Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_MOF-48 _database_code_CSD 171766 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' _publ_section_title ; Metal-organic frameworks constructed from pentagonal antiprismatic and cuboctahedral 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 'David T. Vodak' ; Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; 'Matthew E. Braun' ; 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 ; 'Omar M. Yaghi' ;Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H74 N6 O28 Zn6' _chemical_formula_weight 1935.65 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.5043(16) _cell_length_b 16.4817(14) _cell_length_c 14.6396(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.902(2) _cell_angle_gamma 90.00 _cell_volume 4681.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.586 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19056 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.1581 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4284 _reflns_number_gt 1563 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1838P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4284 _refine_ls_number_parameters 386 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1973 _refine_ls_R_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.3033 _refine_ls_wR_factor_gt 0.2546 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 0.062 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 0.86752(11) 0.5000 0.51865(19) 0.0751(11) Uani 1 2 d S . . Zn2 Zn 0.91678(10) 0.59741(14) 0.33421(16) 0.0864(10) Uani 1 1 d . . . O1 O 0.8312(5) 0.6525(8) 0.3423(8) 0.091(4) Uani 1 1 d . A . O2 O 0.7984(5) 0.5834(8) 0.4620(8) 0.071(3) Uani 1 1 d . A . O3 O 0.4885(5) 0.8199(8) 0.3657(9) 0.091(4) Uani 1 1 d . . . O4 O 0.5584(5) 0.9136(8) 0.4229(8) 0.072(4) Uani 1 1 d . . . O5 O 0.9270(6) 0.5000 0.4100(8) 0.055(4) Uani 1 2 d S . . C7 C 0.7887(7) 0.6320(13) 0.4027(14) 0.071(5) Uani 1 1 d . . . C8 C 0.5484(7) 0.8469(14) 0.3959(11) 0.066(5) Uani 1 1 d . . . C1 C 0.7212(7) 0.6845(14) 0.3926(13) 0.073(5) Uani 1 1 d . A 1 C2 C 0.6962(16) 0.740(3) 0.302(3) 0.073(12) Uani 0.50 1 d P A 1 C3 C 0.6403(15) 0.788(2) 0.307(2) 0.061(10) Uani 0.50 1 d P A 1 C4 C 0.6069(7) 0.7861(12) 0.3936(13) 0.070(5) Uani 1 1 d . A 1 C5 C 0.6283(18) 0.750(3) 0.459(3) 0.072(15) Uani 0.50 1 d P A 1 C6 C 0.6849(17) 0.697(3) 0.463(2) 0.063(11) Uani 0.50 1 d P A 1 C9 C 0.7280(16) 0.733(3) 0.216(2) 0.106(16) Uani 0.50 1 d P A 1 C10 C 0.7021(18) 0.774(3) 0.137(2) 0.112(17) Uani 0.50 1 d P A 1 C11 C 0.639(3) 0.824(3) 0.136(4) 0.091(16) Uani 0.50 1 d P A 1 C12 C 0.6113(17) 0.832(3) 0.224(3) 0.093(13) Uani 0.50 1 d P A 1 C2' C 0.7217(17) 0.752(3) 0.358(3) 0.061(10) Uani 0.50 1 d P B 2 C3' C 0.6665(14) 0.807(2) 0.366(3) 0.054(8) Uani 0.50 1 d P B 2 C5' C 0.6075(16) 0.702(3) 0.444(3) 0.073(14) Uani 0.50 1 d P . 2 C6' C 0.6622(19) 0.649(3) 0.444(3) 0.081(14) Uani 0.50 1 d P . 2 C9' C 0.6578(17) 0.565(3) 0.477(4) 0.13(2) Uani 0.50 1 d P . 2 C10' C 0.604(2) 0.539(2) 0.508(4) 0.14(2) Uani 0.50 1 d P . 2 C11' C 0.5470(19) 0.598(3) 0.522(4) 0.131(19) Uani 0.50 1 d P . 2 C12' C 0.5477(16) 0.678(3) 0.494(3) 0.102(15) Uani 0.50 1 d P . 2 O7 O 0.962(2) 0.567(3) 0.221(3) 0.081(13) Uani 0.50 1 d P . 3 C13 C 0.974(3) 0.5000 0.182(4) 0.063(14) Uani 0.50 2 d SPU . 3 C14 C 1.008(3) 0.5000 0.103(3) 0.063(10) Uani 0.50 2 d SPU . 3 C15 C 0.9881(18) 0.450(2) 0.047(2) 0.069(8) Uani 0.50 1 d PU . 3 C16 C 1.050(3) 0.419(4) 0.076(4) 0.055(13) Uani 0.25 1 d PU . 3 C17 C 1.077(4) 0.360(5) 0.138(4) 0.08(2) Uani 0.25 1 d PU C 3 C18 C 1.113(5) 0.288(6) 0.118(6) 0.064(19) Uani 0.25 1 d PU C 3 C19 C 1.145(4) 0.301(5) 0.034(6) 0.11(3) Uani 0.25 1 d PU C 3 C20 C 1.123(4) 0.358(4) -0.034(5) 0.077(19) Uani 0.25 1 d PU C 3 C21 C 1.076(3) 0.419(4) -0.016(4) 0.056(13) Uani 0.25 1 d PU . 