# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_UTSA-61 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C330 H534 N51 O75 Tb3' _chemical_formula_weight 6892.84 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I432 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' _cell_length_a 33.0001(4) _cell_length_b 33.0001(4) _cell_length_c 33.0001(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 35937.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35845 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 25.05 _exptl_crystal_description block _exptl_crystal_colour 'light red' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14664 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 35845 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5329 _reflns_number_gt 2091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.002 -0.009 -0.003 28491 5993 ' ' _platon_squeeze_details ; About three Me~2~NH~2~ cations and 48 DMA disordered lattice molecules were removed from each formular unit by the SQUEEZE process. ; _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^)+(0.0595P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 5329 _refine_ls_number_parameters 114 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1777 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _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 Tb1 Tb 0.0000 0.60602(3) 0.0000 0.1191(5) Uani 1 4 d S . . O1 O 0.0463(5) 0.6503(5) 0.0327(5) 0.281(6) Uani 1 1 d U . . O2 O 0.0404(6) 0.5884(4) 0.0565(6) 0.252(9) Uani 1 1 d . . . O3 O 0.0000 0.5305(3) 0.0000 0.125(3) Uani 1 4 d S . . C1 C 0.2802(4) 0.7500 0.2198(4) 0.093(6) Uani 1 2 d S . . H1A H 0.3001 0.7500 0.1999 0.111 Uiso 1 2 calc SR . . C2 C 0.2500 0.7195(5) 0.2195(5) 0.134(9) Uani 1 2 d S . . C3 C 0.2500 0.6876(5) 0.1876(5) 0.145(7) Uani 1 2 d S . . C4 C 0.2152(4) 0.6743(4) 0.1717(4) 0.129(4) Uani 1 1 d . . . H4A H 0.1909 0.6843 0.1819 0.155 Uiso 1 1 calc R . . C5 C 0.2139(4) 0.6464(5) 0.1407(4) 0.150(5) Uani 1 1 d D . . C6 C 0.2500 0.6312(4) 0.1312(4) 0.160(7) Uani 1 2 d S . . H6A H 0.2500 0.6113 0.1113 0.192 Uiso 1 2 calc SR . . C7 C 0.1726(4) 0.6351(5) 0.1193(4) 0.177(5) Uani 1 1 d GDU . . C8 C 0.1639(6) 0.5965(4) 0.1050(6) 0.62(3) Uani 1 1 d GU . . H8A H 0.1817 0.5753 0.1101 0.746 Uiso 1 1 calc R . . C9 C 0.1285(7) 0.5895(5) 0.0833(5) 0.333(15) Uani 1 1 d G . . H9A H 0.1227 0.5637 0.0737 0.399 Uiso 1 1 calc R . . C10 C 0.1018(4) 0.6212(8) 0.0758(4) 0.211(8) Uani 1 1 d GD . . C11 C 0.1105(5) 0.6599(6) 0.0900(6) 0.47(2) Uani 1 1 d GU . . H11A H 0.0926 0.6811 0.0850 0.569 Uiso 1 1 calc R . . C12 C 0.1459(5) 0.6669(4) 0.1118(5) 0.398(19) Uani 1 1 d G . . H12A H 0.1517 0.6927 0.1213 0.478 Uiso 1 1 calc R . . C13 C 0.0634(8) 0.6135(6) 0.0479(9) 0.245(15) Uani 1 1 d 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 Tb1 0.1208(6) 0.1156(8) 0.1208(6) 0.000 0.000 0.000 O1 0.263(6) 0.281(6) 0.298(6) -0.0634(15) -0.0011(15) -0.0014(15) O2 0.29(2) 0.183(13) 0.29(2) -0.070(12) -0.020(16) -0.009(12) O3 0.104(5) 0.169(9) 0.104(5) 0.000 0.000 0.000 C1 0.109(9) 0.061(11) 0.109(9) 0.031(7) 0.031(12) 0.031(7) C2 0.20(2) 0.100(11) 0.100(11) -0.002(15) 0.056(11) -0.056(11) C3 0.093(14) 0.170(12) 0.170(12) -0.012(14) -0.039(9) 0.039(9) C4 0.121(11) 0.131(10) 0.134(11) -0.019(8) 0.011(8) 0.020(8) C5 0.126(12) 0.173(14) 0.152(13) -0.020(10) 0.026(9) 0.011(10) C6 0.18(2) 0.152(12) 0.152(12) -0.048(13) 0.015(13) -0.015(13) C7 0.176(6) 0.177(6) 0.177(6) -0.0005(15) -0.0008(15) -0.0001(15) C8 0.62(3) 0.62(3) 0.62(3) 0.0000(15) -0.0001(15) -0.0001(15) C9 0.29(3) 0.31(3) 0.40(4) -0.11(3) -0.03(3) 