535(13) 0.0588 0.5600 Uani . U . 1 8 . C16 C 0.8891(19) 1.1576(16) 0.8519(13) 0.0567 0.5600 Uani D U . 1 8 . C17 C 0.683(3) 0.441(3) 0.7349(16) 0.0463 0.4850 Uani . U . 1 6 . C18 C 0.487(2) 0.492(2) 0.8251(13) 0.0412 0.4850 Uani D U . 1 6 . C19 C 0.451(2) 0.9141(18) 0.9186(12) 0.0348 0.5000 Uani . U . 1 3 . C20 C 0.305(2) 0.857(2) 0.8134(15) 0.0318 0.5000 Uani . U . 1 3 . C21 C 0.5921(19) 1.1319(15) 0.7137(11) 0.0313 0.4200 Uani . U . 1 1 . C22 C 0.508(2) 1.0612(19) 0.5883(13) 0.0393 0.4200 Uani . U . 1 1 . C23 C 0.742(3) 1.1718(16) 0.8358(15) 0.0582 0.4400 Uani D U . 1 7 . C24 C 0.924(2) 1.114(2) 0.8793(15) 0.0471 0.4400 Uani . U . 1 7 . C25 C 0.4317(9) 0.7333(7) 0.5810(6) 0.0401 1.0000 Uani . U . . . . C26 C 0.2153(10) 0.6796(8) 0.5336(7) 0.0509 1.0000 Uani . U . . . . S1 S 0.94302(19) 0.99800(15) 0.68059(10) 0.0254 1.0000 Uani . U . . . . S2 S 0.83777(18) 0.70699(18) 0.59219(11) 0.0298 1.0000 Uani . U . . . . S3 S 0.96901(18) 0.58261(15) 0.76784(10) 0.0238 1.0000 Uani . U . . . . S4 S 0.74157(18) 0.65803(17) 0.93404(10) 0.0256 1.0000 Uani . U . . . . S5 S 0.5515(11) 0.5696(13) 0.7520(10) 0.0270 0.5150 Uani D U . 1 5 . S6 S 0.4655(6) 0.8451(5) 0.8682(3) 0.0274 0.5000 Uani . U . 1 4 . S7 S 0.5979(3) 1.0540(3) 0.68575(17) 0.0248 0.5800 Uani . U . 1 2 . S8 S 0.7792(12) 1.0527(10) 0.8779(9) 0.0283 0.5600 Uani D U . 1 8 . S9 S 0.5781(11) 0.5566(13) 0.7511(11) 0.0238 0.4850 Uani D U . 1 6 . S10 S 0.4505(6) 0.8195(5) 0.8468(3) 0.0277 0.5000 Uani . U . 1 3 . S11 S 0.5294(4) 1.0103(4) 0.6799(2) 0.0237 0.4200 Uani . U . 1 1 . S12 S 0.7971(15) 1.0395(12) 0.8787(12) 0.0342 0.4400 Uani D U . 1 7 . S13 S 0.2750(2) 0.78174(19) 0.58577(13) 0.0382 1.0000 Uani . U . . . . O1 O 0.9127(6) 0.8747(5) 0.6926(3) 0.0359 1.0000 Uani . U . . . . O2 O 0.7550(5) 0.7016(4) 0.6616(3) 0.0291 1.0000 Uani . U . . . . O3 O 0.9092(5) 0.6850(4) 0.8033(3) 0.0256 1.0000 Uani . U . . . . O4 O 0.7246(5) 0.7757(4) 0.8960(3) 0.0252 1.0000 Uani . U . . . . O5 O 0.6076(12) 0.6637(11) 0.7904(8) 0.0238 0.5150 Uani . U . 1 5 . O6 O 0.5614(11) 0.9027(10) 0.8181(7) 0.0280 0.5000 Uani . U . 1 4 . O7 O 0.6444(12) 0.9283(11) 0.6767(7) 0.0296 0.5800 Uani . U . 1 2 . O8 O 0.8254(12) 0.9643(12) 0.8186(8) 0.0261 0.5600 Uani . U . 1 8 . O9 O 0.6503(14) 0.6391(13) 0.7881(9) 0.0292 0.4850 Uani . U . 1 6 . O10 O 0.5405(11) 0.8669(10) 0.7876(7) 0.0288 0.5000 Uani . U . 1 3 . O11 O 0.6812(16) 0.9489(14) 0.6690(11) 0.0230 0.4200 Uani . U . 1 1 . O12 O 0.7866(16) 0.9803(14) 0.8122(11) 0.0255 0.4400 Uani . U . 1 7 . Tb1 Tb 0.74360(3) 0.80969(3) 0.766459(17) 0.0185 1.0000 Uani . . . . . . I1 I 0.40574(5) 0.39808(4) 0.61373(3) 0.0294 1.0000 Uani . . . . . . Cu1 Cu 0.23548(9) 0.31026(8) 0.69242(6) 0.0291 1.0000 Uani . . . . . . I3 I 0.28482(6) 0.21183(5) 0.81478(3) 0.0359 1.0000 Uani . . . . . . I2 I 0.01410(5) 0.32260(5) 0.65014(3) 0.0327 1.0000 Uani . . . . . . I4 I 0.76628(5) 0.34014(5) 1.01799(3) 0.0329 1.0000 Uani . . . . . . O13 O 0.2645(7) 0.8929(5) 0.5425(4) 0.0438 1.0000 Uani . U . . . . H21 H 1.0955 0.9749 0.7621 0.0559 1.0000 Uiso R . . . . . H23 H 1.1509 0.9538 0.6840 0.0559 1.0000 Uiso R . . . . . H22 H 1.1220 1.0765 0.7069 0.0559 1.0000 Uiso R . . . . . H13 H 0.9014 1.0077 0.5600 0.0448 1.0000 Uiso R . . . . . H11 H 1.0374 0.9625 0.5708 0.0449 1.0000 Uiso R . . . . . H12 H 1.0032 1.0912 0.5735 0.0450 1.0000 Uiso R . . . . . H233 H 0.6788 1.1624 0.8019 0.0900 0.4400 Uiso R . . 1 7 . H231 H 0.8135 1.2013 0.8094 0.0900 0.4400 Uiso R . . 1 7 . H232 H 0.7119 1.2241 0.8709 0.0900 0.4400 Uiso R . . 1 7 . H243 H 0.9901 1.0684 0.8997 0.0720 0.4400 Uiso R . . 1 7 . H242 H 0.9456 1.1396 0.8299 0.0721 0.4400 Uiso R . . 1 7 . H241 H 0.9060 1.1779 0.9081 0.0720 0.4400 Uiso R . . 1 7 . H163 H 0.9710 1.1235 0.8551 0.0821 0.5600 Uiso R . . 1 8 . H162 H 0.8769 1.1877 0.8028 0.0820 0.5600 Uiso R . . 1 8 . H161 H 0.8787 1.2171 0.8848 0.0820 0.5600 Uiso R . . 1 8 . H152 H 0.5893 1.1467 0.8679 0.0831 0.5600 Uiso R . . 1 8 . H153 H 0.6765 1.1824 0.8014 0.0831 0.5600 Uiso R . . 1 8 . H151 H 0.6920 1.2312 0.8780 0.0830 0.5600 Uiso R . . 1 8 . H141 H 0.7480 1.1743 0.6511 0.0670 0.5800 Uiso R . . 1 2 . H142 H 0.6872 1.1344 0.5821 0.0669 0.5800 Uiso R . . 1 2 . H143 H 0.6194 1.2266 0.6283 0.0670 0.5800 Uiso R . . 1 2 . H132 H 0.4186 0.9833 0.6507 0.0630 0.5800 Uiso R . . 1 2 . H131 H 0.4871 1.0430 0.5833 0.0628 0.5800 Uiso R . . 1 2 . H133 H 0.4114 1.1145 0.6397 0.0630 0.5800 Uiso R . . 1 2 . H212 H 0.6216 1.1139 0.7618 0.0470 0.4200 Uiso R . . 1 1 . H211 H 0.5296 1.1915 0.7155 0.0470 0.4200 Uiso R . . 1 1 . H213 H 0.6593 1.1559 0.6817 0.0470 0.4200 Uiso R . . 1 1 . H223 H 0.4780 1.0028 0.5614 0.0590 0.4200 Uiso R . . 1 1 . H221 H 0.4490 1.1238 0.5874 0.0590 0.4200 Uiso R . . 1 1 . H222 H 0.5850 1.0847 0.5666 0.0590 0.4200 Uiso R . . 1 1 . H252 H 0.4804 0.7807 0.6067 0.0600 1.0000 Uiso R . . . . . H251 H 0.4604 0.7335 0.5312 0.0600 1.0000 Uiso R . . . . . H253 H 0.4388 0.6584 0.6031 0.0601 1.0000 Uiso R . . . . . H262 H 0.1288 0.6955 0.5277 0.0760 1.0000 Uiso R . . . . . H263 H 0.2573 0.6812 0.4868 0.0758 1.0000 Uiso R . . . . . H261 H 0.2285 0.6070 0.5580 0.0758 1.0000 Uiso R . . . . . H51 H 1.1226 0.6799 0.7079 0.0660 1.0000 Uiso R . . . . . H52 H 1.1681 0.5547 0.7274 0.0661 1.0000 Uiso R . . . . . H53 H 1.1603 0.6412 0.7878 0.0659 1.0000 Uiso R . . . . . H61 H 0.9248 0.4629 0.8656 0.0571 1.0000 Uiso R . . . . . H62 H 1.0444 0.4201 0.8241 0.0571 1.0000 Uiso R . . . . . H63 H 1.0510 0.5169 0.8765 0.0570 1.0000 Uiso R . . . . . H73 H 0.9389 0.6753 0.9682 0.0682 1.0000 Uiso R . . . . . H72 H 0.8672 0.6001 1.0274 0.0681 1.0000 Uiso R . . . . . H71 H 0.8456 0.7308 1.0241 0.0678 1.0000 Uiso R . . . . . H82 H 0.5412 0.6428 0.9723 0.0520 1.0000 Uiso R . . . . . H81 H 0.6281 0.5835 1.0308 0.0519 1.0000 Uiso R . . . . . H83 H 0.6084 0.7154 1.0253 0.0520 1.0000 Uiso R . . . . . H201 H 0.2906 0.8113 0.7738 0.0480 0.5000 Uiso R . . 1 3 . H203 H 0.2435 0.8448 0.8517 0.0479 0.5000 Uiso R . . 