data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lu, Tong-Bu' _publ_contact_author_email lutongbu@mail.sysu.edu.cn _publ_section_title ; A three-dimensional microporous metal-organic framework with large hydrogen sorption hysteresis ; loop_ _publ_author_name 'Di-Chang Zhong' 'Wei-Xiong Zhang' 'Feng-Lei Cao' 'Long Jiang' ; Tong-Bu Lu ; # Attachment '- 1_revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 790706' #TrackingRef '- 1_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Cd2 N8 O6' _chemical_formula_weight 484.95 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 11.7470(14) _cell_length_b 9.1555(11) _cell_length_c 11.5381(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1240.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3865 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 27.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 3.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4658 _exptl_absorpt_correction_T_max 0.6810 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5707 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.01 _reflns_number_total 2014 _reflns_number_gt 1813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0237P)^2^+7.6595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _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 0.03(5) _refine_ls_number_reflns 2014 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cd1 Cd 1.05997(4) -0.12649(5) 0.1532(5) 0.01331(12) Uani 1 1 d . . . Cd2 Cd 1.03121(4) 0.37028(5) 0.1226(5) 0.01151(12) Uani 1 1 d . . . N1 N 0.9035(4) 0.1652(5) 0.1331(7) 0.0147(12) Uani 1 1 d . . . N2 N 0.9016(5) 0.0191(5) 0.1272(7) 0.0161(12) Uani 1 1 d . . . N3 N 0.7947(4) -0.0278(6) 0.1227(8) 0.0189(13) Uani 1 1 d . . . N4 N 0.7262(5) 0.0860(6) 0.1229(8) 0.0175(12) Uani 1 1 d . . . N5 N 1.0126(6) 0.5772(6) -0.0036(7) 0.0167(13) Uani 1 1 d . . . N6 N 0.9988(5) 0.7179(6) -0.0036(8) 0.0165(12) Uani 1 1 d . . . N7 N 0.9748(7) 0.7652(7) -0.1085(8) 0.0212(13) Uani 1 1 d . . . N8 N 0.9717(6) 0.6496(6) -0.1792(7) 0.0191(14) Uani 1 1 d . . . O1 O 0.8356(4) 0.4502(4) 0.1382(7) 0.0227(14) Uani 1 1 d . . . O2 O 0.6503(3) 0.3811(5) 0.1296(7) 0.0177(10) Uani 1 1 d . . . O3 O 1.0199(5) 0.2859(5) -0.0720(7) 0.0208(12) Uani 1 1 d . . . O4 O 0.9749(5) 0.3532(5) -0.2549(7) 0.0191(11) Uani 1 1 d . . . O5 O 1.0855(5) -0.0549(5) 0.3383 0.0264(13) Uani 1 1 d . . . O6 O 1.2274(4) -0.1871(5) 0.0815(7) 0.0285(14) Uani 1 1 d . . . C1 C 0.7939(5) 0.2037(6) 0.1298(8) 0.0144(13) Uani 1 1 d . . . C2 C 0.7560(5) 0.3581(6) 0.1341(8) 0.0139(14) Uani 1 1 d . . . C3 C 0.9970(6) 0.5348(7) -0.1120(8) 0.0140(14) Uani 1 1 d . . . C4 C 0.9996(6) 0.3788(7) -0.1506(8) 0.0165(14) 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 Cd1 0.0151(2) 0.0088(2) 0.0160(3) -0.0010(2) -0.00088(18) 0.00132(17) Cd2 