3 O7' O 0.9239(17) 0.566(3) 0.209(3) 0.075(12) Uani 0.50 1 d P . 4 C13' C 0.927(4) 0.5000 0.171(4) 0.074(17) Uani 0.50 2 d SP . 4 C14' C 0.942(2) 0.5000 0.076(3) 0.061(13) Uani 0.50 2 d SP . 4 O1S O 0.8189(8) 0.5000 0.6354(11) 0.087(5) Uani 1 2 d SD . . N1S N 0.735(4) 0.462(5) 0.726(5) 0.30(2) Uiso 0.50 1 d PD . . C1S C 0.7558(12) 0.5000 0.644(6) 0.30(2) Uiso 1 2 d SD . . C2S C 0.679(5) 0.410(6) 0.748(7) 0.30(2) Uiso 0.50 1 d PD . . C3S C 0.772(4) 0.5000 0.806(5) 0.30(2) Uiso 1 2 d SD . . C7S C 0.776(5) 0.5000 0.230(7) 0.87(5) Uiso 1 2 d SD . . O3S O 0.840(5) 0.5000 0.226(11) 0.87(5) Uiso 1 2 d SD . . N3S N 0.740(4) 0.5000 0.136(6) 0.87(5) Uiso 1 2 d SD . . C8S C 0.697(6) 0.4296(2) 0.085(6) 0.87(5) Uiso 1 1 d D . . O2S O 0.498(4) 0.391(5) 0.785(5) 0.35(2) Uiso 0.50 1 d PD . . C4S C 0.525(5) 0.368(6) 0.861(5) 0.35(2) Uiso 0.50 1 d PD . . N2S N 0.576(3) 0.314(4) 0.817(4) 0.35(2) Uiso 0.50 1 d PD . . C5S C 0.600(5) 0.231(4) 0.849(7) 0.35(2) Uiso 0.50 1 d PD . . C6S C 0.611(5) 0.336(6) 0.732(6) 0.35(2) Uiso 0.50 1 d PD . . 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 0.0245(12) 0.145(3) 0.0581(18) 0.000 0.0148(11) 0.000 Zn2 0.0595(13) 0.1029(18) 0.1057(19) -0.0279(14) 0.0514(12) -0.0072(11) O1 0.035(6) 0.153(12) 0.085(9) 0.029(8) 0.009(6) 0.020(7) O2 0.047(7) 0.101(10) 0.064(8) 0.017(7) 0.005(6) 0.001(6) O3 0.029(6) 0.113(10) 0.130(11) -0.012(8) 0.004(6) -0.006(6) O4 0.033(6) 0.100(11) 0.082(9) -0.014(7) -0.005(5) -0.004(6) O5 0.037(7) 0.093(11) 0.035(8) 0.000 0.007(6) 0.000 C7 0.020(7) 0.112(16) 0.080(14) -0.018(12) -0.003(8) -0.007(8) C8 0.027(8) 0.126(18) 0.046(10) -0.001(10) 0.013(7) -0.017(9) C1 0.024(8) 0.118(17) 0.077(13) -0.006(12) 0.001(8) 0.001(9) C2 0.028(18) 0.14(4) 0.05(2) 0.02(3) 0.006(16) -0.01(2) C3 0.034(17) 0.12(3) 0.037(19) 0.02(2) 0.015(14) 0.027(18) C4 0.024(8) 0.127(17) 0.060(12) -0.005(11) 0.009(8) 0.001(9) C5 0.021(19) 0.15(5) 0.05(2) -0.03(3) 0.015(17) -0.03(2) C6 0.03(2) 0.11(4) 0.05(2) -0.01(2) 0.015(16) -0.019(19) C9 0.050(19) 0.24(5) 0.025(17) 0.02(2) 0.005(15) 0.02(3) C10 0.06(2) 0.22(5) 0.06(2) 0.03(3) 0.012(19) 0.06(3) C11 0.08(4) 0.12(5) 0.08(3) 0.02(3) 0.03(3) -0.01(3) C12 0.05(2) 0.15(4) 0.08(3) 0.02(3) 0.03(2) 0.02(2) C2' 0.04(2) 0.07(3) 0.07(3) 0.02(2) -0.001(18) 0.018(19) C3' 0.028(16) 0.08(2) 0.06(2) -0.006(19) 0.006(15) 0.003(15) C5' 0.018(18) 0.14(4) 0.06(2) 0.05(3) 0.000(16) -0.01(2) C6' 0.03(2) 0.09(4) 0.11(4) 0.00(3) 0.00(2) 0.02(2) C9' 0.035(19) 0.13(4) 0.22(6) 0.11(4) 0.01(3) 0.01(2) C10' 0.06(2) 0.11(4) 0.24(6) 0.11(3) 0.00(3) 0.00(2) C11' 0.05(2) 0.17(5) 0.18(5) 0.09(4) 0.01(3) -0.02(3) C12' 0.05(2) 0.14(4) 0.12(3) 0.07(3) 0.00(2) -0.02(2) O7 0.10(3) 0.10(3) 0.049(19) -0.016(17) 0.02(2) -0.05(3) C13 0.03(3) 0.11(5) 0.04(2) 0.000 0.003(19) 0.000 C14 0.08(3) 0.08(2) 0.03(2) 0.000 0.007(18) 0.000 C15 0.071(19) 0.07(2) 0.063(19) -0.011(14) -0.003(17) 0.009(17) C16 0.06(2) 0.08(3) 0.03(2) 0.000(19) 0.01(2) -0.01(2) C17 0.08(4) 0.12(5) 0.03(3) 0.02(3) 0.01(3) 0.04(4) C18 0.09(7) 0.06(5) 0.05(4) -0.01(3) 0.01(4) -0.02(3) C19 0.11(6) 0.11(7) 0.10(6) 0.02(4) 0.06(5) 0.04(4) C20 0.11(5) 0.07(5) 0.06(4) 0.00(3) 0.05(4) -0.02(3) C21 0.07(3) 0.07(4) 0.03(2) 0.00(2) 0.02(2) -0.03(2) O7' 0.07(2) 0.11(3) 0.05(2) 0.024(19) 0.01(2) 0.02(3) C13' 0.05(4) 0.12(7) 0.06(4) 0.000 0.00(3) 0.000 C14' 0.04(3) 0.11(4) 0.03(2) 0.000 -0.01(2) 0.000 O1S 0.050(9) 0.146(16) 0.072(11) 0.000 0.032(8) 0.000 _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 O1S 2.038(14) . ? Zn1 O2 2.041(12) 6_565 ? Zn1 O2 2.041(12) . ? Zn1 O5 2.062(12) . ? Zn1 O4 2.143(12) 7_666 ? Zn1 O4 2.143(12) 4_646 ? Zn2 O1 1.914(11) . ? Zn2 O7' 1.93(5) . ? Zn2 O5 1.950(7) . ? Zn2 O3 1.973(12) 8_565 ? Zn2 O7 2.02(4) . ? O1 C7 1.32(2) . ? O2 C7 1.18(2) . ? O3 C8 1.285(17) . ? O3 Zn2 1.973(11) 8_465 ? O4 C8 1.18(2) . ? O4 Zn1 