# Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is (c) The Owner Societies 2010 data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_Cambridge 1326 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Stefan Kaskel' _publ_contact_author_email STEFAN.KASKEL@CHEMIE.TU-DRESDEN.DE _publ_section_title ; Monitoring Adsorption-Induced Switching by 129Xe NMR Spectroscopy in a new Metal-Organic Framework Ni2(2,6-ndc)2(dabco) ; loop_ _publ_author_name 'Stefan Kaskel' 'Eike Brunner' 'Juergen Getzschmann' 'Christian Herzog' 'Nicole Klein' 'Martin R. Lohe' ; S.Paasch ; 'Michal Sabo' 'Irena Senkovska' # Attachment 'Ni2_ndc_2_dabco_-CCDC-760964.cif' data_Ni2(ndc)2dabco-NN8-293K1-c _database_code_depnum_ccdc_archive 'CCDC 760964' #TrackingRef 'Ni2_ndc_2_dabco_-CCDC-760964.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common Ni2(2,6-ndc)2(dabco)-DUT-8(Ni) _chemical_formula_moiety 'C30 H24 N2 Ni2 O8' _chemical_formula_sum 'C30 H24 N2 Ni2 O8' _chemical_properties_physical 'air-sensitive, moisture-sensitive' _exptl_crystal_recrystallization_method DMF/MeOH _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour green _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100 _chemical_formula_weight 657.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n' _symmetry_int_tables_number 85 _symmetry_space_group_name_Hall '-P 4a ' _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 18.4312(16) _cell_length_b 18.4312(16) _cell_length_c 9.3905(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3190.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS II' _diffrn_measurement_method Omega-Scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78281 _diffrn_reflns_av_R_equivalents 0.2694 _diffrn_reflns_av_sigmaI/netI 0.1344 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 30.82 _reflns_number_total 4941 _reflns_number_gt 1987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.35' _computing_cell_refinement 'X-Area 1.35' _computing_data_reduction 'X-Area 1.35' _computing_structure_solution 'SHELXL-96 (Sheldrick, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1a' _computing_publication_material WinGX _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. The space group P4/nmm was considered as possible at the structure solution stage. It is possible to solve and refine isotrop the structure in this space group, however the R-factor is somewhat worse in comparison to P4/n. As in P4/nmm the several atoms get wrong anisotropic displacement parameters, the space group P4/n was adopted, even though the PLATON/ADDSYM proposes a higher Laue class. ; _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^)+(0.1750P)^2^] 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_number_reflns 4941 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2418 _refine_ls_R_factor_gt 0.1546 _refine_ls_wR_factor_ref 0.3858 _refine_ls_wR_factor_gt 0.3428 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.005 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 Ni1 Ni 0.2500 0.2500 0.69595(17) 0.0704(10) Uani 1 4 d S . . Ni2 Ni 0.2500 0.2500 0.41535(16) 0.0678(10) Uani 1 4 d S . . O1 O 0.1735(3) 0.1733(3) 0.4435(5) 0.0890(16) Uani 1 1 d . . . O2 O 0.1739(4) 0.1731(4) 0.6758(6) 0.111(2) Uani 1 1 d . . . C1 C 0.1506(5) 0.1508(5) 0.5555(9) 0.097(2) Uani 1 1 d . . . C2 C 0.0955(5) 0.0956(5) 0.5589(9) 0.105(3) Uani 1 1 d . . . C3 C 0.0664(6) 0.0662(6) 0.4401(9) 0.112(2) Uani 1 1 d . . . H3 H 0.0839 0.0825 0.3528 0.135 Uiso 1 1 calc R . . C4 C 0.0667(6) 0.0681(6) 0.6880(9) 0.112(2) Uani 1 1 d . . . H4 H 0.0831 0.0867 0.7742 0.135 Uiso 1 1 calc R . . C5 C 0.0166(8) 0.0162(8) 0.6881(10) 0.142(5) Uani 1 1 d . . . H5 H 0.0003 -0.0010 0.7755 0.171 Uiso 1 1 calc R . . C6 C 0.0136(5) 0.0147(5) 0.4382(9) 0.107(3) Uani 1 1 d . . . N2 N 0.2500 0.2500 0.9008(6) 0.0385(15) Uani 1 4 d S . . N1 N 0.2500 0.2500 1.2001(6) 0.0421(16) Uani 