1 3 . H202 H 0.3024 0.9343 0.7963 0.0481 0.5000 Uiso R . . 1 3 . H192 H 0.5314 0.9120 0.9383 0.0530 0.5000 Uiso R . . 1 3 . H191 H 0.3921 0.8923 0.9565 0.0530 0.5000 Uiso R . . 1 3 . H193 H 0.4295 0.9890 0.8997 0.0530 0.5000 Uiso R . . 1 3 . H111 H 0.5062 0.9319 0.9696 0.0640 0.5000 Uiso R . . 1 4 . H112 H 0.3640 0.9215 0.9648 0.0639 0.5000 Uiso R . . 1 4 . H113 H 0.4312 1.0142 0.9164 0.0640 0.5000 Uiso R . . 1 4 . H121 H 0.3304 0.8414 0.7766 0.0650 0.5000 Uiso R . . 1 4 . H123 H 0.2583 0.8477 0.8523 0.0650 0.5000 Uiso R . . 1 4 . H122 H 0.3141 0.9560 0.8138 0.0650 0.5000 Uiso R . . 1 4 . H31 H 0.7517 0.8743 0.5437 0.0481 1.0000 Uiso R . . . . . H32 H 0.8006 0.7998 0.4809 0.0479 1.0000 Uiso R . . . . . H33 H 0.6759 0.7745 0.5227 0.0480 1.0000 Uiso R . . . . . H43 H 0.8535 0.5161 0.5805 0.0599 1.0000 Uiso R . . . . . H42 H 0.8543 0.5802 0.5031 0.0599 1.0000 Uiso R . . . . . H41 H 0.7292 0.5669 0.5485 0.0599 1.0000 Uiso R . . . . . H101 H 0.7383 0.4783 0.7244 0.0560 0.5150 Uiso R . . 1 5 . H103 H 0.6348 0.3915 0.7329 0.0559 0.5150 Uiso R . . 1 5 . H102 H 0.6893 0.4364 0.8022 0.0559 0.5150 Uiso R . . 1 5 . H93 H 0.3828 0.5609 0.8273 0.0509 0.5150 Uiso R . . 1 5 . H92 H 0.4240 0.4409 0.8028 0.0509 0.5150 Uiso R . . 1 5 . H91 H 0.4955 0.4943 0.8635 0.0510 0.5150 Uiso R . . 1 5 . H181 H 0.4277 0.5466 0.8435 0.0610 0.4850 Uiso R . . 1 6 . H182 H 0.4456 0.4305 0.8082 0.0610 0.4850 Uiso R . . 1 6 . H183 H 0.5404 0.4650 0.8638 0.0609 0.4850 Uiso R . . 1 6 . H172 H 0.7534 0.4667 0.7068 0.0680 0.4850 Uiso R . . 1 6 . H173 H 0.6427 0.3875 0.7088 0.0679 0.4850 Uiso R . . 1 6 . H171 H 0.7087 0.4064 0.7806 0.0680 0.4850 Uiso R . . 1 6 . 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 C1 0.036(4) 0.032(4) 0.023(3) -0.006(3) 0.001(3) -0.005(3) C2 0.045(4) 0.034(4) 0.035(4) -0.006(3) -0.005(3) -0.003(3) C3 0.043(4) 0.028(3) 0.027(3) -0.008(3) 0.004(3) -0.003(3) C4 0.057(5) 0.032(4) 0.032(4) -0.015(3) -0.007(3) 0.011(3) C5 0.046(4) 0.037(4) 0.048(4) -0.007(4) 0.014(4) 0.002(4) C6 0.045(4) 0.032(4) 0.036(4) 0.002(3) -0.003(3) 0.010(3) C7 0.039(4) 0.061(5) 0.036(4) 0.004(4) -0.011(3) -0.002(4) C8 0.035(4) 0.042(4) 0.026(4) 0.005(3) -0.005(3) -0.001(3) C9 0.036(7) 0.034(7) 0.033(6) -0.004(5) -0.001(6) -0.011(6) C10 0.045(8) 0.029(7) 0.039(7) -0.006(6) -0.004(6) -0.012(6) C11 0.054(8) 0.032(7) 0.043(8) 0.000(7) -0.002(7) -0.011(7) C12 0.051(8) 0.037(8) 0.043(8) -0.002(7) -0.004(7) -0.011(7) C13 0.043(6) 0.039(6) 0.047(7) -0.006(6) -0.008(6) -0.002(5) C14 0.040(6) 0.044(6) 0.052(7) 0.000(6) -0.001(6) 0.006(6) C15 0.050(7) 0.063(8) 0.064(8) -0.016(7) 0.002(7) 0.001(7) C16 0.052(7) 0.056(8) 0.064(8) -0.019(7) 0.006(7) -0.008(7) C17 0.040(8) 0.043(8) 0.057(9) -0.012(7) 0.001(7) -0.004(7) C18 0.037(8) 0.036(8) 0.052(8) -0.010(6) -0.003(7) -0.004(7) C19 0.035(7) 0.030(7) 0.041(8) -0.006(6) -0.011(6) -0.001(6) C20 0.034(7) 0.027(7) 0.036(7) -0.001(6) -0.016(6) 0.002(6) C21 0.035(7) 0.023(6) 0.037(7) -0.004(6) -0.013(6) 0.006(6) C22 0.042(7) 0.034(7) 0.043(8) -0.003(6) -0.018(7) 0.007(6) C23 0.059(8) 0.058(8) 0.061(8) -0.017(7) -0.020(7) 0.006(7) C24 0.043(7) 0.046(7) 0.056(7) -0.022(6) -0.023(6) 0.003(6) C25 0.039(4) 0.029(4) 0.053(5) -0.003(4) -0.015(4) -0.002(3) C26 0.047(5) 0.033(4) 0.075(6) -0.004(4) -0.021(5) -0.002(4) S1 0.0356(10) 0.0189(8) 0.0220(8) -0.0030(6) 0.0024(7) -0.0050(7) S2 0.0259(9) 0.0378(10) 0.0275(9) -0.0162(8) -0.0065(7) 0.0044(8) S3 0.0293(9) 0.0190(8) 0.0226(8) 0.0006(6) -0.0054(7) 0.0026(7) S4 0.0275(9) 0.0314(9) 0.0175(8) 0.0027(7) -0.0047(6) 0.0008(7) S5 0.031(4) 0.024(4) 0.028(3) -0.005(2) -0.009(4) -0.007(3) S6 0.024(2) 0.025(3) 0.031(3) 0.008(2) 0.000(2) 0.0038(19) S7 0.0346(17) 0.0193(14) 0.0200(14) -0.0016(11) -0.0050(12) 0.0069(13) S8 0.039(3) 0.021(3) 0.025(3) -0.006(2) -0.002(2) 0.007(2) S9 0.028(4) 0.019(3) 0.026(3) -0.001(2) -0.009(3) -0.007(3) S10 0.030(2) 0.024(3) 0.028(3) 0.0059(19) -0.004(2) -0.0017(18) S11 0.031(2) 0.0159(17) 0.024(2) 0.0045(15) -0.0071(16) 0.0011(17) S12 0.046(5) 0.024(4) 0.035(4) -0.018(3) 0.011(4) -0.012(4) S13 0.0395(12) 0.0314(10) 0.0432(12) -0.0079(9) 0.0109(9) -0.0015(9) O1 0.051(4) 0.021(3) 0.035(3) -0.005(2) 0.013(3) -0.005(2) O2 0.035(3) 0.021(2) 0.032(3) -0.008(2) -0.003(2) 0.002(2) O3 0.032(3) 0.022(2) 0.022(2) -0.0004(19) -0.002(2) 0.003(2) O4 0.031(3) 0.018(2) 0.027(3) -0.0053(19) 0.001(2) -0.003(2) O5 0.030(5) 0.020(5) 0.022(4) -0.006(4) 0.003(4) -0.010(4) O6 0.036(5) 0.021(4) 0.025(5) 0.003(4) 0.006(4) 0.006(4) O7 0.041(6) 0.025(5) 0.022(4) -0.001(4) -0.003(4) 0.015(4) O8 0.033(6) 0.025(5) 0.021(4) -0.004(4) 0.001(4) -0.002(4) O9 0.035(6) 0.026(5) 0.027(5) -0.006(4) 0.000(5) 0.003(5) O10 0.033(5) 0.024(4) 0.028(4) 0.006(4) 0.001(4) 0.001(4) O11 0.029(5) 0.014(4) 0.024(4) 0.009(4) 0.003(4) -0.001(4) O12 0.033(6) 0.013(4) 0.029(5) 0.006(4) 0.002(5) -0.002(4) Tb1 0.02498(17) 0.01362(14) 0.01720(16) -0.00027(11) -0.00556(12) -0.00056(11) I1 0.0349(3) 0.0238(2) 0.0306(3) -0.00175(19) -0.0113(2) -0.00254(19) Cu1 0.0323(5) 0.0229(4) 0.0331(5) -0.0082(4) -0.0080(4) 0.0041(4) I3 0.0489(3) 0.0316(3) 0.0291(3) -0.0035(2) -0.0103(2) -0.0095(2) I2 0.0287(3) 0.0300(3) 0.0399(3) -0.0080(2) -0.0089(2) 0.0079(2) I4 0.0277(3) 0.0364(3) 0.0346(3) -0.0035(2) 0.0033(2) -0.0049(2) O13 0.049(4) 0.027(3) 0.054(4) -0.005(3) -0.001(3) 0.005(3) _refine_ls_extinction_coef 14.4(13) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 1.735(7) 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 C1 . S1 . 1.772(8) yes C1 . H13 . 0.960 no C1 . H11 . 0.958 no C1 . H12 . 0.960 no C2 . S1 . 1.776(9) yes C2 . H21 . 0.957 no C2 . H23 . 0.961 no C2 . H22 . 0.959 no C3 . S2 . 1.792(9) yes C3 . H31 . 0.958 no C3 . H32 . 0.959 no C3 . H33 . 0.959 no C4 . S2 . 1.797(9) yes C4 . H43 . 0.960 no C4 . H42 . 0.963 no C4 . H41 . 0.962 no C5 . S3 . 1.776(10) yes C5 . H51 . 0.961 no C5 . H52 . 0.962 no C5 . H53 . 0.957 no C6 . S3 . 1.770(9) yes C6 . H61 . 0.958 no C6 . H62 . 0.957 no C6 . H63 . 0.960 no C7 . S4 . 