# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Krista Walton' _publ_contact_author_email krista.walton@chbe.gatech.edu _publ_section_title ; Breathing Effects of CO2 Adsorption on a Flexible 3D Lanthanide Metal-Organic Framework ; loop_ _publ_author_name 'Bin Mu' 'Feng Li' 'Yougui Huang' K.Walton # Attachment '- LaBTB.CIF' data_a _database_code_depnum_ccdc_archive 'CCDC 853237' #TrackingRef '- LaBTB.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H15 La O7' _chemical_formula_weight 590.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6522 _symmetry_space_group_name_Hall P652(001) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+5/6' '-y, x-y, z+2/3' '-x, -y, z+1/2' '-x+y, -x, z+1/3' 'y, -x+y, z+1/6' 'x-y, -y, -z' '-x, -x+y, -z+1/3' 'y, x, -z+2/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' _cell_length_a 16.5428(4) _cell_length_b 16.5428(4) _cell_length_c 24.3988(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5782.5(4) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1758 _cell_measurement_theta_min 3.58 _cell_measurement_theta_max 59.07 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 8.806 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.323 _exptl_absorpt_correction_T_max 0.541 _exptl_absorpt_process_details Multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury2 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 36294 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 69.07 _reflns_number_total 3395 _reflns_number_gt 3300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0917P)^2^+32.1144P] 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 0.044(12) _refine_ls_number_reflns 3395 _refine_ls_number_parameters 163 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1508 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.082 _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 La1 La 0.91902(3) 0.0000 0.0000 0.01531(19) Uani 1 2 d S . . O1 O 1.0359(4) 0.1418(3) 0.06980(19) 0.0212(10) Uani 1 1 d . . . C1 C 1.0260(5) 0.1994(5) 0.0391(3) 0.0232(16) Uani 1 1 d . . . O2 O 0.9630(4) 0.1715(4) 0.0044(3) 0.0433(16) Uani 1 1 d . . . C2 C 1.0927(5) 0.3020(5) 0.0448(3) 0.0249(16) Uani 1 1 d . . . O3 O 0.9984(4) 0.9282(4) 0.0449(2) 0.0317(12) Uani 1 1 d . . . C3 C 1.0702(6) 0.3625(6) 0.0197(4) 0.035(2) Uani 1 1 d . . . H3 H 1.0169 0.3390 -0.0019 0.042 Uiso 1 1 calc R . . O4 O 0.7677(4) 0.0000 0.0000 0.0382(19) Uani 1 2 d SU . . C4 C 1.1273(6) 0.4599(6) 0.0262(4) 0.036(2) Uani 1 1 d . . . H4 H 1.1127 0.5001 0.0077 0.044 Uiso 1 1 calc R . . C5 C 1.2055(5) 0.4966(5) 0.0604(3) 0.0242(16) Uani 1 1 d . . . C6 C 1.2277(5) 0.4326(5) 0.0853(4) 0.0236(16) Uani 1 1 d . . . H6 H 1.2803 0.4555 0.1075 0.028 Uiso 1 1 calc R . . C7 C 1.1727(6) 0.3361(5) 0.0773(3) 0.0251(16) Uani 1 1 d . . . H7 H 1.1891 0.2954 0.0935 0.030 Uiso 1 1 calc R . . C8 C 1.2595(5) 0.5980(5) 0.0724(3) 0.0269(16) Uani 1 1 d . . . C9 C 1.3538(4) 