# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Shashank Mishra' 'Stephane Daniele' 'Erwan Jeanneau' 'G. Ledoux' _publ_contact_author_name 'Shashank Mishra' _publ_contact_author_email MISHRASHASHANK74@REDIFFMAIL.COM _publ_section_title ; Title: Lanthanide complexes in hybrid halometalate materials: Interconversion between a novel 2D microporous framework and a 1D zigzag chain structures of iodoargentates templated by octakis-solvated terbium(III) cation ; # Attachment 'Combined CIF_TbAgI.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 721195' _audit_creation_date 08-12-11 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'scale in P 21/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.39430(20) _cell_length_b 18.69510(40) _cell_length_c 17.68630(29) _cell_angle_alpha 90.0000 _cell_angle_beta 99.6061(12) _cell_angle_gamma 90.0000 _cell_volume 4040.677(128) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 = C24 H72 I4.50 O12 S12 Tb1.50 # Dc = 2.87 Fooo = 2240.00 Mu = 67.30 M = 1747.08 # Found Formula = C16 H48 I3 O8 S8 Tb1 # Dc = 1.91 FOOO = 2240.00 Mu = 44.87 M = 1164.72 _chemical_formula_sum 'C16 H48 I3 O8 S8 Tb1' _chemical_formula_moiety 'C16 H48 I3 O8 S8 Tb1' _chemical_compound_source ? _chemical_formula_weight 1164.72 _cell_measurement_reflns_used 35123 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.38 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_max 0.42 _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 4.487 # Sheldrick geometric approximatio 0.15 0.18 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.1519 _exptl_absorpt_correction_T_max 0.1818 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 17321 _reflns_number_total 9469 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections with Friedels Law is 9469 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9646 _diffrn_reflns_theta_min 1.597 _diffrn_reflns_theta_max 27.888 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.099 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _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 -3.06 _refine_diff_density_max 3.04 # 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 8085 _refine_ls_number_restraints 6 _refine_ls_number_parameters 326 _oxford_refine_ls_R_factor_ref 0.0402 _refine_ls_wR_factor_ref 0.0448 _refine_ls_goodness_of_fit_ref 1.0584 _refine_ls_shift/su_max 0.001107 # The values computed from all data _oxford_reflns_number_all 9440 _refine_ls_R_factor_all 0.0487 _refine_ls_wR_factor_all 0.0477 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8391 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_gt 0.0450 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.24 0.357 0.768 ; 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 C1 C 0.5903(7) 0.8718(4) 0.5508(4) 0.0604 1.0000 Uani . . . . . . . C2 C 0.5120(5) 0.9362(3) 0.4169(4) 0.0425 1.0000 Uani . . . . . . . C3 C 0.8561(5) 0.8992(3) 0.3943(4) 0.0430 1.0000 Uani . . . . . . . C4 C 0.9764(4) 0.7861(3) 0.3657(3) 0.0315 1.0000 Uani . . . . . . . C5 C 0.5730(7) 0.7590(4) 0.0703(4) 0.0565 1.0000 Uani . . . . . . . C6 C 0.6201(8) 0.8964(4) 0.1146(4) 0.0606 1.0000 Uani . . . . . . . C7 C 0.2082(5) 0.7699(4) 0.2777(5) 0.0553 1.0000 Uani . . . . . . . C8 C 0.2934(6) 0.8952(3) 0.2482(4) 0.0468 1.0000 Uani . . . . . . . C9 C 0.3945(4) 0.5621(3) 0.4403(3) 0.0323 1.0000 Uani . . . . . . . C10 C 0.3187(4) 0.6928(3) 0.4730(3) 0.0343 1.0000 Uani . . . . . . . C11 C 0.4986(5) 0.5572(3) 0.1441(4) 0.0411 1.0000 Uani . . . . . . . C12 C 0.3180(5) 0.5545(3) 0.2065(3) 0.0411 1.0000 Uani . . . . . . . C13 C 0.7100(11) 0.6432(8) 0.5425(5) 0.1084 1.0000 Uani . U . . . . . C14 C 0.8318(11) 0.5588(7) 0.4652(7) 0.1175 1.0000 Uani . U . . . . . C15 C 0.7984(4) 0.5517(3) 0.2194(3) 0.0359 1.0000 Uani . . . . . . . C16 C 0.8753(4) 0.6817(3) 0.1832(3) 0.0377 1.0000 Uani . . . . . . . S1 S 0.52396(11) 0.84816(7) 0.45652(8) 0.0357 1.0000 Uani . . . . . . . S2 S 0.84826(9) 0.80410(6) 0.39524(6) 0.0242 1.0000 Uani . . . . . . . S3 S 0.64149(12) 0.80824(8) 0.15004(8) 0.0386 1.0000 Uani . . . . . . . S4 S 0.32623(10) 0.80304(7) 0.24451(7) 0.0305 1.0000 Uani . . . . . . . S5 S 0.38158(9) 0.64970(7) 0.40128(7) 0.0287 1.0000 Uani . . . . . . . S6 S 0.40657(11) 0.61833(7) 0.17477(8) 0.0337 1.0000 Uani . . . . . . . S7 S 0.70969(14) 0.59880(9) 0.45793(9) 0.0439 1.0000 Uani . . . . . . . S8 S 0.80375(9) 0.64257(7) 0.25242(7) 0.0265 1.0000 Uani . . . . . . . O1 O 0.6146(3) 0.8132(2) 0.4207(2) 0.0323 1.0000 Uani . . . . . . . O2 O 0.7644(3) 0.78497(19) 0.32580(19) 0.0271 1.0000 Uani . . . . . . . O3 O 0.5676(3) 0.8022(2) 0.2100(2) 0.0376 1.0000 Uani . . . . . . . O4 O 0.4192(3) 0.7920(2) 0.3114(2) 0.0320 1.0000 Uani . . . . . . . O5 O 0.4992(3) 0.6779(2) 0.4140(2) 0.0345 1.0000 Uani . . . . . . . O6 O 0.4644(3) 0.6526(2) 0.2478(3) 0.0419 1.0000 Uani . . . . . . . O7 O 0.7108(3) 0.6544(2) 0.3963(2) 0.0409 1.0000 Uani . . . . . . . O8 O 0.6858(3) 0.66815(19) 0.23099(19) 0.0278 1.0000 Uani . . . . . . . Tb1 Tb 0.589965(16) 0.729505(11) 0.318547(12) 0.0193 1.0000 Uani . . . . . . . I3 I 0.72324(3) 0.578210(18) -0.016705(18) 0.0303 1.0000 Uani . . . . . . . I1 I 0.08507(3) 0.57209(2) 0.35091(3) 0.0408 1.0000 Uani . . . . . . . I2 I 0.54522(4) 0.40871(3) 0.32677(2) 0.0502 1.0000 Uani . . . . . . . H71 H 0.2109 0.7192 0.2796 0.0682 1.0000 Uiso R . . . . . . H72 H 0.2060 0.7883 0.3275 0.0682 1.0000 Uiso R . . . . . . H73 H 0.1446 0.7847 0.2436 0.0682 1.0000 Uiso R . . . . . . H81 H 0.3496 0.9228 0.2319 0.0571 1.0000 Uiso R . . . . . . H82 H 0.2873 0.9078 0.2994 0.0571 1.0000 Uiso R . . . . . . H83 H 0.2259 0.9043 0.2155 0.0571 1.0000 Uiso R . . . . . . H101 H 0.3061 0.7417 0.4599 0.0429 1.0000 Uiso R . . . . . . H102 H 0.3657 0.6894 0.5212 0.0429 1.0000 Uiso R . . . . . . H103 H 0.2510 0.6701 0.4762 0.0429 1.0000 Uiso R . . . . . . H91 H 0.4276 0.5318 0.4076 0.0403 1.0000 Uiso R . . . . . . H92 H 0.4388 0.5635 0.4896 0.0403 1.0000 Uiso R . . . . . . H93 H 0.3241 0.5442 0.4446 0.0403 1.0000 Uiso R . . . . . . H11 H 0.6033 0.8297 0.5811 0.0754 1.0000 Uiso R . . . . . . H12 H 0.6580 0.8946 0.5480 0.0754 1.0000 Uiso R . . . . . . H13 H 0.5450 0.9034 0.5736 0.0754 1.0000 Uiso R . . . . . . H21 H 0.4771 0.9338 0.3649 0.0532 1.0000 Uiso R . . . . . . H22 H 0.5829 0.9564 0.4195 0.0532 1.0000 Uiso R . . . . . . H23 H 0.4698 0.9652 0.4451 0.0532 1.0000 Uiso R . . . . . . H131 H 0.6418 0.6666 0.5413 0.1278 1.0000 Uiso R . . . . . . H132 H 0.7672 0.6777 0.5487 0.1278 1.0000 Uiso R . . . . . . H133 H 0.7217 0.6104 0.5841 0.1278 1.0000 Uiso R . . . . . . H141 H 0.8362 0.5327 0.4198 0.1416 1.0000 Uiso R . . . . . . H142 H 0.8872 0.5945 0.4725 0.1416 1.0000 Uiso R . . . . . . H143 H 0.8417 0.5272 0.5079 0.1416 1.0000 Uiso R . . . . . . H61 H 0.6540 0.9291 0.1523 0.0770 1.0000 Uiso R . . . . . . H62 H 0.6512 0.9014 0.0694 0.0770 1.0000 Uiso R . . . . . . H63 H 0.5439 0.9061 0.1033 0.0770 1.0000 Uiso R . . . . . . H51 H 0.5778 0.7093 0.0818 0.0708 1.0000 Uiso R . . . . . . H52 H 0.6056 0.7683 0.0264 0.0708 1.0000 Uiso R . . . . . . H53 H 0.4983 0.7730 0.0604 0.0708 1.0000 Uiso R . . . . . . H111 H 0.5542 0.5826 0.1244 0.0518 1.0000 Uiso R . . . . . . H112 H 0.5309 0.5286 0.1863 0.0518 1.0000 Uiso R . . . . . . H113 H 0.4603 0.5273 0.1051 0.0518 1.0000 Uiso R . . . . . . H121 H 0.2608 0.5787 0.2257 0.0517 1.0000 Uiso R . . . . . . H122 H 0.3582 0.5261 0.2460 0.0517 1.0000 Uiso R . . . . . . H123 H 0.2876 0.5247 0.1648 0.0517 1.0000 Uiso R . . . . . . H41 H 0.9866 0.7358 0.3631 0.0385 1.0000 Uiso R . . . . . . H42 H 1.0338 0.8062 0.4018 0.0385 1.0000 Uiso R . . . . . . H43 H 0.9769 0.8066 0.3167 0.0385 1.0000 Uiso R . . . . . . H31 H 0.7921 0.9188 0.4091 0.0538 1.0000 Uiso R . . . . . . H32 H 0.9186 0.9146 0.4291 0.0538 1.0000 Uiso R . . . . . . H33 H 0.8617 0.9151 0.3441 0.0538 1.0000 Uiso R . . . . . . H151 H 0.7615 0.5231 0.2514 0.0438 1.0000 Uiso R . . . . . . H152 H 0.8707 0.5342 0.2210 0.0438 1.0000 Uiso R . . . . . . H153 H 0.7601 0.5498 0.1682 0.0438 1.0000 Uiso R . . . . . . H161 H 0.8848 0.7314 0.1934 0.0473 1.0000 Uiso R . . . . . . H162 H 0.9448 0.6595 0.1861 0.0473 1.0000 Uiso R . . . . . . H163 H 0.8343 0.6751 0.1333 0.0473 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 0.079(5) 0.065(5) 0.042(3) -0.018(3) 0.023(3) 0.001(4) C2 0.037(3) 0.035(3) 0.058(4) -0.016(3) 0.015(3) -0.004(2) C3 0.047(3) 0.026(3) 0.058(4) -0.008(2) 0.014(3) -0.006(2) C4 0.022(2) 0.034(3) 0.037(3) -0.001(2) 0.0033(19) 0.0017(19) C5 0.079(5) 0.055(4) 0.038(3) -0.006(3) 0.017(3) -0.011(4) C6 0.088(6) 0.041(4) 0.055(4) 0.009(3) 0.020(4) 0.007(4) C7 0.023(3) 0.063(4) 0.079(5) 0.039(4) 0.004(3) 0.002(3) C8 0.054(4) 0.034(3) 0.049(3) 0.008(3) -0.001(3) 0.011(3) C9 0.030(2) 0.026(2) 0.041(3) 0.006(2) 0.008(2) 0.006(2) C10 0.031(2) 0.034(3) 0.040(3) 0.001(2) 0.013(2) 0.002(2) C11 0.038(3) 0.038(3) 0.050(3) -0.019(2) 0.015(2) -0.005(2) C12 0.038(3) 0.045(3) 0.043(3) -0.008(2) 0.012(2) -0.018(2) C13 0.124(8) 0.150(9) 0.056(5) 0.021(6) 0.028(5) 0.052(7) C14 0.137(8) 0.136(8) 0.090(6) 0.069(6) 0.050(6) 0.088(7) C15 0.029(2) 0.031(3) 0.047(3) -0.004(2) 0.003(2) 0.005(2) C16 0.027(2) 0.045(3) 0.043(3) -0.005(2) 0.012(2) -0.003(2) S1 0.0340(6) 0.0331(6) 0.0453(7) -0.0158(5) 0.0220(6) -0.0071(5) S2 0.0235(5) 0.0249(5) 0.0247(5) -0.0013(4) 0.0057(4) -0.0058(4) S3 0.0410(7) 0.0406(7) 0.0367(7) 0.0014(5) 0.0141(6) -0.0022(6) S4 0.0230(5) 0.0338(6) 0.0352(6) -0.0014(5) 0.0063(5) 0.0055(5) S5 0.0217(5) 0.0345(6) 0.0304(6) 0.0057(5) 0.0059(4) -0.0014(5) S6 0.0296(6) 0.0283(6) 0.0440(7) -0.0056(5) 0.0082(5) -0.0026(5) S7 0.0471(8) 0.0417(8) 0.0431(8) 0.0120(6) 0.0079(6) -0.0054(6) S8 0.0188(5) 0.0319(6) 0.0283(5) -0.0090(4) 0.0030(4) 0.0041(4) O1 0.0259(17) 0.0356(19) 0.0387(19) -0.0150(15) 0.0145(14) -0.0032(14) O2 0.0205(15) 0.0314(17) 0.0299(16) -0.0068(13) 0.0059(13) -0.0063(13) O3 0.043(2) 0.040(2) 0.0309(18) 0.0106(15) 0.0096(16) 0.0107(17) O4 0.0221(16) 0.0356(19) 0.0382(19) -0.0045(15) 0.0054(14) 0.0062(14) O5 0.0226(16) 0.044(2) 0.0378(19) 0.0062(16) 0.0072(14) -0.0070(15) O6 0.0273(18) 0.043(2) 0.057(2) -0.0237(19) 0.0120(17) -0.0122(16) O7 0.037(2) 0.047(2) 0.041(2) 0.0164(18) 0.0120(17) 0.0163(18) O8 0.0198(15) 0.0324(18) 0.0309(17) -0.0071(14) 0.0035(13) 0.0040(13) Tb1 0.01632(10) 0.01881(11) 0.02393(11) -0.00296(7) 0.00636(7) -0.00039(7) I3 0.03139(16) 0.03257(17) 0.02709(15) -0.00297(12) 0.00518(12) -0.00290(12) I1 0.02371(16) 0.03690(19) 0.0592(2) 0.00758(16) -0.00097(15) 0.00028(13) I2 0.0622(3) 0.0559(3) 0.02908(18) -0.00871(16) -0.00245(16) 0.0272(2) _refine_ls_extinction_coef 67(8) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2015(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 C1 . S1 . 