# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_C:zif8_4barprop.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZIF8_4barProp _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 N4 Zn, C3.3 H8.8' _chemical_formula_sum 'C11.30 H18.80 N4 Zn' _chemical_formula_weight 276.07 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, z, -y' 'x, -y, -z' '-x, -z, y' '-z, -y, x' '-x, y, -z' 'z, -y, -x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+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, -y+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' '-z+1/2, -y+1/2, x+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, -y+1/2, -x+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' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, z+1/2, -x+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, -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' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 16.9956(12) _cell_length_b 16.9956(12) _cell_length_c 16.9956(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4909.2(6) _cell_formula_units_Z 12 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4678 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.19 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1735 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7554 _exptl_absorpt_correction_T_max 0.7757 _exptl_absorpt_process_details 'Symmetry-related measurements' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15553 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.18 _reflns_number_total 1144 _reflns_number_gt 995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001;Atwood & Barbour,2003)' _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. ; _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^)+(0.0530P)^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 0.01(2) _refine_ls_number_reflns 1144 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 Zn1 Zn 0.5000 0.0000 0.2500 0.04807(18) Uani 1 4 d S . . C2 C 0.62318(12) 0.0080(3) 0.37682(12) 0.0475(8) Uani 1 2 d S . . N1 N 0.59028(13) -0.03172(11) 0.31759(12) 0.0518(5) Uani 1 1 d . . . C1 C 0.63108(18) -0.10149(16) 0.31382(18) 0.0672(7) Uani 1 1 d . . . H1 H 0.6215 -0.1421 0.2784 0.081 Uiso 1 1 calc R . . C3 C 0.5948(2) 0.0861(2) 0.4052(2) 0.0713(11) Uani 1 2 d S . . H3A H 0.5878 0.0844 0.4613 0.107 Uiso 0.50 1 calc PR . . H3B H 0.5455 0.0984 0.3805 0.107 Uiso 0.50 1 calc PR . . H3C H 0.6328 0.1258 0.3922 0.107 Uiso 0.50 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 Zn1 0.0499(2) 0.0499(2) 0.0444(3) 0.000 0.000 0.000 C2 0.0505(9) 0.041(2) 0.0505(9) -0.0005(12) -0.0007(11) 0.0005(12) N1 0.0544(11) 0.0493(10) 0.0518(11) -0.0033(8) -0.0069(9) 0.0054(9) C1 0.0758(18) 0.0547(14) 0.0710(18) -0.0171(13) -0.0153(14) 0.0098(13) C3 0.0787(17) 0.056(2) 0.0787(17) -0.0151(16) -0.018(2) 0.0151(16) _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 Zn1 N1 1.9910(19) 3_655 ? Zn1 N1 1.9911(19) . ? Zn1 N1 1.9911(19) 26 ? Zn1 N1 1.991(2) 28_545 ? C2 N1 1.334(3) . ? C2 N1 1.334(3) 23_656 ? C2 C3 1.494(7) . ? N1 C1 1.375(3) . ? C1 C1 1.324(6) 23_656 ? C1 H1 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 Zn1 N1 109.53(13) 3_655 . ? N1 Zn1 N1 109.44(6) 3_655 26 ? N1 Zn1 N1 109.44(6) . 26 ? N1 Zn1 N1 109.44(6) 3_655 28_545 ? N1 Zn1 N1 109.44(6) . 28_545 ? N1 Zn1 N1 109.53(13) 26 28_545 ? N1 C2 N1 112.1(4) . 23_656 ? N1 C2 C3 123.9(2) . . ? N1 C2 C3 123.9(2) 23_656 . ? C2 N1 C1 105.0(3) . . ? C2 N1 Zn1 128.4(2) . . ? C1 N1 Zn1 126.52(18) . . ? C1 C1 N1 108.88(15) 23_656 . ? C1 C1 H1 125.6 23_656 . ? N1 C1 H1 125.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 N1 C1 0.8(4) 23_656 . . . ? C3 C2 N1 C1 -176.7(4) . . . . ? N1 C2 N1 Zn1 179.34(10) 23_656 . . . ? C3 C2 N1 Zn1 1.9(5) . . . . ? N1 Zn1 N1 C2 -51.8(3) 3_655 . . . ? N1 Zn1 N1 C2 -171.8(3) 26 . . . ? N1 Zn1 N1 C2 68.2(2) 28_545 . . . ? N1 Zn1 N1 C1 126.4(3) 3_655 . . . ? N1 Zn1 N1 C1 6.5(3) 26 . . . ? N1 Zn1 N1 C1 -113.6(3) 28_545 . . . ? C2 N1 C1 C1 -0.5(3) . . . 23_656 ? Zn1 N1 C1 C1 -179.05(14) . . . 23_656 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.282 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.084 #============================================================================== _iucr_refine_instruction_details ; TITL MDPZIF8_4barProp_0m in I-43m CELL 0.71073 16.9956 16.9956 16.9956 90.000 90.000 90.000 ZERR 12.0000 0.0012 0.0012 0.0012 0.000 0.000 0.000 LATT -2 SYMM Y, -X, -Z SYMM -X, -Y, Z SYMM -Y, X, -Z SYMM -X, Z, -Y SYMM X, -Y, -Z SYMM -X, -Z, Y SYMM -Z, -Y, X SYMM -X, Y, -Z SYMM Z, -Y, -X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM -Y, -X, Z SYMM Y, X, Z SYMM X, -Z, -Y SYMM X, Z, Y SYMM -Z, Y, -X SYMM Z, Y, X SFAC C H N ZN UNIT 135.6 225.6 48 12 MERG 2 FMAP 2 GRID PLAN 5 TEMP 25 SIZE 0.2 0.19 0.18 OMIT 