0.6462(4) 0.0833 0.020(2) Uani 1 2 d S . . H9 H 1.3862 0.6138 0.0833 0.024 Uiso 1 2 calc SR . . C10 C 1.2129(6) 0.6508(5) 0.0710(4) 0.0334(19) Uani 1 1 d . . . H10 H 1.1502 0.6213 0.0612 0.040 Uiso 1 1 calc R . . C11 C 1.2577(4) 0.7423(4) 0.0833 0.031(3) Uani 1 2 d S . . C12 C 1.2047(4) 0.7953(4) 0.0833 0.032(3) Uani 1 2 d S . . C13 C 1.1372(8) 0.7762(7) 0.0435(5) 0.051(3) Uani 1 1 d . . . H13 H 1.1252 0.7318 0.0166 0.061 Uiso 1 1 calc R . . C14 C 1.0878(8) 0.8238(7) 0.0440(4) 0.044(2) Uani 1 1 d . . . H14 H 1.0415 0.8098 0.0180 0.052 Uiso 1 1 calc R . . C15 C 1.1073(4) 0.8927(4) 0.0833 0.030(3) Uani 1 2 d S . . C16 C 1.0551(4) 0.9449(4) 0.0833 0.023(2) Uani 1 2 d S . . 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 La1 0.0112(2) 0.0104(3) 0.0240(3) -0.0030(2) -0.00148(11) 0.00520(14) O1 0.022(2) 0.011(2) 0.025(2) 0.0003(18) 0.000(2) 0.004(2) C1 0.024(4) 0.012(3) 0.031(4) -0.007(3) -0.005(3) 0.007(3) O2 0.042(3) 0.017(3) 0.070(4) -0.011(3) -0.035(3) 0.015(3) C2 0.020(4) 0.012(3) 0.037(4) -0.003(3) -0.007(3) 0.004(3) O3 0.035(3) 0.034(3) 0.039(3) -0.002(2) -0.008(3) 0.027(3) C3 0.030(5) 0.016(4) 0.056(5) -0.002(3) -0.017(4) 0.009(4) O4 0.016(2) 0.054(5) 0.057(5) 0.014(4) 0.007(2) 0.027(2) C4 0.034(5) 0.015(4) 0.059(5) 0.001(4) -0.019(4) 0.011(3) C5 0.018(4) 0.006(3) 0.042(4) 0.003(3) -0.005(3) 0.001(3) C6 0.011(3) 0.006(3) 0.049(5) -0.002(3) -0.009(3) 0.001(3) C7 0.023(4) 0.013(3) 0.037(4) -0.001(3) -0.009(3) 0.006(3) C8 0.015(4) 0.017(4) 0.047(5) -0.004(3) -0.005(3) 0.007(3) C9 0.010(3) 0.010(3) 0.041(6) -0.009(4) -0.009(4) 0.006(4) C10 0.018(4) 0.014(4) 0.065(6) -0.002(4) -0.007(4) 0.006(3) C11 0.017(4) 0.017(4) 0.060(8) -0.007(5) -0.007(5) 0.010(5) C12 0.020(4) 0.020(4) 0.054(7) -0.010(5) -0.010(5) 0.009(5) C13 0.060(7) 0.028(5) 0.082(7) -0.028(5) -0.026(6) 0.034(5) C14 0.051(6) 0.036(5) 0.059(6) -0.024(5) -0.034(5) 0.033(5) C15 0.031(5) 0.031(5) 0.036(6) -0.004(4) -0.004(4) 0.022(5) C16 0.018(4) 0.018(4) 0.035(5) 0.007(4) 0.007(4) 0.012(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 La1 O3 2.427(5) 1_545 ? La1 O3 2.427(5) 7_665 ? La1 O4 2.504(7) . ? La1 O1 2.521(5) 2_544 ? La1 O1 2.521(5) 10_665 ? La1 O2 2.554(5) 7 ? La1 O2 2.554(5) . ? La1 O1 2.758(5) . ? La1 O1 2.758(5) 7 ? La1 C1 3.014(7) 7 ? O1 C1 1.285(9) . ? O1 La1 2.521(5) 6_665 ? C1 O2 1.238(9) . ? C1 C2 1.499(9) . ? C2 C3 1.374(11) . ? C2 C7 1.397(11) . ? O3 C16 1.256(7) . ? O3 La1 2.427(5) 1_565 ? C3 C4 1.412(11) . ? C3 H3 0.9300 . ? C4 C5 1.396(11) . ? C4 H4 0.9300 . ? C5 C6 1.418(10) . ? C5 C8 1.484(10) . ? C6 C7 1.401(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.376(9) . ? C8 C10 1.425(11) . ? C9 C8 1.376(9) 10_775 ? C9 H9 0.9300 . ? C10 C11 1.347(10) . ? C10 H10 0.9300 . ? C11 C10 1.347(10) 10_775 ? C11 C12 1.516(16) . ? C12 C13 1.392(12) . ? C12 C13 1.392(12) 10_775 ? C13 C14 1.390(12) . ? C13 H13 0.9300 . ? C14 C15 1.398(10) . ? C14 H14 0.9300 . ? C15 C14 1.398(10) 10_775 ? C15 C16 1.497(14) . ? C16 O3 1.256(7) 10_775 ? 