# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2059 data_global _publ_contact_author ; Magnus Sandström Department of Chemistry Royal institute of technology S-100-44 Stockholm Sweden ; _publ_contact_author_phone '46 8 7908156' _publ_contact_author_fax '46 8 212626' _publ_contact_author_email magnus@inorg.kth.se _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' # ============================================================= loop_ _publ_author_name _publ_author_address 'Patric Lindquist-Reis'' ; Department of Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; 'Jan Näslund' ; Departement of Chemistry, SLU Box 7015 S-750 07 Uppsala Sweden ; 'Ingmar Persson' ; Departement of Chemistry, SLU Box 7015 S-750 07 Uppsala Sweden ; 'Magnus Sandström' ; Department of Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; #======================================= data_[Y(dmso)8]I3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; octakis(dimethylsulfoxide)yttrium(III)iodide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 I3 O8 S8 Y' _chemical_formula_weight 1094.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3726(13) _cell_length_b 18.883(2) _cell_length_c 18.035(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.977(2) _cell_angle_gamma 90.00 _cell_volume 4149.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6198 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 1.84 _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 4.070 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24595 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9536 _reflns_number_gt 6198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc, and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+0.5777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9536 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y Y 0.90878(3) 0.22820(2) 0.68408(2) 0.03944(14) Uani 1 1 d . . . S1A S 0.69486(11) 0.13947(8) 0.74671(8) 0.0556(3) Uani 1 1 d . . . S2A S 0.65126(11) 0.30493(7) 0.60813(8) 0.0518(3) Uani 1 1 d . . . S3A S 1.17380(12) 0.29980(9) 0.76148(9) 0.0659(4) Uani 1 1 d . . . S4A S 1.11657(12) 0.14952(9) 0.60349(9) 0.0620(4) Uani 1 1 d . . . S5A S 0.7915(2) 0.09995(13) 0.54714(13) 0.0691(9) Uani 0.760(6) 1 d P . . S5B S 0.7197(7) 0.1376(4) 0.5350(5) 0.079(3) Uani 0.240(6) 1 d P . . S6A S 1.0256(3) 0.0814(2) 0.7941(2) 0.0712(14) Uani 0.538(7) 1 d P . . S6B S 1.0891(3) 0.1170(2) 0.8215(2) 0.0627(14) Uani 0.462(7) 1 d P . . S7 S 0.98151(15) 0.34793(10) 0.55500(11) 0.0796(5) Uani 1 1 d . . . S8 S 0.85318(16) 