1 14 15 BOND $H CONF HTAB OMIT 11 11 14 L.S. 20 ACTA WGHT 0.053000 FVAR 0.07475 ZN1 4 0.500000 0.000000 0.250000 10.25000 0.04988 0.04988 = 0.04443 0.00000 0.00000 0.00000 C2 1 0.623179 0.007960 0.376821 10.50000 0.05052 0.04143 = 0.05052 -0.00049 -0.00073 0.00049 N1 3 0.590277 -0.031718 0.317591 11.00000 0.05440 0.04930 = 0.05176 -0.00334 -0.00693 0.00538 C1 1 0.631078 -0.101494 0.313824 11.00000 0.07577 0.05472 = 0.07105 -0.01710 -0.01530 0.00977 AFIX 43 H1 2 0.621532 -0.142064 0.278367 11.00000 -1.20000 AFIX 0 C3 1 0.594760 0.086112 0.405240 10.50000 0.07873 0.05644 = 0.07873 -0.01513 -0.01815 0.01513 AFIX 137 H3A 2 0.587753 0.084364 0.461262 10.50000 -1.50000 H3B 2 0.545495 0.098374 0.380477 10.50000 -1.50000 H3C 2 0.632764 0.125829 0.392248 10.50000 -1.50000 HKLF 4 REM MDPZIF8_4barProp_0m in I-43m REM R1 = 0.0322 for 995 Fo > 4sig(Fo) and 0.0425 for all 1144 data REM 34 parameters refined using 0 restraints END WGHT 0.0530 0.0000 REM Highest difference peak 0.282, deepest hole -0.189, 1-sigma level 0.084 Q1 1 0.6705 0.3295 0.4375 10.50000 0.05 0.28 Q2 1 0.6298 -0.3392 0.3392 10.50000 0.05 0.28 Q3 1 0.6812 0.3188 0.3188 10.16667 0.05 0.28 Q4 1 0.6772 -0.3228 0.3228 10.16667 0.05 0.26 Q5 1 0.6361 -0.3221 0.3639 10.50000 0.05 0.26 ; #====================================================================== _database_code_depnum_ccdc_archive 'CCDC 963851' ####################################################################### # # 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_C:zif8_prop87bar.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZIF8_Prop87bar _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 N4 Zn, C3 H8' _chemical_formula_sum 'C11 H18 N4 Zn' _chemical_formula_weight 271.66 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, z, -y' 'x, -y, -z' '-x, -z, y' '-z, -y, x' '-x, y, -z' 'z, -y, -x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+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, -y+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' '-z+1/2, -y+1/2, x+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, -y+1/2, -x+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' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, z+1/2, -x+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, -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' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 17.000(4) _cell_length_b 17.000(4) _cell_length_c 17.000(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4913.2(18) _cell_formula_units_Z 12 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4861 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.50 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7557 _exptl_absorpt_correction_T_max 0.7760 _exptl_absorpt_process_details 'Symmetry-related measurements' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15447 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1127 _reflns_number_gt 1001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001;Atwood & Barbour,2003)' _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. ; _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^)+(0.0460P)^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 0.02(2) _refine_ls_number_reflns 1127 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Zn1 Zn 0.5000 0.0000 0.2500 0.04812(17) Uani 1 4 d S . . N1 N 0.40980(11) -0.03166(10) 0.31784(11) 0.0517(4) Uani 1 1 d . . . C2 C 0.37687(10) 0.0081(3) 0.37687(10) 0.0470(8) Uani 1 2 d S . . C1 C 0.36920(16) -0.10150(14) 0.31388(16) 0.0660(6) Uani 1 1 d . . . H1 H 0.3788 -0.1420 0.2784 0.079 Uiso 1 1 calc R . . C3 C 0.40524(19) 0.0860(2) 0.40524(19) 0.0709(10) Uani 1 2 d S . . H3A H 0.3658 0.1251 0.3953 0.106 Uiso 0.50 1 calc PR . . H3B H 0.4528 0.0997 0.3780 0.106 Uiso 0.50 1 calc PR . . H3C H 0.4154 0.0832 0.4607 0.106 Uiso 0.50 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 Zn1 0.04996(19) 0.04996(19) 0.0444(2) 0.000 0.000 0.000 N1 0.0547(10) 0.0487(9) 0.0519(10) -0.0043(7) 0.0078(8) -0.0043(8) C2 0.0507(8) 0.0395(19) 0.0507(8) -0.0009(11) -0.0002(10) -0.0009(11) C1 0.0747(16) 0.0524(13) 0.0708(16) -0.0164(12) 0.0145(12) -0.0098(12) C3 0.0769(14) 0.059(2) 0.0769(14) -0.0143(14) 0.017(2) -0.0143(14) _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 Zn1 N1 1.9927(18) 26 ? Zn1 N1 1.9927(18) . ? Zn1 N1 1.9928(18) 28_545 ? Zn1 N1 1.9928(18) 3_655 ? N1 C2 1.333(3) . ? N1 C1 1.375(3) . ? C2 N1 1.333(3) 24 ? C2 C3 1.489(6) . ? C1 C1 1.330(5) 24 ? C1 H1 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 Zn1 N1 109.57(6) 26 . ? N1 Zn1 N1 109.28(11) 26 28_545 ? N1 Zn1 N1 109.57(6) . 28_545 ? N1 Zn1 N1 109.57(6) 26 3_655 ? N1 Zn1 N1 109.28(11) . 