1.788(7) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . S1 . 1.785(7) yes C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . S2 . 1.781(6) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C3 . H33 . 0.950 no C4 . S2 . 1.784(5) yes C4 . H41 . 0.950 no C4 . H42 . 0.950 no C4 . H43 . 0.950 no C5 . S3 . 1.777(7) yes C5 . H51 . 0.950 no C5 . H52 . 0.950 no C5 . H53 . 0.950 no C6 . S3 . 1.767(7) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . S4 . 1.775(6) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C7 . H73 . 0.950 no C8 . S4 . 1.774(6) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . S5 . 1.773(5) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . S5 . 1.788(5) yes C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . S6 . 1.763(6) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . S6 . 1.774(6) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . S7 . 1.710(11) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . S7 . 1.673(11) yes C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . S8 . 1.794(6) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C15 . H153 . 0.950 no C16 . S8 . 1.784(6) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no S1 . O1 . 1.525(3) yes S2 . O2 . 1.513(3) yes S3 . O3 . 1.517(4) yes S4 . O4 . 1.521(4) yes S5 . O5 . 1.531(4) yes S6 . O6 . 1.511(4) yes S7 . O7 . 1.508(4) yes S8 . O8 . 1.524(3) yes O1 . Tb1 . 2.372(3) yes O2 . Tb1 . 2.382(3) yes O3 . Tb1 . 2.330(4) yes O4 . Tb1 . 2.402(3) yes O5 . Tb1 . 2.383(4) yes O6 . Tb1 . 2.325(4) yes O7 . Tb1 . 2.327(4) yes O8 . Tb1 . 2.396(3) 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 . H11 . 109.2 no S1 . C1 . H12 . 109.6 no H11 . C1 . H12 . 109.5 no S1 . C1 . H13 . 109.7 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no S1 . C2 . H21 . 109.4 no S1 . C2 . H22 . 109.4 no H21 . C2 . H22 . 109.5 no S1 . C2 . H23 . 109.6 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no S2 . C3 . H31 . 109.4 no S2 . C3 . H32 . 109.6 no H31 . C3 . H32 . 109.5 no S2 . C3 . H33 . 109.4 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no S2 . C4 . H41 . 109.5 no S2 . C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no S2 . C4 . H43 . 109.4 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no S3 . C5 . H51 . 109.4 no S3 . C5 . H52 . 109.9 no H51 . C5 . H52 . 109.5 no S3 . C5 . H53 . 109.0 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no S3 . C6 . H61 . 109.2 no S3 . C6 . H62 . 109.4 no H61 . C6 . H62 . 109.5 no S3 . C6 . H63 . 109.7 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no S4 . C7 . H71 . 109.5 no S4 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no S4 . C7 . H73 . 109.4 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no S4 . C8 . H81 . 109.4 no S4 . C8 . H82 . 109.4 no H81 . C8 . H82 . 109.5 no S4 . C8 . H83 . 109.6 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no S5 . C9 . H91 . 109.6 no S5 . C9 . H92 . 109.4 no H91 . C9 . H92 . 109.5 no S5 . C9 . H93 . 109.4 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no S5 . C10 . H101 . 109.5 no S5 . C10 . H102 . 109.4 no H101 . C10 . H102 . 109.5 no S5 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no S6 . C11 . H111 . 109.5 no S6 . C11 . H112 . 109.3 no H111 . C11 . H112 . 109.5 no S6 . C11 . H113 . 109.5 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no S6 . C12 . H121 . 109.4 no S6 . C12 . H122 . 109.4 no H121 . C12 . H122 . 109.5 no S6 . C12 . H123 . 109.6 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no S7 . C13 . H131 . 109.4 no S7 . C13 . H132 . 108.9 no H131 . C13 . H132 . 109.5 no S7 . C13 . H133 . 110.0 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no S7 . C14 . H141 . 110.1 no S7 . C14 . H142 . 108.7 no H141 . C14 . H142 . 109.5 no S7 . C14 . H143 . 109.6 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no S8 . C15 . H151 . 109.6 no S8 . C15 . H152 . 109.4 no H151 . C15 . H152 . 109.5 no S8 . C15 . H153 . 109.4 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no S8 . C16 . H161 . 109.3 no S8 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no S8 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C1 . S1 . C2 . 97.7(3) yes C1 . S1 . O1 . 103.7(3) yes C2 . S1 . O1 . 104.5(2) yes C4 . S2 . C3 . 97.7(3) yes C4 . S2 . O2 . 104.0(2) yes C3 . S2 . O2 . 105.1(3) yes C5 . S3 . C6 . 100.3(4) yes C5 . S3 . O3 . 104.6(3) yes C6 . S3 . O3 . 104.2(3) yes C7 . S4 . C8 . 96.9(4) yes C7 . S4 . O4 . 104.8(3) yes C8 . S4 . O4 . 104.6(3) yes C10 . S5 . C9 . 99.3(3) yes C10 . S5 . O5 . 104.9(2) yes C9 . S5 . O5 . 103.8(2) yes C12 . S6 . C11 . 97.3(3) yes C12 . S6 . O6 . 104.2(3) yes C11 . S6 . O6 . 107.4(3) yes C13 . S7 . C14 . 106.2(7) yes C13 . S7 . O7 . 107.4(5) yes C14 . S7 . O7 . 104.3(4) yes C15 . S8 . C16 . 99.2(3) yes C15 . S8 . O8 . 103.5(2) yes C16 . S8 . O8 . 105.5(2) yes S1 . O1 . Tb1 . 126.1(2) yes S2 . O2 . Tb1 . 129.86(19) yes S3 . O3 . Tb1 . 128.1(2) yes S4 . O4 . Tb1 . 130.8(2) yes S5 . O5 . Tb1 . 125.9(2) yes S6 . O6 . Tb1 . 154.4(3) yes S7 . O7 . Tb1 . 139.5(2) yes S8 . O8 . Tb1 . 123.22(19) yes O4 . Tb1 . O8 . 136.57(12) yes O4 . Tb1 . O5 . 73.63(13) yes O8 . Tb1 . O5 . 127.43(14) yes O4 . Tb1 . O2 . 125.10(13) yes O8 . Tb1 . O2 . 72.52(12) yes O5 . Tb1 . O2 . 132.05(12) yes O4 . Tb1 . O1 . 73.71(13) yes O8 . Tb1 . O1 . 142.56(12) yes O5 . Tb1 . O1 . 75.11(13) yes O2 . Tb1 . O1 . 70.83(12) yes O4 . Tb1 . O3 . 71.96(13) yes O8 . Tb1 . O3 . 75.54(13) yes O5 . Tb1 . O3 . 144.49(13) yes O2 . Tb1 . O3 . 76.87(14) yes O1 . Tb1 . O3 . 103.06(15) yes O4 . Tb1 . O7 . 143.03(13) yes O8 . Tb1 . O7 . 75.73(13) yes O5 . Tb1 . O7 . 70.79(14) yes O2 . Tb1 . O7 . 75.04(14) yes O1 . Tb1 . O7 . 87.67(15) yes O4 . Tb1 . O6 . 76.54(14) yes O8 . Tb1 . O6 . 73.48(13) yes O5 . Tb1 . O6 . 77.20(14) yes O2 . Tb1 . O6 . 144.91(12) yes O1 . Tb1 . O6 . 143.86(12) yes O3 . Tb1 . O7 . 144.56(14) yes O3 . Tb1 . O6 . 86.54(16) yes O7 . Tb1 . O6 . 104.62(17) yes #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 721196' _audit_creation_date 08-12-11 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'scale in C 2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 22.41940(80) _cell_length_b 16.00380(50) _cell_length_c 11.70790(29) _cell_angle_alpha 90.0000 _cell_angle_beta 100.0558(19) _cell_angle_gamma 90.0000 _cell_volume 4136.212(224) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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 = C36 H48 I3 N12 O12 Tb1.50 # Dc = 2.34 Fooo = 2176.00 Mu = 48.70 M = 729.98 # Found Formula = C24 H56 I3 N8 O8 Tb1 # Dc = 1.81 FOOO = 2176.00 Mu = 39.96 M = 562.20 _chemical_formula_sum 'C24 H56 I3 N8 O8 Tb1' _chemical_formula_moiety 'C24 H56 I3 N8 O8 Tb1' _chemical_compound_source ? _chemical_formula_weight 1124.40 _cell_measurement_reflns_used 19065 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 3.996 # Sheldrick geometric approximatio 0.49 0.57 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4871 _exptl_absorpt_correction_T_max 0.5716 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9094 _reflns_number_total 4901 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 4901 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4928 _diffrn_reflns_theta_min 1.572 _diffrn_reflns_theta_max 27.865 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.307 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -29 _reflns_limit_h_max 28 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _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 -1.09 _refine_diff_density_max 1.94 # 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>3.0\s(I) _refine_ls_number_reflns 3797 _refine_ls_number_restraints 0 _refine_ls_number_parameters 201 _oxford_refine_ls_R_factor_ref 0.0330 _refine_ls_wR_factor_ref 0.0351 _refine_ls_goodness_of_fit_ref 1.0974 _refine_ls_shift/su_max 0.000805 # The values computed from all data _oxford_reflns_number_all 4884 _refine_ls_R_factor_all 0.0465 _refine_ls_wR_factor_all 0.0482 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3987 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_gt 0.0352 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.367 0.126 0.112 ; 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 C1 C 0.4494(2) 0.3835(3) 0.4333(4) 0.0246 1.0000 Uani . . . . . . . C2 C 0.4085(3) 0.4650(3) 0.5753(4) 0.0370 1.0000 Uani . . . . . . . C3 C 0.4209(2) 0.5262(3) 0.3853(4) 0.0313 1.0000 Uani . . . . . . . C4 C 0.6335(2) 0.3219(3) 0.4097(4) 0.0264 1.0000 Uani . . . . . . . C5 C 0.6545(3) 0.2789(3) 0.6116(4) 0.0367 1.0000 Uani . . . . . . . C6 C 0.7300(2) 0.3600(3) 0.5250(4) 0.0366 1.0000 Uani . . . . . . . C7 C 0.4571(2) 0.1179(3) 0.0354(4) 0.0270 1.0000 Uani . . . . . . . C8 C 0.4252(3) 0.0443(3) -0.1456(4) 0.0370 1.0000 Uani . . . . . . . C9 C 0.3890(4) 0.0019(5) 0.0345(6) 0.0709 1.0000 Uani . . . . . . . C10 C 0.3719(2) 0.1768(3) 0.3279(4) 0.0253 1.0000 Uani . . . . . . . C11 C 0.3455(2) 0.2236(3) 0.5081(4) 0.0316 1.0000 Uani . . . . . . . C12 C 0.2712(2) 0.1460(4) 0.3633(4) 0.0366 1.0000 Uani . . . . . . . Tb1 Tb 0.5000 0.251976(17) 0.2500 0.0185 1.0000 Uani S T . . . . . O3 O 0.45913(16) 0.1315(2) 0.1413(3) 0.0318 1.0000 Uani . . . . . . . N3 N 0.4257(2) 0.0581(3) -0.0225(3) 0.0318 1.0000 Uani . . . . . . . O2 O 0.58170(15) 0.2920(2) 0.3939(3) 0.0330 1.0000 Uani . . . . . . . N2 N 0.67098(18) 0.3194(2) 0.5099(3) 0.0270 1.0000 Uani . . . . . . . O4 O 0.42378(16) 0.2074(2) 0.3513(3) 0.0309 1.0000 Uani . . . . . . . N4 N 0.33213(17) 0.1793(2) 0.3976(3) 0.0241 1.0000 Uani . . . . . . . O1 O 0.46440(16) 0.3717(2) 0.3364(3) 0.0310 1.0000 Uani . . . . . . . N1 N 0.42916(18) 0.4557(2) 0.4648(3) 0.0249 1.0000 Uani . . . . . . . I1 I 0.5000 0.26069(3) 0.7500 0.0310 1.0000 Uani S T . . . . . I2 I 0.256997(16) 0.41599(2) 0.30370(3) 0.0346 1.0000 Uani . . . . . . . H71 H 0.4793 0.1524 -0.0059 0.0320 1.0000 Uiso R . . . . . . H82 H 0.3839 0.0445 -0.1862 0.0549 1.0000 Uiso R . . . . . . H81 H 0.4437 -0.0086 -0.1565 0.0548 1.0000 Uiso R . . . . . . H83 H 0.4477 0.0885 -0.1748 0.0549 1.0000 Uiso R . . . . . . H92 H 0.3500 -0.0051 -0.0132 0.1079 1.0000 Uiso R . . . . . . H91 H 0.4085 -0.0516 0.0469 0.1080 1.0000 Uiso R . . . . . . H93 H 0.3839 0.0253 0.1076 0.1079 1.0000 Uiso R . . . . . . H41 H 0.6478 0.3474 0.3471 0.0309 1.0000 Uiso R . . . . . . H62 H 0.7605 0.3229 0.5641 0.0530 1.0000 Uiso R . . . . . . H61 