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 O3 La1 O3 76.4(3) 1_545 7_665 ? O3 La1 O4 141.79(15) 1_545 . ? O3 La1 O4 141.79(15) 7_665 . ? O3 La1 O1 136.90(17) 1_545 2_544 ? O3 La1 O1 73.25(18) 7_665 2_544 ? O4 La1 O1 73.66(11) . 2_544 ? O3 La1 O1 73.25(18) 1_545 10_665 ? O3 La1 O1 136.90(17) 7_665 10_665 ? O4 La1 O1 73.66(11) . 10_665 ? O1 La1 O1 147.3(2) 2_544 10_665 ? O3 La1 O2 79.9(2) 1_545 7 ? O3 La1 O2 126.91(19) 7_665 7 ? O4 La1 O2 74.33(14) . 7 ? O1 La1 O2 94.6(2) 2_544 7 ? O1 La1 O2 76.5(2) 10_665 7 ? O3 La1 O2 126.91(19) 1_545 . ? O3 La1 O2 79.9(2) 7_665 . ? O4 La1 O2 74.33(14) . . ? O1 La1 O2 76.5(2) 2_544 . ? O1 La1 O2 94.6(2) 10_665 . ? O2 La1 O2 148.7(3) 7 . ? O3 La1 O1 79.44(17) 1_545 . ? O3 La1 O1 75.51(16) 7_665 . ? O4 La1 O1 106.01(11) . . ? O1 La1 O1 120.42(15) 2_544 . ? O1 La1 O1 69.44(17) 10_665 . ? O2 La1 O1 144.0(2) 7 . ? O2 La1 O1 48.70(17) . . ? O3 La1 O1 75.51(16) 1_545 7 ? O3 La1 O1 79.44(17) 7_665 7 ? O4 La1 O1 106.01(11) . 7 ? O1 La1 O1 69.44(17) 2_544 7 ? O1 La1 O1 120.42(15) 10_665 7 ? O2 La1 O1 48.70(17) 7 7 ? O2 La1 O1 144.0(2) . 7 ? O1 La1 O1 148.0(2) . 7 ? O3 La1 C1 73.1(2) 1_545 7 ? O3 La1 C1 103.1(2) 7_665 7 ? O4 La1 C1 92.29(15) . 7 ? O1 La1 C1 84.70(18) 2_544 7 ? O1 La1 C1 96.60(18) 10_665 7 ? O2 La1 C1 23.9(2) 7 7 ? O2 La1 C1 159.3(2) . 7 ? O1 La1 C1 151.96(18) . 7 ? O1 La1 C1 25.22(18) 7 7 ? C1 O1 La1 138.6(5) . 6_665 ? C1 O1 La1 88.6(4) . . ? La1 O1 La1 108.33(17) 6_665 . ? O2 C1 O1 121.1(6) . . ? O2 C1 C2 119.4(7) . . ? O1 C1 C2 119.4(6) . . ? C1 O2 La1 99.3(4) . . ? C3 C2 C7 120.4(7) . . ? C3 C2 C1 118.0(7) . . ? C7 C2 C1 121.5(7) . . ? C16 O3 La1 139.1(5) . 1_565 ? C2 C3 C4 120.7(8) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.6(7) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 117.4(6) . . ? C4 C5 C8 120.9(7) . . ? C6 C5 C8 121.6(7) . . ? C7 C6 C5 121.9(7) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C2 C7 C6 118.9(7) . . ? C2 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C10 116.9(7) . . ? C9 C8 C5 124.2(7) . . ? C10 C8 C5 118.9(7) . . ? C8 C9 C8 122.8(9) . 10_775 ? C8 C9 H9 118.6 . . ? C8 C9 H9 118.6 10_775 . ? C11 C10 C8 121.5(7) . . ? C11 C10 H10 119.3 . . ? C8 C10 H10 119.3 . . ? C10 C11 C10 120.2(10) . 10_775 ? C10 C11 C12 119.9(5) . . ? C10 C11 C12 119.9(5) 10_775 . ? C13 C12 C13 120.1(11) . 10_775 ? C13 C12 C11 119.9(6) . . ? C13 C12 C11 119.9(6) 10_775 . ? C14 C13 C12 119.9(9) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.4(8) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C14 119.2(11) . 10_775 ? C14 C15 C16 120.4(5) . . ? C14 C15 C16 120.4(5) 10_775 . ? O3 C16 O3 125.8(9) . 10_775 ? O3 C16 C15 117.1(5) . . ? O3 C16 C15 117.1(5) 10_775 . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 69.07 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.108 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.151