3_655 ? N1 Zn1 N1 109.57(6) 28_545 3_655 ? C2 N1 C1 105.3(2) . . ? C2 N1 Zn1 128.44(19) . . ? C1 N1 Zn1 126.24(16) . . ? N1 C2 N1 112.0(4) 24 . ? N1 C2 C3 123.96(17) 24 . ? N1 C2 C3 123.96(17) . . ? C1 C1 N1 108.68(13) 24 . ? C1 C1 H1 125.7 24 . ? N1 C1 H1 125.7 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 N1 C2 -68.0(2) 26 . . . ? N1 Zn1 N1 C2 172.1(3) 28_545 . . . ? N1 Zn1 N1 C2 52.0(2) 3_655 . . . ? N1 Zn1 N1 C1 113.5(3) 26 . . . ? N1 Zn1 N1 C1 -6.4(2) 28_545 . . . ? N1 Zn1 N1 C1 -126.5(2) 3_655 . . . ? C1 N1 C2 N1 -0.6(4) . . . 24 ? Zn1 N1 C2 N1 -179.37(9) . . . 24 ? C1 N1 C2 C3 176.5(3) . . . . ? Zn1 N1 C2 C3 -2.2(5) . . . . ? C2 N1 C1 C1 0.4(2) . . . 24 ? Zn1 N1 C1 C1 179.15(12) . . . 24 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.259 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.075 #============================================================================== _iucr_refine_instruction_details ; TITL MDPZIF8_Prop87bar_0m in I-43m CELL 0.71073 17.0002 17.0002 17.0002 90.000 90.000 90.000 ZERR 12.0000 0.0036 0.0036 0.0036 0.000 0.000 0.000 LATT -2 SYMM Y, -X, -Z SYMM -X, -Y, Z SYMM -Y, X, -Z SYMM -X, Z, -Y SYMM X, -Y, -Z SYMM -X, -Z, Y SYMM -Z, -Y, X SYMM -X, Y, -Z SYMM Z, -Y, -X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM -Y, -X, Z SYMM Y, X, Z SYMM X, -Z, -Y SYMM X, Z, Y SYMM -Z, Y, -X SYMM Z, Y, X SFAC C H N ZN UNIT 132 216 48 12 MERG 2 FMAP 2 GRID PLAN 5 TEMP 25 SIZE 0.2 0.19 0.18 BOND $H CONF HTAB OMIT 9 13 14 OMIT 8 11 15 OMIT 10 12 14 OMIT 8 10 18 OMIT 1 3 22 OMIT 5 6 21 L.S. 20 ACTA 54 WGHT 0.046000 FVAR 0.07458 ZN1 4 0.500000 0.000000 0.250000 10.25000 0.04996 0.04996 = 0.04443 0.00000 0.00000 0.00000 N1 3 0.409797 -0.031657 0.317835 11.00000 0.05471 0.04866 = 0.05186 -0.00431 0.00778 -0.00427 C2 1 0.376874 0.008116 0.376874 10.50000 0.05073 0.03950 = 0.05073 -0.00093 -0.00023 -0.00093 C1 1 0.369202 -0.101496 0.313878 11.00000 0.07473 0.05243 = 0.07075 -0.01638 0.01454 -0.00980 AFIX 43 H1 2 0.378828 -0.142013 0.278405 11.00000 -1.20000 AFIX 0 C3 1 0.405240 0.085961 0.405240 10.50000 0.07686 0.05911 = 0.07686 -0.01429 0.01672 -0.01429 AFIX 137 H3A 2 0.365814 0.125138 0.395263 10.50000 -1.50000 H3B 2 0.452769 0.099731 0.378033 10.50000 -1.50000 H3C 2 0.415428 0.083209 0.460715 10.50000 -1.50000 HKLF 4 REM MDPZIF8_Prop87bar_0m in I-43m REM R1 = 0.0300 for 1001 Fo > 4sig(Fo) and 0.0387 for all 1127 data REM 34 parameters refined using 0 restraints END WGHT 0.0460 0.0000 REM Highest difference peak 0.259, deepest hole -0.188, 1-sigma level 0.075 Q1 1 0.4491 -0.0031 0.2881 11.00000 0.05 0.26 Q2 1 0.3414 0.3206 0.4409 11.00000 0.05 0.23 Q3 1 0.3738 -0.3406 0.3738 10.50000 0.05 0.22 Q4 1 0.3507 0.3507 0.4991 10.50000 0.05 0.22 Q5 1 0.3843 -0.3554 0.3554 10.50000 0.05 0.21 ; #====================================================================== _database_code_depnum_ccdc_archive 'CCDC 963852' ####################################################################### # # 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_C:zif8_2barprop.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZIF8_2barProp _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 N4 Zn, C2.1 H5.6' _chemical_formula_sum 'C10.10 H15.60 N4 Zn' _chemical_formula_weight 258.44 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, z, -y' 'x, -y, -z' '-x, -z, y' '-z, -y, x' '-x, y, -z' 'z, -y, -x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+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, -y+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' '-z+1/2, -y+1/2, x+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, -y+1/2, -x+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' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, z+1/2, -x+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, -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' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 16.987(3) _cell_length_b 16.987(3) _cell_length_c 16.987(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4901.4(13) _cell_formula_units_Z 12 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4305 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.41 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1610 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7596 _exptl_absorpt_correction_T_max 0.7718 _exptl_absorpt_process_details 'Symmetry-related measurements' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15458 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.19 _reflns_number_total 1135 _reflns_number_gt 983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001;Atwood & Barbour,2003)' _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. ; _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^)+(0.0496P)^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(2) _refine_ls_number_reflns 1135 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 Zn1 Zn 0.5000 0.0000 