H 0.7396 0.3748 0.4509 0.0530 1.0000 Uiso R . . . . . . H63 H 0.7296 0.4093 0.5705 0.0535 1.0000 Uiso R . . . . . . H52 H 0.6563 0.3186 0.6736 0.0550 1.0000 Uiso R . . . . . . H51 H 0.6140 0.2575 0.5936 0.0552 1.0000 Uiso R . . . . . . H53 H 0.6821 0.2337 0.6366 0.0550 1.0000 Uiso R . . . . . . H101 H 0.3606 0.1502 0.2567 0.0300 1.0000 Uiso R . . . . . . H122 H 0.2585 0.1196 0.4293 0.0560 1.0000 Uiso R . . . . . . H121 H 0.2679 0.1044 0.3023 0.0547 1.0000 Uiso R . . . . . . H123 H 0.2434 0.1909 0.3386 0.0561 1.0000 Uiso R . . . . . . H112 H 0.3238 0.1976 0.5620 0.0502 1.0000 Uiso R . . . . . . H111 H 0.3881 0.2209 0.5382 0.0499 1.0000 Uiso R . . . . . . H113 H 0.3333 0.2808 0.4977 0.0498 1.0000 Uiso R . . . . . . H11 H 0.4530 0.3392 0.4867 0.0297 1.0000 Uiso R . . . . . . H22 H 0.4273 0.5126 0.6165 0.0569 1.0000 Uiso R . . . . . . H21 H 0.4184 0.4160 0.6218 0.0569 1.0000 Uiso R . . . . . . H23 H 0.3655 0.4729 0.5620 0.0567 1.0000 Uiso R . . . . . . H32 H 0.4302 0.5773 0.4283 0.0459 1.0000 Uiso R . . . . . . H31 H 0.4474 0.5208 0.3298 0.0459 1.0000 Uiso R . . . . . . H33 H 0.3796 0.5280 0.3454 0.0460 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 0.026(2) 0.023(2) 0.025(2) -0.0033(16) 0.0056(17) -0.0013(17) C2 0.058(3) 0.028(2) 0.026(2) -0.0047(19) 0.012(2) 0.004(2) C3 0.042(3) 0.025(2) 0.026(2) 0.0026(18) 0.006(2) 0.005(2) C4 0.032(2) 0.023(2) 0.024(2) -0.0029(16) 0.0014(18) 0.0024(18) C5 0.043(3) 0.039(3) 0.026(2) 0.005(2) 0.000(2) 0.000(2) C6 0.032(3) 0.045(3) 0.030(2) -0.008(2) -0.003(2) -0.003(2) C7 0.029(2) 0.023(2) 0.029(2) -0.0016(17) 0.0037(18) -0.0019(18) C8 0.049(3) 0.035(3) 0.024(2) -0.0088(19) 0.000(2) -0.002(2) C9 0.115(7) 0.061(4) 0.044(3) -0.023(3) 0.031(4) -0.052(4) C10 0.029(2) 0.025(2) 0.022(2) 0.0019(16) 0.0044(17) -0.0011(18) C11 0.036(3) 0.038(2) 0.024(2) -0.0056(19) 0.0139(19) -0.005(2) C12 0.028(2) 0.050(3) 0.033(3) -0.006(2) 0.007(2) -0.003(2) Tb1 0.02072(14) 0.01888(13) 0.01563(13) 0.0000 0.00277(10) 0.0000 O3 0.044(2) 0.0261(16) 0.0240(16) -0.0044(12) 0.0008(14) -0.0034(14) N3 0.043(2) 0.028(2) 0.0234(18) -0.0047(15) 0.0047(17) -0.0092(18) O2 0.0290(18) 0.0392(19) 0.0276(16) 0.0007(14) -0.0045(14) -0.0069(15) N2 0.030(2) 0.0268(19) 0.0230(18) -0.0019(14) 0.0021(15) 0.0021(16) O4 0.0343(18) 0.0351(18) 0.0261(16) -0.0036(13) 0.0133(14) -0.0071(15) N4 0.0254(18) 0.0267(19) 0.0205(17) 0.0019(14) 0.0046(14) 0.0016(15) O1 0.0417(19) 0.0239(15) 0.0305(17) -0.0047(13) 0.0148(15) 0.0028(14) N1 0.033(2) 0.0230(18) 0.0189(17) -0.0006(13) 0.0043(15) 0.0049(15) I1 0.0362(2) 0.0330(2) 0.0234(2) 0.0000 0.00419(17) 0.0000 I2 0.03924(18) 0.03427(18) 0.03103(16) -0.00172(12) 0.00782(13) -0.00507(13) _refine_ls_extinction_coef 5(2) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.07235(10) 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 . O1 . 1.253(5) yes C1 . N1 . 1.317(6) yes C1 . H11 . 0.939 no C2 . N1 . 1.456(6) yes C2 . H22 . 0.960 no C2 . H21 . 0.959 no C2 . H23 . 0.957 no C3 . N1 . 1.454(6) yes C3 . H32 . 0.964 no C3 . H31 . 0.958 no C3 . H33 . 0.962 no C4 . O2 . 1.241(6) yes C4 . N2 . 1.319(6) yes C4 . H41 . 0.942 no C5 . N2 . 1.459(6) yes C5 . H52 . 0.960 no C5 . H51 . 0.958 no C5 . H53 . 0.963 no C6 . N2 . 1.457(6) yes C6 . H62 . 0.959 no C6 . H61 . 0.960 no C6 . H63 . 0.953 no C7 . O3 . 1.252(5) yes C7 . N3 . 1.306(6) yes C7 . H71 . 0.932 no C8 . N3 . 1.457(6) yes C8 . H82 . 0.963 no C8 . H81 . 0.962 no C8 . H83 . 0.964 no C9 . N3 . 1.457(7) yes C9 . H92 . 0.957 no C9 . H91 . 0.962 no C9 . H93 . 0.959 no C10 . O4 . 1.248(5) yes C10 . N4 . 1.309(6) yes C10 . H101 . 0.932 no C11 . N4 . 1.460(6) yes C11 . H112 . 0.957 no C11 . H111 . 0.960 no C11 . H113 . 0.958 no C12 . N4 . 1.457(6) yes C12 . H122 . 0.967 no C12 . H121 . 0.970 no C12 . H123 . 0.961 no Tb1 . O3 5_655 2.402(3) yes Tb1 . O1 5_655 2.369(3) yes Tb1 . O4 5_655 2.355(3) yes Tb1 . O2 5_655 2.351(3) yes Tb1 . O3 . 2.402(3) yes Tb1 . O2 . 2.351(3) yes Tb1 . O4 . 2.355(3) yes Tb1 . O1 . 2.369(3) 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 . C1 . N1 . 123.0(4) yes O1 . C1 . H11 . 119.0 no N1 . C1 . H11 . 118.0 no N1 . C2 . H22 . 110.4 no N1 . C2 . H21 . 110.0 no H22 . C2 . H21 . 109.0 no N1 . C2 . H23 . 109.7 no H22 . C2 . H23 . 108.6 no H21 . C2 . H23 . 109.1 no N1 . C3 . H32 . 109.5 no N1 . C3 . H31 . 109.8 no H32 . C3 . H31 . 109.2 no N1 . C3 . H33 . 109.8 no H32 . C3 . H33 . 109.2 no H31 . C3 . H33 . 109.3 no O2 . C4 . N2 . 123.7(4) yes O2 . C4 . H41 . 119.2 no N2 . C4 . H41 . 117.1 no N2 . C5 . H52 . 109.8 no N2 . C5 . H51 . 110.1 no H52 . C5 . H51 . 108.5 no N2 . C5 . H53 . 109.9 no H52 . C5 . H53 . 109.1 no H51 . C5 . H53 . 109.4 no N2 . C6 . H62 . 109.8 no N2 . C6 . H61 . 110.0 no H62 . C6 . H61 . 109.3 no N2 . C6 . H63 . 109.8 no H62 . C6 . H63 . 108.8 no H61 . C6 . H63 . 109.1 no O3 . C7 . N3 . 124.3(4) yes O3 . C7 . H71 . 118.7 no N3 . C7 . H71 . 117.0 no N3 . C8 . H82 . 109.1 no N3 . C8 . H81 . 109.6 no H82 . C8 . H81 . 109.7 no N3 . C8 . H83 . 109.0 no H82 . C8 . H83 . 109.9 no H81 . C8 . H83 . 109.5 no N3 . C9 . H92 . 109.6 no N3 . C9 . H91 . 109.9 no H92 . C9 . H91 . 109.1 no N3 . C9 . H93 . 109.4 no H92 . C9 . H93 . 109.2 no H91 . C9 . H93 . 109.6 no O4 . C10 . N4 . 124.2(4) yes O4 . C10 . H101 . 118.2 no N4 . C10 . H101 . 117.6 no N4 . C11 . H112 . 108.9 no N4 . C11 . H111 . 109.9 no H112 . C11 . H111 . 109.1 no N4 . C11 . H113 . 110.0 no H112 . C11 . H113 . 109.4 no H111 . C11 . H113 . 109.5 no N4 . C12 . H122 . 109.4 no N4 . C12 . H121 . 113.6 no H122 . C12 . H121 . 107.1 no N4 . C12 . H123 . 109.7 no H122 . C12 . H123 . 107.5 no H121 . C12 . H123 . 109.3 no O3 5_655 Tb1 . O1 5_655 138.55(12) yes O3 5_655 Tb1 . O4 5_655 77.32(12) yes O1 5_655 Tb1 . O4 5_655 72.66(12) yes O3 5_655 Tb1 . O2 5_655 140.87(12) yes O1 5_655 Tb1 . O2 5_655 75.66(13) yes O4 5_655 Tb1 . O2 5_655 105.33(12) yes O3 5_655 Tb1 . O3 . 73.23(16) yes O1 5_655 Tb1 . O3 . 123.29(12) yes O4 5_655 Tb1 . O3 . 74.52(13) yes O2 5_655 Tb1 . O3 . 70.20(12) yes O3 5_655 Tb1 . O2 . 70.20(12) yes O1 5_655 Tb1 . O2 . 78.89(12) yes O4 5_655 Tb1 . O2 . 84.29(13) yes O2 5_655 Tb1 . O2 . 148.41(17) yes O3 . Tb1 . O2 . 140.87(12) yes O3 5_655 Tb1 . O4 . 74.52(12) yes O1 5_655 Tb1 . O4 . 142.02(12) yes O4 5_655 Tb1 . O4 . 144.73(17) yes O2 5_655 Tb1 . O4 . 84.29(13) yes O3 . Tb1 . O4 . 77.32(12) yes O3 5_655 Tb1 . O1 . 123.29(12) yes O1 5_655 Tb1 . O1 . 72.03(16) yes O4 5_655 Tb1 . O1 . 142.02(12) yes O2 5_655 Tb1 . O1 . 78.89(12) yes O3 . Tb1 . O1 . 138.55(12) yes O2 . Tb1 . O4 . 105.33(12) yes O2 . Tb1 . O1 . 75.66(13) yes O4 . Tb1 . O1 . 72.66(12) yes Tb1 . O3 . C7 . 127.5(3) yes C9 . N3 . C8 . 116.9(4) yes C9 . N3 . C7 . 120.8(4) yes C8 . N3 . C7 . 122.3(4) yes Tb1 . O2 . C4 . 143.5(3) yes C5 . N2 . C6 . 116.9(4) yes C5 . N2 . C4 . 121.8(4) yes C6 . N2 . C4 . 121.2(4) yes Tb1 . O4 . C10 . 137.7(3) yes C11 . N4 . C12 . 117.4(4) yes C11 . N4 . C10 . 120.6(4) yes C12 . N4 . C10 . 121.7(4) yes Tb1 . O1 . C1 . 132.2(3) yes C2 . N1 . C3 . 117.6(4) yes C2 . N1 . C1 . 121.2(4) yes C3 . N1 . C1 . 120.9(4) yes #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 721197' _audit_creation_date 08-07-08 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'scale in C 2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 42.80100(100) _cell_length_b 12.80720(20) _cell_length_c 18.62970(40) _cell_angle_alpha 90.0000 _cell_angle_beta 102.5088(9) _cell_angle_gamma 90.0000 _cell_volume 9969.668(354) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 '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 4 # Given Formula = C80 H100 Ag5 I22.50 O2.50 S40 Tb2.50 # Dc = 4.11 Fooo = 7280.00 Mu = 105.75 M = 3088.16 # Found Formula = C32 H96 Ag7 I13 O16 S16 Tb2 # Dc = 2.65 FOOO = 7280.00 Mu = 71.44 M = 1986.42 _chemical_formula_sum 'C32 H96 Ag7 I13 O16 S16 Tb2' _chemical_formula_moiety '2(C16 H48 O8 S8 Tb), Ag5 I8, Ag2 I5' _chemical_compound_source ? _chemical_formula_weight 3972.84 _cell_measurement_reflns_used 9597 _cell_measurement_theta_min 0.679 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.24 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.48 _exptl_crystal_density_diffrn 2.647 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 7280 _exptl_absorpt_coefficient_mu 7.144 # Sheldrick geometric approximatio 0.18 0.16 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1606 _exptl_absorpt_correction_T_max 0.1787 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 20717 _reflns_number_total 11718 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections with Friedels Law is 11718 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11908 _diffrn_reflns_theta_min 1.663 _diffrn_reflns_theta_max 27.903 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.950 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -56 _reflns_limit_h_max 54 _reflns_limit_k_min 0 _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 -2.08 _refine_diff_density_max 1.53 # 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 9092 _refine_ls_number_restraints 0 _refine_ls_number_parameters 394 _oxford_refine_ls_R_factor_ref 0.0340 _refine_ls_wR_factor_ref 0.0380 _refine_ls_goodness_of_fit_ref 1.0492 _refine_ls_shift/su_max 0.002397 # The values computed from all data _oxford_reflns_number_all 11678 _refine_ls_R_factor_all 0.0489 _refine_ls_wR_factor_all 0.0471 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9707 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_gt 0.0394 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.667 0.343 0.395 ; 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 C1 C 0.4531(3) 0.6857(10) 0.8157(6) 0.1070 1.0000 Uani . . . . . . . C2 C 0.4162(2) 0.8555(7) 0.8034(5) 0.0526 1.0000 Uani . . . . . . . C3 C 0.48480(18) 0.9510(6) 0.6292(5) 0.0484 1.0000 Uani . . . . . . . C4 C 0.45845(17) 0.9341(5) 0.4852(4) 0.0333 1.0000 Uani . . . . . . . C5 C 0.34499(17) 1.0359(5) 0.6716(4) 0.0358 1.0000 Uani . . . . . . . C6 C 0.37923(17) 1.1036(5) 0.5768(4) 0.0352 1.0000 Uani . . . . . . . C7 C 0.36445(18) 0.8008(5) 0.3401(3) 0.0339 1.0000 Uani . . . . . . . C8 C 0.35953(18) 1.0038(5) 0.3759(4) 0.0378 1.0000 Uani . . . . . . . C9 C 0.30387(18) 0.5773(6) 0.3794(4) 0.0426 1.0000 Uani . . . . . . . C10 C 0.28570(14) 0.7314(5) 0.4608(4) 0.0325 1.0000 Uani . . . . . . . C11 C 0.3314(3) 0.6057(6) 0.7140(5) 0.0617 1.0000 Uani . . . . . . . C12 C 0.29017(17) 0.7666(7) 0.6741(4) 0.0460 1.0000 Uani . . . . . . . C13 C 0.4464(2) 0.5687(7) 0.4032(5) 0.0500 1.0000 Uani . . . . . . . C14 C 0.47392(16) 0.5938(6) 0.5466(4) 