0.30842(10) 0.84552(11) 0.0697(7) Uani 0.886(5) 1 d P . . S8B S 0.9504(13) 0.3170(9) 0.8664(10) 0.080(6) Uani 0.114(5) 1 d P . . O1 O 0.8123(3) 0.1672(2) 0.7670(2) 0.0553(9) Uani 1 1 d . . . O2 O 0.7357(3) 0.2835(2) 0.6755(2) 0.0561(9) Uani 1 1 d . . . O3 O 1.0804(3) 0.2864(2) 0.6967(2) 0.0697(11) Uani 1 1 d . . . O4 O 1.0011(3) 0.1794(2) 0.5914(2) 0.0716(11) Uani 1 1 d . . . O5 O 0.7887(4) 0.1565(2) 0.6041(2) 0.0772(13) Uani 1 1 d . . . O6A O 1.0298(4) 0.1498(3) 0.7532(3) 0.0853(15) Uani 1 1 d . . . O7 O 0.8898(3) 0.3145(2) 0.5887(2) 0.0687(12) Uani 1 1 d . . . O8 O 0.9299(3) 0.2978(2) 0.7912(2) 0.0695(11) Uani 1 1 d . . . I1 I 1.27787(4) 0.42183(2) 0.51636(2) 0.07010(15) Uani 1 1 d . . . I2 I 0.54160(5) 0.39942(3) 0.83368(3) 0.0916(2) Uani 1 1 d . . . I3 I 0.41248(4) 0.06521(3) 0.65044(4) 0.0985(2) Uani 1 1 d . . . C1A C 0.6238(5) 0.1768(4) 0.8153(4) 0.0755(19) Uani 1 1 d . . . C1B C 0.7044(6) 0.0503(3) 0.7809(4) 0.0769(19) Uani 1 1 d . . . C2A C 0.5216(5) 0.2837(4) 0.6349(4) 0.0708(17) Uani 1 1 d . . . C2B C 0.6416(7) 0.3990(3) 0.6155(5) 0.085(2) Uani 1 1 d . . . C3A C 1.2921(7) 0.2625(6) 0.7329(8) 0.150(5) Uani 1 1 d . . . C3B C 1.2082(8) 0.3900(4) 0.7526(5) 0.105(3) Uani 1 1 d . . . C4A C 1.1013(6) 0.0640(3) 0.5617(4) 0.0731(18) Uani 1 1 d . . . C4B C 1.1807(6) 0.1917(4) 0.5347(4) 0.079(2) Uani 1 1 d . . . C5A C 0.7836(11) 0.1420(8) 0.4612(5) 0.160(5) Uani 1 1 d . . . C5B C 0.6668(14) 0.0591(8) 0.5396(7) 0.211(9) Uani 1 1 d . . . C6A C 1.0212(13) 0.0791(10) 0.8765(9) 0.251(12) Uani 1 1 d . . . C6B C 1.1699(9) 0.0484(6) 0.7920(5) 0.128(4) Uani 1 1 d . . . C7A C 0.9884(7) 0.4385(4) 0.5891(6) 0.105(3) Uani 1 1 d . . . C7B C 0.9206(10) 0.3644(7) 0.4581(5) 0.143(4) Uani 1 1 d . . . C8A C 0.8689(11) 0.3972(5) 0.8762(8) 0.147(5) Uani 1 1 d . . . C8B C 0.9208(11) 0.2654(7) 0.9305(5) 0.151(5) Uani 1 1 d . . . 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 Y 0.0337(2) 0.0412(3) 0.0457(3) 0.00484(19) 0.01313(18) 0.00019(18) S1A 0.0424(7) 0.0656(9) 0.0589(8) 0.0176(7) 0.0088(6) -0.0086(6) S2A 0.0473(7) 0.0561(8) 0.0529(7) 0.0012(6) 0.0110(6) 0.0088(6) S3A 0.0497(8) 0.0782(10) 0.0712(10) -0.0018(8) 0.0145(7) -0.0152(7) S4A 0.0460(8) 0.0762(10) 0.0664(9) -0.0142(8) 0.0164(7) 0.0018(7) S5A 0.0756(17) 0.0663(15) 0.0645(13) -0.0168(10) 0.0100(11) 0.0047(12) S5B 0.080(6) 0.056(4) 0.100(6) 0.001(4) 0.015(4) -0.002(4) S6A 0.064(2) 0.068(2) 0.081(2) 0.0140(17) 0.0109(17) 0.0159(19) S6B 0.060(2) 0.053(2) 0.075(2) 0.0103(17) 0.0135(19) 0.0052(18) S7 0.0729(11) 0.0736(10) 0.1046(13) 0.0406(10) 0.0499(10) 0.0139(8) S8 