0.2500 0.04783(18) Uani 1 4 d S . . C2 C 0.37669(11) 0.0082(3) 0.37669(11) 0.0463(8) Uani 1 2 d S . . N1 N 0.40948(13) -0.03175(11) 0.31770(12) 0.0518(5) Uani 1 1 d . . . C1 C 0.36914(17) -0.10135(16) 0.31403(18) 0.0668(7) Uani 1 1 d . . . H1 H 0.3788 -0.1420 0.2786 0.080 Uiso 1 1 calc R . . C3 C 0.4051(2) 0.0860(2) 0.4051(2) 0.0719(11) Uani 1 2 d S . . H3A H 0.4030 0.1234 0.3628 0.108 Uiso 0.50 1 calc PR . . H3B H 0.4584 0.0811 0.4233 0.108 Uiso 0.50 1 calc PR . . H3C H 0.3722 0.1037 0.4475 0.108 Uiso 0.50 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 Zn1 0.0497(2) 0.0497(2) 0.0441(3) 0.000 0.000 0.000 C2 0.0509(9) 0.037(2) 0.0509(9) -0.0026(12) -0.0002(11) -0.0026(12) N1 0.0533(11) 0.0501(11) 0.0522(11) -0.0044(8) 0.0081(9) -0.0051(9) C1 0.0757(18) 0.0534(15) 0.0713(18) -0.0189(13) 0.0176(14) -0.0093(13) C3 0.0784(17) 0.059(2) 0.0784(17) -0.0149(16) 0.019(2) -0.0149(16) _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 Zn1 N1 1.9944(19) 28_545 ? Zn1 N1 1.9944(19) . ? Zn1 N1 1.9944(19) 3_655 ? Zn1 N1 1.9944(19) 26 ? C2 N1 1.332(3) 24 ? C2 N1 1.332(3) . ? C2 C3 1.488(6) . ? N1 C1 1.368(3) . ? C1 C1 1.324(6) 24 ? C1 H1 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 Zn1 N1 109.42(6) 28_545 . ? N1 Zn1 N1 109.42(6) 28_545 3_655 ? N1 Zn1 N1 109.57(13) . 3_655 ? N1 Zn1 N1 109.57(13) 28_545 26 ? N1 Zn1 N1 109.42(6) . 26 ? N1 Zn1 N1 109.42(6) 3_655 26 ? N1 C2 N1 111.7(4) 24 . ? N1 C2 C3 124.10(19) 24 . ? N1 C2 C3 124.10(19) . . ? C2 N1 C1 105.3(3) . . ? C2 N1 Zn1 128.2(2) . . ? C1 N1 Zn1 126.42(17) . . ? C1 C1 N1 108.78(15) 24 . ? C1 C1 H1 125.6 24 . ? N1 C1 H1 125.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 N1 C1 -0.8(4) 24 . . . ? C3 C2 N1 C1 176.3(4) . . . . ? N1 C2 N1 Zn1 -179.21(10) 24 . . . ? C3 C2 N1 Zn1 -2.1(5) . . . . ? N1 Zn1 N1 C2 171.9(3) 28_545 . . . ? N1 Zn1 N1 C2 52.0(3) 3_655 . . . ? N1 Zn1 N1 C2 -68.0(2) 26 . . . ? N1 Zn1 N1 C1 -6.2(3) 28_545 . . . ? N1 Zn1 N1 C1 -126.2(3) 3_655 . . . ? N1 Zn1 N1 C1 113.9(3) 26 . . . ? C2 N1 C1 C1 0.5(3) . . . 24 ? Zn1 N1 C1 C1 178.93(14) . . . 24 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.257 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.069 #============================================================================== _iucr_refine_instruction_details ; TITL MDPZIF8_2barProp_0m in I-43m CELL 0.71073 16.9866 16.9866 16.9866 90.000 90.000 90.000 ZERR 12.0000 0.0026 0.0026 0.0026 0.000 0.000 0.000 LATT -2 SYMM Y, -X, -Z SYMM -X, -Y, Z SYMM -Y, X, -Z SYMM -X, Z, -Y SYMM X, -Y, -Z SYMM -X, -Z, Y SYMM -Z, -Y, X SYMM -X, Y, -Z SYMM Z, -Y, -X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM -Y, -X, Z SYMM Y, X, Z SYMM X, -Z, -Y SYMM X, Z, Y SYMM -Z, Y, -X SYMM Z, Y, X SFAC C H N ZN UNIT 121.2 187.2 48 12 MERG 2 FMAP 2 GRID PLAN 5 TEMP 25 SIZE 0.196 0.189 0.184 OMIT 2 14 16 OMIT 0 15 15 OMIT 4 12 18 OMIT -7 14 15 OMIT 12 12 14 OMIT 8 10 18 OMIT -12 13 13 OMIT 6 10 16 OMIT -8 13 13 BOND $H CONF HTAB L.S. 20 ACTA 54 WGHT 0.049600 FVAR 0.07522 ZN1 4 0.500000 0.000000 0.250000 10.25000 0.04971 0.04971 = 0.04406 0.00000 0.00000 0.00000 C2 1 0.376692 0.008163 0.376692 10.50000 0.05092 0.03695 = 0.05092 -0.00259 -0.00022 -0.00259 N1 3 0.409484 -0.031748 0.317702 11.00000 0.05328 0.05006 = 0.05215 -0.00443 0.00814 -0.00505 C1 1 0.369140 -0.101347 0.314032 11.00000 0.07573 0.05344 = 0.07132 -0.01890 0.01759 -0.00934 AFIX 43 H1 2 0.378831 -0.141981 0.278642 11.00000 -1.20000 AFIX 0 C3 1 0.405110 0.086010 0.405110 10.50000 0.07837 0.05907 = 0.07837 -0.01494 0.01949 -0.01494 AFIX 137 H3A 2 0.403038 0.123414 0.362794 10.50000 -1.50000 H3B 2 0.458382 0.081112 0.423332 10.50000 -1.50000 H3C 2 0.372241 0.103722 0.447535 10.50000 -1.50000 HKLF 4 REM MDPZIF8_2barProp_0m in I-43m REM R1 = 0.0331 for 983 Fo > 4sig(Fo) and 0.0446 for all 1135 data REM 34 parameters refined using 0 restraints END WGHT 0.0496 0.0000 REM Highest difference peak 0.257, deepest hole -0.210, 1-sigma level 0.069 Q1 1 0.4726 0.3161 0.3161 10.50000 0.05 0.26 Q2 1 0.4489 -0.0038 0.2893 11.00000 0.05 0.25 Q3 1 0.4601 -0.0261 0.2979 11.00000 0.05 0.25 Q4 1 0.4013 -0.3338 0.3338 10.50000 0.05 0.24 Q5 1 0.4008 0.3325 0.3325 10.50000 0.05 0.24 ; #====================================================================== _database_code_depnum_ccdc_archive 'CCDC 963853' ####################################################################### # # 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_C:eth35bar.