2.143(12) 7_666 ? O5 Zn2 1.950(7) 6_565 ? C7 C1 1.57(2) . ? C8 C4 1.52(2) . ? C1 C6 1.32(4) . ? C1 C2 1.65(4) . ? C2 C3 1.35(5) . ? C2 C9 1.47(4) . ? C3 C12 1.48(5) . ? C3 C4 1.49(3) . ? C4 C5 1.17(5) . ? C5 C6 1.41(6) . ? C9 C10 1.39(5) . ? C10 C11 1.47(6) . ? C11 C12 1.47(6) . ? C2' C3' 1.42(4) . ? C5' C6' 1.38(5) . ? C5' C12' 1.49(4) . ? C6' C9' 1.47(6) . ? C9' C10' 1.25(5) . ? C10' C10' 1.30(8) 6_565 ? C10' C11' 1.50(6) . ? C11' C12' 1.39(5) . ? C11' C11' 1.88(8) 2_656 ? C12' C12' 1.89(6) 2_656 ? O7 C13 1.28(5) . ? C13 O7 1.28(5) 6_565 ? C13 C14 1.39(6) . ? C14 C15 1.20(4) . ? C14 C15 1.20(4) 6_565 ? C14 C16 1.64(7) 6_565 ? C14 C16 1.64(7) . ? C15 C16 1.35(7) . ? C15 C21 1.38(7) 2_755 ? C15 C15 1.49(6) 2_755 ? C15 C15 1.65(7) 6_565 ? C15 C16 1.95(7) 2_755 ? C16 C17 1.39(9) . ? C16 C21 1.48(7) . ? C16 C15 1.95(7) 2_755 ? C17 C18 1.43(13) . ? C18 C19 1.45(12) . ? C19 C20 1.40(10) . ? C20 C21 1.42(9) . ? C21 C15 1.38(7) 2_755 ? O7' C13' 1.22(5) . ? C13' O7' 1.22(5) 6_565 ? C13' C14' 1.45(7) . ? C13' O3S 1.94(12) . ? O1S C1S 1.249(8) . ? N1S N1S 1.25(16) 6_565 ? N1S C1S 1.451(8) . ? N1S C3S 1.452(8) . ? N1S C2S 1.450(8) . ? C1S N1S 1.451(8) 6_565 ? C2S C6S 1.80(12) . ? C3S N1S 1.452(8) 6_565 ? C7S O3S 1.252(8) . ? C7S N3S 1.497(10) . ? N3S C8S 1.566(8) . ? N3S C8S 1.566(8) 6_565 ? C8S C8S 2.320(8) 6_565 ? O2S C4S 1.251(8) . ? C4S N2S 1.524(6) . ? N2S C5S 1.515(7) . ? N2S C6S 1.525(7) . ? 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 O1S Zn1 O2 89.8(5) . 6_565 ? O1S Zn1 O2 89.8(5) . . ? O2 Zn1 O2 84.7(7) 6_565 . ? O1S Zn1 O5 173.6(6) . . ? O2 Zn1 O5 95.0(4) 6_565 . ? O2 Zn1 O5 95.0(4) . . ? O1S Zn1 O4 91.0(5) . 7_666 ? O2 Zn1 O4 178.9(4) 6_565 7_666 ? O2 Zn1 O4 96.0(4) . 7_666 ? O5 Zn1 O4 84.2(4) . 7_666 ? O1S Zn1 O4 91.0(5) . 4_646 ? O2 Zn1 O4 96.0(4) 6_565 4_646 ? O2 Zn1 O4 178.9(4) . 4_646 ? O5 Zn1 O4 84.2(4) . 4_646 ? O4 Zn1 O4 83.2(6) 7_666 4_646 ? O1 Zn2 O7' 109.5(10) . . ? O1 Zn2 O5 113.2(5) . . ? O7' Zn2 O5 108.0(14) . . ? O1 Zn2 O3 105.1(5) . 8_565 ? O7' Zn2 O3 106.8(14) . 8_565 ? O5 Zn2 O3 114.0(5) . 8_565 ? O1 Zn2 O7 128.8(14) . . ? O7' Zn2 O7 21.8(10) . . ? O5 Zn2 O7 103.6(15) . . ? O3 Zn2 O7 90.0(10) 8_565 . ? C7 O1 Zn2 122.2(12) . . ? C7 O2 Zn1 143.6(11) . . ? C8 O3 Zn2 116.1(13) . 8_465 ? C8 O4 Zn1 146.6(11) . 7_666 ? Zn2 O5 Zn2 110.8(6) . 6_565 ? Zn2 O5 Zn1 114.0(4) . . ? Zn2 O5 Zn1 114.0(4) 6_565 . ? O2 C7 O1 127.0(15) . . ? O2 C7 C1 120.9(16) . . ? O1 C7 C1 112.1(18) . . ? O4 C8 O3 123.4(17) . . ? O4 C8 C4 121.6(14) . . ? O3 C8 C4 115.0(18) . . ? C6 C1 C7 122(2) . . ? C6 C1 C2 114(3) . . ? C7 C1 C2 124.1(18) . . ? C3 C2 C9 120(4) . . ? C3 C2 C1 117(3) . . ? C9 C2 C1 122(3) . . ? C2 C3 C12 120(3) . . ? C2 C3 C4 117(3) . . ? C12 C3 C4 123(2) . . ? C5 C4 C3 124(3) . . ? C5 C4 C8 121(3) . . ? C3 C4 C8 113.8(19) . . ? C4 C5 C6 124(3) . . ? C1 C6 C5 123(4) . . ? C10 C9 C2 122(3) . . ? C9 C10 C11 121(4) . . ? C12 C11 C10 116(4) . . ? C11 C12 C3 122(4) . . ? C6' C5' C12' 118(4) . . ? C5' C6' C9' 122(4) . . ? C10' C9' C6' 121(4) . . ? C9' C10' C10' 110(3) . 6_565 ? C9' C10' C11' 119(4) . . ? C10' C10' C11' 130(2) 6_565 . ? C12' C11' C10' 123(3) . . ? C12' C11' C11' 86(2) . 2_656 ? C10' C11' C11' 132(4) . 2_656 ? C11' C12' C5' 116(4) . . ? C11' C12' C12' 86(2) . 2_656 ? C5' C12' C12' 151(3) . 2_656 ? C13 O7 Zn2 134(3) . . ? O7 C13 O7 120(5) . 6_565 ? O7 C13 C14 120(2) . . ? O7 C13 C14 120(2) 6_565 . ? C15 C14 C15 87(4) . 6_565 ? C15 C14 C13 115(4) . . ? C15 C14 C13 115(4) 6_565 . ? C15 C14 C16 122(4) . 6_565 ? C15 C14 C16 54(3) 6_565 6_565 ? C13 C14 C16 120(3) . 6_565 ? C15 C14 C16 54(3) . . ? C15 C14 C16 122(4) 6_565 . ? C13 C14 C16 120(3) . . ? C16 C14 C16 109(5) 6_565 . ? C14 C15 C16 80(4) . . ? C14 C15 C21 134(4) . 2_755 ? C16 C15 C21 136(5) . 2_755 ? C14 C15 C15 121(4) . 2_755 ? C16 C15 C15 86(4) . 