0.0639(14) 0.0723(12) 0.0798(13) -0.0167(9) 0.0319(10) -0.0044(9) S8B 0.059(10) 0.092(12) 0.095(12) -0.021(9) 0.029(8) -0.006(8) O1 0.042(2) 0.065(2) 0.061(2) 0.0153(19) 0.0147(17) -0.0064(17) O2 0.0415(19) 0.068(2) 0.060(2) 0.0085(18) 0.0125(16) 0.0127(17) O3 0.050(2) 0.085(3) 0.074(3) 0.007(2) 0.012(2) -0.022(2) O4 0.054(2) 0.084(3) 0.079(3) -0.008(2) 0.017(2) 0.010(2) O5 0.077(3) 0.084(3) 0.076(3) -0.029(2) 0.027(2) -0.027(2) O6A 0.058(3) 0.096(3) 0.106(4) 0.055(3) 0.027(2) 0.027(2) O7 0.053(2) 0.073(3) 0.085(3) 0.038(2) 0.026(2) 0.006(2) O8 0.065(3) 0.080(3) 0.066(3) -0.021(2) 0.021(2) -0.016(2) I1 0.0683(3) 0.0782(3) 0.0631(3) -0.0058(2) 0.0092(2) -0.0061(2) I2 0.0858(4) 0.1159(4) 0.0701(3) -0.0238(3) 0.0045(2) 0.0261(3) I3 0.0528(3) 0.0865(4) 0.1489(5) -0.0205(3) -0.0030(3) 0.0003(2) C1A 0.052(3) 0.101(5) 0.081(4) 0.005(4) 0.031(3) 0.001(3) C1B 0.077(4) 0.057(4) 0.095(5) 0.022(3) 0.012(4) -0.014(3) C2A 0.044(3) 0.082(4) 0.085(4) -0.002(4) 0.007(3) 0.000(3) C2B 0.103(6) 0.050(4) 0.104(6) 0.006(4) 0.023(5) 0.008(4) C3A 0.051(4) 0.160(10) 0.232(12) -0.113(9) 0.008(6) -0.007(5) C3B 0.120(7) 0.067(5) 0.122(7) -0.012(4) 0.006(6) -0.030(5) C4A 0.072(4) 0.063(4) 0.087(5) -0.012(3) 0.024(4) -0.005(3) C4B 0.075(4) 0.088(5) 0.083(5) -0.004(4) 0.039(4) -0.007(4) C5A 0.170(11) 0.247(15) 0.064(5) 0.015(7) 0.021(6) -0.023(10) C5B 0.278(18) 0.233(15) 0.139(10) -0.098(10) 0.085(11) -0.204(15) C6A 0.203(14) 0.35(2) 0.246(16) 0.235(17) 0.160(13) 0.181(15) C6B 0.135(8) 0.159(9) 0.098(6) 0.040(6) 0.038(6) 0.098(7) C7A 0.094(6) 0.061(4) 0.166(9) 0.027(5) 0.043(6) 0.004(4) C7B 0.170(11) 0.183(11) 0.080(6) 0.034(7) 0.036(6) -0.014(9) C8A 0.176(11) 0.067(5) 0.218(12) -0.043(7) 0.092(10) -0.021(6) C8B 0.225(14) 0.151(10) 0.085(6) 0.035(6) 0.053(8) 0.043(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y O6A 2.311(4) . ? Y O8 2.314(4) . ? Y O5 2.320(4) . ? Y O7 2.352(4) . ? Y O2 2.363(3) . ? Y O3 2.367(4) . ? Y O4 2.367(4) . ? Y O1 2.368(3) . ? S1A O1 1.528(4) . ? S1A C1A 1.782(7) . ? S1A C1B 1.791(6) . ? S2A O2 1.514(4) . ? S2A C2B 1.787(7) . ? S2A C2A 1.799(6) . ? S3A O3 1.516(4) . ? S3A C3B 1.770(8) . ? S3A C3A 1.779(9) . ? S4A O4 1.517(4) . ? S4A C4B 1.774(7) . ? S4A C4A 1.778(7) . ? S5A S5B 1.130(9) . ? S5A O5 1.486(5) . ? S5A C5B 1.709(12) . ? S5A C5A 1.729(10) . ? S5B O5 1.429(9) . ? S5B C5B 1.627(13) . ? S5B C5A 1.663(13) . ? S6A S6B 1.086(5) . ? S6A O6A 1.493(5) . ? S6A C6A 1.498(15) . ? S6A C6B 1.898(9) . ? S6B O6A 1.459(5) . ? S6B C6A 1.577(12) . ? S6B C6B 1.773(9) . ? S7 O7 1.515(4) . ? S7 C7B 1.806(10) . ? S7 