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZIF8_Eth35bar _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 N4 Zn, C H3' _chemical_formula_sum 'C9 H13 N4 Zn' _chemical_formula_weight 242.60 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, z, -y' 'x, -y, -z' '-x, -z, y' '-z, -y, x' '-x, y, -z' 'z, -y, -x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+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, -y+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' '-z+1/2, -y+1/2, x+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, -y+1/2, -x+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' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, z+1/2, -x+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, -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' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 16.986(14) _cell_length_b 16.986(14) _cell_length_c 16.986(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4901(7) _cell_formula_units_Z 12 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3084 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.20 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.986 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_correction_T_max 0.7764 _exptl_absorpt_process_details 'Symmetry-related measurements' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10664 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.37 _reflns_number_total 1128 _reflns_number_gt 915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001;Atwood & Barbour,2003)' _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. ; _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^)+(0.0449P)^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 0.01(2) _refine_ls_number_reflns 1128 _refine_ls_number_parameters 33 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Zn1 Zn 0.5000 0.0000 0.2500 0.05055(18) Uani 1 4 d S . . C2 C 0.62300(11) 0.0079(3) 0.37700(11) 0.0493(8) Uani 1 2 d S . . N1 N 0.59022(12) -0.03157(11) 0.31760(11) 0.0540(5) Uani 1 1 d . . . C1 C 0.63070(16) -0.10137(15) 0.31391(17) 0.0686(7) Uani 1 1 d . . . H1 H 0.6210 -0.1420 0.2785 0.082 Uiso 1 1 calc R . . C3 C 0.5946(2) 0.0858(2) 0.4054(2) 0.0731(11) Uani 1 2 d S . . H3A H 0.5516 0.1031 0.3731 0.110 Uiso 0.25 1 calc PR . . H3B H 0.6367 0.1234 0.4025 0.110 Uiso 0.25 1 calc PR . . H3C H 0.5772 0.0811 0.4590 0.110 Uiso 0.25 1 calc PR . . H3D H 0.6254 0.1020 0.4499 0.110 Uiso 0.25 1 calc PR . . H3E H 0.5403 0.0816 0.4205 0.110 Uiso 0.25 1 calc PR . . H3F H 0.5998 0.1239 0.3640 0.110 Uiso 0.25 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 Zn1 0.0523(2) 0.0523(2) 0.0471(3) 0.000 0.000 0.000 C2 0.0526(9) 0.043(2) 0.0526(9) -0.0010(12) 0.0004(12) 0.0010(12) N1 0.0577(11) 0.0505(10) 0.0538(11) -0.0044(8) -0.0087(9) 0.0042(9) C1 0.0761(17) 0.0549(14) 0.0749(18) -0.0190(13) -0.0160(13) 0.0112(13) C3 0.0805(16) 0.058(2) 0.0805(16) -0.0158(15) -0.017(2) 0.0158(15) _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 Zn1 N1 1.989(2) 3_655 ? Zn1 N1 1.989(2) 28_545 ? Zn1 N1 1.989(2) . ? Zn1 N1 1.989(2) 26 ? C2 N1 1.334(3) . ? C2 N1 1.334(3) 23_656 ? C2 C3 1.488(6) . ? N1 C1 1.372(3) . ? C1 C1 1.331(5) 23_656 ? C1 H1 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C3 H3E 0.9600 . ? C3 H3F 0.9600 . ? 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 N1 Zn1 N1 109.47(6) 3_655 28_545 ? N1 Zn1 N1 109.46(12) 3_655 . ? N1 Zn1 N1 109.48(6) 28_545 . ? N1 Zn1 N1 109.48(6) 3_655 26 ? N1 Zn1 N1 109.46(12) 28_545 26 ? N1 Zn1 N1 109.47(6) . 26 ? N1 C2 N1 112.3(4) . 23_656 ? N1 C2 C3 123.85(19) . . ? N1 C2 C3 123.85(19) 23_656 . ? C2 N1 C1 105.1(3) . . ? C2 N1 Zn1 128.5(2) . . ? C1 N1 Zn1 126.36(17) . . ? C1 C1 N1 108.79(14) 23_656 . ? C1 C1 H1 125.6 23_656 . ? N1 C1 H1 125.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C3 H3D 109.5 . . ? H3A C3 H3D 141.1 . . ? H3B C3 H3D 56.3 . . ? H3C C3 H3D 56.3 . . ? C2 C3 H3E 109.5 . . ? H3A C3 H3E 56.3 . . ? H3B C3 H3E 141.1 . . ? H3C C3 H3E 56.3 . . ? H3D C3 H3E 109.5 . . ? C2 C3 H3F 109.5 . . ? H3A C3 H3F 56.3 . . ? H3B C3 H3F 56.3 . . ? H3C C3 H3F 141.1 . . ? H3D C3 H3F 109.5 . . ? H3E C3 H3F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 N1 C1 1.3(4) 23_656 . . . ? C3 C2 N1 C1 -176.5(4) . . . . ? N1 C2 N1 Zn1 179.47(10) 23_656 . . . ? C3 C2 N1 Zn1 1.6(5) . . . . ? N1 Zn1 N1 C2 -51.6(2) 3_655 . . . ? N1 Zn1 N1 C2 68.4(2) 28_545 . . . ? N1 Zn1 N1 C2 -171.6(3) 26 . . . ? N1 Zn1 N1 C1 126.2(3) 3_655 . . . ? N1 Zn1 N1 C1 -113.8(3) 28_545 . . . ? N1 Zn1 N1 C1 6.2(2) 26 . . . ? C2 N1 C1 C1 -0.8(2) . . . 23_656 ? Zn1 N1 C1 C1 -178.96(13) . . . 