0.0103(2) 0.0120(2) 0.0122(3) 0.0009(3) -0.00042(17) -0.00099(17) N1 0.016(3) 0.013(2) 0.015(3) -0.001(2) 0.001(3) 0.0026(19) N2 0.023(3) 0.003(2) 0.022(3) 0.000(2) -0.001(3) -0.0023(19) N3 0.015(3) 0.015(3) 0.027(4) 0.000(3) -0.004(3) -0.002(2) N4 0.019(3) 0.011(2) 0.023(3) 0.000(2) 0.000(3) 0.0002(19) N5 0.026(4) 0.010(3) 0.015(3) -0.002(2) -0.001(3) 0.000(2) N6 0.013(3) 0.019(3) 0.018(3) 0.000(2) -0.002(3) 0.000(2) N7 0.030(4) 0.021(3) 0.012(3) 0.002(3) 0.001(3) -0.002(3) N8 0.037(4) 0.003(3) 0.018(3) -0.001(2) 0.000(3) -0.003(2) O1 0.011(2) 0.006(2) 0.051(5) 0.001(2) -0.001(3) 0.0006(15) O2 0.014(2) 0.015(2) 0.025(3) -0.002(2) 0.001(2) -0.0015(16) O3 0.035(4) 0.010(2) 0.017(3) 0.0021(19) -0.005(2) 0.001(2) O4 0.026(3) 0.019(3) 0.013(3) 0.000(2) -0.001(2) -0.002(2) O5 0.050(4) 0.006(2) 0.022(3) -0.001(2) 0.000(3) -0.001(2) O6 0.016(3) 0.017(2) 0.053(4) -0.007(2) 0.007(3) -0.0001(19) C1 0.018(3) 0.012(3) 0.013(4) -0.001(3) 0.003(3) 0.001(2) C2 0.005(3) 0.017(3) 0.020(4) -0.003(3) 0.003(3) 0.000(2) C3 0.019(4) 0.011(3) 0.012(4) 0.000(3) 0.000(3) -0.004(3) C4 0.017(4) 0.018(3) 0.015(3) 0.002(3) 0.001(3) -0.002(3) _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 Cd1 O6 2.205(5) . ? Cd1 O5 2.254(5) . ? Cd1 N2 2.308(5) . ? Cd1 O4 2.367(5) 2_755 ? Cd1 N6 2.413(6) 1_545 ? Cd1 O2 2.500(4) 3 ? Cd2 N8 2.295(7) 2_765 ? Cd2 N4 2.325(5) 3 ? Cd2 O3 2.377(6) . ? Cd2 N5 2.399(6) . ? Cd2 N1 2.407(5) . ? Cd2 O1 2.418(4) . ? N1 C1 1.335(8) . ? N1 N2 1.339(7) . ? N2 N3 1.329(7) . ? N3 N4 1.316(7) . ? N4 C1 1.342(8) . ? N4 Cd2 2.325(5) 3_455 ? N5 C3 1.323(9) . ? N5 N6 1.298(8) . ? N6 N7 1.316(9) . ? N6 Cd1 2.413(6) 1_565 ? N7 N8 1.336(9) . ? N8 C3 1.340(9) . ? N8 Cd2 2.295(7) 2_764 ? O1 C2 1.260(7) . ? O2 C2 1.261(7) . ? O2 Cd1 2.500(4) 3_455 ? O3 C4 1.266(9) . ? O4 C4 1.259(9) . ? O4 Cd1 2.367(5) 2_754 ? C1 C2 1.483(8) . ? C3 C4 1.496(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 O6 Cd1 O5 108.1(2) . . ? O6 Cd1 N2 144.6(2) . . ? O5 Cd1 N2 93.6(2) . . ? O6 Cd1 O4 95.85(19) . 2_755 ? O5 Cd1 O4 81.58(18) . 2_755 ? N2 Cd1 O4 115.17(18) . 2_755 ? O6 Cd1 N6 80.5(2) . 1_545 ? O5 Cd1 N6 157.2(2) . 1_545 ? N2 Cd1 N6 90.2(2) . 1_545 ? O4 Cd1 N6 76.50(19) 2_755 1_545 ? O6 Cd1 O2 78.85(17) . 3 ? O5 Cd1 O2 77.60(19) . 3 ? N2 Cd1 O2 78.98(15) . 3 ? O4 Cd1 O2 155.60(18) 2_755 3 ? N6 Cd1 O2 125.1(2) 1_545 3 ? N8 Cd2 N4 91.5(2) 2_765 3 ? N8 Cd2 O3 156.1(2) 2_765 . ? N4 Cd2 O3 96.5(2) 3 . ? N8 Cd2 N5 131.8(2) 2_765 . ? N4 Cd2 N5 87.4(2) 3 . ? O3 Cd2 N5 71.24(18) . . ? N8 Cd2 N1 83.0(2) 2_765 . ? N4 Cd2 N1 138.46(18) 3 . ? O3 Cd2 N1 76.1(2) . . ? N5 Cd2 N1 126.1(2) . . ? N8 Cd2 O1 86.3(2) 2_765 . ? N4 Cd2 O1 152.10(17) 3 . ? O3 Cd2 O1 96.6(2) . . ? N5 Cd2 O1 73.7(2) . . ? N1 Cd2 O1 68.89(15) . . ? C1 N1 N2 104.3(5) . . ? C1 N1 Cd2 113.2(4) . . ? N2 N1 Cd2 141.9(4) . . ? N3 N2 N1 109.9(5) . . ? N3 N2 Cd1 125.5(4) . . ? N1 N2 Cd1 123.9(4) . . ? N2 N3 N4 108.8(5) . . ? N3 N4 C1 105.9(5) . . ? N3 N4 Cd2 137.6(4) . 