data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Linhong Weng' _publ_contact_author_email LHWENG@FUDAN.EDU.CN _publ_section_title ; Unprecedented trinodal four-connected FRL MOF based on mixed ligands ; loop_ _publ_author_name 'Linhong Weng' 'Zhen-Xia Chen' 'Peng Li' 'Xiaofeng Liu' 'Jiaying Lou' ; Yaming Zhou ; # Attachment 'wlh-frl-r.cif' data_f70908c _database_code_depnum_ccdc_archive 'CCDC 721200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 N4 O20 Zn4' _chemical_formula_weight 1024.03 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.623(4) _cell_length_b 9.466(4) _cell_length_c 11.371(5) _cell_angle_alpha 80.005(6) _cell_angle_beta 79.760(6) _cell_angle_gamma 69.169(5) _cell_volume 847.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1017 _cell_measurement_theta_min 2.319 _cell_measurement_theta_max 27.191 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.006 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 514 _exptl_absorpt_coefficient_mu 2.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6707 _exptl_absorpt_correction_T_max 0.8688 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4240 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2939 _reflns_number_gt 2588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.4908P] 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 2939 _refine_ls_number_parameters 281 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _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 0.89140(5) 0.34932(4) 0.65509(3) 0.02410(14) Uani 1 1 d . . . Zn2 Zn 0.56275(5) 0.22564(4) 1.00250(3) 0.02835(15) Uani 1 1 d . . . O1 O 0.7539(3) 0.2485(3) 0.7756(2) 0.0338(6) Uani 1 1 d . . . O2 O 0.5492(4) 0.1596(3) 0.8459(2) 0.0359(6) Uani 1 1 d . . . O3 O 0.2570(3) 0.4911(3) 0.4478(2) 0.0345(6) Uani 1 1 d . . . O4 O 0.3348(4) 0.3610(3) 0.2918(2) 0.0551(9) Uani 1 1 d . . . O5 O 0.9537(3) -0.2042(3) 0.4546(2) 0.0306(6) Uani 1 1 d . . . O6 O 0.8571(3) -0.0835(3) 0.2836(2) 0.0396(7) Uani 1 1 d . . . O7 O 1.2866(3) 0.7085(3) 0.9204(2) 0.0356(6) Uani 1 1 d . . . N2 N 1.4551(4) 0.4640(3) 0.9752(2) 0.0258(6) Uani 1 1 d . . . O8 O 0.7187(4) 0.0005(3) 1.0490(3) 0.0443(7) Uani 1 1 d D . . H8B H 0.820(2) -0.008(6) 1.013(3) 0.053 Uiso 1 1 d D . . H8A H 0.739(5) -0.009(6) 1.1235(13) 0.053 Uiso 1 1 d D . . O9 O 0.3877(4) 0.1777(4) 1.1310(2) 0.0403(7) Uani 1 1 d D . . H9A H 0.367(6) 0.227(4) 1.194(3) 0.048 Uiso 1 1 d D . . N1 N 1.0164(3) 0.4259(3) 0.7497(3) 0.0250(6) Uani 1 1 d . . . C1 C 0.6319(4) 0.1690(4) 0.6357(3) 0.0236(7) Uani 1 1 d . . . C2 C 0.5009(4) 0.2747(4) 0.5778(3) 0.0268(7) Uani 1 1 d . . . H2 H 0.4244 0.3547 0.6170 0.032 Uiso 1 1 calc R . . C3 C 0.4848(4) 0.2604(4) 0.4615(3) 0.0254(7) Uani 1 1 d . . . C4 C 0.6001(4) 0.1396(4) 0.4040(3) 0.0247(7) Uani 1 1 d . . . H4 H 0.5900 0.1304 0.3258 0.030 Uiso 1 1 calc R . . C5 C 0.7303(4) 0.0323(4) 0.4619(3) 0.0220(7) Uani 1 1 d . . . C6 C 0.7462(4) 0.0475(4) 0.5789(3) 0.0245(7) Uani 1 1 d . . . H6 H 0.8326 -0.0231 0.6185 0.029 Uiso 1 1 calc R . . C7 C 0.6489(4) 0.1933(4) 0.7597(3) 0.0235(7) Uani 1 1 d . . . C8 C 0.3490(4) 0.3774(4) 0.3945(3) 0.0301(8) Uani 1 1 d . . . C9 C 0.8536(4) -0.0932(4) 0.3946(3) 0.0261(7) Uani 1 1 d . . . C10 C 