23_656 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.295 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.051 #============================================================================== _iucr_refine_instruction_details ; TITL MDPZIF8_Eth35bar_0m in I-43m CELL 0.71073 16.9860 16.9860 16.9860 90.000 90.000 90.000 ZERR 12.0000 0.0143 0.0143 0.0143 0.000 0.000 0.000 LATT -2 SYMM Y, -X, -Z SYMM -X, -Y, Z SYMM -Y, X, -Z SYMM -X, Z, -Y SYMM X, -Y, -Z SYMM -X, -Z, Y SYMM -Z, -Y, X SYMM -X, Y, -Z SYMM Z, -Y, -X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM -Y, -X, Z SYMM Y, X, Z SYMM X, -Z, -Y SYMM X, Z, Y SYMM -Z, Y, -X SYMM Z, Y, X SFAC C H N ZN UNIT 108 156 48 12 MERG 2 FMAP 2 GRID PLAN 5 TEMP 25 SIZE 0.2 0.19 0.18 BOND $H CONF HTAB OMIT -2 7 19 OMIT -10 10 16 OMIT -5 5 16 OMIT 5 10 19 OMIT -10 12 14 OMIT 3 9 20 OMIT 5 9 20 OMIT -8 14 14 OMIT -5 8 19 OMIT 4 11 19 OMIT 4 12 18 OMIT -2 6 20 OMIT 4 7 17 OMIT -4 8 18 L.S. 20 ACTA 54 WGHT 0.044900 FVAR 0.07330 ZN1 4 0.500000 0.000000 0.250000 10.25000 0.05228 0.05228 = 0.04709 0.00000 0.00000 0.00000 C2 1 0.622997 0.007931 0.377003 10.50000 0.05260 0.04270 = 0.05260 -0.00098 0.00039 0.00098 N1 3 0.590218 -0.031570 0.317599 11.00000 0.05765 0.05047 = 0.05383 -0.00438 -0.00869 0.00425 C1 1 0.630696 -0.101366 0.313907 11.00000 0.07609 0.05491 = 0.07489 -0.01897 -0.01601 0.01122 AFIX 43 H1 2 0.621014 -0.141998 0.278509 11.00000 -1.20000 AFIX 0 C3 1 0.594609 0.085777 0.405391 10.50000 0.08046 0.05846 = 0.08046 -0.01578 -0.01684 0.01578 AFIX 123 H3A 2 0.551590 0.103071 0.373073 10.25000 -1.50000 H3B 2 0.636689 0.123391 0.402450 10.25000 -1.50000 H3C 2 0.577231 0.081099 0.458966 10.25000 -1.50000 H3D 2 0.625417 0.101970 0.449920 10.25000 -1.50000 H3E 2 0.540318 0.081650 0.420543 10.25000 -1.50000 H3F 2 0.599775 0.123941 0.364027 10.25000 -1.50000 HKLF 4 REM MDPZIF8_Eth35bar_0m in I-43m REM R1 = 0.0291 for 915 Fo > 4sig(Fo) and 0.0481 for all 1128 data REM 33 parameters refined using 0 restraints END WGHT 0.0449 0.0000 REM Highest difference peak 0.295, deepest hole -0.184, 1-sigma level 0.051 Q1 1 0.5000 0.2560 0.5000 10.25000 0.05 0.29 Q2 1 0.5510 -0.0043 0.2976 11.00000 0.05 0.22 Q3 1 0.5442 -0.0328 0.2927 11.00000 0.05 0.22 Q4 1 0.7491 -0.2509 0.2509 10.16667 0.05 0.20 Q5 1 0.4548 -0.0289 0.2935 11.00000 0.05 0.20 ; #====================================================================== _database_code_depnum_ccdc_archive 'CCDC 963854' ####################################################################### # # 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_C:zif8_methane50bar.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZIF8_Methane50bar _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 N4 Zn, C3.9 H15.6' _chemical_formula_sum 'C11.90 H25.60 N4 Zn' _chemical_formula_weight 290.13 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, z, -y' 'x, -y, -z' '-x, -z, y' '-z, -y, x' '-x, y, -z' 'z, -y, -x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+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, -y+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' '-z+1/2, -y+1/2, x+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, -y+1/2, -x+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' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, z+1/2, -x+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, -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' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 17.001(6) _cell_length_b 17.001(6) _cell_length_c 17.001(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4914(3) _cell_formula_units_Z 12 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4333 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.18 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7552 _exptl_absorpt_correction_T_max 0.7756 _exptl_absorpt_process_details 'Symmetry-related measurements' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15408 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.17 _reflns_number_total 1138 _reflns_number_gt 965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001;Atwood & Barbour,2003)' _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. ; _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^)+(0.0600P)^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(3) _refine_ls_number_reflns 1138 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 Zn1 Zn 0.5000 0.0000 0.2500 0.0477(2) Uani 1 4 d S . . C2 C 0.62304(14) 0.0077(4) 0.37696(14) 0.0485(10) Uani 1 2 d S . . N1 N 0.59026(15) -0.03131(13) 0.31750(14) 0.0514(5) Uani 1 1 d . . . C1 C 0.6313(2) -0.10084(19) 0.3131(2) 0.0659(8) Uani 1 1 d . . . H1 H 0.6219 -0.1412 0.2774 0.079 Uiso 1 1 calc R . . C3 C 0.5942(3) 0.0859(3) 0.4058(3) 0.0720(14) Uani 1 2 d S . . H3A H 0.6353 0.1242 0.4004 0.108 Uiso 0.50 1 calc PR . . H3B H 0.5794 0.0816 0.4601 0.108 Uiso 0.50 1 calc PR . . H3C H 0.5495 0.1019 0.3752 0.108 Uiso 0.50 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 Zn1 0.0494(2) 0.0494(2) 0.0443(3) 0.000 0.000 0.000 C2 0.0505(10) 0.044(3) 0.0505(10) -0.0003(15) 0.0001(13) 0.0003(15) N1 0.0558(14) 0.0477(12) 0.0508(13) -0.0030(9) -0.0083(11) 0.0046(10) C1 0.074(2) 0.0551(17) 0.068(2) -0.0179(15) -0.0146(16) 0.0109(15) C3 0.080(2) 0.055(2) 0.080(2) -0.0153(19) -0.019(3) 0.0153(19) _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 Zn1 N1 1.989(2) 26 ? Zn1 N1 1.989(2) 28_545 ? Zn1 N1 1.989(2) 3_655 ? Zn1 N1 1.989(2) . ? C2 N1 1.331(4) . ? C2 N1 1.331(4) 23_656 ? C2 C3 1.499(8) . ? N1 C1 1.374(4) . ? C1 C1 1.337(7) 23_656 ? C1 H1 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 Zn1 N1 109.52(15) 26 28_545 ? N1 Zn1 N1 109.45(8) 26 3_655 ? N1 Zn1 N1 109.45(8) 28_545 3_655 ? N1 Zn1 N1 109.45(8) 26 . ? N1 Zn1 N1 109.45(8) 28_545 . ? N1 Zn1 N1 109.52(15) 3_655 . ? N1 C2 N1 112.8(5) . 