1.780(9) yes C7 . H73 . 0.962 no C7 . H72 . 0.960 no C7 . H71 . 0.956 no C8 . S4 . 1.775(9) yes C8 . H82 . 0.958 no C8 . H81 . 0.960 no C8 . H83 . 0.965 no C9 . S5 . 1.74(2) yes C9 . H93 . 0.962 no C9 . H92 . 0.960 no C9 . H91 . 0.965 no C10 . S5 . 1.800(5) yes C10 . H101 . 0.959 no C10 . H103 . 0.959 no C10 . H102 . 0.960 no C11 . S6 . 1.76(2) yes C11 . H111 . 0.958 no C11 . H112 . 0.958 no C11 . H113 . 0.958 no C12 . S6 . 1.77(3) yes C12 . H121 . 0.961 no C12 . H123 . 0.962 no C12 . H122 . 0.961 no C13 . S7 . 1.789(17) yes C13 . H132 . 0.959 no C13 . H131 . 0.959 no C13 . H133 . 0.957 no C14 . S7 . 1.769(18) yes C14 . H141 . 0.957 no C14 . H142 . 0.962 no C14 . H143 . 0.957 no C15 . S8 . 1.78(2) yes C15 . H152 . 0.963 no C15 . H153 . 0.965 no C15 . H151 . 0.963 no C16 . S8 . 1.803(5) yes C16 . H163 . 0.961 no C16 . H162 . 0.962 no C16 . H161 . 0.963 no C17 . S9 . 1.77(3) yes C17 . H172 . 0.959 no C17 . H173 . 0.958 no C17 . H171 . 0.959 no C18 . S9 . 1.801(5) yes C18 . H181 . 0.961 no C18 . H182 . 0.960 no C18 . H183 . 0.963 no C19 . S10 . 1.79(2) yes C19 . H192 . 0.958 no C19 . H191 . 0.959 no C19 . H193 . 0.959 no C20 . S10 . 1.74(2) yes C20 . H201 . 0.959 no C20 . H203 . 0.961 no C20 . H202 . 0.960 no C21 . S11 . 1.796(19) yes C21 . H212 . 0.959 no C21 . H211 . 0.959 no C21 . H213 . 0.962 no C22 . S11 . 1.77(2) yes C22 . H223 . 0.958 no C22 . H221 . 0.958 no C22 . H222 . 0.960 no C23 . S12 . 1.804(5) yes C23 . H233 . 0.966 no C23 . H231 . 0.964 no C23 . H232 . 0.964 no C24 . S12 . 1.68(3) yes C24 . H243 . 0.960 no C24 . H242 . 0.962 no C24 . H241 . 0.961 no C25 . S13 . 1.769(9) yes C25 . H252 . 0.954 no C25 . H251 . 0.955 no C25 . H253 . 0.958 no C26 . S13 . 1.767(10) yes C26 . H262 . 0.959 no C26 . H263 . 0.956 no C26 . H261 . 0.956 no S1 . O1 . 1.526(6) yes S2 . O2 . 1.529(6) yes S3 . O3 . 1.528(5) yes S4 . O4 . 1.534(5) yes S5 . O5 . 1.53(2) yes S6 . O6 . 1.522(13) yes S7 . O7 . 1.577(13) yes S8 . O8 . 1.61(2) yes S9 . O9 . 1.50(3) yes S10 . O10 . 1.532(13) yes S11 . O11 . 1.779(19) yes S12 . O12 . 1.46(3) yes S13 . O13 . 1.504(7) yes O1 . Tb1 . 2.370(6) yes O2 . Tb1 . 2.386(5) yes O3 . Tb1 . 2.367(5) yes O4 . Tb1 . 2.390(5) yes O5 . Tb1 . 2.352(13) yes O6 . Tb1 . 2.409(11) yes O7 . Tb1 . 2.361(13) yes O8 . Tb1 . 2.367(14) yes O9 . Tb1 . 2.327(16) yes O10 . Tb1 . 2.300(12) yes O11 . Tb1 . 2.454(18) yes O12 . Tb1 . 2.333(19) yes I1 . Cu1 . 2.5275(12) yes Cu1 . I3 . 2.5327(12) yes Cu1 . I2 . 2.5525(11) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . C1 . H13 . 109.1 no S1 . C1 . H11 . 109.6 no H13 . C1 . H11 . 109.1 no S1 . C1 . H12 . 109.9 no H13 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.7 no S1 . C2 . H21 . 108.9 no S1 . C2 . H23 . 110.4 no H21 . C2 . H23 . 109.3 no S1 . C2 . H22 . 109.8 no H21 . C2 . H22 . 109.2 no H23 . C2 . H22 . 109.2 no S2 . C3 . H31 . 110.0 no S2 . C3 . H32 . 109.9 no H31 . C3 . H32 . 109.3 no S2 . C3 . H33 . 109.5 no H31 . C3 . H33 . 109.0 no H32 . C3 . H33 . 109.1 no S2 . C4 . H43 . 109.5 no S2 . C4 . H42 . 109.1 no H43 . C4 . H42 . 109.4 no S2 . C4 . H41 . 109.4 no H43 . C4 . H41 . 109.7 no H42 . C4 . H41 . 109.7 no S3 . C5 . H51 . 109.6 no S3 . C5 . H52 . 108.4 no H51 . C5 . H52 . 109.9 no S3 . C5 . H53 . 109.3 no H51 . C5 . H53 . 110.4 no H52 . C5 . H53 . 109.1 no S3 . C6 . H61 . 109.1 no S3 . C6 . H62 . 109.0 no H61 . C6 . H62 . 108.9 no S3 . C6 . H63 . 110.9 no H61 . C6 . H63 . 110.1 no H62 . C6 . H63 . 108.8 no S4 . C7 . H73 . 109.0 no S4 . C7 . H72 . 109.5 no H73 . C7 . H72 . 109.8 no S4 . C7 . H71 . 109.6 no H73 . C7 . H71 . 109.4 no H72 . C7 . H71 . 109.6 no S4 . C8 . H82 . 108.7 no S4 . C8 . H81 . 109.2 no H82 . C8 . H81 . 109.9 no S4 . C8 . H83 . 109.4 no H82 . C8 . H83 . 109.7 no H81 . C8 . H83 . 109.9 no S5 . C9 . H93 . 109.4 no S5 . C9 . H92 . 109.6 no H93 . C9 . H92 . 109.5 no S5 . C9 . H91 . 109.4 no H93 . C9 . H91 . 109.4 no H92 . C9 . H91 . 109.6 no S5 . C10 . H101 . 109.6 no S5 . C10 . H103 . 110.0 no H101 . C10 . H103 . 109.4 no S5 . C10 . H102 . 109.2 no H101 . C10 . H102 . 109.2 no H103 . C10 . H102 . 109.4 no S6 . C11 . H111 . 109.3 no S6 . C11 . H112 . 109.8 no H111 . C11 . H112 . 109.3 no S6 . C11 . H113 . 109.6 no H111 . C11 . H113 . 109.3 no H112 . C11 . H113 . 109.5 no S6 . C12 . H121 . 109.7 no S6 . C12 . H123 . 109.4 no H121 . C12 . H123 . 109.6 no S6 . C12 . H122 . 109.3 no H121 . C12 . H122 . 109.5 no H123 . C12 . H122 . 109.4 no S7 . C13 . H132 . 109.6 no S7 . C13 . H131 . 109.2 no H132 . C13 . H131 . 109.5 no S7 . C13 . H133 . 109.4 no H132 . C13 . H133 . 109.6 no H131 . C13 . H133 . 109.5 no S7 . C14 . H141 . 109.4 no S7 . C14 . H142 . 109.5 no H141 . C14 . H142 . 109.5 no S7 . C14 . H143 . 109.3 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.8 no S8 . C15 . H152 . 110.4 no S8 . C15 . H153 . 109.9 no H152 . C15 . H153 . 108.6 no S8 . C15 . H151 . 109.1 no H152 . C15 . H151 . 109.0 no H153 . C15 . H151 . 109.9 no S8 . C16 . H163 . 108.8 no S8 . C16 . H162 . 110.6 no H163 . C16 . H162 . 109.3 no S8 . C16 . H161 . 109.1 no H163 . C16 . H161 . 109.6 no H162 . C16 . H161 . 109.4 no S9 . C17 . H172 . 109.7 no S9 . C17 . H173 . 109.4 no H172 . C17 . H173 . 109.6 no S9 . C17 . H171 . 109.5 no H172 . C17 . H171 . 109.2 no H173 . C17 . H171 . 109.4 no S9 . C18 . H181 . 109.5 no S9 . C18 . H182 . 109.7 no H181 . C18 . H182 . 109.5 no S9 . C18 . H183 . 109.5 no H181 . C18 . H183 . 109.1 no H182 . C18 . H183 . 109.5 no S10 . C19 . H192 . 109.8 no S10 . C19 . H191 . 109.7 no H192 . C19 . H191 . 109.2 no S10 . C19 . H193 . 109.7 no H192 . C19 . H193 . 109.3 no H191 . C19 . H193 . 109.2 no S10 . C20 . H201 . 109.5 no S10 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.6 no S10 . C20 . H202 . 109.4 no H201 . C20 . H202 . 109.3 no H203 . C20 . H202 . 109.5 no S11 . C21 . H212 . 109.7 no S11 . C21 . H211 . 109.8 no H212 . C21 . H211 . 109.5 no S11 . C21 . H213 . 109.3 no H212 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.1 no S11 . C22 . H223 . 