1 4 d S . . C8 C 0.3239(11) 0.2545(10) 1.147(2) 0.084(3) Uani 0.38 1 d P . . H8A H 0.3487 0.2084 1.1574 0.101 Uiso 0.38 1 calc PR . . H8B H 0.3511 0.2915 1.1972 0.101 Uiso 0.38 1 calc PR . . C9 C 0.3004(11) 0.3060(9) 1.137(2) 0.084(3) Uani 0.38 1 d P . . H9A H 0.3501 0.2887 1.1370 0.101 Uiso 0.38 1 calc PR . . H9B H 0.2980 0.3511 1.1900 0.101 Uiso 0.38 1 calc PR . . C10 C 0.2697(13) 0.3178(10) 0.967(2) 0.084(3) Uani 0.38 1 d P . . H10A H 0.2278 0.3497 0.9683 0.101 Uiso 0.38 1 calc PR . . H10B H 0.3072 0.3411 0.9107 0.101 Uiso 0.38 1 calc PR . . C11 C 0.3137(12) 0.2776(11) 0.963(2) 0.084(3) Uani 0.38 1 d P . . H11A H 0.3136 0.3300 0.9542 0.101 Uiso 0.38 1 calc PR . . H11B H 0.3552 0.2593 0.9110 0.101 Uiso 0.38 1 calc PR . . 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 Ni1 0.0675(11) 0.0675(11) 0.0764(13) 0.000 0.000 0.000 Ni2 0.0651(10) 0.0651(10) 0.0732(14) 0.000 0.000 0.000 O1 0.098(3) 0.098(3) 0.072(3) 0.008(2) 0.008(2) -0.035(2) O2 0.129(5) 0.129(5) 0.075(3) 0.003(3) 0.004(3) -0.021(4) C1 0.100(5) 0.105(5) 0.087(4) -0.011(4) -0.013(4) -0.007(4) C2 0.112(6) 0.117(6) 0.087(5) 0.006(4) 0.003(4) -0.028(5) C3 0.130(5) 0.128(5) 0.079(3) 0.000(3) -0.002(3) -0.037(4) C4 0.130(5) 0.128(5) 0.079(3) 0.000(3) -0.002(3) -0.037(4) C5 0.178(11) 0.170(10) 0.079(5) 0.010(5) 0.007(5) -0.083(9) C6 0.118(6) 0.112(6) 0.090(5) 0.002(4) 0.003(4) -0.046(5) N2 0.0341(17) 0.0341(17) 0.047(3) 0.000 0.000 0.000 N1 0.054(2) 0.054(2) 0.017(2) 0.000 0.000 0.000 C8 0.094(6) 0.065(4) 0.094(5) -0.001(4) -0.016(5) -0.036(4) C9 0.094(6) 0.065(4) 0.094(5) -0.001(4) -0.016(5) -0.036(4) C10 0.094(6) 0.065(4) 0.094(5) -0.001(4) -0.016(5) -0.036(4) C11 0.094(6) 0.065(4) 0.094(5) -0.001(4) -0.016(5) -0.036(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 Ni1 N2 1.924(6) . ? Ni1 O2 2.003(7) . ? Ni1 O2 2.003(7) 3 ? Ni1 Ni2 2.635(2) . ? Ni2 O1 2.014(4) . ? Ni2 N1 2.022(5) 1_554 ? O1 C1 1.207(10) . ? O2 C1 1.277(9) . ? C1 C2 1.437(12) . ? C2 C3 1.352(12) . ? C2 C4 1.417(12) . ? C3 C6 1.360(12) . ? C4 C5 1.329(14) . ? C5 C6 1.428(13) 5_556 ? C6 C6 1.376(16) 5_556 ? N2 C11 1.407(16) . ? N2 C10 1.443(15) . ? N1 C8 1.45(2) . ? N1 C9 1.510(16) . ? C8 C11 1.79(3) . ? C9 C10 1.71(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? 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 N2 Ni1 O2 95.42(17) . . ? O2 Ni1 O2 89.49(3) 4 . ? O2 Ni1 O2 169.2(3) . 2 ? N2 Ni1 Ni2 180.000(1) . . ? O2 Ni1 Ni2 84.58(17) . . ? O1 Ni2 O1 89.01(4) 4 . ? O1 Ni2 O1 164.9(3) 2 . ? O1 Ni2 N1 97.55(15) . 1_554 ? O1 Ni2 Ni1 82.45(15) . . ? N1 Ni2 Ni1 180.0 1_554 . ? C1 O1 Ni2 127.0(5) . . ? C1 O2 Ni1 123.2(6) . . ? O1 C1 O2 122.8(8) . . ? O1 C1 C2 120.7(7) . . ? O2 C1 C2 116.5(8) . . ? C3 C2 C4 114.4(8) . . ? C3 C2 C1 123.0(8) . . ? C4 C2 C1 122.5(8) . . ? C2 C3 C6 125.1(8) . . ? C5 C4 C2 121.3(8) . . ? C4 C5 C6 123.8(8) . 5_556 ? C3 C6 C6 121.7(10) . 5_556 ? C3 C6 C5 124.6(8) . 5_556 ? C6 C6 C5 113.7(9) 5_556 5_556 ? C11 N2 C11 130.8(17) 2 . ? C11 N2 C11 80.0(6) . 4 ? C11 N2 C10 110.1(10) 2 . ? C11 N2 C10 45.4(10) . . ? C11 N2 C10 116.9(11) 4 . ? C10 N2 C10 79.3(6) . 4 ? C10 N2 C10 129.0(15) . 2 ? C11 N2 Ni1 114.6(8) . . ? C10 N2 Ni1 115.5(8) . . ? C8 N1 C8 139.8(15) 2 . ? C8 N1 C8 83.2(5) 4 . ? C8 N1 C9 118.7(10) . 2 ? C9 N1 C9 133.7(14) 2 . ? C8 N1 C9 118.1(10) . 3 ? C9 N1 C9 81.1(5) 2 3 ? C8 N1 Ni2 110.1(8) . 1_556 ? C9 N1 Ni2 113.1(7) . 1_556 ? N1 C8 C11 104.3(13) . . ? N1 C9 C10 104.5(10) . . ? N2 C10 C9 112.0(13) . . ? N2 C11 C8 113.8(12) . . ? H8A C8 H8B 108.9 . . ? H9A C9 H9B 108.8 . . ? N2 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N2 C11 H11A 108.5 . . ? N2 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.82 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.674 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.039 # 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 -0.019 0.081 -0.008 2104 638 ' ' _platon_squeeze_details ; ;