C7A 1.815(9) . ? S8 S8B 1.208(16) . ? S8 O8 1.490(4) . ? S8 C8A 1.766(9) . ? S8 C8B 1.807(10) . ? S8B O8 1.384(17) . ? S8B C8B 1.60(2) . ? S8B C8A 1.84(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6A Y O8 86.83(18) . . ? O6A Y O5 104.3(2) . . ? O8 Y O5 144.94(14) . . ? O6A Y O7 144.26(14) . . ? O8 Y O7 101.51(17) . . ? O5 Y O7 88.72(17) . . ? O6A Y O2 144.46(14) . . ? O8 Y O2 76.92(14) . . ? O5 Y O2 75.04(15) . . ? O7 Y O2 70.80(13) . . ? O6A Y O3 76.06(16) . . ? O8 Y O3 71.71(15) . . ? O5 Y O3 142.96(15) . . ? O7 Y O3 73.88(15) . . ? O2 Y O3 126.04(16) . . ? O6A Y O4 77.55(16) . . ? O8 Y O4 144.26(15) . . ? O5 Y O4 70.69(15) . . ? O7 Y O4 75.69(15) . . ? O2 Y O4 131.92(14) . . ? O3 Y O4 73.39(15) . . ? O6A Y O1 72.44(13) . . ? O8 Y O1 75.23(14) . . ? O5 Y O1 76.73(14) . . ? O7 Y O1 143.29(13) . . ? O2 Y O1 72.92(13) . . ? O3 Y O1 135.01(14) . . ? O4 Y O1 127.89(16) . . ? O1 S1A C1A 105.1(3) . . ? O1 S1A C1B 103.7(3) . . ? C1A S1A C1B 98.3(4) . . ? O2 S2A C2B 104.6(3) . . ? O2 S2A C2A 104.4(3) . . ? C2B S2A C2A 97.3(4) . . ? O3 S3A C3B 104.7(4) . . ? O3 S3A C3A 105.5(4) . . ? C3B S3A C3A 97.6(5) . . ? O4 S4A C4B 104.9(3) . . ? O4 S4A C4A 104.4(3) . . ? C4B S4A C4A 98.0(3) . . ? S5B S5A O5 64.6(5) . . ? S5B S5A C5B 66.4(8) . . ? O5 S5A C5B 104.5(5) . . ? S5B S5A C5A 67.4(7) . . ? O5 S5A C5A 106.5(5) . . ? C5B S5A C5A 103.0(7) . . ? S5A S5B O5 69.9(5) . . ? S5A S5B C5B 74.2(8) . . ? O5 S5B C5B 111.5(7) . . ? S5A S5B C5A 73.7(7) . . ? O5 S5B C5A 112.9(7) . . ? C5B S5B C5A 109.8(8) . . ? S6B S6A O6A 66.8(4) . . ? S6B S6A C6A 73.3(9) . . ? O6A S6A C6A 121.7(8) . . ? S6B S6A C6B 66.6(5) . . ? O6A S6A C6B 99.2(4) . . ? C6A S6A C6B 101.9(6) . . ? S6A S6B O6A 70.1(4) . . ? S6A S6B C6A 65.4(9) . . ? O6A S6B C6A 118.6(6) . . ? S6A S6B C6B 79.2(5) . . ? O6A S6B C6B 106.5(4) . . ? C6A S6B C6B 104.4(7) . . ? O7 S7 C7B 104.1(4) . . ? O7 S7 C7A 104.5(3) . . ? C7B S7 C7A 98.7(5) . . ? S8B S8 O8 60.6(8) . . ? S8B S8 C8A 74.0(9) . . ? O8 S8 C8A 106.6(4) . . ? S8B S8 C8B 60.4(10) . . ? O8 S8 C8B 104.1(4) . . ? C8A S8 C8B 98.7(6) . . ? S8 S8B O8 69.8(9) . . ? S8 S8B C8B 78.6(10) . . ? O8 S8B C8B 121.4(12) . . ? S8 S8B C8A 67.0(8) . . ? O8 S8B C8A 107.4(12) . . ? C8B S8B C8A 103.4(10) . . ? S1A O1 Y 125.3(2) . . ? S2A O2 Y 131.5(2) . . ? S3A O3 Y 134.7(2) . . ? S4A O4 Y 127.0(3) . . ? S5B O5 S5A 45.6(4) . . ? S5B O5 Y 155.5(4) . . ? S5A O5 Y 139.5(3) . . ? S6B O6A S6A 43.1(2) . . ? S6B O6A Y 155.7(3) . . ? S6A O6A Y 138.2(3) . . ? S7 O7 Y 126.5(2) . . ? S8B O8 S8 49.5(6) . . ? S8B O8 Y 160.4(8) . . ? S8 O8 Y 