109.6 no S11 . C22 . H221 . 109.5 no H223 . C22 . H221 . 109.5 no S11 . C22 . H222 . 109.3 no H223 . C22 . H222 . 109.6 no H221 . C22 . H222 . 109.3 no S12 . C23 . H233 . 111.9 no S12 . C23 . H231 . 105.0 no H233 . C23 . H231 . 109.1 no S12 . C23 . H232 . 112.2 no H233 . C23 . H232 . 109.2 no H231 . C23 . H232 . 109.3 no S12 . C24 . H243 . 109.7 no S12 . C24 . H242 . 108.6 no H243 . C24 . H242 . 109.7 no S12 . C24 . H241 . 109.2 no H243 . C24 . H241 . 109.6 no H242 . C24 . H241 . 109.9 no S13 . C25 . H252 . 110.0 no S13 . C25 . H251 . 109.6 no H252 . C25 . H251 . 109.5 no S13 . C25 . H253 . 109.0 no H252 . C25 . H253 . 109.1 no H251 . C25 . H253 . 109.6 no S13 . C26 . H262 . 109.8 no S13 . C26 . H263 . 108.9 no H262 . C26 . H263 . 109.5 no S13 . C26 . H261 . 109.3 no H262 . C26 . H261 . 109.8 no H263 . C26 . H261 . 109.5 no C2 . S1 . C1 . 99.3(4) yes C2 . S1 . O1 . 103.8(4) yes C1 . S1 . O1 . 104.3(4) yes C4 . S2 . C3 . 98.1(4) yes C4 . S2 . O2 . 104.4(4) yes C3 . S2 . O2 . 106.0(4) yes C5 . S3 . C6 . 98.0(5) yes C5 . S3 . O3 . 104.6(4) yes C6 . S3 . O3 . 104.3(4) yes C7 . S4 . C8 . 99.0(4) yes C7 . S4 . O4 . 105.6(4) yes C8 . S4 . O4 . 104.5(4) yes C10 . S5 . C9 . 96.8(13) yes C10 . S5 . O5 . 105.8(12) yes C9 . S5 . O5 . 103.5(14) yes C12 . S6 . C11 . 97.6(14) yes C12 . S6 . O6 . 103.3(12) yes C11 . S6 . O6 . 103.0(10) yes C13 . S7 . C14 . 98.0(9) yes C13 . S7 . O7 . 95.6(8) yes C14 . S7 . O7 . 117.5(8) yes C16 . S8 . C15 . 81.9(12) yes C16 . S8 . O8 . 97.1(11) yes C15 . S8 . O8 . 120.2(12) yes C18 . S9 . C17 . 98.4(14) yes C18 . S9 . O9 . 103.2(15) yes C17 . S9 . O9 . 105.8(14) yes C19 . S10 . C20 . 99.3(11) yes C19 . S10 . O10 . 105.0(10) yes C20 . S10 . O10 . 104.2(11) yes C21 . S11 . C22 . 99.2(10) yes C21 . S11 . O11 . 89.6(9) yes C22 . S11 . O11 . 98.7(10) yes C23 . S12 . C24 . 78.8(14) yes C23 . S12 . O12 . 92.8(15) yes C24 . S12 . O12 . 114.1(17) yes C25 . S13 . C26 . 97.8(5) yes C25 . S13 . O13 . 107.7(4) yes C26 . S13 . O13 . 107.9(5) yes S1 . O1 . Tb1 . 124.0(3) yes S2 . O2 . Tb1 . 132.1(3) yes S3 . O3 . Tb1 . 130.8(3) yes S4 . O4 . Tb1 . 122.7(3) yes S5 . O5 . Tb1 . 140.4(10) yes S6 . O6 . Tb1 . 124.7(6) yes S7 . O7 . Tb1 . 125.4(7) yes S8 . O8 . Tb1 . 136.5(9) yes S9 . O9 . Tb1 . 141.8(12) yes S10 . O10 . Tb1 . 127.3(7) yes S11 . O11 . Tb1 . 115.3(8) yes S12 . O12 . Tb1 . 144.7(12) yes O11 . Tb1 . O4 . 140.8(5) yes O11 . Tb1 . O2 . 77.6(5) yes O4 . Tb1 . O2 . 137.43(18) yes O11 . Tb1 . O1 . 67.1(4) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O11 . Tb1 . O3 . 142.5(4) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O2 . 137.43(18) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O7 . 136.6(3) yes O2 . Tb1 . O7 . 76.3(3) yes O1 . Tb1 . O7 . 77.9(3) yes O3 . Tb1 . O7 . 150.8(3) yes O4 . Tb1 . O2 . 137.43(18) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O10 . 79.4(3) yes O2 . Tb1 . O10 . 107.9(4) yes O1 . Tb1 . O10 . 136.5(3) yes O3 . Tb1 . O10 . 146.3(3) yes O6 . Tb1 . O4 . 67.7(3) yes O6 . Tb1 . O2 . 126.6(4) yes O4 . Tb1 . O2 . 137.43(18) yes O6 . Tb1 . O1 . 133.0(3) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O6 . Tb1 . O3 . 139.6(3) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O2 . 137.43(18) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O5 . 72.7(4) yes O2 . Tb1 . O5 . 73.2(4) yes O1 . Tb1 . O5 . 145.5(3) yes O3 . Tb1 . O5 . 89.4(4) yes O4 . Tb1 . O2 . 137.43(18) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O9 . 73.4(4) yes O2 . Tb1 . O9 . 67.7(4) yes O1 . Tb1 . O9 . 135.4(4) yes O3 . Tb1 . O9 . 77.0(4) yes O4 . Tb1 . O2 . 137.43(18) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O12 . 75.6(5) yes O2 . Tb1 . O12 . 145.4(5) yes O1 . Tb1 . O12 . 75.2(5) yes O3 . Tb1 . O12 . 104.5(4) yes O4 . Tb1 . O2 . 137.43(18) yes O4 . Tb1 . O1 . 129.7(2) yes O2 . Tb1 . O1 . 73.8(2) yes O4 . Tb1 . O3 . 72.00(18) yes O2 . Tb1 . O3 . 82.89(18) yes O1 . Tb1 . O3 . 76.9(2) yes O4 . Tb1 . O8 . 73.0(4) yes O2 . Tb1 . O8 . 143.8(4) yes O1 . Tb1 . O8 . 70.3(4) yes O3 . Tb1 . O8 . 93.2(3) yes I1 . Cu1 . I3 . 119.65(4) yes I1 . Cu1 . I2 . 120.43(4) yes I3 . Cu1 . I2 . 119.91(5) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C15 . H233 . C21 . 145(3) 0.95(4) 1.97(3) 2.81(3) yes C23 . H233 . C21 . 163 0.97 1.97 2.91(3) yes C15 . H153 . C21 . 137 0.96 2.03 2.81(3) yes C23 . H153 . C21 . 150(2) 0.97(3) 2.03(3) 2.91(3) yes C14 . H142 . O13 2_676 169 0.96 2.37 3.32(3) yes C21 . H212 . C15 . 148 0.96 1.95 2.81(3) yes C21 . H212 . C23 . 141 0.96 2.10 2.91(3) yes C21 . H212 . O12 . 134 0.96 2.50 3.24(3) yes C14 . H213 . C21 . 132.7(16) 0.94(3) 0.962 1.75(3) yes C22 . H222 . O13 2_676 151 0.96 2.54 3.41(3) yes C11 . H111 . C11 2_677 129 0.96 2.49 3.18(3) yes C19 . H111 . C11 2_677 150(3) 1.17(4) 2.49(5) 3.55(3) yes C3 . H31 . O11 . 131 0.96 2.60 3.30(3) yes _iucr_refine_instruction_details_constraints ; # # Punched on 31/01/11 at 16:45:24 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 11,X'S) H ( 12,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 23,X'S) H ( 22,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 4,X'S) H ( 43,X'S) H ( 42,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S) RIDE C ( 7,X'S) H ( 73,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) H ( 83,X'S) RIDE C ( 9,X'S) H ( 93,X'S) H ( 92,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 103,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 123,X'S) H ( 122,X'S) RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 153,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 163,X'S) H ( 162,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 172,X'S) H ( 173,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 19,X'S) H ( 192,X'S) H ( 191,X'S) H ( 193,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 203,X'S) H ( 202,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) H ( 213,X'S) RIDE C ( 22,X'S) H ( 223,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 