2_755 ? C21 C15 C15 93(4) 2_755 2_755 ? C14 C15 C15 47(2) . 6_565 ? C16 C15 C15 112(3) . 6_565 ? C21 C15 C15 111(3) 2_755 6_565 ? C15 C15 C15 89.995(3) 2_755 6_565 ? C14 C15 C16 152(4) . 2_755 ? C16 C15 C16 116(4) . 2_755 ? C21 C15 C16 49(3) 2_755 2_755 ? C15 C15 C16 44(2) 2_755 2_755 ? C15 C15 C16 105(2) 6_565 2_755 ? C15 C16 C17 137(6) . . ? C15 C16 C21 95(4) . . ? C17 C16 C21 118(6) . . ? C15 C16 C14 46(3) . . ? C17 C16 C14 125(5) . . ? C21 C16 C14 116(5) . . ? C15 C16 C15 50(3) . 2_755 ? C17 C16 C15 150(5) . 2_755 ? C21 C16 C15 45(3) . 2_755 ? C14 C16 C15 81(3) . 2_755 ? C16 C17 C18 127(6) . . ? C17 C18 C19 108(8) . . ? C20 C19 C18 125(7) . . ? C21 C20 C19 120(6) . . ? C15 C21 C20 142(6) 2_755 . ? C15 C21 C16 86(4) 2_755 . ? C20 C21 C16 117(6) . . ? C13' O7' Zn2 132(4) . . ? O7' C13' O7' 126(7) . 6_565 ? O7' C13' C14' 117(4) . . ? O7' C13' C14' 117(4) 6_565 . ? O7' C13' O3S 75(5) . . ? O7' C13' O3S 75(5) 6_565 . ? C14' C13' O3S 132(7) . . ? C1S O1S Zn1 129(4) . . ? N1S N1S C1S 65(3) 6_565 . ? N1S N1S C3S 65(3) 6_565 . ? C1S N1S C3S 109(8) . . ? N1S N1S C2S 127(6) 6_565 . ? C1S N1S C2S 136(7) . . ? C3S N1S C2S 113(7) . . ? O1S C1S N1S 116(6) . 6_565 ? O1S C1S N1S 116(6) . . ? N1S C1S N1S 51(7) 6_565 . ? N1S C2S C6S 159(9) . . ? N1S C3S N1S 51(7) . 6_565 ? O3S C7S N3S 110(10) . . ? C7S O3S C13' 159(10) . . ? C8S N3S C8S 95.6(7) . 6_565 ? C8S N3S C7S 128.3(8) . . ? C8S N3S C7S 128.3(8) 6_565 . ? C8S C8S N3S 42.2(4) 6_565 . ? O2S C4S N2S 92(5) . . ? C5S N2S C4S 126.2(7) . . ? C5S N2S C6S 108.5(6) . . ? C4S N2S C6S 125.4(7) . . ? N2S C6S C2S 116(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.273 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.133 data_MOF-49 _database_code_CSD 171767 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' _publ_section_title ; Metal-organic frameworks constructed from pentagonal antiprismatic and cuboctahedral 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 'David T. Vodak' ; Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; 'Matthew E. Braun' ; 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 ; 'Omar M. Yaghi' ;Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64.50 H79.50 N5.50 O39 Zn7' _chemical_formula_weight 2013.43 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.509(2) _cell_length_b 11.9838(19) _cell_length_c 27.039(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.459(3) _cell_angle_gamma 90.00 _cell_volume 4369.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 985 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 19.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .25 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2054 _exptl_absorpt_coefficient_mu 1.977 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Siemens APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16427 _diffrn_reflns_av_R_equivalents 0.1431 _diffrn_reflns_av_sigmaI/netI 0.3684 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.21 _reflns_number_total 7224 _reflns_number_gt 2240 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0951P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7224 _refine_ls_number_parameters 462 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.2306 _refine_ls_R_factor_gt 0.0983 _refine_ls_wR_factor_ref 0.2720 _refine_ls_wR_factor_gt 0.2348 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 5.573 _refine_ls_shift/su_mean 0.142 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 0.82305(16) 1.17349(16) 0.54204(7) 0.0357(6) Uani 1 1 d . . . Zn2 Zn 1.19848(16) 1.17317(17) 0.55638(7) 0.0352(6) Uani 1 1 d . . . Zn3 Zn 1.0000 1.0000 0.5000 0.0317(8) Uani 1 2 d S . . Zn4 Zn 1.01156(17) 1.07594(15) 0.61105(7) 0.0343(6) Uani 1 1 d . . . O1W O 1.0056(9) 0.8977(9) 0.6290(4) 0.045(3) Uani 1 1 d . . . O1 O 0.9019(10) 1.1105(9) 0.6566(4) 0.037(3) Uani 1 1 