129.2(2) . . ? S5B C5A S5A 38.9(4) . . ? S5B C5B S5A 39.5(4) . . ? S6A C6A S6B 41.2(3) . . ? S6B C6B S6A 34.2(2) . . ? S8 C8A S8B 39.0(5) . . ? S8B C8B S8 40.9(6) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.387 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.126 CIF [Y(dmpu)6]I3 data_global _publ_contact_author ; Magnus Sandström Department of Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; _publ_contact_author_phone '46 8 7908156 ' _publ_contact_author_fax '46 8 212626' _publ_contact_author_email magnus@inorg.kth.se _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' # ============================================================= loop_ _publ_author_name _publ_author_address 'Patric Lindquist-Reis'' ; Department of Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; 'Jan Näslund' ; Departement of Chemistry, SLU Box 7015 S-750 07 Uppsala Sweden ; 'Ingmar Persson' ; Departement of Chemistry, SLU Box 7015 S-750 07 Uppsala Sweden ; 'Magnus Sandström' ; Department of Chemistry Royal Institute of Technology S-100 44 Stockholm Sweden ; #======================================= data_[Y(dmpu)6]I3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(N,N'-dimethylpropyleneurea)yttrium(III)iodide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 I3 N12 O6 Y' _chemical_formula_weight 1238.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ' monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1696(12) _cell_length_b 12.1227(13) _cell_length_c 17.9365(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.905(2) _cell_angle_gamma 90.00 _cell_volume 2644.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0 _cell_measurement_theta_max 58 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 2.902 _exptl_absorpt_correction_type 'empirical ' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD-area detector' _diffrn_measurement_method 'hemisphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15031 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6078 _reflns_number_gt 3586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6078 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y Y 0.5000 0.5000 0.0000 0.04125(15) Uani 1 2 d S . . I1 I 0.47672(3) 0.97039(5) 0.23337(2) 0.0916(2) Uani 1 1 d . . . I2 I 0.0000 0.0000 0.0000 0.0825(2) Uani 1 2 d S . . O1 O 0.4392(2) 0.5552(3) 0.10888(16) 0.0573(7) Uani 1 1 d . . . O2 O 0.6476(2) 0.6060(2) 0.01703(15) 0.0521(7) Uani 1 1 d . . . N31 N 0.7430(3) 0.2953(3) 0.1095(2) 0.0574(9) Uani 1 1 d . . . O3 O 0.5845(2) 0.3597(2) 0.05705(16) 0.0541(7) Uani 