233,X'S) H ( 231,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 243,X'S) H ( 242,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 252,X'S) H ( 251,X'S) H ( 253,X'S) RIDE C ( 26,X'S) H ( 262,X'S) H ( 263,X'S) H ( 261,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 31/01/11 at 16:45:24 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = S(1) TO S(2) U(IJ)'S 0.0, 0.010000 = S(2) TO S(3) U(IJ)'S 0.0, 0.010000 = S(3) TO S(4) U(IJ)'S 0.0, 0.010000 = S(4) TO S(5) U(IJ)'S 0.0, 0.010000 = S(5) TO S(6) U(IJ)'S 0.0, 0.010000 = S(6) TO S(7) U(IJ)'S 0.0, 0.010000 = S(7) TO S(8) U(IJ)'S 0.0, 0.010000 = S(8) TO S(9) U(IJ)'S 0.0, 0.010000 = S(9) TO S(10) U(IJ)'S 0.0, 0.010000 = S(10) TO S(11) U(IJ)'S 0.0, 0.010000 = S(11) TO S(12) U(IJ)'S 0.0, 0.010000 = S(12) TO S(13) U(IJ)'S 0.0, 0.010000 = O(1) TO O(2) U(IJ)'S 0.0, 0.010000 = O(2) TO O(3) U(IJ)'S 0.0, 0.010000 = O(3) TO O(4) U(IJ)'S 0.0, 0.010000 = O(4) TO O(5) U(IJ)'S 0.0, 0.010000 = O(5) TO O(6) U(IJ)'S 0.0, 0.010000 = O(6) TO O(7) U(IJ)'S 0.0, 0.010000 = O(7) TO O(8) U(IJ)'S 0.0, 0.010000 = O(8) TO O(9) U(IJ)'S 0.0, 0.010000 = O(9) TO O(10) U(IJ)'S 0.0, 0.0050000 = O(10) TO O(11) U(IJ)'S 0.0, 0.0050000 = O(11) TO O(12) U(IJ)'S 0.0, 0.010000 = O(12) TO O(13) U(IJ)'S 0.0, 0.010000 = C(1) TO C(2) U(IJ)'S 0.0, 0.010000 = C(2) TO C(3) U(IJ)'S 0.0, 0.010000 = C(3) TO C(4) U(IJ)'S 0.0, 0.010000 = C(4) TO C(5) U(IJ)'S 0.0, 0.010000 = C(5) TO C(6) U(IJ)'S 0.0, 0.010000 = C(6) TO C(7) U(IJ)'S 0.0, 0.010000 = C(7) TO C(8) U(IJ)'S 0.0, 0.010000 = C(8) TO C(9) U(IJ)'S 0.0, 0.010000 = C(9) TO C(10) U(IJ)'S 0.0, 0.010000 = C(10) TO C(11) U(IJ)'S 0.0, 0.010000 = C(11) TO C(12) U(IJ)'S 0.0, 0.010000 = C(12) TO C(13) U(IJ)'S 0.0, 0.010000 = C(13) TO C(14) U(IJ)'S 0.0, 0.010000 = C(14) TO C(15) U(IJ)'S 0.0, 0.010000 = C(15) TO C(16) U(IJ)'S 0.0, 0.010000 = C(16) TO C(17) U(IJ)'S 0.0, 0.010000 = C(17) TO C(18) U(IJ)'S 0.0, 0.010000 = C(18) TO C(19) U(IJ)'S 0.0, 0.010000 = C(19) TO C(20) U(IJ)'S 0.0, 0.010000 = C(20) TO C(21) U(IJ)'S 0.0, 0.010000 = C(21) TO C(22) U(IJ)'S 0.0, 0.010000 = C(22) TO C(23) U(IJ)'S 0.0, 0.010000 = C(23) TO C(24) U(IJ)'S 0.0, 0.010000 = C(24) TO C(25) U(IJ)'S 0.0, 0.010000 = C(25) TO C(26) DISTANCE 1.800000 , 0.0050000 = C(18) TO S(9) DISTANCE 1.800000 , 0.0050000 = C(10) TO S(5) DISTANCE 1.800000 , 0.0050000 = C(23) TO S(12) DISTANCE 1.800000 , 0.0050000 = C(16) TO S(8) END ; #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 864818' #TrackingRef '- Combined CIFs_TbCuI-CEC-Jan 2012.cif' _audit_creation_date 11-01-31 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'smr265a in P m n a' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.4740(10) _cell_length_b 18.5970(10) _cell_length_c 12.222(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4426.3(8) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b n a ' _symmetry_space_group_name_Hall '-P 2ac 2b' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,z x,-y+1/2,-z -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C8 Cu2.50 I0.50 O4 # Dc = 1.15 Fooo = 2664.00 Mu = 30.79 M = 382.40 # Found Formula = C8 H24 I2.50 O4 S4 Tb0.50 # Dc = 2.13 FOOO = 2664.00 Mu = 54.93 M = 709.26 _chemical_formula_sum 'C16 H48 I5 O8 S8 Tb' _chemical_formula_moiety 'C16 H48 O8 S8 Tb, I3, 2(I)' _chemical_compound_source ? _chemical_formula_weight 1418.53 _cell_measurement_reflns_used 6773 _cell_measurement_theta_min 3.4453 _cell_measurement_theta_max 30.0387 _cell_measurement_temperature 110 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_min 0.266 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_max 0.481 _exptl_crystal_density_diffrn 2.129 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 5.493 # Sheldrick geometric approximatio 0.21 0.23 _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_T_max 0.374 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.4685 _diffrn_measurement_method '\w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _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 110 _diffrn_reflns_number 15199 _reflns_number_total 5276 _diffrn_reflns_av_R_equivalents 0.055 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5276 # Theoretical number of reflections is about 12404 _diffrn_reflns_theta_min 3.458 _diffrn_reflns_theta_max 29.560 _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 26.309 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min 0 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 2.10 _oxford_diffrn_Wilson_scale 0.25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -6.49 _refine_diff_density_max 4.81 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5276 _refine_ls_number_restraints 6 _refine_ls_number_parameters 174 _oxford_refine_ls_R_factor_ref 0.1141 _refine_ls_wR_factor_ref 0.1739 _refine_ls_goodness_of_fit_ref 1.0551 _refine_ls_shift/su_max 0.0003862 _refine_ls_shift/su_mean 0.0000249 # The values computed from all data _oxford_reflns_number_all 5276 _refine_ls_R_factor_all 0.1141 _refine_ls_wR_factor_all 0.1739 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4493 _refine_ls_R_factor_gt 0.1006 _refine_ls_wR_factor_gt 0.1689 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # 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: 0.295E+04 0.377E+04 0.217E+04 678. 