d . . . O2 O 0.7918(9) 1.2087(9) 0.6096(4) 0.037(3) Uani 1 1 d . . . O3 O 0.8739(11) 1.0961(9) 0.8350(4) 0.048(4) Uani 1 1 d . . . O4 O 0.7539(10) 1.1837(10) 0.8726(5) 0.054(4) Uani 1 1 d . . . O5 O 1.1356(9) 1.3200(9) 0.5522(4) 0.039(3) Uani 1 1 d . . . O6 O 1.0140(10) 1.2493(10) 0.5977(5) 0.049(4) Uani 1 1 d . . . O7 O 1.1133(10) 1.7092(9) 0.4966(5) 0.047(4) Uani 1 1 d . . . O8 O 1.0114(9) 1.8286(9) 0.5323(4) 0.041(3) Uani 1 1 d . . . O9 O 0.6890(9) 1.1477(10) 0.5113(5) 0.046(3) Uani 1 1 d . . . O10 O 0.7510(11) 1.1187(10) 0.4387(5) 0.055(4) Uani 1 1 d . . . O11 O 0.3215(9) 1.1629(10) 0.5229(5) 0.047(3) Uani 1 1 d . . . O12 O 0.2249(11) 1.1350(10) 0.4508(6) 0.061(4) Uani 1 1 d . . . O13 O 1.1070(8) 1.0457(8) 0.5538(4) 0.030(3) Uani 1 1 d . . . O14 O 0.9043(9) 1.0424(7) 0.5526(4) 0.030(3) Uani 1 1 d . . . C1 C 0.7765(15) 1.2066(16) 0.6946(8) 0.050(5) Uani 1 1 d . . . C2 C 0.8043(15) 1.1712(15) 0.7426(7) 0.042(5) Uani 1 1 d . . . H2A H 0.8612 1.1246 0.7461 0.050 Uiso 1 1 calc R . . C3 C 0.7602(15) 1.1953(16) 0.7845(8) 0.049(5) Uani 1 1 d . . . C4 C 0.6746(18) 1.264(2) 0.7793(9) 0.072(7) Uani 1 1 d . . . H4A H 0.6389 1.2824 0.8074 0.086 Uiso 1 1 calc R . . C5 C 0.6447(18) 1.302(3) 0.7345(9) 0.097(10) Uani 1 1 d . . . H5A H 0.5883 1.3493 0.7319 0.116 Uiso 1 1 calc R . . C6 C 0.6913(17) 1.276(2) 0.6914(8) 0.074(7) Uani 1 1 d . . . H6A H 0.6665 1.3051 0.6604 0.088 Uiso 1 1 calc R . . C7 C 0.8276(17) 1.1732(16) 0.6517(6) 0.044(5) Uani 1 1 d . . . C8 C 0.7981(14) 1.1577(14) 0.8357(7) 0.033(4) Uani 1 1 d . . . C9 C 1.0112(14) 1.4432(13) 0.5796(6) 0.036(5) Uani 1 1 d . . . C10 C 1.0515(14) 1.5332(14) 0.5536(7) 0.044(5) Uani 1 1 d . . . H10A H 1.1088 1.5230 0.5355 0.053 Uiso 1 1 calc R . . C11 C 1.0051(14) 1.6385(12) 0.5552(7) 0.037(3) Uani 1 1 d . . . C12 C 0.9202(13) 1.6507(12) 0.5803(7) 0.037(3) Uani 1 1 d . . . H12A H 0.8905 1.7224 0.5815 0.045 Uiso 1 1 calc R . . C13 C 0.8777(16) 1.5651(15) 0.6031(8) 0.060(6) Uani 1 1 d . . . H13A H 0.8165 1.5749 0.6181 0.072 Uiso 1 1 calc R . . C14 C 0.9268(14) 1.4573(13) 0.6043(8) 0.055(7) Uani 1 1 d . . . H14A H 0.9006 1.3970 0.6222 0.066 Uiso 1 1 calc R . . C15 C 1.0569(15) 1.3297(15) 0.5758(6) 0.037(5) Uani 1 1 d . . . C16 C 1.0474(17) 1.7309(15) 0.5261(7) 0.047(6) Uani 1 1 d . . . C17 C 0.568(3) 1.079(3) 0.4444(13) 0.040(9) Uiso 0.50 1 d P . . C17' C 0.584(3) 1.167(3) 0.4401(13) 0.037(9) Uiso 0.50 1 d P . . C18 C 0.4924(16) 1.1392(19) 0.4702(8) 0.064(7) Uani 1 1 d . . . H18A H 0.5025 1.1968 0.4941 0.077 Uiso 0.50 1 calc PR . . C19 C 0.390(2) 1.088(3) 0.4498(11) 0.024(8) Uiso 0.50 1 d P . . C19' C 0.406(3) 1.174(4) 0.4471(15) 0.052(10) Uiso 0.50 1 d P . . C20 C 0.384(3) 1.037(3) 0.4063(14) 0.043(10) Uiso 0.50 1 d P . . H20A H 0.3196 1.0322 0.3904 0.052 Uiso 0.50 1 calc PR . . C20' C 0.390(4) 1.207(4) 0.3980(17) 0.072(14) Uiso 0.50 1 d P . . H20' H 0.3258 1.2203 0.3825 0.087 Uiso 0.50 1 calc PR . . C21 C 0.461(3) 0.989(3) 0.3806(15) 0.051(11) Uiso 0.50 1 d P . . H21A H 0.4522 0.9399 0.3530 0.061 Uiso 0.50 1 calc PR . . C21' C 0.486(4) 1.221(4) 0.372(2) 0.086(16) Uiso 0.50 1 d P . . H21' H 0.4819 1.2500 0.3394 0.103 Uiso 0.50 1 calc PR . . C22 C 0.557(3) 1.025(3) 0.4021(12) 0.034(9) Uiso 0.50 1 d P . . H22A H 0.6144 1.0084 0.3849 0.041 Uiso 0.50 1 calc PR . . C22' C 0.576(3) 1.195(3) 0.3917(15) 0.059(12) Uiso 0.50 1 d P . . H22' H 0.6324 1.1958 0.3722 0.071 Uiso 0.50 1 calc PR . . C23 C 0.6825(17) 1.1311(18) 0.4654(9) 0.064(5) Uani 1 1 d . . . C24 C 0.3075(18) 1.1431(18) 0.4743(9) 0.064(5) Uani 1 1 d . . . O1S O 0.319(3) 1.039(3) 0.3092(15) 0.110(13) Uiso 0.50 1 d P . . N1S N 0.455(5) 0.946(6) 0.335(3) 0.18(2) Uiso 0.50 1 d P . . C1S C 0.339(6) 0.998(6) 0.351(3) 0.16(3) Uiso 0.50 1 d P . . H1SA H 0.3049 0.9953 0.3807 0.195 Uiso 0.50 1 calc PR . . C2S C 0.553(12) 0.986(14) 0.310(5) 0.58(2) Uiso 0.50 1 d