1 1 d . . . N12 N 0.4120(3) 0.5110(4) 0.2297(2) 0.0658(11) Uani 1 1 d . . . N11 N 0.3288(3) 0.6640(3) 0.1755(2) 0.0601(9) Uani 1 1 d . . . C1 C 0.3945(3) 0.5770(4) 0.1702(2) 0.0526(10) Uani 1 1 d . . . N21 N 0.7543(3) 0.7039(4) 0.0979(2) 0.0655(10) Uani 1 1 d . . . C3 C 0.6432(3) 0.2778(4) 0.0770(2) 0.0486(10) Uani 1 1 d . . . N22 N 0.8237(3) 0.6340(3) -0.0118(2) 0.0618(10) Uani 1 1 d . . . C2 C 0.7407(3) 0.6473(3) 0.0336(2) 0.0496(10) Uani 1 1 d . . . N32 N 0.6063(3) 0.1750(3) 0.0669(2) 0.0611(10) Uani 1 1 d . . . C32 C 0.8194(4) 0.2043(5) 0.1287(3) 0.0738(14) Uani 1 1 d . . . H32A H 0.8645 0.2243 0.1722 0.089 Uiso 1 1 calc R . . H32B H 0.8676 0.1914 0.0876 0.089 Uiso 1 1 calc R . . C34 C 0.6753(4) 0.0793(4) 0.0828(3) 0.0777(15) Uani 1 1 d . . . H34A H 0.7136 0.0588 0.0383 0.093 Uiso 1 1 calc R . . H34B H 0.6294 0.0176 0.0966 0.093 Uiso 1 1 calc R . . C16 C 0.4796(5) 0.4135(7) 0.2227(3) 0.100(2) Uani 1 1 d . . . H16A H 0.4930 0.4006 0.1710 0.149 Uiso 1 1 calc R . . H16B H 0.4422 0.3510 0.2429 0.149 Uiso 1 1 calc R . . H16C H 0.5483 0.4243 0.2495 0.149 Uiso 1 1 calc R . . C35 C 0.7866(4) 0.4058(5) 0.1148(3) 0.0879(17) Uani 1 1 d . . . H35A H 0.7312 0.4545 0.1328 0.132 Uiso 1 1 calc R . . H35B H 0.8082 0.4298 0.0665 0.132 Uiso 1 1 calc R . . H35C H 0.8492 0.4065 0.1488 0.132 Uiso 1 1 calc R . . C12 C 0.3560(5) 0.5282(6) 0.2989(3) 0.0892(18) Uani 1 1 d . . . H12A H 0.4005 0.4989 0.3402 0.107 Uiso 1 1 calc R . . H12B H 0.2864 0.4891 0.2971 0.107 Uiso 1 1 calc R . . C27 C 0.8065(4) 0.5805(5) -0.0828(3) 0.0847(17) Uani 1 1 d . . . H27A H 0.8040 0.5021 -0.0756 0.127 Uiso 1 1 calc R . . H27B H 0.8659 0.5985 -0.1146 0.127 Uiso 1 1 calc R . . H27C H 0.7383 0.6051 -0.1055 0.127 Uiso 1 1 calc R . . C26 C 0.6626(5) 0.7231(6) 0.1465(3) 0.0921(18) Uani 1 1 d . . . H26A H 0.6876 0.7163 0.1976 0.138 Uiso 1 1 calc R . . H26B H 0.6059 0.6697 0.1359 0.138 Uiso 1 1 calc R . . H26C H 0.6339 0.7960 0.1380 0.138 Uiso 1 1 calc R . . C22 C 0.9327(4) 0.6801(5) 0.0040(4) 0.0917(19) Uani 1 1 d . . . H22A H 0.9388 0.7514 -0.0201 0.110 Uiso 1 1 calc R . . H22B H 0.9881 0.6317 -0.0157 0.110 Uiso 1 1 calc R . . C15 C 0.3036(4) 0.7331(5) 0.1102(3) 0.0814(16) Uani 1 1 d . . . H15A H 0.2541 0.6944 0.0766 0.122 Uiso 1 1 calc R . . H15B H 0.3703 0.7496 0.0853 0.122 Uiso 1 1 calc R . . H15C H 0.2699 0.8005 0.1258 0.122 Uiso 1 1 calc R . . C36 C 0.4977(4) 0.1541(5) 0.0359(4) 0.0938(19) Uani 1 1 d . . . H36A H 0.4600 0.2228 0.0278 0.141 Uiso 1 1 calc R . . H36B H 0.4575 0.1096 0.0699 0.141 Uiso 1 1 calc R . . H36C H 0.5031 0.1158 -0.0107 0.141 