23_656 ? N1 C2 C3 123.6(2) . . ? N1 C2 C3 123.6(2) 23_656 . ? C2 N1 C1 104.9(3) . . ? C2 N1 Zn1 128.9(3) . . ? C1 N1 Zn1 126.2(2) . . ? C1 C1 N1 108.69(18) 23_656 . ? C1 C1 H1 125.7 23_656 . ? N1 C1 H1 125.7 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 N1 C1 1.0(5) 23_656 . . . ? C3 C2 N1 C1 -176.9(5) . . . . ? N1 C2 N1 Zn1 179.46(13) 23_656 . . . ? C3 C2 N1 Zn1 1.5(7) . . . . ? N1 Zn1 N1 C2 -171.3(3) 26 . . . ? N1 Zn1 N1 C2 68.6(3) 28_545 . . . ? N1 Zn1 N1 C2 -51.4(3) 3_655 . . . ? N1 Zn1 N1 C1 6.8(3) 26 . . . ? N1 Zn1 N1 C1 -113.2(4) 28_545 . . . ? N1 Zn1 N1 C1 126.8(3) 3_655 . . . ? C2 N1 C1 C1 -0.6(3) . . . 23_656 ? Zn1 N1 C1 C1 -179.10(16) . . . 23_656 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.362 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.095 #============================================================================== _iucr_refine_instruction_details ; TITL MDPZIF8_Methane50bar_0m in I-43m CELL 0.71073 17.0013 17.0013 17.0013 90.000 90.000 90.000 ZERR 12.0000 0.0060 0.0060 0.0060 0.000 0.000 0.000 LATT -2 SYMM Y, -X, -Z SYMM -X, -Y, Z SYMM -Y, X, -Z SYMM -X, Z, -Y SYMM X, -Y, -Z SYMM -X, -Z, Y SYMM -Z, -Y, X SYMM -X, Y, -Z SYMM Z, -Y, -X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM -Y, -X, Z SYMM Y, X, Z SYMM X, -Z, -Y SYMM X, Z, Y SYMM -Z, Y, -X SYMM Z, Y, X SFAC C H N ZN UNIT 142.8 307.2 48 12 MERG 2 FMAP 2 GRID PLAN 5 TEMP 25 SIZE 0.2 0.19 0.18 OMIT -1 12 17 OMIT -1 1 20 OMIT 1 7 20 BOND $H CONF HTAB L.S. 20 ACTA 54 WGHT 0.060000 FVAR 0.07578 ZN1 4 0.500000 0.000000 0.250000 10.25000 0.04944 0.04944 = 0.04428 0.00000 0.00000 0.00000 C2 1 0.623042 0.007704 0.376958 10.50000 0.05050 0.04438 = 0.05050 -0.00028 0.00007 0.00028 N1 3 0.590259 -0.031315 0.317502 11.00000 0.05582 0.04774 = 0.05076 -0.00295 -0.00832 0.00456 C1 1 0.631280 -0.100838 0.313115 11.00000 0.07415 0.05508 = 0.06842 -0.01786 -0.01459 0.01094 AFIX 43 H1 2 0.621911 -0.141190 0.277391 11.00000 -1.20000 AFIX 0 C3 1 0.594234 0.085870 0.405766 10.50000 0.08040 0.05517 = 0.08040 -0.01534 -0.01851 0.01534 AFIX 137 H3A 2 0.635348 0.124207 0.400446 10.50000 -1.50000 H3B 2 0.579386 0.081606 0.460078 10.50000 -1.50000 H3C 2 0.549514 0.101868 0.375227 10.50000 -1.50000 HKLF 4 REM MDPZIF8_Methane50bar_0m in I-43m REM R1 = 0.0337 for 965 Fo > 4sig(Fo) and 0.0481 for all 1138 data REM 34 parameters refined using 0 restraints END WGHT 0.0600 0.0000 REM Highest difference peak 0.362, deepest hole -0.208, 1-sigma level 0.095 Q1 1 0.4991 -0.3045 0.3045 10.50000 0.05 0.36 Q2 1 0.6629 -0.3371 0.3371 10.16667 0.05 0.36 Q3 1 0.6784 0.3216 0.3216 10.16667 0.05 0.35 Q4 1 0.6809 -0.3191 0.3191 10.16667 0.05 0.35 Q5 1 0.5000 0.2613 0.5000 10.25000 0.05 0.27 ; #====================================================================== _database_code_depnum_ccdc_archive 'CCDC 963855' ####################################################################### # # 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_C: _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZIF8Vacuum _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 N4 Zn' _chemical_formula_sum 'C8 H10 N4 Zn' _chemical_formula_weight 227.57 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m _symmetry_space_group_name_Hall I-423 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, z, -y' 'x, -y, -z' '-x, -z, y' '-z, -y, x' '-x, y, -z' 'z, -y, -x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+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, -y+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' '-z+1/2, -y+1/2, x+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, -y+1/2, -x+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' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, z+1/2, -x+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, -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' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 17.033(2) _cell_length_b 17.033(2) _cell_length_c 17.033(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4941.2(10) _cell_formula_units_Z 12 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6164 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.70 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7581 _exptl_absorpt_correction_T_max 0.7783 _exptl_absorpt_process_details 'Symmetry-related measurements' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17433 