0.0394 1.0000 Uani . . . . . . . C15 C 0.40154(18) 0.3865(6) 0.6677(5) 0.0468 1.0000 Uani . . . . . . . C16 C 0.37666(18) 0.3999(6) 0.5218(4) 0.0444 1.0000 Uani . . . . . . . S1 S 0.43672(5) 0.77922(16) 0.75027(9) 0.0419 1.0000 Uani . . . . . . . S2 S 0.44664(3) 0.93049(11) 0.57121(8) 0.0251 1.0000 Uani . . . . . . . S3 S 0.35884(3) 0.98777(10) 0.59464(8) 0.0218 1.0000 Uani . . . . . . . S4 S 0.35314(3) 0.87808(11) 0.40970(7) 0.0231 1.0000 Uani . . . . . . . S5 S 0.31463(3) 0.62762(11) 0.47070(8) 0.0228 1.0000 Uani . . . . . . . S6 S 0.33194(4) 0.73992(11) 0.69037(8) 0.0246 1.0000 Uani . . . . . . . S7 S 0.44649(4) 0.65997(11) 0.47559(8) 0.0260 1.0000 Uani . . . . . . . S8 S 0.40255(3) 0.47080(11) 0.59245(9) 0.0255 1.0000 Uani . . . . . . . O1 O 0.41135(11) 0.7187(3) 0.6971(2) 0.0308 1.0000 Uani . . . . . . . O2 O 0.43919(9) 0.8156(3) 0.5837(2) 0.0228 1.0000 Uani . . . . . . . O3 O 0.38482(9) 0.9093(3) 0.6276(2) 0.0219 1.0000 Uani . . . . . . . O4 O 0.38083(9) 0.8673(3) 0.4765(2) 0.0230 1.0000 Uani . . . . . . . O5 O 0.34661(9) 0.6815(3) 0.4732(2) 0.0227 1.0000 Uani . . . . . . . O6 O 0.33912(10) 0.7423(3) 0.6139(2) 0.0249 1.0000 Uani . . . . . . . O7 O 0.41385(9) 0.6435(3) 0.4948(2) 0.0241 1.0000 Uani . . . . . . . O8 O 0.38273(11) 0.5654(3) 0.6047(2) 0.0298 1.0000 Uani . . . . . . . Tb1 Tb 0.387371(6) 0.740866(18) 0.571654(13) 0.0150 1.0000 Uani . . . . . . . I2 I 0.5000 0.55048(4) 0.2500 0.0314 1.0000 Uani S T . . . . . I3 I 0.540749(10) 0.75384(3) 0.47282(2) 0.0281 1.0000 Uani . . . . . . . I4 I 0.805513(9) 0.82133(3) 0.66054(2) 0.0295 1.0000 Uani . . . . . . . I7 I 0.728626(10) 1.05371(3) 0.72245(2) 0.0298 1.0000 Uani . . . . . . . I5 I 0.734705(10) 0.96505(3) 0.47591(2) 0.0270 1.0000 Uani . . . . . . . I1 I 0.450274(9) 0.85228(3) 0.27405(2) 0.0299 1.0000 Uani . . . . . . . I6 I 0.691068(9) 0.74103(3) 0.60621(2) 0.0294 1.0000 Uani . . . . . . . Ag4 Ag 0.741369(14) 0.89797(4) 0.62704(3) 0.0372 1.0000 Uani . . . . . . . Ag3 Ag 0.755431(14) 0.66569(4) 0.64383(3) 0.0360 1.0000 Uani . . . . . . . Ag1 Ag 0.512919(14) 0.75085(4) 0.32620(3) 0.0381 1.0000 Uani . . . . . . . Ag2 Ag 0.77094(3) 0.76658(8) 0.51027(5) 0.0354 0.5000 Uani . . . . . . . H91 H 0.3179 0.5208 0.3736 0.0640 1.0000 Uiso R . . . . . . H92 H 0.3057 0.6313 0.3444 0.0640 1.0000 Uiso R . . . . . . H93 H 0.2821 0.5520 0.3694 0.0640 1.0000 Uiso R . . . . . . H101 H 0.2910 0.7783 0.5022 0.0470 1.0000 Uiso R . . . . . . H102 H 0.2856 0.7696 0.4166 0.0472 1.0000 Uiso R . . . . . . H103 H 0.2646 0.7030 0.4586 0.0472 1.0000 Uiso R . . . . . . H111 H 0.3530 0.5807 0.7289 0.1030 1.0000 Uiso R . . . . . . H112 H 0.3204 0.5976 0.7535 0.1030 1.0000 Uiso R . . . . . . H113 H 0.3204 0.5667 0.6718 0.1030 1.0000 Uiso R . . . . . . H121 H 0.2871 0.8382 0.6583 0.0712 1.0000 Uiso R . . . . . . H122 H 0.2829 0.7566 0.7190 0.0711 1.0000 Uiso R . . . . . . H123 H 0.2790 0.7205 0.6364 0.0710 1.0000 Uiso R . . . . . . H151 H 0.4143 0.4159 0.7120 0.0680 1.0000 Uiso R . . . . . . H152 H 0.4099 0.3191 0.6594 0.0680 1.0000 Uiso R . . . . . . H153 H 0.3799 0.3789 0.6735 0.0681 1.0000 Uiso R . . . . . . H161 H 0.3724 0.4415 0.4779 0.0650 1.0000 Uiso R . . . . . . H162 H 0.3872 0.3363 0.5125 0.0649 1.0000 Uiso R . . . . . . H163 H 0.3568 0.3839 0.5362 0.0651 1.0000 Uiso R . . . . . . H21 H 0.4073 0.9167 0.7756 0.0761 1.0000 Uiso R . . . . . . H22 H 0.4310 0.8773 0.8479 0.0763 1.0000 Uiso R . . . . . . H23 H 0.3994 0.8137 0.8161 0.0760 1.0000 Uiso R . . . . . . H11 H 0.4672 0.6412 0.7959 0.1380 1.0000 Uiso R . . . . . . H12 H 0.4649 0.7198 0.8592 0.1381 1.0000 Uiso R . . . . . . H13 H 0.4361 0.6445 0.8277 0.1381 1.0000 Uiso R . . . . . . H71 H 0.3676 0.7302 0.3566 0.0490 1.0000 Uiso R . . . . . . H72 H 0.3839 0.8285 0.3295 0.0493 1.0000 Uiso R . . . . . . H73 H 0.3478 0.8032 0.2964 0.0492 1.0000 Uiso R . . . . . . H81 H 0.3551 1.0556 0.4095 0.0552 1.0000 Uiso R . . . . . . H82 H 0.3815 1.0093 0.3718 0.0551 1.0000 Uiso R . . . . . . H83 H 0.3456 1.0134 0.3289 0.0549 1.0000 Uiso R . . . . . . H31 H 0.4828 0.9464 0.6793 0.0689 1.0000 Uiso R . . . . . . H32 H 0.4925 1.0189 0.6200 0.0691 1.0000 Uiso R . . . . . . H33 H 0.4993 0.8984 0.6201 0.0690 1.0000 Uiso R . . . . . . H41 H 0.4407 0.9139 0.4463 0.0500 1.0000 Uiso R . . . . . . H42 H 0.4649 1.0037 0.4763 0.0502 1.0000 Uiso R . . . . . . H43 H 0.4762 0.8872 0.4865 0.0501 1.0000 Uiso R . . . . . . H141 H 0.4750 0.6295 0.5923 0.0571 1.0000 Uiso R . . . . . . H142 H 0.4946 0.5947 0.5348 0.0571 1.0000 Uiso R . . . . . . H143 H 0.4672 0.5231 0.5504 0.0571 1.0000 Uiso R . . . . . . H131 H 0.4299 0.5876 0.3617 0.0801 1.0000 Uiso R . . . . . . H132 H 0.4667 0.5689 0.3893 0.0798 1.0000 Uiso R . . . . . . H133 H 0.4421 0.4998 0.4197 0.0799 1.0000 Uiso R . . . . . . H61 H 0.3910 1.0903 0.5392 0.0531 1.0000 Uiso R . . . . . . H62 H 0.3938 1.1254 0.6212 0.0531 1.0000 Uiso R . . . . . . H63 H 0.3638 1.1580 0.5605 0.0530 1.0000 Uiso R . . . . . . H51 H 0.3333 0.9814 0.6901 0.0531 1.0000 Uiso R . . . . . . H52 H 0.3631 1.0565 0.7095 0.0531 1.0000 Uiso R . . . . . . H53 H 0.3312 1.0946 0.6570 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 0.143(11) 0.092(8) 0.053(6) -0.037(6) -0.050(6) 0.092(8) C2 0.050(5) 0.053(5) 0.047(4) -0.024(4) -0.006(4) 0.015(4) C3 0.036(4) 0.049(4) 0.055(5) -0.011(4) 0.000(3) -0.029(3) C4 0.038(3) 0.027(3) 0.038(3) 0.001(3) 0.016(3) -0.004(3) C5 0.043(4) 0.034(3) 0.034(3) -0.007(3) 0.016(3) 0.014(3) C6 0.039(4) 0.018(3) 0.048(4) 0.010(3) 0.009(3) 0.001(2) C7 0.046(4) 0.036(3) 0.020(3) -0.001(2) 0.007(3) -0.005(3) C8 0.042(4) 0.032(3) 0.035(3) 0.013(3) -0.002(3) -0.004(3) C9 0.038(4) 0.050(4) 0.038(4) -0.017(3) 0.004(3) -0.018(3) C10 0.014(3) 0.037(3) 0.043(4) -0.001(3) 0.000(2) 0.000(2) C11 0.111(8) 0.032(4) 0.062(5) 0.019(4) 0.062(6) 0.014(4) C12 0.026(3) 0.073(5) 0.043(4) 0.003(4) 0.016(3) -0.004(3) C13 0.047(4) 0.053(5) 0.057(5) -0.017(4) 0.029(4) 0.005(4) C14 0.024(3) 0.037(4) 0.055(4) 0.011(3) 0.003(3) 0.007(3) C15 0.034(4) 0.044(4) 0.059(5) 0.028(4) 0.005(3) 0.006(3) C16 0.040(4) 0.038(4) 0.050(4) -0.018(3) 0.001(3) -0.003(3) S1 0.0415(10) 0.0532(11) 0.0276(8) -0.0069(7) 0.0003(7) -0.0060(8) S2 0.0195(6) 0.0213(6) 0.0351(7) -0.0062(5) 0.0075(5) -0.0047(5) S3 0.0201(6) 0.0196(6) 0.0240(6) -0.0023(5) 0.0011(5) 0.0040(5) S4 0.0198(6) 0.0266(7) 0.0214(6) 0.0043(5) 0.0012(5) -0.0001(5) S5 0.0177(6) 0.0249(6) 0.0242(6) 0.0008(5) 0.0012(5) -0.0050(5) S6 0.0266(7) 0.0252(7) 0.0242(6) -0.0003(5) 0.0101(5) 0.0006(5) S7 0.0267(7) 0.0215(6) 0.0336(7) -0.0007(5) 0.0150(6) 0.0023(5) S8 0.0196(6) 0.0181(6) 0.0370(7) 0.0026(5) 0.0023(5) -0.0012(5) O1 0.035(2) 0.026(2) 0.027(2) 0.0038(17) -0.0018(18) -0.0053(18) O2 0.0187(18) 0.0198(18) 0.030(2) 0.0004(15) 0.0044(15) -0.0021(15) O3 0.0246(19) 0.0180(18) 0.0225(18) 0.0002(14) 0.0038(15) -0.0002(15) O4 0.0226(19) 0.0237(19) 0.0205(18) 0.0027(15) -0.0002(15) -0.0034(15) O5 0.0180(18) 0.027(2) 0.0237(19) 0.0005(15) 0.0065(15) -0.0032(15) O6 0.027(2) 0.028(2) 0.0222(19) -0.0020(16) 0.0121(16) -0.0024(16) O7 0.0185(18) 0.025(2) 0.029(2) -0.0050(16) 0.0062(15) 0.0032(15) O8 0.042(2) 0.0155(18) 0.035(2) -0.0005(16) 0.0141(19) -0.0015(17) Tb1 0.01377(11) 0.01433(11) 0.01639(11) -0.00102(8) 0.00193(8) 0.00017(8) I2 0.0441(3) 0.0216(2) 0.0318(3) 0.0000 0.0153(2) 0.0000 I3 0.0302(2) 0.03065(19) 0.02239(17) 0.00173(14) 0.00353(14) 0.00220(15) I4 0.02336(18) 0.02433(18) 0.0389(2) 0.00256(15) 0.00279(15) 0.00002(14) I7 0.02987(19) 0.0334(2) 0.02515(18) -0.00883(15) 0.00363(15) -0.00018(16) I5 0.0327(2) 0.02585(18) 0.02238(17) 0.00053(14) 0.00580(14) 0.00202(15) I1 0.02052(17) 0.0381(2) 0.03021(19) -0.00933(16) 0.00353(14) 0.00017(15) I6 0.02378(18) 0.02716(19) 0.0343(2) -0.00125(15) -0.00021(15) -0.00154(14) Ag4 0.0462(3) 0.0319(2) 0.0332(2) -0.0022(2) 0.0082(2) 0.0078(2) Ag3 0.0460(3) 0.0308(2) 0.0308(2) 0.00543(19) 0.0074(2) 0.0065(2) Ag1 0.0449(3) 0.0423(3) 0.0242(2) -0.0010(2) 0.0009(2) 0.0004(2) Ag2 0.0476(6) 0.0332(5) 0.0257(4) 0.0030(4) 0.0084(4) 0.0070(4) _refine_ls_extinction_coef 21(3) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.03799(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 . S1 . 1.744(10) yes C1 . H11 . 0.960 no C1 . H12 . 0.962 no C1 . H13 . 0.963 no C2 . S1 . 1.756(8) yes C2 . H21 . 0.971 no C2 . H22 . 0.969 no C2 . H23 . 0.966 no C3 . S2 . 1.772(7) yes C3 . H31 . 0.958 no C3 . H32 . 0.958 no C3 . H33 . 0.957 no C4 . S2 . 1.782(7) yes C4 . H41 . 0.965 no C4 . H42 . 0.959 no C4 . H43 . 0.963 no C5 . S3 . 1.776(6) yes C5 . H51 . 0.964 no C5 . H52 . 0.965 no C5 . H53 . 0.958 no C6 . S3 . 1.788(6) yes C6 . H61 . 0.962 no C6 . H62 . 0.963 no C6 . H63 . 0.964 no C7 . S4 . 1.780(7) yes C7 . H71 . 0.955 no C7 . H72 . 0.962 no C7 . H73 . 0.959 no C8 . S4 . 1.771(7) yes C8 . H81 . 0.958 no C8 . H82 . 0.963 no C8 . H83 . 0.956 no C9 . S5 . 1.783(7) yes C9 . H91 . 0.963 no C9 . H92 . 0.965 no C9 . H93 . 0.966 no C10 . S5 . 1.799(6) yes C10 . H101 . 0.964 no C10 . H102 . 0.957 no C10 . H103 . 0.964 no C11 . S6 . 1.776(8) yes C11 . H111 . 0.962 no C11 . H112 . 0.962 no C11 . H113 . 0.963 no C12 . S6 . 1.780(7) yes C12 . H121 . 0.963 no C12 . H122 . 0.962 no C12 . H123 . 0.962 no C13 . S7 . 1.784(8) yes C13 . H131 . 0.959 no C13 . H132 . 0.958 no C13 . H133 . 0.965 no C14 . S7 . 1.781(7) yes C14 . H141 . 0.959 no C14 . H142 . 0.958 no C14 . H143 . 0.958 no C15 . S8 . 1.778(7) yes C15 . H151 . 0.962 no C15 . H152 . 0.960 no C15 . H153 . 0.961 no C16 . S8 . 1.775(7) yes C16 . H161 . 0.960 no C16 . H162 . 0.966 no C16 . H163 . 0.965 no S1 . O1 . 1.515(5) yes S2 . O2 . 1.534(4) yes S3 . O3 . 1.526(4) yes S4 . O4 . 1.527(4) yes S5 . O5 . 1.524(4) yes S6 . O6 . 1.522(4) yes S7 . O7 . 1.530(4) yes S8 . O8 . 1.524(4) yes O1 . Tb1 . 2.358(4) yes O2 . Tb1 . 2.381(4) yes O3 . Tb1 . 2.408(4) yes O4 . Tb1 . 2.372(4) yes O5 . Tb1 . 2.366(4) yes O6 . Tb1 . 2.364(4) yes O7 . Tb1 . 2.365(4) yes O8 . Tb1 . 2.350(4) yes I2 . Ag1 5_655 2.9267(12) yes I2 . Ag1 . 2.9267(12) yes I3 . Ag1 . 2.7336(9) yes I4 . Ag4 . 2.8544(7) yes I4 . Ag3 . 2.8942(9) yes I4 . Ag2 . 2.9536(13) yes I7 . Ag3 7_656 2.8271(9) yes I7 . Ag4 . 2.8027(9) yes I5 . Ag2 4_666 2.9919(16) yes I5 . Ag3 4_666 2.8924(9) yes I5 . Ag4 . 2.8980(10) yes I5 . Ag2 . 2.9743(14) yes I1 . Ag1 5_655 2.9886(8) yes I1 . Ag1 . 2.9483(8) yes I6 . Ag2 4_666 2.9817(12) yes I6 . Ag4 . 2.9092(9) yes I6 . Ag3 . 2.8592(8) yes Ag4 . Ag2 4_666 3.2677(14) yes Ag4 . Ag3 . 3.0378(13) yes Ag4 . Ag2 . 3.2186(13) yes Ag3 . Ag2 4_666 2.9773(13) yes Ag3 . Ag2 . 3.0028(13) yes Ag1 . Ag1 5_655 2.8149(12) yes Ag2 . Ag2 4_666 1.801(2) 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 . H11 . 