Uiso 1 1 calc R . . C33 C 0.7571(4) 0.1022(5) 0.1444(3) 0.0815(16) Uani 1 1 d . . . H33A H 0.7195 0.1104 0.1909 0.098 Uiso 1 1 calc R . . H33B H 0.8076 0.0405 0.1497 0.098 Uiso 1 1 calc R . . C13 C 0.2765(5) 0.6964(5) 0.2455(3) 0.0833(17) Uani 1 1 d . . . H13A H 0.2759 0.7762 0.2494 0.100 Uiso 1 1 calc R . . H13B H 0.2009 0.6710 0.2443 0.100 Uiso 1 1 calc R . . C14 C 0.3357(6) 0.6492(6) 0.3113(3) 0.099(2) Uani 1 1 d . . . H14A H 0.2924 0.6592 0.3552 0.119 Uiso 1 1 calc R . . H14B H 0.4052 0.6872 0.3195 0.119 Uiso 1 1 calc R . . C23 C 0.9512(5) 0.6928(6) 0.0863(5) 0.113(3) Uani 1 1 d . . . H23A H 0.9585 0.6204 0.1090 0.135 Uiso 1 1 calc R . . H23B H 1.0193 0.7326 0.0961 0.135 Uiso 1 1 calc R . . C24 C 0.8603(5) 0.7523(6) 0.1198(3) 0.095(2) Uani 1 1 d . . . H24A H 0.8696 0.7502 0.1737 0.114 Uiso 1 1 calc R . . H24B H 0.8618 0.8289 0.1043 0.114 Uiso 1 1 calc 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 Y 0.0389(3) 0.0374(3) 0.0471(3) -0.0011(2) -0.0037(2) 0.0016(2) I1 0.0771(3) 0.1150(4) 0.0828(3) 0.0062(2) 0.0031(2) 0.0039(2) I2 0.1091(4) 0.0644(3) 0.0742(3) -0.0088(2) 0.0063(3) -0.0148(3) O1 0.0609(16) 0.061(2) 0.0503(16) -0.0048(14) 0.0040(14) 0.0069(14) O2 0.0451(14) 0.0512(18) 0.0597(17) -0.0050(14) -0.0041(13) -0.0051(13) N31 0.0497(19) 0.048(2) 0.074(2) 0.0118(19) -0.0080(18) 0.0034(16) O3 0.0555(15) 0.0379(16) 0.0680(18) 0.0045(14) -0.0132(14) 0.0037(13) N12 0.070(2) 0.076(3) 0.051(2) 0.003(2) -0.0001(18) 0.003(2) N11 0.068(2) 0.053(2) 0.060(2) -0.0086(19) 0.0105(19) 0.0056(19) C1 0.045(2) 0.061(3) 0.051(2) -0.006(2) -0.0052(19) -0.009(2) N21 0.066(2) 0.060(3) 0.070(2) -0.008(2) -0.005(2) -0.0153(19) C3 0.055(2) 0.046(3) 0.045(2) 0.0063(19) 0.0015(19) 0.0063(19) N22 0.0509(19) 0.055(2) 0.080(3) -0.002(2) 0.0144(19) -0.0150(17) C2 0.050(2) 0.036(2) 0.063(3) 0.004(2) -0.005(2) -0.0045(18) N32 0.067(2) 0.039(2) 0.076(3) 0.0048(18) -0.0138(19) 0.0021(17) C32 0.063(3) 0.066(3) 0.091(4) 0.010(3) -0.005(3) 0.019(2) C34 0.090(3) 0.040(3) 0.102(4) 0.015(3) -0.003(3) 0.015(3) C16 0.103(4) 0.115(6) 0.080(4) 0.035(4) 0.004(3) 0.038(4) C35 0.072(3) 0.060(3) 0.129(5) 0.014(3) -0.034(3) -0.009(3) C12 0.102(4) 0.113(5) 0.053(3) 0.004(3) 0.009(3) 0.008(4) C27 0.089(4) 0.080(4) 0.087(4) -0.013(3) 0.030(3) -0.013(3) C26 0.093(4) 0.104(5) 0.080(4) -0.034(4) 0.010(3) -0.012(4) C22 0.056(3) 0.087(5) 0.133(6) -0.009(4) 0.008(3) -0.017(3) C15 0.088(3) 0.075(4) 0.081(4) -0.002(3) -0.001(3) 0.025(3) C36 0.089(4) 0.050(3) 0.139(5) 0.019(4) -0.041(4) -0.018(3) C33 0.077(3) 0.058(3) 0.109(4) 0.025(3) -0.007(3) 0.017(3) C13 