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1173 _reflns_number_gt 1089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001;Atwood & Barbour,2003)' _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. ; _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^)+(0.0607P)^2^+0.6848P] 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 -0.04(3) _refine_ls_number_reflns 1173 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _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 Zn1 Zn 0.5000 1.0000 0.7500 0.0461(2) Uani 1 4 d S . . N1 N 0.40996(14) 1.03182(13) 0.68241(14) 0.0496(5) Uani 1 1 d . . . C2 C 0.37704(12) 0.9935(4) 0.62296(12) 0.0456(8) Uani 1 2 d S . . C1 C 0.3691(2) 1.10145(18) 0.6866(2) 0.0629(8) Uani 1 1 d . . . H1 H 0.3786 1.1418 0.7222 0.075 Uiso 1 1 calc R . . C3 C 0.4053(2) 0.9143(3) 0.5947(2) 0.0686(12) Uani 1 2 d S . . H3A H 0.4010 0.8768 0.6365 0.103 Uiso 0.50 1 calc PR . . H3B H 0.4592 0.9183 0.5785 0.103 Uiso 0.50 1 calc PR . . H3C H 0.3738 0.8976 0.5511 0.103 Uiso 0.50 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 Zn1 0.0481(2) 0.0481(2) 0.0419(3) 0.000 0.000 0.000 N1 0.0530(12) 0.0472(10) 0.0486(11) -0.0032(9) -0.0082(9) 0.0045(9) C2 0.0468(9) 0.043(2) 0.0468(9) -0.0003(14) -0.0005(11) 0.0003(14) C1 0.0718(19) 0.0510(14) 0.0659(18) -0.0166(14) -0.0147(15) 0.0114(13) C3 0.0756(18) 0.055(2) 0.0756(18) -0.0173(17) -0.018(2) 0.0173(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 Zn1 N1 1.993(2) 26_466 ? Zn1 N1 1.993(2) 28_656 ? Zn1 N1 1.993(2) . ? Zn1 N1 1.993(2) 3_675 ? N1 C2 1.329(4) . ? N1 C1 1.376(4) . ? C2 N1 1.329(4) 23_656 ? C2 C3 1.511(7) . ? C1 C1 1.343(6) 23_656 ? C1 H1 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 Zn1 N1 109.42(14) 26_466 28_656 ? N1 Zn1 N1 109.50(7) 26_466 . ? N1 Zn1 N1 109.49(7) 28_656 . ? N1 Zn1 N1 109.49(7) 26_466 3_675 ? N1 Zn1 N1 109.50(7) 28_656 3_675 ? N1 Zn1 N1 109.42(14) . 3_675 ? C2 N1 C1 104.5(3) . . ? C2 N1 Zn1 129.2(3) . . ? C1 N1 Zn1 126.36(19) . . ? N1 C2 N1 113.7(5) 23_656 . ? N1 C2 C3 123.1(2) 23_656 . ? N1 C2 C3 123.2(2) . . ? C1 C1 N1 108.68(16) 23_656 . ? C1 C1 H1 125.7 23_656 . ? N1 C1 H1 125.7 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 N1 C2 171.1(3) 26_466 . . . ? N1 Zn1 N1 C2 -68.9(3) 28_656 . . . ? N1 Zn1 N1 C2 51.1(3) 3_675 . . . ? N1 Zn1 N1 C1 -6.9(3) 26_466 . . . ? N1 Zn1 N1 C1 113.1(3) 28_656 . . . ? N1 Zn1 N1 C1 -126.9(3) 3_675 . . . ? C1 N1 C2 N1 -1.5(5) . . . 23_656 ? Zn1 N1 C2 N1 -179.84(12) . . . 23_656 ? C1 N1 C2 C3 177.7(4) . . . . ? Zn1 N1 C2 C3 -0.7(6) . . . . ? C2 N1 C1 C1 0.9(3) . . . 23_656 ? Zn1 N1 C1 C1 179.26(16) . . . 23_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.790 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.054 #============================================================================== _iucr_refine_instruction_details ; TITL mo_MDPZIF8Vacuum_0m in I-43m CELL 0.71073 17.0325 17.0325 17.0325 90.000 90.000 90.000 ZERR 12.0000 0.0020 0.0020 0.0020 0.000 0.000 0.000 LATT -2 SYMM Y, -X, -Z SYMM -X, -Y, Z SYMM -Y, X, -Z SYMM -X, Z, -Y SYMM X, -Y, -Z SYMM -X, -Z, Y SYMM -Z, -Y, X SYMM -X, Y, -Z SYMM Z, -Y, -X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM -Y, -X, Z SYMM Y, X, Z SYMM X, -Z, -Y SYMM X, Z, Y SYMM -Z, Y, -X SYMM Z, Y, X SFAC C H N ZN UNIT 96 120 48 12 MERG 2 FMAP GRID PLAN 5 TEMP 25 SIZE 0.2 0.19 0.18 OMIT -11 12 15 OMIT -9 12 17 OMIT -8 14 16 OMIT -11 11 16 BOND $H CONF HTAB L.S. 20 ACTA WGHT 0.060700 0.684800 FVAR 0.07517 ZN1 4 0.500000 1.000000 0.750000 10.25000 0.04812 0.04812 = 0.04191 0.00000 0.00000 0.00000 N1 3 0.409957 1.031820 0.682410 11.00000 0.05298 0.04719 = 0.04862 -0.00324 -0.00819 0.00445 C2 1 0.377043 0.993504 0.622957 10.50000 0.04680 0.04312 = 0.04680 -0.00030 -0.00047 0.00030 C1 1 0.369144 1.101446 0.686614 11.00000 0.07175 0.05100 = 0.06594 -0.01660 -0.01473 0.01142 AFIX 43 H1 2 0.378607 1.141792 0.722166 11.00000 -1.20000 AFIX 0 C3 1 0.405323 0.914341 0.594677 10.50000 0.07561 0.05473 = 0.07561 -0.01732 -0.01770 0.01732 AFIX 137 H3A 2 0.400991 0.876805 0.636498 10.50000 -1.50000 H3B 2 0.459167 0.918308 0.578495 10.50000 -1.50000 H3C 2 0.373783 0.897604 0.551067 10.50000 -1.50000 HKLF 4 REM mo_MDPZIF8Vacuum_0m in I-43m REM R1 = 0.0325 for 1089 Fo > 4sig(Fo) and 0.0385 for all 1173 data REM 34 parameters refined using 0 restraints END WGHT 0.0607 0.6848 REM Highest difference peak 0.790, deepest hole -0.376, 1-sigma level 0.054 Q1 1 0.2502 1.2502 0.7498 10.16667 0.05 0.79 Q2 1 0.5000 0.7506 0.5000 10.25000 0.05 0.59 Q3 1 0.5000 1.0000 0.7181 10.50000 0.05 0.40 Q4 1 0.5000 1.0000 0.6957 10.50000 0.05 0.35 Q5 1 0.4457 1.0019 0.7191 11.00000 0.05 0.34 ; #====================================================================== _database_code_depnum_ccdc_archive 'CCDC 963856'