0.00(3) C10 0.132(14) 0.26(2) 0.242(18) -0.004(16) 0.051(13) -0.041(13) C11 0.47(2) 0.47(2) 0.47(2) -0.0002(15) -0.0002(15) -0.0001(15) C12 0.26(3) 0.50(4) 0.43(4) -0.14(3) -0.12(3) 0.12(3) C13 0.21(2) 0.156(18) 0.37(4) 0.02(2) -0.13(3) 0.014(17) _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 Tb1 O1 2.373(13) . ? Tb1 O1 2.373(13) 23 ? Tb1 O1 2.373(13) 21 ? Tb1 O1 2.373(13) 3 ? Tb1 O2 2.366(18) 3 ? Tb1 O2 2.366(18) 23 ? Tb1 O2 2.366(18) 21 ? Tb1 O2 2.366(18) . ? Tb1 O3 2.494(11) . ? Tb1 C13 2.633(15) . ? Tb1 C13 2.633(15) 3 ? Tb1 C13 2.633(15) 23 ? O1 C13 1.43(2) . ? O2 C13 1.16(3) . ? C1 C2 1.417(8) . ? C1 C2 1.417(8) 12_665 ? C2 C1 1.417(8) 6_566 ? C2 C3 1.49(3) . ? C3 C4 1.337(14) 42_554 ? C3 C4 1.337(14) . ? C4 C5 1.375(15) . ? C5 C6 1.329(13) . ? C5 C7 1.582(11) . ? C6 C5 1.329(13) 42_554 ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C10 C13 1.587(12) . ? C11 C12 1.3900 . ? 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 Tb1 O1 67.7(4) . 23 ? O1 Tb1 O1 67.7(4) . 21 ? O1 Tb1 O1 104.0(8) 23 21 ? O1 Tb1 O1 104.0(8) . 3 ? O1 Tb1 O1 67.7(4) 23 3 ? O1 Tb1 O1 67.7(4) 21 3 ? O1 Tb1 O2 150.8(6) . 3 ? O1 Tb1 O2 113.7(6) 23 3 ? O1 Tb1 O2 84.3(6) 21 3 ? O1 Tb1 O2 55.3(5) 3 3 ? O1 Tb1 O2 113.7(6) . 23 ? O1 Tb1 O2 55.3(5) 23 23 ? O1 Tb1 O2 150.8(6) 21 23 ? O1 Tb1 O2 84.3(6) 3 23 ? O2 Tb1 O2 86.53(15) 3 23 ? O1 Tb1 O2 84.3(6) . 21 ? O1 Tb1 O2 150.8(6) 23 21 ? O1 Tb1 O2 55.3(5) 21 21 ? O1 Tb1 O2 113.7(6) 3 21 ? O2 Tb1 O2 86.53(15) 3 21 ? O2 Tb1 O2 151.5(6) 23 21 ? O1 Tb1 O2 55.3(5) . . ? O1 Tb1 O2 84.3(6) 23 . ? O1 Tb1 O2 113.7(6) 21 . ? O1 Tb1 O2 150.8(6) 3 . ? O2 Tb1 O2 151.5(6) 3 . ? O2 Tb1 O2 86.53(15) 23 . ? O2 Tb1 O2 86.53(15) 21 . ? O1 Tb1 O3 128.0(4) . . ? O1 Tb1 O3 128.0(4) 23 . ? O1 Tb1 O3 128.0(4) 21 . ? O1 Tb1 O3 128.0(4) 3 . ? O2 Tb1 O3 75.8(3) 3 . ? O2 Tb1 O3 75.8(3) 23 . ? O2 Tb1 O3 75.8(3) 21 . ? O2 Tb1 O3 75.8(3) . . ? O1 Tb1 C13 32.7(5) . . ? O1 Tb1 C13 85.3(9) 23 . ? O1 Tb1 C13 88.1(9) 21 . ? O1 Tb1 C13 136.6(7) 3 . ? O2 Tb1 C13 160.8(10) 3 . ? O2 Tb1 C13 108.1(10) 23 . ? O2 Tb1 C13 74.6(11) 21 . ? O2 Tb1 C13 26.1(7) . . ? O3 Tb1 C13 95.4(4) . . ? O1 Tb1 C13 136.6(7) . 3 ? O1 Tb1 C13 88.1(9) 23 3 ? O1 Tb1 C13 85.3(9) 21 3 ? O1 Tb1 C13 32.7(5) 3 3 ? O2 Tb1 C13 26.1(7) 3 3 ? O2 Tb1 C13 74.6(11) 23 3 ? O2 Tb1 C13 108.1(10) 21 3 ? O2 Tb1 C13 160.8(10) . 3 ? O3 Tb1 C13 95.4(4) . 3 ? C13 Tb1 C13 169.3(9) . 3 ? O1 Tb1 C13 88.1(9) . 23 ? O1 Tb1 C13 32.7(5) 23 23 ? O1 Tb1 C13 136.6(7) 21 23 ? O1 Tb1 C13 85.3(9) 3 23 ? O2 Tb1 C13 108.1(10) 3 23 ? O2 Tb1 C13 26.1(7) 23 23 ? O2 Tb1 C13 160.8(10) 21 23 ? O2 Tb1 C13 74.7(10) . 23 ? O3 Tb1 C13 95.4(4) . 23 ? C13 Tb1 C13 89.50(8) . 23 ? C13 Tb1 C13 89.50(8) 3 23 ? C13 O1 Tb1 83.7(9) . . ? C13 O2 Tb1 90.0(15) . . ? C2 C1 C2 121(3) . 12_665 ? C1 C2 C1 119(3) . 6_566 ? C1 C2 C3 120.7(13) . . ? C1 C2 C3 120.6(13) 6_566 . ? C4 C3 C4 118.6(19) 42_554 . ? C4 C3 C2 120.7(10) 42_554 . ? C4 C3 C2 120.7(10) . . ? C3 C4 C5 122.6(14) . . ? C6 C5 C4 113.6(13) . . ? C6 C5 C7 125.4(14) . . ? C4 C5 C7 121.0(12) . . ? C5 C6 C5 128.6(19) 42_554 . ? C8 C7 C12 120.0 . . ? C8 C7 C5 123.0(13) . . ? C12 C7 C5 116.8(13) . . ? C9 C8 C7 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 C13 119.2(17) . . ? C11 C10 C13 120.6(17) . . ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? O2 C13 O1 116(2) . . ? O2 C13 C10 120(2) . . ? O1 C13 C10 112.4(17) . . ? O2 C13 Tb1 64.0(12) . . ? O1 C13 Tb1 63.6(7) . . ? C10 C13 Tb1 175.9(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.492 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.044 _database_code_depnum_ccdc_archive 'CCDC 940070'