3_455 ? C1 N4 Cd2 116.5(4) . 3_455 ? C3 N5 N6 105.9(6) . . ? C3 N5 Cd2 110.8(4) . . ? N6 N5 Cd2 142.7(5) . . ? N7 N6 N5 110.7(6) . . ? N7 N6 Cd1 124.0(4) . 1_565 ? N5 N6 Cd1 123.3(5) . 1_565 ? N6 N7 N8 107.8(6) . . ? N7 N8 C3 105.2(6) . . ? N7 N8 Cd2 132.2(5) . 2_764 ? C3 N8 Cd2 121.2(4) . 2_764 ? C2 O1 Cd2 120.0(3) . . ? C2 O2 Cd1 124.3(4) . 3_455 ? C4 O3 Cd2 118.0(4) . . ? C4 O4 Cd1 129.1(4) . 2_754 ? N1 C1 N4 111.2(5) . . ? N1 C1 C2 122.7(5) . . ? N4 C1 C2 126.1(5) . . ? O2 C2 O1 128.4(5) . . ? O2 C2 C1 116.9(5) . . ? O1 C2 C1 114.6(5) . . ? N5 C3 N8 110.3(6) . . ? N5 C3 C4 124.0(6) . . ? N8 C3 C4 125.6(6) . . ? O4 C4 O3 127.1(6) . . ? O4 C4 C3 117.2(6) . . ? O3 C4 C3 115.5(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.177 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.150 # Attachment '- 1d_revised.cif' data_Pna21_from_1_ori_moving_rot_min(2) _database_code_depnum_ccdc_archive 'CCDC 790707' #TrackingRef '- 1d_revised.cif' _audit_creation_date 2010-10-26 _audit_creation_method 'Materials Studio' _symmetry_space_group_name_H-M PNA21 _symmetry_Int_Tables_number 33 _symmetry_cell_setting orthorhombic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z+1/2 x+1/2,-y+1/2,z -x+1/2,y+1/2,z+1/2 _cell_length_a 11.8184 _cell_length_b 8.3244 _cell_length_c 11.9153 _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 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 N1 N 0.852(2) 0.161(3) 0.122(2) 0.02080 Uiso 1.00 N2 N 0.845(2) 0.00428(3) 0.123(3) 0.02080 Uiso 1.00 N3 N 0.737(2) -0.0284(3) 0.131(2) 0.02080 Uiso 1.00 N4 N 0.671(2) 0.100(4) 0.131(1) 0.02080 Uiso 1.00 N5 N 1.01(2) 0.579(3) -0.0173(2) 0.02080 Uiso 1.00 N6 N 1.02(2) 0.735(3) -0.0272(2) 0.02080 Uiso 1.00 N7 N 1.01(2) 0.786(3) -0.131(2) 0.02080 Uiso 1.00 N8 N 0.988(2) 0.660(3) -0.191(2) 0.02080 Uiso 1.00 O1 O 0.766(3) 0.511(3) 0.172(3) 0.02080 Uiso 1.00 O2 O 0.621(3) 0.431(4) 0.0638(4) 0.02080 Uiso 1.00 O3 O 1.00(3) 0.234(3) -0.102(2) 0.02080 Uiso 1.00 O4 O 0.976(5) 0.329(3) -0.272(2) 0.02080 Uiso 1.00 C1 C 0.745(2) 0.226(3) 0.124(1) 0.02080 Uiso 1.00 C2 C 0.716(3) 0.401(4) 0.125(1) 0.02080 Uiso 1.00 C3 C 0.995(2) 0.525(3) -0.125(2) 0.02080 Uiso 1.00 C4 C 0.991(2) 0.353(3) -0.160(2) 0.02080 Uiso 1.00 Cd1 Cd 0.992(1) 0.117(1) -1.364(2) 0.02080 Uiso 1.00 Cd2 Cd 0.980(1) 0.378(1) 1.12(2) 0.02080 Uiso 1.00 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _ccdc_geom_bond_type N1 C1 1.372 . S N1 N2 1.311 . S N2 N3 1.310 . D N3 N4 1.321 . S N4 C1 1.366 . D N5 C3 1.365 . D N5 N6 1.322 . S N6 N7 1.310 . D N7 N8 1.312 . S N8 C3 1.377 . S O1 C2 1.220 . D O2 C2 1.357 . S O3 C4 1.214 . D O4 C4 1.358 . S C1 C2 1.498 . S C3 C4 1.496 . S