0.099(4) 0.066(4) 0.087(4) -0.017(3) 0.037(3) -0.004(3) C14 0.131(5) 0.109(6) 0.057(3) -0.020(3) 0.020(3) -0.007(4) C23 0.059(3) 0.104(5) 0.173(7) 0.018(5) -0.029(4) -0.036(3) C24 0.086(4) 0.100(5) 0.097(4) -0.013(4) -0.021(3) -0.043(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y O1 2.215(3) 3_665 ? Y O1 2.215(3) . ? Y O3 2.220(3) 3_665 ? Y O3 2.220(3) . ? Y O2 2.221(3) 3_665 ? Y O2 2.221(3) . ? O1 C1 1.271(5) . ? O2 C2 1.265(4) . ? N31 C3 1.346(5) . ? N31 C35 1.443(6) . ? N31 C32 1.476(6) . ? O3 C3 1.268(5) . ? N12 C1 1.346(6) . ? N12 C16 1.448(8) . ? N12 C12 1.450(6) . ? N11 C1 1.329(6) . ? N11 C15 1.465(6) . ? N11 C13 1.479(6) . ? N21 C2 1.346(6) . ? N21 C26 1.458(6) . ? N21 C24 1.459(6) . ? C3 N32 1.334(6) . ? N22 C2 1.329(5) . ? N22 C27 1.437(6) . ? N22 C22 1.458(6) . ? N32 C36 1.440(6) . ? N32 C34 1.456(6) . ? C32 C33 1.483(7) . ? C34 C33 1.487(7) . ? C12 C14 1.506(9) . ? C22 C23 1.494(9) . ? C13 C14 1.478(8) . ? C23 C24 1.467(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y O1 180.0 3_665 . ? O1 Y O3 89.34(11) 3_665 3_665 ? O1 Y O3 90.66(11) . 3_665 ? O1 Y O3 90.66(11) 3_665 . ? O1 Y O3 89.34(11) . . ? O3 Y O3 180.00(16) 3_665 . ? O1 Y O2 89.78(10) 3_665 3_665 ? O1 Y O2 90.22(10) . 3_665 ? O3 Y O2 91.12(10) 3_665 3_665 ? O3 Y O2 88.88(10) . 3_665 ? O1 Y O2 90.22(10) 3_665 . ? O1 Y O2 89.78(10) . . ? O3 Y O2 88.88(10) 3_665 . ? O3 Y O2 91.12(10) . . ? O2 Y O2 180.00(18) 3_665 . ? C1 O1 Y 172.3(3) . . ? C2 O2 Y 167.2(3) . . ? C3 N31 C35 120.0(4) . . ? C3 N31 C32 122.4(4) . . ? C35 N31 C32 116.8(4) . . ? C3 O3 Y 168.0(3) . . ? C1 N12 C16 119.4(4) . . ? C1 N12 C12 121.8(5) . . ? C16 N12 C12 118.5(5) . . ? C1 N11 C15 120.4(4) . . ? C1 N11 C13 123.3(4) . . ? C15 N11 C13 116.2(4) . . ? O1 C1 N11 120.2(4) . . ? O1 C1 N12 120.2(4) . . ? N11 C1 N12 119.6(4) . . ? C2 N21 C26 121.2(4) . . ? C2 N21 C24 121.2(4) . . ? C26 N21 C24 117.5(4) . . ? O3 C3 N32 120.6(4) . . ? O3 C3 N31 119.4(4) . . ? N32 C3 N31 120.0(4) . . ? C2 N22 C27 120.5(4) . . ? C2 N22 C22 122.6(4) . . ? C27 N22 C22 116.7(4) . . ? O2 C2 N22 120.0(4) . . ? O2 C2 N21 119.2(4) . . ? N22 C2 N21 120.8(4) . . ? C3 N32 C36 121.2(4) . . ? C3 N32 C34 121.9(4) . . ? C36 N32 C34 116.8(4) . . ? N31 C32 C33 110.3(4) . . ? N32 C34 C33 111.4(5) . . ? N12 C12 C14 110.5(5) . . ? N22 C22 C23 109.8(5) . . ? C32 C33 C34 110.4(5) . . ? C14 C13 N11 111.2(5) . . ? C13 C14 C12 109.7(5) . . ? C24 C23 C22 111.4(5) . . ? N21 C24 C23 111.3(5) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.022 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.100