P . . H2SA H 0.5953 1.0288 0.3342 0.694 Uiso 0.50 1 calc PR . . H2SB H 0.5350 1.0334 0.2814 0.694 Uiso 0.50 1 calc PR . . H2SC H 0.5900 0.9209 0.2992 0.694 Uiso 0.50 1 calc PR . . C3S C 0.487(5) 0.876(5) 0.387(2) 0.12(2) Uiso 0.50 1 d P . . H3SA H 0.5266 0.9240 0.4098 0.141 Uiso 0.50 1 calc PR . . H3SB H 0.5256 0.8100 0.3790 0.141 Uiso 0.50 1 calc PR . . H3SC H 0.4268 0.8524 0.4028 0.141 Uiso 0.50 1 calc PR . . O2S O 0.711(4) 1.425(4) 0.395(2) 0.58(2) Uiso 1 1 d D . . N2S N 0.786(3) 1.347(4) 0.3434(18) 0.58(2) Uiso 1 1 d D . . C4S C 0.748(4) 1.456(4) 0.356(2) 0.58(2) Uiso 1 1 d D . . H4SA H 0.7506 1.5268 0.3400 0.694 Uiso 1 1 calc R . . C5S C 0.807(5) 1.229(4) 0.346(2) 0.58(2) Uiso 1 1 d D . . H5SA H 0.7526 1.1886 0.3278 0.694 Uiso 1 1 calc R . . H5SB H 0.8116 1.2051 0.3804 0.694 Uiso 1 1 calc R . . H5SC H 0.8691 1.2137 0.3305 0.694 Uiso 1 1 calc R . . C6S C 0.830(5) 1.373(6) 0.296(2) 0.58(2) Uiso 1 1 d D . . H6SA H 0.9026 1.3744 0.3007 0.694 Uiso 1 1 calc R . . H6SB H 0.8068 1.4469 0.2842 0.694 Uiso 1 1 calc R . . H6SC H 0.8100 1.3167 0.2712 0.694 Uiso 1 1 calc R . . O3S O 0.501(3) 1.510(3) 0.3350(13) 0.230(14) Uiso 1 1 d D . . N3S N 0.411(7) 1.560(7) 0.421(2) 0.54(4) Uiso 1 1 d D . . C7S C 0.453(6) 1.508(8) 0.376(2) 0.54(4) Uiso 1 1 d D . . H7SA H 0.4326 1.4324 0.3776 0.646 Uiso 1 1 calc R . . C8S C 0.502(7) 1.627(9) 0.427(3) 0.58(9) Uiso 1 1 d D . . H8SA H 0.5259 1.6457 0.3945 0.698 Uiso 1 1 calc R . . H8SB H 0.5533 1.5852 0.4463 0.698 Uiso 1 1 calc R . . H8SC H 0.4879 1.6966 0.4447 0.698 Uiso 1 1 calc R . . C9S C 0.369(4) 1.534(4) 0.4697(17) 0.25(2) Uiso 1 1 d D . . H9SA H 0.3098 1.4872 0.4642 0.300 Uiso 1 1 calc R . . H9SB H 0.3509 1.6037 0.4858 0.300 Uiso 1 1 calc R . . H9SC H 0.4186 1.4942 0.4909 0.300 Uiso 1 1 calc R . . O4S O 0.175(3) 1.141(5) 0.300(2) 0.07(2) Uiso 0.25 1 d PD . . N4S N 0.0000 1.102(6) 0.2500 0.13(3) Uiso 0.50 2 d SPD . . C10S C 0.091(4) 1.118(7) 0.281(3) 0.06(3) Uiso 0.25 1 d PD . . C11S C 0.0000 0.982(6) 0.2500 0.54(4) Uiso 1 2 d SD . . O2W O 0.147(3) 1.170(3) 0.3209(14) 0.116(17) Uani 0.50 1 d P . . O3W O 0.362(4) 1.160(3) 0.2457(18) 0.18(2) Uani 0.50 1 d P . . O4W O 1.0000 1.533(5) 0.2500 0.18(2) Uani 0.50 2 d SP . . O5W O 0.441(3) 1.387(3) 0.253(3) 0.25(3) Uani 0.50 1 d P . . 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 0.0480(15) 0.0230(11) 0.0362(13) 0.0008(10) 0.0029(11) 0.0026(11) Zn2 0.0423(15) 0.0270(12) 0.0370(13) 0.0023(10) 0.0083(11) 0.0057(11) Zn3 0.038(2) 0.0234(16) 0.0344(18) -0.0019(13) 0.0050(15) 0.0075(14) Zn4 0.0486(15) 0.0194(11) 0.0355(13) 0.0000(9) 0.0065(10) 0.0027(10) O1W 0.063(10) 0.019(7) 0.055(9) 0.012(5) 0.010(7) 0.003(6) O1 0.064(10) 0.023(7) 0.025(7) 0.000(5) 0.007(7) -0.004(6) O2 0.029(8) 0.046(8) 0.036(8) 0.008(6) 0.000(6) -0.004(6) O3 0.077(11) 0.029(7) 0.038(8) 0.004(6) 0.011(7) 0.016(7) O4 0.086(11) 0.040(8) 0.041(8) -0.004(6) 0.035(8) 0.001(7) O5 0.044(8) 0.026(7) 0.048(8) -0.003(6) 0.017(7) 0.005(6) O6 0.063(10) 0.024(7) 0.064(9) 0.004(6) 0.028(8) 0.005(7) O7 0.066(10) 0.025(7) 0.054(9) 0.008(6) 0.029(8) -0.005(6) O8 0.066(9) 0.006(6) 0.049(8) -0.007(5) -0.009(7) 0.007(6) O9 0.033(8) 0.045(8) 0.060(10) 0.007(7) -0.003(7) 0.004(6) O10 0.066(11) 0.048(9) 0.051(9) -0.003(6) 0.010(8) 0.010(7) O11 0.037(8) 0.056(8) 0.049(9) 0.017(7) 0.009(7) 0.018(7) O12 0.045(10) 0.038(8) 0.101(12) -0.007(7) 0.013(9) 0.002(7) O13 0.032(8) 0.022(6) 0.037(7) 0.005(5) -0.006(6) 0.002(5) O14 0.049(9) 0.012(6) 0.027(7) 0.004(4) 0.000(6) 0.012(5) C1 0.034(13) 0.056(14) 0.059(16) -0.003(10) 0.003(11) -0.003(10) C2 0.055(13) 0.045(11) 0.026(10) -0.003(10) 0.000(9) -0.025(11) C3 0.034(13) 0.051(14) 0.061(15) -0.005(11) 0.000(11) 0.005(10) C4 0.064(18) 0.103(19) 0.051(16) 0.031(13) 0.026(14) 0.027(14) C5 0.050(17) 0.19(3) 0.050(16) -0.019(18) 0.014(14) 0.039(18) C6 0.072(19) 0.11(2) 