109.3 no S1 . C1 . H12 . 109.6 no H11 . C1 . H12 . 109.6 no S1 . C1 . H13 . 109.2 no H11 . C1 . H13 . 109.4 no H12 . C1 . H13 . 109.8 no S1 . C2 . H21 . 109.5 no S1 . C2 . H22 . 109.2 no H21 . C2 . H22 . 109.5 no S1 . C2 . H23 . 108.7 no H21 . C2 . H23 . 110.5 no H22 . C2 . H23 . 109.5 no S2 . C3 . H31 . 108.7 no S2 . C3 . H32 . 109.3 no H31 . C3 . H32 . 109.7 no S2 . C3 . H33 . 109.6 no H31 . C3 . H33 . 109.2 no H32 . C3 . H33 . 110.3 no S2 . C4 . H41 . 109.7 no S2 . C4 . H42 . 109.2 no H41 . C4 . H42 . 109.2 no S2 . C4 . H43 . 109.6 no H41 . C4 . H43 . 109.9 no H42 . C4 . H43 . 109.2 no S3 . C5 . H51 . 109.1 no S3 . C5 . H52 . 109.3 no H51 . C5 . H52 . 109.4 no S3 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.9 no S3 . C6 . H61 . 110.1 no S3 . C6 . H62 . 109.4 no H61 . C6 . H62 . 109.4 no S3 . C6 . H63 . 109.2 no H61 . C6 . H63 . 109.3 no H62 . C6 . H63 . 109.5 no S4 . C7 . H71 . 109.5 no S4 . C7 . H72 . 109.1 no H71 . C7 . H72 . 110.2 no S4 . C7 . H73 . 109.3 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.3 no S4 . C8 . H81 . 109.3 no S4 . C8 . H82 . 108.9 no H81 . C8 . H82 . 109.7 no S4 . C8 . H83 . 109.3 no H81 . C8 . H83 . 109.6 no H82 . C8 . H83 . 110.0 no S5 . C9 . H91 . 109.9 no S5 . C9 . H92 . 110.1 no H91 . C9 . H92 . 108.5 no S5 . C9 . H93 . 110.1 no H91 . C9 . H93 . 109.1 no H92 . C9 . H93 . 109.2 no S5 . C10 . H101 . 109.9 no S5 . C10 . H102 . 109.9 no H101 . C10 . H102 . 109.1 no S5 . C10 . H103 . 110.0 no H101 . C10 . H103 . 108.9 no H102 . C10 . H103 . 108.9 no S6 . C11 . H111 . 109.3 no S6 . C11 . H112 . 109.2 no H111 . C11 . H112 . 110.1 no S6 . C11 . H113 . 109.3 no H111 . C11 . H113 . 109.4 no H112 . C11 . H113 . 109.6 no S6 . C12 . H121 . 107.4 no S6 . C12 . H122 . 109.2 no H121 . C12 . H122 . 110.2 no S6 . C12 . H123 . 109.2 no H121 . C12 . H123 . 110.4 no H122 . C12 . H123 . 110.5 no S7 . C13 . H131 . 109.0 no S7 . C13 . H132 . 110.4 no H131 . C13 . H132 . 109.5 no S7 . C13 . H133 . 109.1 no H131 . C13 . H133 . 109.2 no H132 . C13 . H133 . 109.6 no S7 . C14 . H141 . 109.2 no S7 . C14 . H142 . 108.5 no H141 . C14 . H142 . 109.4 no S7 . C14 . H143 . 110.1 no H141 . C14 . H143 . 110.0 no H142 . C14 . H143 . 109.7 no S8 . C15 . H151 . 109.5 no S8 . C15 . H152 . 110.2 no H151 . C15 . H152 . 109.3 no S8 . C15 . H153 . 109.8 no H151 . C15 . H153 . 108.9 no H152 . C15 . H153 . 109.2 no S8 . C16 . H161 . 108.7 no S8 . C16 . H162 . 108.9 no H161 . C16 . H162 . 108.9 no S8 . C16 . H163 . 110.4 no H161 . C16 . H163 . 109.8 no H162 . C16 . H163 . 110.1 no C2 . S1 . C1 . 99.4(5) yes C2 . S1 . O1 . 106.1(3) yes C1 . S1 . O1 . 103.2(5) yes C4 . S2 . C3 . 98.1(4) yes C4 . S2 . O2 . 105.7(3) yes C3 . S2 . O2 . 104.1(3) yes C6 . S3 . C5 . 97.2(3) yes C6 . S3 . O3 . 106.2(3) yes C5 . S3 . O3 . 104.2(3) yes C7 . S4 . C8 . 99.2(3) yes C7 . S4 . O4 . 104.9(3) yes C8 . S4 . O4 . 102.7(3) yes C10 . S5 . C9 . 98.0(4) yes C10 . S5 . O5 . 105.2(3) yes C9 . S5 . O5 . 103.8(3) yes C12 . S6 . C11 . 99.3(5) yes C12 . S6 . O6 . 103.6(3) yes C11 . S6 . O6 . 105.5(3) yes C13 . S7 . C14 . 98.2(4) yes C13 . S7 . O7 . 103.5(3) yes C14 . S7 . O7 . 104.4(3) yes C15 . S8 . C16 . 99.0(4) yes C15 . S8 . O8 . 104.8(3) yes C16 . S8 . O8 . 103.8(3) yes S1 . O1 . Tb1 . 133.1(3) yes S2 . O2 . Tb1 . 126.2(2) yes S3 . O3 . Tb1 . 120.9(2) yes S4 . O4 . Tb1 . 128.0(2) yes S5 . O5 . Tb1 . 132.5(2) yes S6 . O6 . Tb1 . 132.8(2) yes S7 . O7 . Tb1 . 130.6(2) yes S8 . O8 . Tb1 . 129.8(3) yes O3 . Tb1 . O2 . 74.20(13) yes O3 . Tb1 . O4 . 72.75(13) yes O2 . Tb1 . O4 . 75.70(13) yes O3 . Tb1 . O5 . 121.90(13) yes O2 . Tb1 . O5 . 135.87(13) yes O4 . Tb1 . O5 . 72.07(13) yes O3 . Tb1 . O7 . 143.79(14) yes O2 . Tb1 . O7 . 73.17(14) yes O4 . Tb1 . O7 . 84.34(14) yes O5 . Tb1 . O7 . 74.39(13) yes O3 . Tb1 . O6 . 74.00(14) yes O2 . Tb1 . O6 . 145.94(14) yes O4 . Tb1 . O6 . 105.88(14) yes O5 . Tb1 . O6 . 73.13(14) yes O7 . Tb1 . O6 . 140.66(14) yes O3 . Tb1 . O1 . 74.28(14) yes O2 . Tb1 . O1 . 75.99(15) yes O4 . Tb1 . O1 . 141.13(14) yes O5 . Tb1 . O1 . 145.02(14) yes O7 . Tb1 . O1 . 111.98(15) yes O3 . Tb1 . O8 . 136.79(14) yes O2 . Tb1 . O8 . 119.30(15) yes O4 . Tb1 . O8 . 147.71(14) yes O5 . Tb1 . O8 . 78.79(15) yes O7 . Tb1 . O8 . 74.52(15) yes O6 . Tb1 . O1 . 83.97(16) yes O6 . Tb1 . O8 . 77.91(15) yes O1 . Tb1 . O8 . 70.66(15) yes Ag1 5_655 I2 . Ag1 . 57.49(3) yes Ag4 . I4 . Ag3 . 63.80(2) yes Ag4 . I4 . Ag2 . 67.28(3) yes Ag3 . I4 . Ag2 . 61.78(3) yes Ag3 7_656 I7 . Ag4 . 151.27(2) yes Ag2 4_666 I5 . Ag3 4_666 61.34(2) yes Ag2 4_666 I5 . Ag4 . 67.37(3) yes Ag3 4_666 I5 . Ag4 . 125.28(3) yes Ag2 4_666 I5 . Ag2 . 35.14(4) yes Ag3 4_666 I5 . Ag2 . 60.98(3) yes Ag4 . I5 . Ag2 . 66.46(3) yes Ag1 5_655 I1 . Ag1 . 56.60(2) yes Ag2 4_666 I6 . Ag4 . 67.37(3) yes Ag2 4_666 I6 . Ag3 . 61.25(3) yes Ag4 . I6 . Ag3 . 63.55(3) yes Ag2 4_666 Ag4 . I6 . 57.37(3) yes Ag2 4_666 Ag4 . I5 . 57.68(3) yes I6 . Ag4 . I5 . 99.26(2) yes Ag2 4_666 Ag4 . I4 . 86.21(3) yes I6 . Ag4 . I4 . 116.14(3) yes I5 . Ag4 . I4 . 101.65(2) yes Ag2 4_666 Ag4 . I7 . 159.20(3) yes I6 . Ag4 . I7 . 109.65(3) yes I5 . Ag4 . I7 . 114.42(2) yes I4 . Ag4 . I7 . 114.59(3) yes Ag2 4_666 Ag4 . Ag3 . 56.21(3) yes I6 . Ag4 . Ag3 . 57.42(3) yes I5 . Ag4 . Ag3 . 111.47(3) yes I4 . Ag4 . Ag3 . 58.74(2) yes I7 . Ag4 . Ag3 . 133.87(3) yes Ag2 4_666 Ag4 . Ag2 . 32.23(4) yes I6 . Ag4 . Ag2 . 86.37(3) yes I5 . Ag4 . Ag2 . 57.91(3) yes I4 . Ag4 . Ag2 . 57.83(2) yes I7 . Ag4 . Ag2 . 163.69(3) yes Ag3 . Ag4 . Ag2 . 57.28(2) yes I4 . Ag3 . I5 4_666 104.67(3) yes I4 . Ag3 . I6 . 116.47(3) yes I5 4_666 Ag3 . I6 . 107.47(3) yes I4 . Ag3 . Ag4 . 57.47(3) yes I5 4_666 Ag3 . Ag4 . 123.11(3) yes I6 . Ag3 . Ag4 . 59.03(2) yes I4 . Ag3 . I7 7_646 102.87(2) yes I5 4_666 Ag3 . I7 7_646 109.77(3) yes I6 . Ag3 . I7 7_646 115.02(2) yes Ag4 . Ag3 . I7 7_646 126.31(2) yes I4 . Ag3 . Ag2 4_666 91.17(4) yes I5 4_666 Ag3 . Ag2 4_666 60.87(3) yes I6 . Ag3 . Ag2 4_666 61.41(3) yes Ag4 . Ag3 . Ag2 4_666 65.80(3) yes I7 7_646 Ag3 . Ag2 4_666 165.07(3) yes I4 . Ag3 . Ag2 . 60.08(3) yes I5 4_666 Ag3 . Ag2 . 60.96(3) yes I6 . Ag3 . Ag2 . 91.49(3) yes Ag4 . Ag3 . Ag2 . 64.39(2) yes I7 7_646 Ag3 . Ag2 . 153.38(3) yes Ag2 4_666 Ag3 . Ag2 . 35.05(4) yes I1 5_655 Ag1 . I1 . 99.64(3) yes I1 5_655 Ag1 . I2 . 98.50(3) yes I1 . Ag1 . I2 . 99.42(3) yes I1 5_655 Ag1 . I3 . 116.35(3) yes I1 . Ag1 . I3 . 119.44(2) yes I2 . Ag1 . I3 . 119.51(3) yes I1 5_655 Ag1 . Ag1 5_655 60.98(3) yes I1 . Ag1 . Ag1 5_655 62.42(2) yes I2 . Ag1 . Ag1 5_655 61.26(3) yes I3 . Ag1 . Ag1 5_655 177.25(4) yes Ag4 4_666 Ag2 . Ag4 . 147.77(4) yes Ag4 4_666 Ag2 . I5 4_666 54.94(3) yes Ag4 . Ag2 . I5 4_666 114.16(4) yes Ag4 4_666 Ag2 . I6 4_666 55.26(3) yes Ag4 . Ag2 . I6 4_666 149.92(4) yes I5 4_666 Ag2 . I6 4_666 95.58(4) yes Ag4 4_666 Ag2 . I5 . 113.24(4) yes Ag4 . Ag2 . I5 . 55.64(3) yes I5 4_666 Ag2 . I5 . 144.86(4) yes I6 4_666 Ag2 . I5 . 102.27(4) yes Ag4 4_666 Ag2 . I4 . 149.07(4) yes Ag4 . Ag2 . I4 . 54.89(3) yes I5 4_666 Ag2 . I4 . 100.78(3) yes I6 4_666 Ag2 . I4 . 117.22(4) yes I5 . Ag2 . I4 . 97.58(4) yes Ag4 4_666 Ag2 . Ag3 . 110.12(4) yes Ag4 . Ag2 . Ag3 . 58.33(3) yes I5 4_666 Ag2 . Ag3 . 57.70(2) yes I6 4_666 Ag2 . Ag3 . 147.38(4) yes I5 . Ag2 . Ag3 . 110.33(4) yes Ag4 4_666 Ag2 . Ag3 4_666 57.99(3) yes Ag4 . Ag2 . Ag3 4_666 112.14(4) yes I5 4_666 Ag2 . Ag3 4_666 110.55(4) yes I6 4_666 Ag2 . Ag3 4_666 57.35(3) yes I5 . Ag2 . Ag3 4_666 58.15(2) yes Ag4 4_666 Ag2 . Ag2 4_666 72.38(6) yes Ag4 . Ag2 . Ag2 4_666 75.39(7) yes I5 4_666 Ag2 . Ag2 4_666 71.89(6) yes I6 4_666 Ag2 . Ag2 4_666 120.82(8) yes I5 . Ag2 . Ag2 4_666 72.97(7) yes I4 . Ag2 . Ag3 . 58.13(3) yes I4 . Ag2 . Ag3 4_666 148.45(4) yes Ag3 . Ag2 . Ag3 4_666 144.95(4) yes I4 . Ag2 . Ag2 4_666 121.91(8) yes Ag3 . Ag2 . Ag2 4_666 71.70(6) yes Ag3 4_666 Ag2 . Ag2 4_666 73.25(6) yes #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 721198' _audit_creation_date 08-12-11 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'scale in C 2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 20.48990(40) _cell_length_b 18.35680(29) _cell_length_c 16.83410(29) _cell_angle_alpha 90.0000 _cell_angle_beta 114.6262(10) _cell_angle_gamma 90.0000 _cell_volume 5755.889(184) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 '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 = C36 H81 Ag9 I13.50 N12 O12 Tb1.50 # Dc = 4.38 Fooo = 4576.00 Mu = 121.20 M = 1898.26 # Found Formula = C24 H56.00 Ag6 I9 N8 O8 Tb1 # Dc = 2.92 FOOO = 4576.00 Mu = 80.80 M = 1266.52 _chemical_formula_sum 'C24 H56 Ag6 I9 N8 O8 Tb ' _chemical_formula_moiety 'C24 H56 N8 O8 Tb, Ag6 I9' _chemical_compound_source ? _chemical_formula_weight 2533.03 _cell_measurement_reflns_used 22596 _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 0.25 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 2.923 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4576 _exptl_absorpt_coefficient_mu 8.080 # Sheldrick geometric approximatio 0.12 0.14 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 13417 _reflns_number_total 6888 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections with Friedels Law is 6888 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7152 _diffrn_reflns_theta_min 1.727 _diffrn_reflns_theta_max 28.293 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.445 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -26 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _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 -1.49 _refine_diff_density_max 1.03 # 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 5641 _refine_ls_number_restraints 6 _refine_ls_number_parameters 282 _oxford_refine_ls_R_factor_ref 0.0303 _refine_ls_wR_factor_ref 0.0335 _refine_ls_goodness_of_fit_ref 1.1168 _refine_ls_shift/su_max 0.001085 # The values computed from all data _oxford_reflns_number_all 6867 _refine_ls_R_factor_all 0.0397 _refine_ls_wR_factor_all 0.0393 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5888 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_gt 0.0342 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.509 0.294 0.298 ; 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 C1 C 0.1494(2) 0.3471(3) -0.2588(3) 0.0305 1.0000 Uani . . . . . . . C2 C 0.2415(3) 0.4005(4) -0.2941(4) 0.0432 1.0000 Uani . . . . . . . C3 C 0.1938(4) 0.4653(3) -0.1995(5) 0.0503 1.0000 Uani . . . . . . . C4 C 0.0486(3) 0.4130(3) -0.0916(3) 0.0338 1.0000 Uani . . . . . . . C5 C 0.1068(4) 0.4856(5) 0.0381(7) 0.0900 1.0000 Uani . . . . . . . C6 C 0.0506(4) 0.3664(6) 0.0418(5) 0.0759 1.0000 Uani . . . . . . . C7 C 0.1503(3) 0.2007(3) -0.1066(4) 0.0385 1.0000 Uani . . . . . . . C8 C 0.2640(3) 0.1429(3) -0.0208(4) 0.0388 1.0000 Uani . . . . . . . C9 C 0.1752(3) 0.1683(4) 0.0410(4) 0.0437 1.0000 Uani . . . . . . . C10 C -0.0746(9) 0.1354(10) -0.2133(11) 0.0390 0.3401 Uani . . . 