93.9 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2006). Gemini User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Tb1 Tb 0.66503(5) 0.7500 1.0000 0.0170 1.0000 Uani S T . . . . O3 O 0.6238(6) 0.6485(6) 1.1033(9) 0.0227 1.0000 Uani . . . . . . S3 S 0.6008(3) 0.6483(3) 1.2215(4) 0.0370 1.0000 Uani . . . . . . C6 C 0.5240(10) 0.6023(19) 1.226(2) 0.0809 1.0000 Uani . U . . . . H63 H 0.4994 0.6099 1.1589 0.1210 1.0000 Uiso R . . . . . H62 H 0.4969 0.6191 1.2859 0.1210 1.0000 Uiso R . . . . . H61 H 0.5330 0.5519 1.2347 0.1210 1.0000 Uiso R . . . . . C5 C 0.6517(12) 0.587(2) 1.288(2) 0.0925 1.0000 Uani . U . . . . H53 H 0.6940 0.6096 1.3085 0.1380 1.0000 Uiso R . . . . . H52 H 0.6285 0.5697 1.3523 0.1380 1.0000 Uiso R . . . . . H51 H 0.6610 0.5467 1.2401 0.1380 1.0000 Uiso R . . . . . O4 O 0.5739(6) 0.7031(7) 0.8964(9) 0.0261 1.0000 Uani . . . . . . S4 S 0.5079(2) 0.6693(2) 0.9393(3) 0.0231 1.0000 Uani . . . . . . C8 C 0.5143(9) 0.5773(10) 0.9035(16) 0.0332 1.0000 Uani . . . . . . H83 H 0.5530 0.5559 0.9402 0.0500 1.0000 Uiso R . . . . . H82 H 0.5203 0.5726 0.8259 0.0501 1.0000 Uiso R . . . . . H81 H 0.4733 0.5525 0.9250 0.0500 1.0000 Uiso R . . . . . C7 C 0.4437(8) 0.6949(10) 0.8449(18) 0.0342 1.0000 Uani . . . . . . H73 H 0.4313 0.7441 0.8575 0.0510 1.0000 Uiso R . . . . . H72 H 0.4612 0.6897 0.7720 0.0510 1.0000 Uiso R . . . . . H71 H 0.4040 0.6648 0.8540 0.0510 1.0000 Uiso R . . . . . O2 O 0.7093(5) 0.7592(6) 1.1773(9) 0.0234 1.0000 Uani . . . . . . S2 S 0.7508(2) 0.8139(2) 1.2426(4) 0.0233 1.0000 Uani . . . . . . C4 C 0.7398(11) 0.7867(13) 1.3810(15) 0.0428 1.0000 Uani . . . . . . H43 H 0.7533 0.7373 1.3886 0.0640 1.0000 Uiso R . . . . . H42 H 0.7676 0.8162 1.4276 0.0640 1.0000 Uiso R . . . . . H41 H 0.6923 0.7917 1.4010 0.0639 1.0000 Uiso R . . . . . C3 C 0.7025(9) 0.8943(10) 1.2441(18) 0.0366 1.0000 Uani . . . . . . H33 H 0.6973 0.9118 1.1708 0.0550 1.0000 Uiso R . . . . . H32 H 0.7259 0.9297 1.2875 0.0550 1.0000 Uiso R . . . . . H31 H 0.6580 0.8851 1.2750 0.0550 1.0000 Uiso R . . . . . O1 O 0.7537(6) 0.8362(6) 1.0049(10) 0.0265 1.0000 Uani . . . . . . S1 S 0.7844(2) 0.8747(2) 0.9078(4) 0.0259 1.0000 Uani . . . . . . C2 C 0.8610(9) 0.8275(11) 0.8770(15) 0.0350 1.0000 Uani . . . . . . H23 H 0.8501 0.7811 0.8479 0.0520 1.0000 Uiso R . . . . . H22 H 0.8876 0.8219 0.9426 0.0520 1.0000 Uiso R . . . . . H21 H 0.8870 0.8542 0.8242 0.0519 1.0000 Uiso R . . . . . C1 C 0.8204(9) 0.9545(10) 0.9632(16) 0.0349 1.0000 Uani . . . . . . H13 H 0.7846 0.9889 0.9764 0.0530 1.0000 Uiso R . . . . . H12 H 0.8435 0.9440 1.0304 0.0529 1.0000 Uiso R . . . . . H11 H 0.8526 0.9745 0.9119 0.0530 1.0000 Uiso R . . . . . I1 I 0.53259(8) 0.7500 0.5000 0.0324 1.0000 Uani S T . . . . I2 I 0.52718(7) 0.90240(7) 0.43974(11) 0.0402 1.0000 Uani . . . . . . I3 I 0.34184(6) 0.58319(7) 1.07938(12) 0.0392 1.0000 Uani . . . . . . 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 Tb1 0.0144(4) 0.0195(5) 0.0169(5) 0.0018(4) 0.0000 0.0000 O3 0.020(5) 0.025(6) 0.022(6) 0.005(5) -0.006(5) -0.004(5) S3 0.038(2) 0.054(3) 0.019(2) 0.011(2) -0.0086(19) -0.023(2) C6 0.020(8) 0.17(2) 0.054(12) 0.033(16) 0.017(9) 0.000(12) C5 0.036(9) 0.18(2) 0.065(12) 0.048(16) 0.016(9) 0.008(13) O4 0.020(5) 0.038(7) 0.021(6) 0.006(5) 0.004(5) -0.007(5) S4 0.0177(18) 0.0264(19) 0.025(2) 0.0038(17) 0.0004(16) -0.0038(16) C8 0.030(9) 0.036(10) 0.033(10) -0.001(8) 0.000(8) 0.004(8) C7 0.020(8) 0.026(9) 0.056(13) 0.005(9) -0.002(8) -0.007(7) O2 0.024(5) 0.017(6) 0.029(6) 0.009(5) -0.007(5) -0.011(5) S2 0.0218(18) 0.031(2) 0.0173(19) -0.0006(17) -0.0010(15) -0.0033(17) C4 0.044(12) 0.064(14) 0.020(10) 0.002(10) 0.000(8) -0.008(11) C3 0.023(8) 0.043(11) 0.044(11) -0.023(10) 0.003(8) -0.005(8) O1 0.031(6) 0.031(6) 0.017(5) 0.005(5) 0.003(6) -0.001(5) S1 0.0209(19) 0.036(2) 0.021(2) 0.0126(18) -0.0015(16) -0.0041(17) C2 0.030(9) 0.051(12) 0.025(9) -0.009(9) 0.001(8) -0.002(9) C1 0.029(9) 0.036(10) 0.040(11) -0.004(8) 0.006(8) -0.006(8) I1 0.0206(7) 0.0360(9) 0.0406(10) -0.0112(8) 0.0000 0.0000 I2 0.0429(7) 0.0373(7) 0.0402(7) -0.0077(6) 0.0151(6) -0.0141(6) I3 0.0234(5) 0.0362(6) 0.0581(8) 0.0025(6) 0.0037(6) 0.0030(5) _refine_ls_extinction_coef 37(3) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 1.194(8) 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 Tb1 . O3 4_567 2.408(11) yes Tb1 . O1 4_567 2.357(11) yes Tb1 . O4 4_567 2.349(11) yes Tb1 . O2 4_567 2.338(11) yes Tb1 . O3 . 2.408(11) yes Tb1 . O4 . 2.349(11) yes Tb1 . O2 . 2.338(11) yes Tb1 . O1 . 2.357(11) yes O3 . S3 . 1.513(12) yes S3 . C6 . 1.72(2) yes S3 . C5 . 1.72(3) yes C6 . H63 . 0.956 no C6 . H62 . 0.958 no C6 . H61 . 0.959 no C5 . H53 . 0.961 no C5 . H52 . 0.961 no C5 . H51 . 0.963 no O4 . S4 . 1.524(11) yes S4 . C8 . 1.770(19) yes S4 . C7 . 1.766(19) yes C8 . H83 . 0.962 no C8 . H82 . 0.960 no C8 . H81 . 0.959 no C7 . H73 . 0.959 no C7 . H72 . 0.959 no C7 . H71 . 0.960 no O2 . S2 . 1.525(11) yes S2 . C4 . 1.778(19) yes S2 . C3 . 1.768(19) yes C4 . H43 . 0.960 no C4 . H42 . 0.959 no C4 . H41 . 0.960 no C3 . H33 . 0.959 no C3 . H32 . 0.960 no C3 . H31 . 0.959 no O1 . S1 . 1.509(12) yes S1 . C2 . 1.771(18) yes S1 . C1 . 1.776(18) yes C2 . H23 . 0.958 no C2 . H22 . 0.960 no C2 . H21 . 0.957 no C1 . H13 . 0.959 no C1 . H12 . 0.957 no C1 . H11 . 0.962 no I1 . I2 4_566 2.9302(14) yes I1 . I2 . 2.9302(14) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 4_567 Tb1 . O1 4_567 139.8(4) yes O3 4_567 Tb1 . O4 4_567 74.9(4) yes O1 4_567 Tb1 . O4 4_567 145.1(4) yes O3 4_567 Tb1 . O2 4_567 72.2(4) yes O1 4_567 Tb1 . O2 4_567 69.9(4) yes O4 4_567 Tb1 . O2 4_567 143.6(4) yes O3 4_567 Tb1 . O3 . 141.0(5) yes O1 4_567 Tb1 . O3 . 74.0(4) yes O4 4_567 Tb1 . O3 . 75.9(4) yes O2 4_567 Tb1 . O3 . 123.5(4) yes O3 4_567 Tb1 . O4 . 75.9(4) yes O1 4_567 Tb1 . O4 . 106.7(4) yes O4 4_567 Tb1 . O4 . 81.8(6) yes O2 4_567 Tb1 . O4 . 75.7(4) yes O3 . Tb1 . O4 . 74.9(4) yes O3 4_567 Tb1 . O2 . 123.5(4) yes O1 4_567 Tb1 . O2 . 78.6(4) yes O4 4_567 Tb1 . O2 . 75.7(4) yes O2 4_567 Tb1 . O2 . 136.7(5) yes O3 . Tb1 . O2 . 72.2(4) yes O3 4_567 Tb1 . O1 . 74.0(4) yes O1 4_567 Tb1 . O1 . 85.8(5) yes O4 4_567 Tb1 . O1 . 106.7(4) yes O2 4_567 Tb1 . O1 . 78.6(4) yes O3 . Tb1 . O1 . 139.8(4) yes O4 . Tb1 . O2 . 143.6(4) yes O4 . Tb1 . O1 . 145.1(4) yes O2 . Tb1 . O1 . 69.9(4) yes Tb1 . O3 . S3 . 127.0(7) yes O3 . S3 . C6 . 106.6(10) yes O3 . S3 . C5 . 106.3(11) yes C6 . S3 . C5 . 98.9(14) yes S3 . C6 . H63 . 109.6 no S3 . C6 . H62 . 109.7 no H63 . C6 . H62 . 109.4 no S3 . C6 . H61 . 109.3 no H63 . C6 . H61 . 109.5 no H62 . C6 . H61 . 109.3 no S3 . C5 . H53 . 108.8 no S3 . C5 . H52 . 