0.037(14) -0.010(12) -0.010(13) 0.036(15) C7 0.091(18) 0.028(11) 0.012(10) 0.006(9) -0.006(11) -0.018(12) C8 0.045(13) 0.021(10) 0.032(12) 0.001(8) -0.010(10) -0.004(9) C9 0.043(13) 0.023(10) 0.043(12) -0.001(8) 0.014(10) -0.003(9) C10 0.037(13) 0.052(13) 0.044(12) 0.009(9) 0.003(10) 0.014(9) C11 0.046(9) 0.008(6) 0.059(9) 0.001(6) 0.009(7) 0.008(6) C12 0.046(9) 0.008(6) 0.059(9) 0.001(6) 0.009(7) 0.008(6) C13 0.060(16) 0.024(11) 0.100(18) 0.006(11) 0.032(13) -0.001(10) C14 0.038(14) 0.015(10) 0.118(19) -0.004(10) 0.049(13) 0.002(8) C15 0.058(14) 0.028(10) 0.025(10) -0.011(9) -0.001(10) -0.002(11) C16 0.086(18) 0.027(11) 0.029(11) 0.008(9) 0.021(12) -0.015(11) C18 0.044(15) 0.089(18) 0.059(15) -0.003(12) -0.008(12) 0.030(12) C23 0.050(12) 0.083(12) 0.058(12) -0.013(9) 0.010(10) 0.039(9) C24 0.050(12) 0.083(12) 0.058(12) -0.013(9) 0.010(10) 0.039(9) O2W 0.19(4) 0.07(2) 0.10(3) 0.03(2) 0.11(3) 0.02(3) O3W 0.22(5) 0.11(3) 0.19(4) -0.04(3) -0.14(4) 0.02(3) O4W 0.22(5) 0.11(3) 0.19(4) -0.04(3) -0.14(4) 0.02(3) O5W 0.17(5) 0.04(2) 0.52(10) -0.04(4) -0.05(7) 0.02(2) _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 O14 1.928(10) . ? Zn1 O2 1.945(11) . ? Zn1 O9 1.971(12) . ? Zn1 O7 1.979(11) 3_786 ? Zn2 O11 1.944(12) 1_655 ? Zn2 O5 1.954(11) . ? Zn2 O13 1.964(10) . ? Zn2 O4 1.991(13) 2_756 ? Zn3 O14 2.043(10) . ? Zn3 O14 2.043(10) 3_776 ? Zn3 O13 2.061(11) . ? Zn3 O13 2.061(11) 3_776 ? Zn3 O8 2.234(11) 3_786 ? Zn3 O8 2.234(11) 1_545 ? Zn3 Zn4 3.132(2) . ? Zn3 Zn4 3.132(2) 3_776 ? Zn4 O1 2.026(12) . ? Zn4 O3 2.075(14) 2_756 ? Zn4 O13 2.106(11) . ? Zn4 O6 2.109(12) . ? Zn4 O14 2.117(11) . ? Zn4 O1W 2.193(10) . ? O1 C7 1.25(2) . ? O2 C7 1.284(19) . ? O3 C8 1.26(2) . ? O3 Zn4 2.075(14) 2_756 ? O4 C8 1.23(2) . ? O4 Zn2 1.991(13) 2_756 ? O5 C15 1.278(19) . ? O6 C15 1.29(2) . ? O7 C16 1.26(2) . ? O7 Zn1 1.979(11) 3_786 ? O8 C16 1.28(2) . ? O8 Zn3 2.234(11) 1_565 ? O9 C23 1.25(2) . ? O10 C23 1.22(2) . ? O11 C24 1.34(2) . ? O11 Zn2 1.944(12) 1_455 ? O12 C24 1.25(3) . ? C1 C2 1.40(3) . ? C1 C6 1.42(3) . ? C1 C7 1.44(3) . ? C2 C3 1.34(2) . ? C3 C4 1.42(3) . ? C3 C8 1.52(3) . ? C4 C5 1.33(3) . ? C5 C6 1.39(3) . ? C9 C14 1.37(2) . ? C9 C10 1.41(2) . ? C9 C15 1.50(2) . ? C10 C11 1.41(2) . ? C11 C12 1.37(2) . ? C11 C16 1.49(2) . ? C12 C13 1.34(2) . ? C13 C14 1.45(2) . ? C17 C22 1.31(4) . ? C17 C18 1.46(4) . ? C17 C23 1.73(4) . ? C17' C22' 1.35(5) . ? C17' C23 1.52(4) . ? C17' C22 2.01(5) . ? C18 C19 1.58(4) . ? C19 C20 1.32(4) . ? C19 C24 1.48(3) . ? C19' C20' 1.39(5) . ? C19' C24 1.60(4) . ? C19' C20 1.99(5) . ? C20 C21 1.41(5) . ? C20' C21' 1.53(6) . ? C21 C22 1.45(5) . ? C21' C22' 1.33(6) . ? O1S C1S 1.25(8) . ? N1S C2S 1.60(16) . ? N1S C3S 1.66(8) . ? N1S C1S 1.76(9) . ? O2S C4S 1.25(2) . ? N2S C5S 1.44(2) . ? N2S C4S 1.46(2) . ? N2S C6S 1.48(2) . ? O3S C7S 1.31(2) . ? N3S C8S 1.48(2) . ? N3S C9S 1.50(2) . ? N3S C7S 1.51(3) . ? O4S O2W 0.78(6) . ? O4S C10S 1.25(2) . ? N4S C11S 1.45(2) . ? N4S C10S 1.46(2) . ? N4S C10S 1.46(2) 2 ? C10S O2W 1.42(6) . ? O5W O5W 1.62(10) 2_655 ? 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 O14 Zn1 O2 101.0(5) . . ? O14 Zn1 O9 115.8(5) . . ? O2 Zn1 O9 100.6(5) . . ? O14 Zn1 O7 113.3(5) . 3_786 ? O2 Zn1 O7 117.9(5) . 3_786 ? O9 Zn1 O7 107.8(5) . 3_786 ? O11 Zn2 O5 114.2(5) 1_655 . ? O11 Zn2 O13 119.2(5) 1_655 . ? O5 Zn2 O13 115.3(5) . . ? O11 Zn2 O4 102.6(6) 1_655 2_756 ? O5 Zn2 O4 96.5(5) . 2_756 ? O13 Zn2 O4 104.5(5) . 2_756 ? O14 Zn3 O14 179.998(3) . 3_776 ? O14 Zn3 O13 83.6(4) . . ? O14 Zn3 O13 96.4(4) 3_776 . ? O14 Zn3 O13 96.4(4) . 3_776 ? O14 Zn3 O13 83.6(4) 3_776 3_776 ? O13 Zn3 O13 179.999(2) . 3_776 ? O14 Zn3 O8 90.7(4) . 3_786 ? O14 Zn3 O8 89.3(4) 3_776 3_786 ? O13 Zn3 O8 93.5(4) . 3_786 ? O13 Zn3 O8 86.5(4) 3_776 3_786 ? O14 Zn3 O8 89.3(4) . 1_545 ? O14 Zn3 O8 90.7(4) 3_776 1_545 ? O13 Zn3 O8 86.5(4) . 