1 2 . . C11 C -0.0519(5) 0.1599(5) -0.1350(5) 0.0384 0.6599 Uani . . . 1 1 . . C12 C -0.0748(12) 0.0556(7) -0.2274(10) 0.1017 0.6599 Uani . U . 1 1 . . C13 C -0.0262(11) 0.1233(11) -0.0561(11) 0.0500 0.3401 Uani . . . 1 2 . . C14 C -0.0813(16) 0.0147(11) -0.1494(15) 0.0825 0.3401 Uani . . . 1 2 . . C15 C -0.0491(13) 0.0414(8) -0.0724(11) 0.1064 0.6599 Uani . U . 1 1 . . Tb1 Tb 0.0000 0.283525(17) -0.2500 0.0248 1.0000 Uani S T . . . . . I5 I 0.436509(17) 0.318620(18) -0.17745(2) 0.0314 1.0000 Uani . . . . . . . I4 I 0.5000 0.08434(2) -0.2500 0.0281 1.0000 Uani S T . . . . . I3 I 0.641308(17) 0.207217(18) -0.02541(2) 0.0313 1.0000 Uani . . . . . . . I2 I 0.741173(18) 0.164699(19) -0.22683(2) 0.0343 1.0000 Uani . . . . . . . I1 I 0.83699(2) 0.04449(2) 0.05701(3) 0.0405 1.0000 Uani . . . . . . . Ag2 Ag 0.60829(2) 0.18912(2) -0.21492(3) 0.0361 1.0000 Uani . . . . . . . Ag3 Ag 0.58518(2) 0.33276(2) -0.14266(3) 0.0378 1.0000 Uani . . . . . . . Ag1 Ag 0.76854(3) 0.16450(3) -0.04856(3) 0.0475 1.0000 Uani . . . . . . . O1 O 0.11014(19) 0.3442(2) -0.2184(2) 0.0353 1.0000 Uani . . . . . . . O3 O 0.0887(2) 0.2231(2) -0.1219(3) 0.0428 1.0000 Uani . . . . . . . O4 O -0.0595(2) 0.2032(2) -0.1976(3) 0.0434 1.0000 Uani . . . . . . . O2 O 0.0156(2) 0.3601(3) -0.1331(3) 0.0443 1.0000 Uani . . . . . . . N3 N 0.1952(2) 0.1734(2) -0.0324(3) 0.0326 1.0000 Uani . . . . . . . N1 N 0.1920(2) 0.4020(2) -0.2520(3) 0.0297 1.0000 Uani . . . . . . . N4 N -0.0586(3) 0.0906(3) -0.1445(3) 0.0365 1.0000 Uani . . . . . . . N2 N 0.0672(2) 0.4222(3) -0.0080(3) 0.0384 1.0000 Uani . . . . . . . H11 H 0.1484 0.3087 -0.2951 0.0333 1.0000 Uiso R . . . . . . H71 H 0.1649 0.2026 -0.1522 0.0447 1.0000 Uiso R . . . . . . H82 H 0.3012 0.1648 0.0291 0.0511 1.0000 Uiso R . . . . . . H83 H 0.2724 0.1535 -0.0716 0.0511 1.0000 Uiso R . . . . . . H81 H 0.2636 0.0907 -0.0133 0.0510 1.0000 Uiso R . . . . . . H92 H 0.2144 0.1836 0.0934 0.0589 1.0000 Uiso R . . . . . . H93 H 0.1341 0.1985 0.0295 0.0590 1.0000 Uiso R . . . . . . H91 H 0.1635 0.1185 0.0473 0.0590 1.0000 Uiso R . . . . . . H41 H 0.0612 0.4494 -0.1214 0.0393 1.0000 Uiso R . . . . . . H23 H 0.2342 0.4424 -0.3306 0.0611 1.0000 Uiso R . . . . . . H21 H 0.2340 0.3572 -0.3291 0.0614 1.0000 Uiso R . . . . . . H22 H 0.2901 0.4009 -0.2507 0.0610 1.0000 Uiso R . . . . . . H31 H 0.2318 0.4969 -0.1964 0.0734 1.0000 Uiso R . . . . . . H33 H 0.1489 0.4901 -0.2251 0.0733 1.0000 Uiso R . . . . . . H32 H 0.2019 0.4496 -0.1421 0.0732 1.0000 Uiso R . . . . . . H111 H -0.0407 0.1798 -0.0798 0.0371 0.6599 Uiso R . . 1 1 . . H62 H 0.0240 0.3887 0.0710 0.1059 1.0000 Uiso R . . . . . . H63 H 0.0223 0.3290 0.0028 0.1061 1.0000 Uiso R . . . . . . H61 H 0.0945 0.3462 0.0840 0.1060 1.0000 Uiso R . . . . . . H53 H 0.0835 0.5066 0.0715 0.1649 1.0000 Uiso R . . . . . . H51 H 0.1083 0.5206 -0.0031 0.1650 1.0000 Uiso R . . . . . . H52 H 0.1549 0.4723 0.0766 0.1650 1.0000 Uiso R . . . . . . H122 H -0.0791 0.0041 -0.2217 0.1160 0.6599 Uiso R . . 1 1 . . H121 H -0.1190 0.0747 -0.2701 0.1161 0.6599 Uiso R . . 1 1 . . H123 H -0.0366 0.0654 -0.2449 0.1161 0.6599 Uiso R . . 1 1 . . H131 H 0.0150 0.0953 -0.0196 0.0570 0.3401 Uiso R . . 1 2 . . H133 H -0.0609 0.1231 -0.0314 0.0570 0.3401 Uiso R . . 1 2 . . H132 H -0.0117 0.1726 -0.0595 0.0569 0.3401 Uiso R . . 1 2 . . H101 H -0.0936 0.1174 -0.2702 0.0501 0.3401 Uiso R . . 1 2 . . H153 H -0.0028 -0.0036 -0.0720 0.3870 0.6599 Uiso R . . 1 1 . . H152 H -0.1104 0.0147 -0.0939 0.3870 0.6599 Uiso R . . 1 1 . . H151 H -0.0285 0.0811 -0.0063 0.3870 0.6599 Uiso R . . 1 1 . . H143 H -0.1070 0.0017 -0.2098 0.1160 0.3401 Uiso R . . 1 2 . . H141 H -0.1120 0.0084 -0.1196 0.1160 0.3401 Uiso R . . 1 2 . . H142 H -0.0398 -0.0160 -0.1228 0.1160 0.3401 Uiso R . . 1 2 . . 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 0.021(2) 0.036(3) 0.031(2) 0.0035(19) 0.0068(18) -0.0021(18) C2 0.027(2) 0.058(4) 0.052(3) 0.015(3) 0.023(2) 0.001(2) C3 0.046(3) 0.032(3) 0.076(4) -0.005(3) 0.028(3) -0.005(2) C4 0.028(2) 0.038(3) 0.036(3) 0.006(2) 0.014(2) 0.001(2) C5 0.042(4) 0.088(6) 0.120(8) -0.073(6) 0.014(4) -0.003(4) C6 0.059(4) 0.135(8) 0.035(3) 0.023(4) 0.021(3) -0.005(5) C7 0.032(3) 0.039(3) 0.052(3) 0.017(2) 0.025(2) 0.006(2) C8 0.023(2) 0.037(3) 0.053(3) 0.003(2) 0.012(2) 0.002(2) C9 0.034(3) 0.057(4) 0.038(3) 0.010(3) 0.013(2) 0.010(2) C10 0.039(8) 0.049(9) 0.032(7) -0.003(7) 0.017(6) -0.008(7) C11 0.039(4) 0.036(4) 0.030(4) -0.002(3) 0.005(3) 0.006(3) C12 0.199(16) 0.043(6) 0.079(8) 0.012(5) 0.074(9) 0.031(7) C13 0.058(11) 0.060(11) 0.030(8) 0.003(8) 0.016(8) -0.011(9) C14 0.12(2) 0.033(10) 0.054(13) 0.013(9) -0.001(13) -0.030(12) C15 0.209(16) 0.051(6) 0.086(8) 0.026(6) 0.087(9) 0.035(8) Tb1 0.01980(14) 0.02536(15) 0.02883(15) 0.0000 0.00977(11) 0.0000 I5 0.02927(16) 0.03557(17) 0.03092(16) -0.00413(12) 0.01414(13) 0.00256(12) I4 0.0271(2) 0.0253(2) 0.0305(2) 0.0000 0.01084(16) 0.0000 I3 0.02930(16) 0.03468(17) 0.02686(15) -0.00028(12) 0.00870(12) -0.00191(12) I2 0.02992(16) 0.03602(17) 0.03948(18) -0.00262(13) 0.01684(14) -0.00349(12) I1 0.03909(19) 0.03189(17) 0.0480(2) -0.01020(14) 0.01561(16) -0.00565(13) Ag2 0.0372(2) 0.0342(2) 0.0404(2) -0.00180(16) 0.01968(17) -0.00368(15) Ag3 0.0380(2) 0.0359(2) 0.0384(2) -0.00674(16) 0.01485(17) -0.00549(16) Ag1 0.0477(3) 0.0473(3) 0.0475(2) -0.00505(19) 0.0200(2) -0.0017(2) O1 0.0303(18) 0.040(2) 0.0359(18) -0.0002(15) 0.0143(15) -0.0105(15) O3 0.0264(18) 0.053(2) 0.047(2) 0.0238(19) 0.0139(16) 0.0101(16) O4 0.033(2) 0.035(2) 0.064(3) 0.0128(18) 0.0216(19) -0.0025(15) O2 0.038(2) 0.062(3) 0.0335(19) -0.0167(19) 0.0165(16) -0.0063(19) N3 0.0225(19) 0.032(2) 0.041(2) 0.0057(17) 0.0117(17) 0.0032(16) N1 0.0259(19) 0.031(2) 0.033(2) 0.0074(16) 0.0121(16) 0.0011(16) N4 0.039(2) 0.035(2) 0.044(2) 0.0100(19) 0.026(2) 0.0065(18) N2 0.031(2) 0.048(3) 0.035(2) -0.0123(19) 0.0125(18) -0.0006(19) _refine_ls_extinction_coef 69(3) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.05230(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . O1 . 1.252(6) yes C1 . N1 . 1.307(6) yes C1 . H11 . 0.928 no C2 . N1 . 1.459(6) yes C2 . H23 . 0.956 no C2 . H21 . 0.963 no C2 . H22 . 0.959 no C3 . N1 . 1.451(7) yes C3 . H31 . 0.955 no C3 . H33 . 0.954 no C3 . H32 . 0.953 no C4 . O2 . 1.223(7) yes C4 . N2 . 1.306(7) yes C4 . H41 . 0.935 no C5 . N2 . 1.445(8) yes C5 . H53 . 0.957 no C5 . H51 . 0.956 no C5 . H52 . 0.958 no C6 . N2 . 1.450(9) yes C6 . H62 . 0.964 no C6 . H63 . 0.959 no C6 . H61 . 0.958 no C7 . O3 . 1.248(6) yes C7 . N3 . 1.304(7) yes C7 . H71 . 0.932 no C8 . N3 . 1.452(6) yes C8 . H82 . 0.957 no C8 . H83 . 0.959 no C8 . H81 . 0.968 no C9 . N3 . 1.457(7) yes C9 . H92 . 0.955 no C9 . H93 . 0.960 no C9 . H91 . 0.961 no C10 . O4 . 1.283(18) yes C10 . N4 . 1.345(17) yes C10 . H101 . 0.931 no C11 . O4 . 1.276(9) yes C11 . N4 . 1.282(9) yes C11 . H111 . 0.934 no C12 . N4 . 1.442(14) yes C12 . H122 . 0.959 no C12 . H121 . 0.958 no C12 . H123 . 0.962 no C13 . N4 . 1.481(18) yes C13 . H131 . 0.960 no C13 . H133 . 0.963 no C13 . H132 . 0.962 no C14 . N4 . 1.461(19) yes C14 . H143 . 0.961 no C14 . H141 . 0.960 no C14 . H142 . 0.961 no C15 . N4 . 1.460(13) yes C15 . H153 . 1.255 no C15 . H152 . 1.254 no C15 . H151 . 1.247 no Tb1 . O3 5_554 2.432(4) yes Tb1 . O1 5_554 2.370(3) yes Tb1 . O2 5_554 2.330(4) yes Tb1 . O4 5_554 2.311(4) yes Tb1 . O1 . 2.370(3) yes Tb1 . O3 . 2.432(4) yes Tb1 . O4 . 2.311(4) yes Tb1 . O2 . 2.330(4) yes I5 . Ag2 5_654 2.8967(8) yes I5 . Ag3 5_654 2.8833(10) yes I5 . Ag3 . 2.8640(9) yes I4 . Ag2 5_654 2.8070(7) yes I4 . Ag2 . 2.8070(7) yes I3 . Ag1 4_655 2.9311(8) yes I3 . Ag2 . 2.9910(11) yes I3 . Ag3 . 2.9391(8) yes I3 . Ag1 . 2.8996(9) yes I2 . Ag2 . 2.8476(8) yes I2 . Ag1 . 2.8138(11) yes I1 . Ag3 4_655 2.7899(8) yes I1 . Ag1 . 2.8111(8) yes Ag2 . Ag3 . 3.0227(9) yes Ag2 . Ag1 . 3.3412(9) yes Ag3 . Ag1 4_655 3.3625(10) 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 . C1 . N1 . 122.9(5) yes O1 . C1 . H11 . 118.9 no N1 . C1 . H11 . 118.2 no N1 . C2 . H23 . 110.0 no N1 . C2 . H21 . 110.2 no H23 . C2 . H21 . 109.2 no N1 . C2 . H22 . 110.0 no H23 . C2 . H22 . 108.6 no H21 . C2 . H22 . 108.8 no N1 . C3 . H31 . 109.4 no N1 . C3 . H33 . 109.4 no H31 . C3 . H33 . 110.2 no N1 . C3 . H32 . 109.0 no H31 . C3 . H32 . 109.5 no H33 . C3 . H32 . 109.3 no O2 . C4 . N2 . 124.2(5) yes O2 . C4 . H41 . 118.2 no N2 . C4 . H41 . 117.6 no N2 . C5 . H53 . 109.5 no N2 . C5 . H51 . 109.4 no H53 . C5 . H51 . 109.2 no N2 . C5 . H52 . 110.3 no H53 . C5 . H52 . 109.2 no H51 . C5 . H52 . 109.2 no N2 . C6 . H62 . 108.4 no N2 . C6 . H63 . 109.3 no H62 . C6 . H63 . 110.0 no N2 . C6 . H61 . 109.1 no H62 . C6 . H61 . 110.0 no H63 . C6 . H61 . 110.1 no O3 . C7 . N3 . 125.0(5) yes O3 . C7 . H71 . 117.4 no N3 . C7 . H71 . 117.6 no N3 . C8 . H82 . 109.3 no N3 . C8 . H83 . 109.1 no H82 . C8 . H83 . 108.9 no N3 . C8 . H81 . 109.9 no H82 . C8 . H81 . 110.3 no H83 . C8 . H81 . 109.3 no N3 . C9 . H92 . 109.8 no N3 . C9 . H93 . 109.0 no H92 . C9 . H93 . 110.2 no N3 . C9 . H91 . 109.0 no H92 . C9 . H91 . 109.3 no H93 . C9 . H91 . 109.5 no O4 . C10 . N4 . 117.6(12) yes O4 . C10 . H101 . 121.2 no N4 . C10 . H101 . 121.1 no O4 . C11 . N4 . 123.1(7) yes O4 . C11 . H111 . 118.2 no N4 . C11 . H111 . 118.8 no N4 . C12 . H122 . 109.7 no N4 . C12 . H121 . 109.1 no H122 . C12 . H121 . 109.7 no N4 . C12 . H123 . 109.0 no H122 . C12 . H123 . 109.7 no H121 . C12 . H123 . 109.7 no N4 . C13 . H131 . 109.5 no N4 . C13 . H133 . 109.3 no H131 . C13 . H133 . 109.3 no N4 . C13 . H132 . 110.0 no H131 . C13 . H132 . 109.3 no H133 . C13 . H132 . 109.4 no N4 . C14 . H143 . 108.5 no N4 . C14 . H141 . 110.4 no H143 . C14 . H141 . 109.4 no N4 . C14 . H142 . 109.6 no H143 . C14 . H142 . 109.6 no H141 . C14 . H142 . 109.3 no N4 . C15 . H153 . 104.6 no N4 . C15 . H152 . 103.4 no H153 . C15 . H152 . 114.1 no N4 . C15 . H151 . 105.0 no H153 . C15 . H151 . 113.9 no H152 . C15 . H151 . 114.3 no O3 5_554 Tb1 . O1 5_554 74.07(13) yes O3 5_554 Tb1 . O2 5_554 74.81(16) yes O1 5_554 Tb1 . O2 5_554 75.19(14) yes O3 5_554 Tb1 . O4 5_554 71.87(14) yes O1 5_554 Tb1 . O4 5_554 145.01(14) yes O2 5_554 Tb1 . O4 5_554 88.32(16) yes O3 5_554 Tb1 . O1 . 134.68(13) yes O1 5_554 Tb1 . O1 . 