data_MOF-77 _publ_requested_journal 'J. Am. Chem. Soc.' _publ_section_title ; Rod Packings and Metal-Organic Frameworks Constructed From Rod-Shaped Secondary Building Units ; _publ_contact_author ; Omar M. Yaghi Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; _publ_contact_author_email oyaghi@umich.edu loop_ _publ_author_name _publ_author_address 'Nathaniel L. Rosi' ; Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; 'Jaheon Kim' ; Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; 'Mohamed Eddaoudi' ; Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; 'Michael O'Keeffe' ; Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287-1604 USA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H6 O4 Zn' _chemical_formula_sum 'C7 H6 O4 Zn' _chemical_formula_weight 219.49 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' 'O' 'O' 0.0106 0.0060 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 7.261(4) _cell_length_b 7.261(4) _cell_length_c 25.471(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1342.8(14) _cell_formula_units_Z 8 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 1272 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 20.86 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 3.619 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; 50KV/40ma; 30 sec. frames; 0.3 deg. steps in omega and phi; 5.008 sample - detector distance; 2132 frames giving full sphere of data ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16739 _diffrn_reflns_av_R_equivalents 0.1505 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 23.26 _reflns_number_total 485 _reflns_number_gt 359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. Due to the paucity of high angle reflections, the resolution of data used in the refinement was limited to 0.90 A^3. ; _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^)+(0.0989P)^2^+10.1334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 485 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.0000 0.2500 0.02854(6) 0.0419(9) Uani 1 2 d S . . O1 O -0.1825(12) 0.3879(12) -0.0124(3) 0.084(3) Uani 1 1 d . . . O2 O -0.1602(10) 0.1012(9) 0.0718(3) 0.051(2) Uani 1 1 d . . . C1 C -0.2207(12) 0.4531(12) -0.0566(3) 0.033(2) Uani 1 1 d . . . C2 C -0.3625(11) 0.3562(11) -0.0900(3) 0.026(2) Uani 1 1 d . . . C3 C -0.2580(12) 0.2174(13) -0.1250(4) 0.029(2) Uani 1 1 d . . . H3A H -0.192(12) 0.270(10) -0.147(3) 0.02(2) Uiso 1 1 d . . . H3B H -0.193(11) 0.121(12) -0.104(3) 0.03(2) Uiso 1 1 d . . . C4 C -0.5000 0.2500 -0.0551(5) 0.027(3) Uani 1 2 d S . . H4 H -0.574(9) 0.343(10) -0.036(3) 0.015(18) Uiso 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 Zn1 0.0555(13) 0.0382(12) 0.0319(11) 0.000 0.000 -0.0229(7) O1 0.087(6) 0.085(6) 0.080(6) 0.021(5) -0.050(5) -0.041(5) O2 0.059(5) 0.051(5) 0.043(4) -0.001(3) 0.006(3) -0.029(4) C1 0.036(5) 0.035(6) 0.027(5) -0.005(4) 0.003(4) -0.006(4) C2 0.026(4) 0.025(4) 0.027(4) 0.002(4) -0.001(4) -0.006(3) C3 0.022(5) 0.035(5) 0.030(5) 0.005(5) 0.000(4) 0.003(4) C4 0.032(7) 0.024(7) 0.025(6) 0.000 0.000 -0.005(6) _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 O2 1.932(6) . ? Zn1 O2 1.932(6) 6_454 ? Zn1 O1 1.962(9) 6_454 ? Zn1 O1 1.962(9) . ? O1 C1 1.252(11) . ? O2 C1 1.224(10) 14_545 ? C1 O2 1.224(10) 14 ? C1 C2 1.508(11) . ? C2 C3 1.533(12) 16_565 ? C2 C4 1.543(10) . ? C2 C3 1.545(12) . ? C3 C2 1.533(12) 11 ? C4 C2 1.543(10) 6_354 ? 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 O2 Zn1 O2 110.5(4) . 6_454 ? O2 Zn1 O1 115.1(3) . 6_454 ? O2 Zn1 O1 100.5(3) 6_454 6_454 ? O2 Zn1 O1 100.5(3) . . ? O2 Zn1 O1 115.1(3) 6_454 . ? O1 Zn1 O1 115.7(6) 6_454 . ? C1 O1 Zn1 145.2(9) . . ? C1 O2 Zn1 121.9(6) 14_545 . ? O2 C1 O1 122.4(8) 14 . ? O2 C1 C2 118.5(8) 14 . ? O1 C1 C2 118.7(8) . . ? C1 C2 C3 111.5(7) . 16_565 ? C1 C2 C4 110.5(6) . . ? C3 C2 C4 109.6(6) 16_565 . ? C1 C2 C3 107.1(6) . . ? C3 C2 C3 109.1(5) 16_565 . ? C4 C2 C3 108.9(6) . . ? C2 C3 C2 110.2(7) 11 . ? C2 C4 C2 109.6(9) . 6_354 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.969 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.137