1_545 ? O13 Zn3 O8 93.5(4) 3_776 1_545 ? O8 Zn3 O8 179.996(2) 3_786 1_545 ? O14 Zn3 Zn4 42.0(3) . . ? O14 Zn3 Zn4 138.0(3) 3_776 . ? O13 Zn3 Zn4 41.8(3) . . ? O13 Zn3 Zn4 138.2(3) 3_776 . ? O8 Zn3 Zn4 96.1(3) 3_786 . ? O8 Zn3 Zn4 83.9(3) 1_545 . ? O14 Zn3 Zn4 138.0(3) . 3_776 ? O14 Zn3 Zn4 42.0(3) 3_776 3_776 ? O13 Zn3 Zn4 138.2(3) . 3_776 ? O13 Zn3 Zn4 41.8(3) 3_776 3_776 ? O8 Zn3 Zn4 83.9(3) 3_786 3_776 ? O8 Zn3 Zn4 96.1(3) 1_545 3_776 ? Zn4 Zn3 Zn4 180.0 . 3_776 ? O1 Zn4 O3 95.2(5) . 2_756 ? O1 Zn4 O13 170.1(5) . . ? O3 Zn4 O13 94.2(5) 2_756 . ? O1 Zn4 O6 85.5(5) . . ? O3 Zn4 O6 89.3(5) 2_756 . ? O13 Zn4 O6 91.6(4) . . ? O1 Zn4 O14 90.0(5) . . ? O3 Zn4 O14 173.9(4) 2_756 . ? O13 Zn4 O14 80.8(4) . . ? O6 Zn4 O14 94.4(5) . . ? O1 Zn4 O1W 91.5(4) . . ? O3 Zn4 O1W 89.6(5) 2_756 . ? O13 Zn4 O1W 91.6(4) . . ? O6 Zn4 O1W 176.7(5) . . ? O14 Zn4 O1W 87.0(4) . . ? O1 Zn4 Zn3 130.3(4) . . ? O3 Zn4 Zn3 134.4(4) 2_756 . ? O13 Zn4 Zn3 40.7(3) . . ? O6 Zn4 Zn3 97.0(3) . . ? O14 Zn4 Zn3 40.3(3) . . ? O1W Zn4 Zn3 85.9(3) . . ? C7 O1 Zn4 131.9(11) . . ? C7 O2 Zn1 132.1(13) . . ? C8 O3 Zn4 128.9(11) . 2_756 ? C8 O4 Zn2 128.3(13) . 2_756 ? C15 O5 Zn2 115.1(11) . . ? C15 O6 Zn4 145.9(12) . . ? C16 O7 Zn1 122.4(11) . 3_786 ? C16 O8 Zn3 143.6(11) . 1_565 ? C23 O9 Zn1 116.7(14) . . ? C24 O11 Zn2 113.2(13) . 1_455 ? Zn2 O13 Zn3 130.2(5) . . ? Zn2 O13 Zn4 104.6(5) . . ? Zn3 O13 Zn4 97.5(5) . . ? Zn1 O14 Zn3 118.5(5) . . ? Zn1 O14 Zn4 108.3(4) . . ? Zn3 O14 Zn4 97.7(5) . . ? C2 C1 C6 114.0(19) . . ? C2 C1 C7 123(2) . . ? C6 C1 C7 123(2) . . ? C3 C2 C1 128(2) . . ? C2 C3 C4 116(2) . . ? C2 C3 C8 124.3(18) . . ? C4 C3 C8 119.4(19) . . ? C5 C4 C3 119(2) . . ? C4 C5 C6 124(2) . . ? C5 C6 C1 119(2) . . ? O1 C7 O2 123.3(18) . . ? O1 C7 C1 120.0(16) . . ? O2 C7 C1 117(2) . . ? O4 C8 O3 126.3(17) . . ? O4 C8 C3 120.7(18) . . ? O3 C8 C3 112.9(16) . . ? C14 C9 C10 120.4(16) . . ? C14 C9 C15 120.3(15) . . ? C10 C9 C15 119.1(16) . . ? C11 C10 C9 118.8(17) . . ? C12 C11 C10 119.7(16) . . ? C12 C11 C16 122.6(15) . . ? C10 C11 C16 117.5(17) . . ? C13 C12 C11 122.5(15) . . ? C12 C13 C14 118.8(17) . . ? C9 C14 C13 119.5(16) . . ? O5 C15 O6 125.0(16) . . ? O5 C15 C9 118.3(16) . . ? O6 C15 C9 116.7(16) . . ? O7 C16 O8 124.1(15) . . ? O7 C16 C11 119.4(16) . . ? O8 C16 C11 116.5(17) . . ? C22 C17 C18 128(3) . . ? C22 C17 C23 121(3) . . ? C18 C17 C23 108(2) . . ? C22' C17' C23 122(3) . . ? C22' C17' C22 73(2) . . ? C23 C17' C22 97(2) . . ? C17 C18 C19 106(2) . . ? C20 C19 C24 127(3) . . ? C20 C19 C18 119(3) . . ? C24 C19 C18 110(2) . . ? C20' C19' C24 114(4) . . ? C20' C19' C20 73(3) . . ? C24 C19' C20 88(2) . . ? C19 C20 C21 128(4) . . ? C19 C20 C19' 29.2(18) . . ? C21 C20 C19' 121(3) . . ? C19' C20' C21' 112(4) . . ? C20 C21 C22 110(4) . . ? C22' C21' C20' 125(5) . . ? C17 C22 C21 123(4) . . ? C17 C22 C17' 29.6(19) . . ? C21 C22 C17' 126(3) . . ? C17' C22' C21' 118(4) . . ? O10 C23 O9 127(2) . . ? O10 C23 C17' 116(2) . . ? O9 C23 C17' 114(2) . . ? O10 C23 C17 117(2) . . ? O9 C23 C17 113(2) . . ? C17' C23 C17 38.4(16) . . ? O12 C24 O11 125.5(19) . . ? O12 C24 C19 114(2) . . ? O11 C24 C19 117(2) . . ? O12 C24 C19' 122(2) . . ? O11 C24 C19' 110(2) . . ? C19 C24 C19' 39.6(17) . . ? C2S N1S C3S 109(7) . . ? C2S N1S C1S 140(8) . . ? C3S N1S C1S 99(5) . . ? O1S C1S N1S 94(6) . . ? C5S N2S C4S 160(5) . . ? C5S N2S C6S 99.5(18) . . ? C4S N2S C6S 100(5) . . ? O2S C4S N2S 95(4) . . ? C8S N3S C9S 112(7) . . ? C8S N3S C7S 88(6) . . ? C9S N3S C7S 144(8) . . ? O3S C7S N3S 154(8) . . ? O2W O4S C10S 86(6) . . ? C11S N4S C10S 97(5) . . ? C11S N4S C10S 97(5) . 2 ? C10S N4S C10S 166(9) . 2 ? O4S C10S O2W 33(3) . . ? O4S C10S N4S 169(9) . . ? O2W C10S N4S 152(8) . . ? O4S O2W C10S 61(4) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 1.318 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.203