123.92(19) yes O2 5_554 Tb1 . O1 . 71.83(14) yes O4 5_554 Tb1 . O1 . 77.33(14) yes O3 5_554 Tb1 . O3 . 125.7(2) yes O1 5_554 Tb1 . O3 . 134.68(13) yes O2 5_554 Tb1 . O3 . 144.35(13) yes O4 5_554 Tb1 . O3 . 74.28(15) yes O1 . Tb1 . O3 . 74.07(13) yes O3 5_554 Tb1 . O4 . 74.28(15) yes O1 5_554 Tb1 . O4 . 77.33(14) yes O2 5_554 Tb1 . O4 . 143.09(14) yes O4 5_554 Tb1 . O4 . 100.7(2) yes O1 . Tb1 . O4 . 145.01(14) yes O3 5_554 Tb1 . O2 . 144.35(13) yes O1 5_554 Tb1 . O2 . 71.83(14) yes O2 5_554 Tb1 . O2 . 105.7(2) yes O4 5_554 Tb1 . O2 . 143.09(14) yes O1 . Tb1 . O2 . 75.19(14) yes O3 . Tb1 . O4 . 71.87(14) yes O3 . Tb1 . O2 . 74.81(16) yes O4 . Tb1 . O2 . 88.32(16) yes Ag2 5_654 I5 . Ag3 5_654 63.06(3) yes Ag2 5_654 I5 . Ag3 . 103.60(2) yes Ag3 5_654 I5 . Ag3 . 83.80(3) yes Ag2 5_654 I4 . Ag2 . 93.48(3) yes Ag1 4_655 I3 . Ag2 . 111.39(2) yes Ag1 4_655 I3 . Ag3 . 69.89(2) yes Ag2 . I3 . Ag3 . 61.284(15) yes Ag1 4_655 I3 . Ag1 . 80.31(3) yes Ag2 . I3 . Ag1 . 69.093(17) yes Ag3 . I3 . Ag1 . 104.12(2) yes Ag2 . I2 . Ag1 . 72.34(3) yes Ag3 4_655 I1 . Ag1 . 73.79(2) yes I3 . Ag2 . I5 5_654 116.608(18) yes I3 . Ag2 . I2 . 107.13(2) yes I5 5_654 Ag2 . I2 . 98.52(2) yes I3 . Ag2 . I4 . 96.21(2) yes I5 5_654 Ag2 . I4 . 114.47(2) yes I2 . Ag2 . I4 . 124.91(2) yes I3 . Ag2 . Ag3 . 58.512(14) yes I5 5_654 Ag2 . Ag3 . 58.25(2) yes I2 . Ag2 . Ag3 . 118.71(2) yes I4 . Ag2 . Ag3 . 116.10(3) yes I3 . Ag2 . Ag1 . 54.164(14) yes I5 5_654 Ag2 . Ag1 . 125.44(2) yes I2 . Ag2 . Ag1 . 53.36(2) yes I4 . Ag2 . Ag1 . 119.88(2) yes Ag3 . Ag2 . Ag1 . 92.56(2) yes Ag1 4_655 Ag3 . I3 . 54.942(15) yes Ag1 4_655 Ag3 . I5 5_654 133.84(3) yes I3 . Ag3 . I5 5_654 118.73(3) yes Ag1 4_655 Ag3 . I5 . 130.16(3) yes I3 . Ag3 . I5 . 98.71(3) yes I5 5_654 Ag3 . I5 . 95.26(3) yes Ag1 4_655 Ag3 . Ag2 . 99.88(2) yes I3 . Ag3 . Ag2 . 60.20(3) yes I5 5_654 Ag3 . Ag2 . 58.686(14) yes I5 . Ag3 . Ag2 . 99.797(19) yes Ag1 4_655 Ag3 . I1 4_655 53.396(15) yes I3 . Ag3 . I1 4_655 107.87(3) yes I5 5_654 Ag3 . I1 4_655 114.85(2) yes I5 . Ag3 . I1 4_655 120.602(19) yes Ag2 . Ag3 . I1 4_655 139.55(2) yes Ag3 4_655 Ag1 . Ag2 . 166.636(19) yes Ag3 4_655 Ag1 . I3 4_655 55.166(15) yes Ag2 . Ag1 . I3 4_655 118.20(2) yes Ag3 4_655 Ag1 . I3 . 111.10(3) yes Ag2 . Ag1 . I3 . 56.74(3) yes I3 4_655 Ag1 . I3 . 99.69(3) yes Ag3 4_655 Ag1 . I2 . 136.30(3) yes Ag2 . Ag1 . I2 . 54.30(2) yes I3 4_655 Ag1 . I2 . 105.21(3) yes I3 . Ag1 . I2 . 110.62(3) yes Ag3 4_655 Ag1 . I1 . 52.817(15) yes Ag2 . Ag1 . I1 . 133.87(2) yes I3 4_655 Ag1 . I1 . 107.52(3) yes I3 . Ag1 . I1 . 111.51(2) yes I2 . Ag1 . I1 . 120.03(2) yes Tb1 . O1 . C1 . 131.7(3) yes Tb1 . O3 . C7 . 130.6(4) yes C11 . O4 . Tb1 . 144.1(5) yes C10 . O4 . Tb1 . 131.3(8) yes Tb1 . O2 . C4 . 144.1(4) yes C9 . N3 . C8 . 117.5(4) yes C9 . N3 . C7 . 120.1(4) yes C8 . N3 . C7 . 122.3(5) yes C2 . N1 . C3 . 117.7(5) yes C2 . N1 . C1 . 121.2(5) yes C3 . N1 . C1 . 121.1(5) yes C15 . N4 . C12 . 115.2(9) yes C15 . N4 . C11 . 122.7(8) yes C12 . N4 . C11 . 122.1(7) yes C13 . N4 . C14 . 116.2(13) yes C13 . N4 . C10 . 117.6(11) yes C14 . N4 . C10 . 125.3(12) yes C6 . N2 . C5 . 118.2(7) yes C6 . N2 . C4 . 119.8(6) yes C5 . N2 . C4 . 121.9(7) 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 C12 . H123 . C12 5_554 164 0.96 2.52 3.451(16) yes #===END data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 721199' _audit_creation_date 09-02-05 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'analytical in C 1 2/c 1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 20.556(2) _cell_length_b 18.1239(13) _cell_length_c 16.868(2) _cell_angle_alpha 90.0 _cell_angle_beta 114.576(13) _cell_angle_gamma 90.0 _cell_volume 5715.0(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 '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 = C18 H50 Ag5 I8.50 N6 O6 S6 Tb1.50 # Dc = 2.90 Fooo = 4586.65 Mu = 83.53 M = 1247.72 # Found Formula = C22.67 H54.67 Ag6 I9 N6.67 O8 S1.33 Tb1 # Dc = 2.95 FOOO = 4586.65 Mu = 81.84 M = 1269.87 _chemical_formula_sum 'C22.67 H54.67 Ag6 I9 N6.67 O8 S1.33 Tb ' _chemical_formula_moiety 'C22.67 H54.67 N6.67 O8 S1.33 Tb, Ag6 I9 ' _chemical_compound_source ? _chemical_formula_weight 2539.74 _cell_measurement_reflns_used 7734 _cell_measurement_theta_min 3.1240 _cell_measurement_theta_max 29.4956 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3935 _exptl_crystal_size_mid 0.2701 _exptl_crystal_size_min 0.1084 _exptl_crystal_density_diffrn 2.952 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4586.651 _exptl_absorpt_coefficient_mu 8.184 # Sheldrick geometric approximatio 0.17 0.47 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) 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 0.13 _exptl_absorpt_correction_T_max 0.47 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _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 ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _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 14329 _reflns_number_total 6843 _diffrn_reflns_av_R_equivalents 0.047 # Number of reflections with Friedels Law is 6843 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8011 _diffrn_reflns_theta_min 3.131 _diffrn_reflns_theta_max 29.565 _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 26.313 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -27 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.19 _refine_diff_density_max 1.53 # 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>2.0\s(I) _refine_ls_number_reflns 5228 _refine_ls_number_restraints 48 _refine_ls_number_parameters 291 _oxford_refine_ls_R_factor_ref 0.0514 _refine_ls_wR_factor_ref 0.0579 _refine_ls_goodness_of_fit_ref 1.0154 _refine_ls_shift/su_max 0.000805 # The values computed from all data _oxford_reflns_number_all 6831 _refine_ls_R_factor_all 0.0702 _refine_ls_wR_factor_all 0.0806 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5228 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_gt 0.0579 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 12.7 -1.84 8.30 ; 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 C1 C 0.5486(5) 0.9096(6) 0.4068(6) 0.0360 1.0000 Uani . . . . . . . C2 C 0.5503(7) 0.8631(10) 0.5399(9) 0.0717 1.0000 Uani . . . . . . . C3 C 0.6034(8) 0.9854(8) 0.5332(11) 0.0797 1.0000 Uani . . . . . . . C4 C 0.6494(5) 0.8387(6) 0.2346(6) 0.0338 1.0000 Uani . . . . . . . C5 C 0.7398(5) 0.8989(7) 0.2026(7) 0.0429 1.0000 Uani . . . . . . . C6 C 0.6849(7) 0.9603(7) 0.2939(9) 0.0536 1.0000 Uani . U . . . . . C7 C 0.3497(5) 0.6949(5) 0.1065(6) 0.0316 1.0000 Uani . U . . . . . C8 C 0.2349(5) 0.6403(5) 0.0200(6) 0.0304 1.0000 Uani . . . . . . . C9 C 0.3187(6) 0.6721(6) -0.0466(6) 0.0400 1.0000 Uani . U . . . . . C10 C 0.4511(14) 0.6597(15) 0.3773(18) 0.0280 0.3343 Uani . U . 1 1 . . C12 C 0.468(2) 0.543(2) 0.444(3) 0.0603 0.3343 Uani . U . 1 1 . . C13 C 0.4655(12) 0.6312(12) 0.4445(13) 0.0603 0.6657 Uani . U . 1 2 . . I1 I 0.64209(3) 0.20693(3) 0.47595(4) 0.0312 1.0000 Uani . . . . . . . I2 I 0.43511(3) 0.32042(3) 0.31977(4) 0.0292 1.0000 Uani . . . . . . . I3 I 0.5000 0.08334(4) 0.2500 0.0295 1.0000 Uani S T . . . . . I4 I 0.73738(3) 0.16177(4) 0.27015(4) 0.0344 1.0000 Uani . . . . . . . I5 I 0.65990(4) 0.45740(4) 0.44829(4) 0.0411 1.0000 Uani . . . . . . . Ag1 Ag 0.58397(4) 0.33414(4) 0.35935(5) 0.0370 1.0000 Uani . . . . . . . Ag2 Ag 0.60754(4) 0.18894(4) 0.28607(5) 0.0368 1.0000 Uani . . . . . . . Ag3 Ag 0.76682(5) 0.16315(5) 0.44961(5) 0.0442 1.0000 Uani . . . . . . . Tb1 Tb 0.5000 0.77436(3) 0.2500 0.0242 1.0000 Uani S T . . . . . N2 N 0.6891(4) 0.8965(4) 0.2422(5) 0.0324 1.0000 Uani . . . . . . . N1 N 0.5656(4) 0.9198(5) 0.4886(5) 0.0361 1.0000 Uani . U . . . . . O2 O 0.6097(4) 0.8312(5) 0.2744(5) 0.0453 1.0000 Uani . U . . . . . O3 O 0.4101(4) 0.7199(4) 0.1186(5) 0.0389 1.0000 Uani . . . . . . . N3 N 0.3024(4) 0.6723(4) 0.0300(5) 0.0257 1.0000 Uani . . . . . . . O1 O 0.5172(4) 0.8557(5) 0.3645(5) 0.0490 1.0000 Uani . U . . . . . S1 S 0.47760(19) 0.6107(2) 0.3477(2) 0.0335 0.6657 Uani . . . 1 2 . . N4 N 0.4496(13) 0.5886(14) 0.3690(17) 0.0313 0.3343 Uani . U . 1 1 . . O4 O 0.4419(12) 0.6969(16) 0.3151(16) 0.0339 0.3343 Uani . U . 1 1 . . O5 O 0.4476(8) 0.6784(8) 0.2887(9) 0.0451 0.6657 Uani . U . 1 2 . . H11 H 0.5615 0.9472 0.3767 0.0404 1.0000 Uiso R . . . . . . H21 H 0.5661 0.8791 0.5985 0.0868 1.0000 Uiso R . . . . . . H22 H 0.5745 0.8189 0.5382 0.0868 1.0000 Uiso R . . . . . . H23 H 0.5002 0.8542 0.5160 0.0868 1.0000 Uiso R . . . . . . H31 H 0.6113 0.9834 0.5928 0.0877 1.0000 Uiso R . . . . . . H32 H 0.6481 0.9879 0.5291 0.0877 1.0000 Uiso R . . . . . . H33 H 0.5758 1.0278 0.5067 0.0877 1.0000 Uiso R . . . . . . H41 H 0.6503 0.8001 0.1970 0.0389 1.0000 Uiso R . . . . . . H51 H 0.7640 0.9450 0.2150 0.0546 1.0000 Uiso R . . . . . . H52 H 0.7736 0.8602 0.2256 0.0546 1.0000 Uiso R . . . . . . H53 H 0.7150 0.8931 0.1412 0.0546 1.0000 Uiso R . . . . . . H61 H 0.7171 0.9975 0.2931 0.0688 1.0000 Uiso R . . . . . . H62 H 0.6971 0.9452 0.3523 0.0688 1.0000 Uiso R . . . . . . H63 H 0.6375 0.9792 0.2696 0.0688 1.0000 Uiso R . . . . . . H71 H 0.3376 0.6919 0.1550 0.0361 1.0000 Uiso R . . . . . . H81 H 0.2078 0.6274 -0.0393 0.0356 1.0000 Uiso R . . . . . . H82 H 0.2089 0.6751 0.0376 0.0356 1.0000 Uiso R . . . . . . H83 H 0.2437 0.5974 0.0553 0.0356 1.0000 Uiso R . . . . . . H91 H 0.2786 0.6543 -0.0957 0.0453 1.0000 Uiso R . . . . . . H92 H 0.3295 0.7209 -0.0579 0.0453 1.0000 Uiso R . . . . . . H93 H 0.3587 0.6410 -0.0359 0.0453 1.0000 Uiso R . . . . . . H101 H 0.4599 0.6811 0.4322 0.0360 0.3343 Uiso R . . 1 1 . . H121 H 0.4647 0.4921 0.4295 0.0784 0.3343 Uiso R . . 1 1 . . H122 H 0.5155 0.5548 0.4827 0.0784 0.3343 Uiso R . . 1 1 . . H123 H 0.4363 0.5541 0.4701 0.0784 0.3343 Uiso R . . 1 1 . . C14 C 0.4105(11) 0.5411(12) 0.3052(16) 0.0471 0.6657 Uani . . . 1 2 . . C11 C 0.430(3) 0.552(3) 0.289(4) 0.0643 0.3343 Uani . U . 1 1 . . H111 H 0.4186 0.5811 0.2386 0.0673 0.3343 Uiso R . . 1 1 . . H112 H 0.4601 0.5120 0.2885 0.0673 0.3343 Uiso R . . 1 1 . . H113 H 0.3875 0.5324 0.2903 0.0673 0.3343 Uiso R . . 1 1 . . H141 H 0.4096 0.5222 0.2522 0.0673 0.6657 Uiso R . . 1 2 . . H142 H 0.3648 0.5606 0.2951 0.0673 0.6657 Uiso R . . 1 2 . . H143 H 0.4223 0.5026 0.3471 0.0673 0.6657 Uiso R . . 1 2 . . H131 H 0.4973 0.6697 0.4755 0.0735 0.6657 Uiso R . . 1 2 . . H132 H 0.4176 0.6466 0.4285 0.0735 0.6657 Uiso R . . 1 2 . . H133 H 0.4750 0.5886 0.4805 0.0735 0.6657 Uiso R . . 1 2 . . 