109.5 no H53 . C5 . H52 . 109.6 no S3 . C5 . H51 . 109.6 no H53 . C5 . H51 . 109.9 no H52 . C5 . H51 . 109.4 no Tb1 . O4 . S4 . 127.3(7) yes O4 . S4 . C8 . 104.8(8) yes O4 . S4 . C7 . 105.1(8) yes C8 . S4 . C7 . 98.6(9) yes S4 . C8 . H83 . 109.8 no S4 . C8 . H82 . 109.9 no H83 . C8 . H82 . 109.1 no S4 . C8 . H81 . 109.8 no H83 . C8 . H81 . 109.1 no H82 . C8 . H81 . 109.2 no S4 . C7 . H73 . 109.4 no S4 . C7 . H72 . 109.2 no H73 . C7 . H72 . 109.5 no S4 . C7 . H71 . 109.7 no H73 . C7 . H71 . 109.5 no H72 . C7 . H71 . 109.5 no Tb1 . O2 . S2 . 136.8(6) yes O2 . S2 . C4 . 104.1(9) yes O2 . S2 . C3 . 106.7(7) yes C4 . S2 . C3 . 99.6(11) yes S2 . C4 . H43 . 109.4 no S2 . C4 . H42 . 109.5 no H43 . C4 . H42 . 109.6 no S2 . C4 . H41 . 109.4 no H43 . C4 . H41 . 109.4 no H42 . C4 . H41 . 109.6 no S2 . C3 . H33 . 109.5 no S2 . C3 . H32 . 109.4 no H33 . C3 . H32 . 109.5 no S2 . C3 . H31 . 109.5 no H33 . C3 . H31 . 109.4 no H32 . C3 . H31 . 109.5 no Tb1 . O1 . S1 . 126.3(7) yes O1 . S1 . C2 . 105.5(8) yes O1 . S1 . C1 . 104.7(8) yes C2 . S1 . C1 . 99.4(9) yes S1 . C2 . H23 . 109.8 no S1 . C2 . H22 . 109.3 no H23 . C2 . H22 . 109.3 no S1 . C2 . H21 . 109.4 no H23 . C2 . H21 . 109.5 no H22 . C2 . H21 . 109.5 no S1 . C1 . H13 . 109.6 no S1 . C1 . H12 . 109.9 no H13 . C1 . H12 . 109.5 no S1 . C1 . H11 . 109.4 no H13 . C1 . H11 . 109.0 no H12 . C1 . H11 . 109.4 no I2 4_566 I1 . I2 . 175.88(8) yes _iucr_refine_instruction_details_constraints ; # # Punched on 31/01/11 at 17:03:47 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 6,X'S) H ( 63,X'S) H ( 62,X'S) H ( 61,X'S) RIDE C ( 5,X'S) H ( 53,X'S) H ( 52,X'S) H ( 51,X'S) RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) H ( 81,X'S) RIDE C ( 7,X'S) H ( 73,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 4,X'S) H ( 43,X'S) H ( 42,X'S) H ( 41,X'S) RIDE C ( 3,X'S) H ( 33,X'S) H ( 32,X'S) H ( 31,X'S) RIDE C ( 2,X'S) H ( 23,X'S) H ( 22,X'S) H ( 21,X'S) RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 31/01/11 at 17:03:47 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = C(6) TO C(5) END ; #===END data_complex5 _database_code_depnum_ccdc_archive 'CCDC 864819' #TrackingRef '- Combined CIFs_TbCuI-CEC-Jan 2012.cif' _audit_creation_date 09-03-18 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'SMR147b in R-3c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.83(2) _cell_length_b 13.83(2) _cell_length_c 61.5(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 10187(84) _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' 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' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 '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' _cell_formula_units_Z 6 # Given Formula = C7.50 H1.00 Cu4.50 I7.00 N3 O4.50 Tb0.50 # Dc = 2.85 Fooo = 8028.00 Mu = 101.79 M = 486.29 # Found Formula = C9 H24 Cu4.50 I7 N3 O4.50 Tb0.50 # Dc = 2.93 FOOO = 8028.00 Mu = 101.83 M = 500.02 _chemical_formula_sum 'C18 H48 Cu9 I14 N6 O9 Tb' _chemical_formula_moiety 'C18 H48 N6 O9 Tb, Cu9 I14 ' _chemical_compound_source ? _chemical_formula_weight 3000.10 _cell_measurement_reflns_used 184 _cell_measurement_theta_min 3.1034 _cell_measurement_theta_max 29.4426 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 2.934 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 8028 _exptl_absorpt_coefficient_mu 10.183 # Sheldrick geometric approximatio 0.14 0.22 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.22 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Atlas (Gemini ultra Mo) ; _diffrn_detector_area_resol_mean 10.4685 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _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 2838 _reflns_number_total 2838 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 2838 # Number of reflections without Friedels Law is 5035 # Theoretical number of reflections is about 3160 _diffrn_reflns_theta_min 3.109 _diffrn_reflns_theta_max 29.535 _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 26.582 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 84 _reflns_limit_h_min -16 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 84 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.08 _refine_diff_density_max 2.39 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 1305 _refine_ls_number_restraints 8 _refine_ls_number_parameters 91 _oxford_refine_ls_R_factor_ref 0.0583 _refine_ls_wR_factor_ref 0.0671 _refine_ls_goodness_of_fit_ref 1.0930 _refine_ls_shift/su_max 0.004177 # The values computed from all data _oxford_reflns_number_all 2831 _refine_ls_R_factor_all 0.1156 _refine_ls_wR_factor_all 0.1363 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1457 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_gt 0.0709 # The Flack parameter was determined before Friedel pairs were merged _refine_ls_abs_structure_Flack . _refine_ls_abs_structure_details 'Flack (1983), 2197 Friedel-pairs' # 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 ad _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: 10.8 0.675 5.74 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Tb1 Tb 0.6667 0.3333 0.0833 0.0655 1.0000 Uani S T . . . . . I1 I 0.06139(10) -0.28787(11) 0.047091(19) 0.0732 1.0000 Uani . . . . . . . I3 I 0.0000 0.0000 0.13844(3) 0.0726 1.0000 Uani S T . . . . . I2 I 0.19594(10) 0.03384(9) 0.07882(2) 0.0751 1.0000 Uani . . . . . . . Cu2 Cu 0.0201(2) -0.10742(19) 0.10409(4) 0.0797 1.0000 Uani . . . . . . . Cu1 Cu 0.1525(2) -0.1808(2) 0.0833 0.0818 1.0000 Uani S T . . . . . O1 O 0.5533(18) 0.2074(16) 0.1111(3) 0.1279 1.0000 Uani . U . . . . . N1 N 0.4301(14) 0.1006(15) 0.1366(3) 0.0891 1.0000 Uani . . . . . . . C1 C 0.459(3) 0.158(2) 0.1189(5) 0.1260 1.0000 Uani . . . . . . . O2 O 0.666667(10) 0.1534(18) 0.083333(10) 0.1316 1.0000 Uani S TU . . . . . C2 C 0.319(2) 0.039(3) 0.1437(5) 0.1523 1.0000 Uani . . . . . . . C3 C 0.511(3) 0.086(3) 0.1483(4) 0.1696 1.0000 Uani . . . . . . . H11 H 0.4036 0.1631 0.1111 0.1560 1.0000 Uiso R . . . . . . H22 H 0.3037 -0.0336 0.1486 0.2010 1.0000 Uiso R . . . . . . H21 H 0.3076 0.0772 0.1555 0.2010 1.0000 Uiso R . . . . . . H23 H 0.2704 0.0303 0.1319 0.2010 1.0000 Uiso R . . . . . . H32 H 0.4727 0.0167 0.1561 0.2880 1.0000 Uiso R . . . . . . H33 H 0.5497 0.1462 0.1584 0.2880 1.0000 Uiso R . . . . . . H31 H 0.5627 0.0840 0.1383 0.2880 1.0000 Uiso R . . . . . . H34 H 0.6763 0.1279 0.0675 0.2072 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 Tb1 0.0524(7) 0.0524(7) 0.0916(14) 0.0000 0.0000 0.0262(3) I1 0.0691(8) 0.0851(9) 0.0740(7) -0.0124(6) -0.0116(6) 0.0449(7) I3 0.0714(8) 0.0714(8) 0.0749(12) 0.0000 0.0000 0.0357(4) I2 0.0647(7) 0.0524(6) 0.1109(10) 0.0095(6) 0.0211(6) 0.0314(6) Cu2 0.0768(15) 0.0682(14) 0.0968(16) 0.0017(12) 0.0015(12) 0.0383(12) Cu1 0.0798(16) 0.0798(16) 0.0810(19) -0.0033(9) 0.0033(9) 0.0362(18) O1 0.144(14) 0.124(10) 0.125(11) 0.011(8) 0.021(11) 0.074(10) N1 0.071(10) 0.091(12) 0.097(12) -0.015(10) -0.005(9) 0.034(9) C1 0.13(2) 0.12(2) 0.15(2) 0.043(19) 0.03(2) 0.072(19) O2 0.157(15) 0.123(10) 0.126(13) 0.007(6) 0.015(12) 0.079(7) C2 0.10(2) 0.17(3) 0.14(2) 0.04(2) 0.026(18) 0.03(2) C3 0.16(3) 0.30(5) 0.11(2) 0.07(3) 0.024(19) 0.16(3) _refine_ls_extinction_coef 80(10) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.490(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Tb1 . O2 34_544 2.49(3) yes Tb1 . O2 22_554 2.49(3) yes Tb1 . O1 22_554 2.38(2) yes Tb1 . O1 34_544 2.38(2) yes Tb1 . O1 28_654 2.38(2) yes Tb1 . O1 13_665 2.38(2) yes Tb1 . O1 7_655 2.38(2) yes Tb1 . O1 . 2.38(2) yes Tb1 . O2 . 2.49(3) yes I1 . Cu2 34_544 2.647(18) yes I1 . Cu1 . 2.624(17) yes I3 . Cu2 13_555 2.676(18) yes I3 . Cu2 7_555 2.676(18) yes I3 . Cu2 . 2.676(18) yes I2 . Cu2 7_555 2.679(18) yes I2 . Cu2 . 2.719(18) yes I2 . Cu1 . 2.733(18) yes Cu2 . Cu2 13_555 2.845(19) yes Cu2 . Cu2 7_555 2.845(19) yes Cu2 . Cu1 . 2.806(19) yes O1 . C1 . 1.23(3) yes N1 . C1 . 1.29(3) yes N1 . C2 . 1.40(3) yes N1 . C3 . 1.42(3) yes C1 . H11 . 0.930 no O2 . H34 28_654 1.069 no O2 . H34 . 1.069 no C2 . H22 . 0.960 no C2 . H21 . 0.959 no C2 . H23 . 0.960 no C3 . H32 . 0.959 no C3 . H33 . 0.960 no C3 . H31 . 0.960 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 34_544 Tb1 . O2 22_554 120.000(10) yes O2 34_544 Tb1 . O1 22_554 73.0(5) yes O2 22_554 Tb1 . O1 22_554 66.3(4) yes O2 34_544 Tb1 . O1 34_544 66.3(4) yes O2 22_554 Tb1 . O1 34_544 134.0(5) yes O1 22_554 Tb1 . O1 34_544 74.3(7) yes O2 34_544 Tb1 . O1 28_654 134.0(5) yes O2 22_554 Tb1 . O1 28_654 73.0(5) yes O1 22_554 Tb1 . O1 28_654 74.3(7) yes O1 34_544 Tb1 . O1 28_654 74.3(7) yes O2 34_544 Tb1 . O1 13_665 66.3(4) yes O2 22_554 Tb1 . O1 13_665 73.0(5) yes O1 22_554 Tb1 . O1 13_665 92.0(10) yes O1 34_544 Tb1 . O1 13_665 132.6(9) yes O1 28_654 Tb1 . O1 13_665 146.0(10) yes O2 34_544 Tb1 . O1 7_655 134.0(5) yes O2 22_554 Tb1 . O1 7_655 66.3(4) yes O1 22_554 Tb1 . O1 7_655 132.6(9) yes O1 34_544 Tb1 . O1 7_655 146.0(10) yes O1 28_654 Tb1 . O1 7_655 92.0(10) yes O2 34_544 Tb1 . O1 . 73.0(5) yes O2 22_554 Tb1 . O1 . 134.0(5) yes O1 22_554 Tb1 . O1 . 146.0(10) yes O1 34_544 Tb1 . O1 . 92.0(10) yes O1 28_654 Tb1 . O1 . 132.6(9) yes O2 34_544 Tb1 . O2 . 120.000(12) yes O2 22_554 Tb1 . O2 . 120.000(9) yes O1 22_554 Tb1 . O2 . 134.0(5) yes O1 34_544 Tb1 . O2 . 73.0(5) yes O1 28_654 Tb1 . O2 . 66.3(4) yes O1 13_665 Tb1 . O1 7_655 74.3(7) yes O1 13_665 Tb1 . O1 . 74.3(7) yes O1 7_655 Tb1 . O1 . 74.3(7) yes O1 13_665 Tb1 . O2 . 134.0(5) yes O1 7_655 Tb1 . O2 . 73.0(5) yes O1 . Tb1 . O2 . 66.3(4) yes Cu2 34_544 I1 . Cu1 . 64.33(6) yes Cu2 13_555 I3 . Cu2 7_555 64.23(9) yes Cu2 13_555 I3 . Cu2 . 64.23(9) yes Cu2 7_555 I3 . Cu2 . 64.23(9) yes Cu2 7_555 I2 . Cu2 . 63.60(10) yes Cu2 7_555 I2 . Cu1 . 124.13(7) yes Cu2 . I2 . Cu1 . 61.94(7) yes Cu2 13_555 Cu2 . Cu2 7_555 60.000(7) yes Cu2 13_555 Cu2 . I2 . 105.60(7) yes Cu2 7_555 Cu2 . I2 . 57.52(8) yes Cu2 13_555 Cu2 . I2 13_555 58.88(9) yes Cu2 7_555 Cu2 . I2 13_555 106.68(8) yes I2 . Cu2 . I2 13_555 107.20(10) yes Cu2 13_555 Cu2 . I3 . 57.88(5) yes Cu2 7_555 Cu2 . I3 . 57.88(5) yes I2 . Cu2 . I3 . 110.86(9) yes I2 13_555 Cu2 . I3 . 112.11(9) yes Cu2 13_555 Cu2 . I1 34_544 142.81(12) yes Cu2 7_555 Cu2 . I1 34_544 144.98(12) yes I2 . Cu2 . I1 34_544 111.59(9) yes I2 13_555 Cu2 . I1 34_544 108.33(9) yes I3 . Cu2 . I1 34_544 106.78(9) yes Cu2 13_555 Cu2 . Cu1 . 152.92(5) yes Cu2 7_555 Cu2 . Cu1 . 115.61(13) yes I2 . Cu2 . Cu1 . 59.27(8) yes I2 13_555 Cu2 . Cu1 . 101.86(10) yes I3 . Cu2 . Cu1 . 145.89(11) yes I1 34_544 Cu2 . Cu1 . 57.43(7) yes I2 . Cu1 . I2 34_544 98.45(12) yes I2 . Cu1 . Cu2 34_544 135.08(10) yes I2 34_544 Cu1 . Cu2 34_544 58.79(6) yes I2 . Cu1 . Cu2 . 58.79(6) yes I2 34_544 Cu1 . Cu2 . 135.08(10) yes Cu2 34_544 Cu1 . Cu2 . 163.28(17) yes I2 . Cu1 . I1 34_544 111.89(4) yes I2 34_544 Cu1 . I1 34_544 108.03(5) yes Cu2 34_544 Cu1 . I1 34_544 112.00(9) yes Cu2 . Cu1 . I1 34_544 58.23(6) yes I2 . Cu1 . I1 . 108.03(5) yes I2 34_544 Cu1 . I1 . 111.89(4) yes Cu2 34_544 Cu1 . I1 . 58.23(6) yes Cu2 . Cu1 . I1 . 112.00(9) yes I1 34_544 Cu1 . I1 . 117.02(14) yes Tb1 . O1 . C1 . 144.3(19) yes C1 . N1 . C2 . 123(2) yes C1 . N1 . C3 . 120(2) yes C2 . N1 . C3 . 117(2) yes N1 . C1 . O1 . 126(3) yes N1 . C1 . H11 . 118.3 no O1 . C1 . H11 . 116.1 no H34 28_654 O2 . Tb1 . 113.1 no H34 28_654 O2 . H34 . 133.8 no Tb1 . O2 . H34 . 113.1 no N1 . C2 . H22 . 109.9 no N1 . C2 . H21 . 109.5 no H22 . C2 . H21 . 109.4 no N1 . C2 . H23 . 109.1 no H22 . C2 . H23 . 109.4 no H21 . C2 . H23 . 109.5 no N1 . C3 . H32 . 108.7 no N1 . C3 . H33 . 110.3 no H32 . C3 . H33 . 109.5 no N1 . C3 . H31 . 109.4 no H32 . C3 . H31 . 109.4 no H33 . C3 . H31 . 109.5 no # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 227 47 ' ' 2 0.000 0.000 0.500 227 47 ' ' 3 0.333 0.667 0.167 226 46 ' ' 4 0.333 0.667 0.667 226 46 ' ' 5 0.667 0.333 0.333 226 46 ' ' 6 0.667 0.333 0.833 226 46 ' ' _platon_squeeze_details ; ; #===END