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 0.031(5) 0.041(5) 0.026(4) 0.004(4) 0.002(4) 0.005(4) C2 0.051(7) 0.126(14) 0.041(7) 0.033(8) 0.022(6) 0.017(8) C3 0.051(8) 0.067(9) 0.098(12) -0.052(9) 0.008(8) -0.001(7) C4 0.026(4) 0.045(5) 0.024(4) 0.004(4) 0.004(3) -0.006(4) C5 0.028(5) 0.069(7) 0.035(5) 0.005(5) 0.015(4) 0.001(5) C6 0.058(6) 0.049(6) 0.061(6) -0.002(5) 0.032(5) -0.008(5) C7 0.029(4) 0.032(4) 0.031(4) 0.000(4) 0.010(4) -0.003(4) C8 0.023(4) 0.034(5) 0.030(4) 0.005(4) 0.007(3) 0.002(3) C9 0.043(5) 0.048(5) 0.032(4) -0.007(4) 0.018(4) -0.012(4) C10 0.029(8) 0.034(9) 0.028(8) 0.004(7) 0.020(7) -0.001(7) C12 0.07(2) 0.031(14) 0.08(2) 0.016(14) 0.037(19) -0.001(14) C13 0.068(7) 0.067(7) 0.048(6) -0.007(6) 0.026(6) -0.014(6) I1 0.0300(3) 0.0332(3) 0.0249(3) 0.0011(2) 0.0060(2) -0.0023(2) I2 0.0298(3) 0.0302(3) 0.0273(3) -0.0005(2) 0.0116(2) 0.0028(2) I3 0.0281(4) 0.0237(4) 0.0330(4) 0.0000 0.0091(3) 0.0000 I4 0.0319(3) 0.0399(3) 0.0313(3) -0.0009(2) 0.0130(2) -0.0031(2) I5 0.0454(4) 0.0294(3) 0.0356(3) -0.0037(2) 0.0040(3) -0.0063(3) Ag1 0.0389(4) 0.0361(4) 0.0326(4) -0.0068(3) 0.0116(3) -0.0062(3) Ag2 0.0402(4) 0.0320(4) 0.0394(4) -0.0016(3) 0.0178(3) -0.0039(3) Ag3 0.0478(5) 0.0441(4) 0.0377(4) 0.0004(3) 0.0149(4) -0.0003(4) Tb1 0.0241(3) 0.0246(3) 0.0198(3) 0.0000 0.0050(2) 0.0000 N2 0.028(4) 0.031(4) 0.032(4) 0.007(3) 0.007(3) 0.000(3) N1 0.031(4) 0.037(4) 0.032(4) -0.007(3) 0.006(3) 0.002(3) O2 0.028(3) 0.065(5) 0.035(3) 0.004(3) 0.006(3) -0.023(3) O3 0.028(3) 0.042(4) 0.038(4) -0.010(3) 0.005(3) -0.003(3) N3 0.018(3) 0.026(3) 0.029(4) 0.002(3) 0.005(3) -0.002(3) O1 0.045(4) 0.056(4) 0.038(4) -0.010(3) 0.008(3) 0.005(3) S1 0.0253(16) 0.0345(18) 0.0328(17) 0.0083(14) 0.0041(14) 0.0000(14) N4 0.024(7) 0.031(8) 0.038(8) 0.002(7) 0.012(7) 0.003(7) O4 0.014(7) 0.060(9) 0.029(8) 0.000(7) 0.011(6) -0.014(7) O5 0.035(5) 0.055(6) 0.033(5) 0.017(4) 0.001(4) -0.009(5) C14 0.036(10) 0.033(10) 0.062(13) -0.013(9) 0.010(8) -0.014(7) C11 0.07(2) 0.031(15) 0.09(2) 0.010(14) 0.033(19) 0.000(15) _refine_ls_extinction_coef 20(3) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.6278(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . N1 . 1.287(13) yes C1 . O1 . 1.224(13) yes C1 . H11 . 0.950 no C2 . N1 . 1.459(16) yes C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . N1 . 1.448(14) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C3 . H33 . 0.950 no C4 . N2 . 1.301(12) yes C4 . O2 . 1.261(12) yes C4 . H41 . 0.950 no C5 . N2 . 1.454(12) yes C5 . H51 . 0.950 no C5 . H52 . 0.950 no C5 . H53 . 0.950 no C6 . N2 . 1.472(15) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . O3 . 1.256(11) yes C7 . N3 . 1.317(11) yes C7 . H71 . 0.950 no C8 . N3 . 1.449(11) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . N3 . 1.463(12) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . N4 . 1.29(4) yes C10 . O4 . 1.19(4) yes C10 . H101 . 0.950 no C12 . N4 . 1.42(4) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . S1 . 1.79(2) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no I1 . Ag3 4_656 2.9447(12) yes I1 . Ag1 . 2.9422(11) yes I1 . Ag2 . 2.9961(13) yes I1 . Ag3 . 2.8894(12) yes I2 . Ag1 5_655 2.8910(13) yes I2 . Ag2 5_655 2.8865(11) yes I2 . Ag1 . 2.8585(12) yes I3 . Ag2 5_655 2.7930(11) yes I3 . Ag2 . 2.7930(11) yes I4 . Ag2 . 2.8345(12) yes I4 . Ag3 . 2.8295(13) yes I5 . Ag3 4_656 2.8019(12) yes I5 . Ag1 . 2.7803(11) yes Ag1 . Ag3 4_656 3.4019(13) yes Ag2 . Ag3 . 3.3220(13) yes Tb1 . O3 5_655 2.429(7) yes Tb1 . O4 5_655 2.39(2) yes Tb1 . O2 5_655 2.354(6) yes Tb1 . O1 5_655 2.337(8) yes Tb1 . O2 . 2.354(6) yes Tb1 . O3 . 2.429(7) yes Tb1 . O1 . 2.337(8) yes Tb1 . O4 . 2.39(2) yes Tb1 . O3 5_655 2.429(7) yes Tb1 . O2 5_655 2.354(6) yes Tb1 . O1 5_655 2.337(8) yes Tb1 . O5 5_655 2.280(14) yes Tb1 . S1 5_655 3.516(4) yes Tb1 . O2 . 2.354(6) yes Tb1 . O3 . 2.429(7) yes Tb1 . O1 . 2.337(8) yes Tb1 . S1 . 3.516(4) yes Tb1 . O5 . 2.280(14) yes S1 . O5 . 1.539(14) yes S1 . C14 . 1.783(18) yes N4 . C11 . 1.40(7) yes C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 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 N1 . C1 . O1 . 125.6(10) yes N1 . C1 . H11 . 117.2 no O1 . C1 . H11 . 117.2 no N1 . C2 . H21 . 109.8 no N1 . C2 . H22 . 109.3 no H21 . C2 . H22 . 109.5 no N1 . C2 . H23 . 109.3 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no N1 . C3 . H31 . 109.8 no N1 . C3 . H32 . 109.2 no H31 . C3 . H32 . 109.5 no N1 . C3 . H33 . 109.5 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no N2 . C4 . O2 . 123.6(10) yes N2 . C4 . H41 . 118.2 no O2 . C4 . H41 . 118.2 no N2 . C5 . H51 . 109.5 no N2 . C5 . H52 . 109.4 no H51 . C5 . H52 . 109.5 no N2 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N2 . C6 . H61 . 109.6 no N2 . C6 . H62 . 109.5 no H61 . C6 . H62 . 109.5 no N2 . C6 . H63 . 109.3 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no O3 . C7 . N3 . 123.1(9) yes O3 . C7 . H71 . 118.4 no N3 . C7 . H71 . 118.4 no N3 . C8 . H81 . 109.6 no N3 . C8 . H82 . 109.5 no H81 . C8 . H82 . 109.5 no N3 . C8 . H83 . 109.3 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no N3 . C9 . H91 . 109.6 no N3 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no N3 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N4 . C10 . O4 . 119(3) yes N4 . C10 . H101 . 120.0 no O4 . C10 . H101 . 121.4 no N4 . C12 . H121 . 112.3 no N4 . C12 . H122 . 107.7 no H121 . C12 . H122 . 109.5 no N4 . C12 . H123 . 108.4 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no S1 . C13 . H131 . 109.3 no S1 . C13 . H132 . 108.9 no H131 . C13 . H132 . 109.5 no S1 . C13 . H133 . 110.2 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no Ag3 4_656 I1 . Ag1 . 70.60(3) yes Ag3 4_656 I1 . Ag2 . 111.65(3) yes Ag1 . I1 . Ag2 . 61.37(3) yes Ag3 4_656 I1 . Ag3 . 80.65(4) yes Ag1 . I1 . Ag3 . 104.59(4) yes Ag2 . I1 . Ag3 . 68.70(3) yes Ag1 5_655 I2 . Ag2 5_655 63.28(3) yes Ag1 5_655 I2 . Ag1 . 84.46(4) yes Ag2 5_655 I2 . Ag1 . 103.68(3) yes Ag2 5_655 I3 . Ag2 . 93.49(5) yes Ag2 . I4 . Ag3 . 71.82(4) yes Ag3 4_656 I5 . Ag1 . 75.10(4) yes Ag3 4_656 Ag1 . I1 . 54.73(2) yes Ag3 4_656 Ag1 . I2 5_655 131.93(4) yes I1 . Ag1 . I2 5_655 118.17(4) yes Ag3 4_656 Ag1 . I2 . 132.71(4) yes I1 . Ag1 . I2 . 100.70(4) yes I2 5_655 Ag1 . I2 . 94.68(4) yes Ag3 4_656 Ag1 . I5 . 52.74(2) yes I1 . Ag1 . I5 . 106.75(4) yes I2 5_655 Ag1 . I5 . 115.77(3) yes I2 . Ag1 . I5 . 120.14(3) yes I1 . Ag2 . I2 5_655 116.57(3) yes I1 . Ag2 . I4 . 107.83(3) yes I2 5_655 Ag2 . I4 . 98.08(3) yes I1 . Ag2 . I3 . 96.99(3) yes I2 5_655 Ag2 . I3 . 114.94(3) yes I4 . Ag2 . I3 . 123.47(3) yes I1 . Ag2 . Ag3 . 54.13(2) yes I2 5_655 Ag2 . Ag3 . 124.79(3) yes I4 . Ag2 . Ag3 . 54.02(3) yes I3 . Ag2 . Ag3 . 120.13(4) yes Ag2 . Ag3 . Ag1 4_656 166.79(4) yes Ag2 . Ag3 . I1 4_656 118.29(3) yes Ag1 4_656 Ag3 . I1 4_656 54.66(2) yes Ag2 . Ag3 . I1 . 57.17(3) yes Ag1 4_656 Ag3 . I1 . 111.01(4) yes I1 4_656 Ag3 . I1 . 99.35(4) yes Ag2 . Ag3 . I4 . 54.16(3) yes Ag1 4_656 Ag3 . I4 . 136.14(4) yes I1 4_656 Ag3 . I4 . 106.17(4) yes I1 . Ag3 . I4 . 110.99(4) yes Ag2 . Ag3 . I5 4_656 135.42(4) yes Ag1 4_656 Ag3 . I5 4_656 52.16(2) yes I1 4_656 Ag3 . I5 4_656 106.11(4) yes I1 . Ag3 . I5 4_656 113.84(4) yes I4 . Ag3 . I5 4_656 118.15(4) yes O3 5_655 Tb1 . O4 5_655 81.0(6) yes O3 5_655 Tb1 . O2 5_655 130.3(3) yes O4 5_655 Tb1 . O2 5_655 143.5(6) yes O3 5_655 Tb1 . O1 5_655 143.8(3) yes O4 5_655 Tb1 . O1 5_655 85.6(7) yes O2 5_655 Tb1 . O1 5_655 77.0(3) yes O3 5_655 Tb1 . O2 . 73.0(3) yes O4 5_655 Tb1 . O2 . 73.2(7) yes O2 5_655 Tb1 . O2 . 128.1(4) yes O1 5_655 Tb1 . O2 . 70.9(3) yes O3 5_655 Tb1 . O3 . 132.0(4) yes O4 5_655 Tb1 . O3 . 71.2(6) yes O2 5_655 Tb1 . O3 . 73.0(2) yes O1 5_655 Tb1 . O3 . 72.9(3) yes O2 . Tb1 . O3 . 130.3(3) yes O3 5_655 Tb1 . O1 . 72.9(3) yes O4 5_655 Tb1 . O1 . 145.0(6) yes O2 5_655 Tb1 . O1 . 70.9(3) yes O1 5_655 Tb1 . O1 . 101.7(4) yes O2 . Tb1 . O1 . 77.0(3) yes O3 5_655 Tb1 . O4 . 71.2(6) yes O4 5_655 Tb1 . O4 . 107.9(13) yes O2 5_655 Tb1 . O4 . 73.2(7) yes O1 5_655 Tb1 . O4 . 145.0(6) yes O2 . Tb1 . O4 . 143.5(6) yes O3 . Tb1 . O1 . 143.8(3) yes O3 . Tb1 . O4 . 81.0(6) yes O1 . Tb1 . O4 . 85.6(7) yes O3 5_655 Tb1 . O2 5_655 130.3(3) yes O3 5_655 Tb1 . O1 5_655 143.8(3) yes O2 5_655 Tb1 . O1 5_655 77.0(3) yes O3 5_655 Tb1 . O5 5_655 71.3(4) yes O2 5_655 Tb1 . O5 5_655 144.7(4) yes O1 5_655 Tb1 . O5 5_655 99.9(4) yes O3 5_655 Tb1 . S1 5_655 83.48(19) yes O2 5_655 Tb1 . S1 5_655 126.1(2) yes O1 5_655 Tb1 . S1 5_655 98.6(2) yes O5 5_655 Tb1 . S1 5_655 18.6(4) yes O3 5_655 Tb1 . O2 . 73.0(3) yes O2 5_655 Tb1 . O2 . 128.1(4) yes O1 5_655 Tb1 . O2 . 70.9(3) yes O5 5_655 Tb1 . O2 . 81.4(5) yes S1 5_655 Tb1 . O2 . 98.5(2) yes O3 5_655 Tb1 . O3 . 132.0(4) yes O2 5_655 Tb1 . O3 . 73.0(2) yes O1 5_655 Tb1 . O3 . 72.9(3) yes O5 5_655 Tb1 . O3 . 72.5(4) yes S1 5_655 Tb1 . O3 . 55.06(18) yes O3 5_655 Tb1 . O1 . 72.9(3) yes O2 5_655 Tb1 . O1 . 70.9(3) yes O1 5_655 Tb1 . O1 . 101.7(4) yes O5 5_655 Tb1 . O1 . 142.3(4) yes S1 5_655 Tb1 . O1 . 156.3(2) yes O3 5_655 Tb1 . S1 . 55.06(18) yes O2 5_655 Tb1 . S1 . 98.5(2) yes O1 5_655 Tb1 . S1 . 156.3(2) yes O5 5_655 Tb1 . S1 . 70.1(4) yes S1 5_655 Tb1 . S1 . 64.91(14) yes O3 5_655 Tb1 . O5 . 72.5(4) yes O2 5_655 Tb1 . O5 . 81.4(5) yes O1 5_655 Tb1 . O5 . 142.3(4) yes O5 5_655 Tb1 . O5 . 80.5(8) yes S1 5_655 Tb1 . O5 . 70.1(4) yes O2 . Tb1 . O3 . 130.3(3) yes O2 . Tb1 . O1 . 77.0(3) yes O3 . Tb1 . O1 . 143.8(3) yes O2 . Tb1 . S1 . 126.1(2) yes O3 . Tb1 . S1 . 83.48(19) yes O1 . Tb1 . S1 . 98.6(2) yes O2 . Tb1 . O5 . 144.7(4) yes O3 . Tb1 . O5 . 71.3(4) yes O1 . Tb1 . O5 . 99.9(4) yes S1 . Tb1 . O5 . 18.6(4) yes C6 . N2 . C5 . 118.6(9) yes C6 . N2 . C4 . 120.0(9) yes C5 . N2 . C4 . 121.3(9) yes C2 . N1 . C3 . 118.1(12) yes C2 . N1 . C1 . 120.4(10) yes C3 . N1 . C1 . 121.4(11) yes Tb1 . O2 . C4 . 137.7(6) yes Tb1 . O3 . C7 . 128.3(7) yes C9 . N3 . C8 . 117.2(7) yes C9 . N3 . C7 . 121.4(8) yes C8 . N3 . C7 . 121.2(8) yes Tb1 . O1 . C1 . 147.9(8) yes C13 . S1 . Tb1 . 110.3(7) yes C13 . S1 . O5 . 104.7(10) yes Tb1 . S1 . O5 . 28.2(6) yes C13 . S1 . C14 . 97.8(11) yes Tb1 . S1 . C14 . 129.6(8) yes O5 . S1 . C14 . 105.6(10) yes C12 . N4 . C10 . 120(3) yes C12 . N4 . C11 . 116(3) yes C10 . N4 . C11 . 124(3) yes Tb1 . O4 . C10 . 144(2) yes Tb1 . O5 . S1 . 133.1(8) yes S1 . C14 . H141 . 110.0 no S1 . C14 . H142 . 110.6 no H141 . C14 . H142 . 109.5 no S1 . C14 . H143 . 107.8 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N4 . C11 . H111 . 117.3 no N4 . C11 . H112 . 116.5 no H111 . C11 . H112 . 109.5 no N4 . C11 . H113 . 93.2 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no #===END