1.0650(5) 0.5458(4) 0.7031(3) 0.0297(8) Uani 1 1 d . . . H10 H 1.0280 0.6011 0.6315 0.036 Uiso 1 1 calc R . . C11 C 1.1681(5) 0.5899(4) 0.7579(3) 0.0304(8) Uani 1 1 d . . . H11 H 1.2008 0.6730 0.7230 0.036 Uiso 1 1 calc R . . C12 C 1.2223(4) 0.5094(4) 0.8653(3) 0.0253(7) Uani 1 1 d . . . C13 C 1.1677(4) 0.3884(4) 0.9159(3) 0.0289(8) Uani 1 1 d . . . H13 H 1.1994 0.3337 0.9890 0.035 Uiso 1 1 calc R . . C14 C 1.0649(4) 0.3508(4) 0.8552(3) 0.0290(8) Uani 1 1 d . . . H14 H 1.0279 0.2698 0.8891 0.035 Uiso 1 1 calc R . . C15 C 1.3286(4) 0.5629(4) 0.9258(3) 0.0269(7) Uani 1 1 d . . . O10 O -0.0332(4) 0.9087(4) 0.8737(3) 0.0644(10) Uani 1 1 d D . . H10A H 0.057(4) 0.852(5) 0.907(5) 0.077 Uiso 1 1 d D . . H10B H 0.002(6) 0.985(4) 0.841(5) 0.077 Uiso 1 1 d D . . H5B H 0.389(7) 0.084(7) 1.152(5) 0.078(19) 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 0.0262(2) 0.0199(2) 0.0248(2) -0.00802(16) -0.01033(16) -0.00018(16) Zn2 0.0397(3) 0.0210(2) 0.0274(2) -0.00610(17) -0.01066(18) -0.00922(19) O1 0.0368(14) 0.0445(16) 0.0247(12) -0.0091(11) -0.0066(10) -0.0156(13) O2 0.0496(16) 0.0397(15) 0.0261(13) -0.0090(11) -0.0056(11) -0.0215(13) O3 0.0377(14) 0.0258(13) 0.0295(13) -0.0122(10) -0.0134(11) 0.0105(11) O4 0.062(2) 0.0514(19) 0.0320(15) -0.0214(13) -0.0267(14) 0.0230(15) O5 0.0328(13) 0.0197(12) 0.0317(13) -0.0067(10) -0.0119(10) 0.0058(10) O6 0.0498(17) 0.0316(15) 0.0258(14) -0.0112(11) -0.0103(12) 0.0066(12) O7 0.0438(15) 0.0184(12) 0.0480(16) -0.0077(11) -0.0224(12) -0.0050(11) N2 0.0330(16) 0.0195(14) 0.0287(15) -0.0065(12) -0.0122(12) -0.0079(13) O8 0.0536(18) 0.0261(14) 0.0495(17) -0.0034(13) -0.0174(14) -0.0041(14) O9 0.0583(18) 0.0364(16) 0.0293(14) -0.0053(12) -0.0056(13) -0.0188(14) N1 0.0240(14) 0.0228(15) 0.0278(14) -0.0082(12) -0.0099(11) -0.0017(12) C1 0.0265(17) 0.0211(17) 0.0219(16) -0.0050(13) -0.0067(13) -0.0035(14) C2 0.0297(18) 0.0213(17) 0.0253(17) -0.0120(14) -0.0051(14) 0.0013(14) C3 0.0260(17) 0.0218(17) 0.0243(17) -0.0074(13) -0.0066(13) 0.0006(14) C4 0.0283(17) 0.0206(17) 0.0223(16) -0.0075(13) -0.0070(13) -0.0004(14) C5 0.0255(17) 0.0159(16) 0.0228(16) -0.0062(13) -0.0062(13) -0.0015(13) C6 0.0260(17) 0.0187(16) 0.0265(17) -0.0042(13) -0.0104(13) -0.0007(13) C7 0.0280(18) 0.0155(15) 0.0240(17) -0.0056(13) -0.0070(14) -0.0005(13) C8 0.0303(19) 0.0244(18) 0.0284(18) -0.0061(14) -0.0093(14) 0.0034(15) C9 0.0281(18) 0.0200(17) 0.0297(18) -0.0092(14) -0.0048(14) -0.0040(14) C10 0.037(2) 0.0286(19) 0.0231(17) -0.0013(14) -0.0107(14) -0.0088(16) C11 0.034(2) 0.0241(18) 0.0331(19) -0.0001(15) -0.0073(15) -0.0096(15) C12 0.0269(17) 0.0213(17) 0.0284(17) -0.0109(14) -0.0077(14) -0.0033(14) C13 0.036(2) 0.0243(18) 0.0278(17) -0.0046(14) -0.0140(15) -0.0068(15) C14 0.0345(19) 0.0213(17) 0.0322(18) -0.0027(14) -0.0118(15) -0.0071(15) C15 0.0330(19) 0.0224(18) 0.0273(17) -0.0066(14) -0.0085(14) -0.0077(15) O10 0.057(2) 0.048(2) 0.069(2) 0.0001(17) -0.0042(17) 0.0004(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 O3 1.958(2) 2_666 ? Zn1 O5 1.981(2) 2_756 ? Zn1 O1 1.992(3) . ? Zn1 N1 2.021(3) . ? Zn2 O7 2.004(3) 2_767 ? Zn2 O2 2.021(3) . ? Zn2 O9 2.023(3) . ? Zn2 N2 2.102(3) 1_455 ? Zn2 O8 2.110(3) . ? O1 C7 1.246(4) . ? O2 C7 1.261(4) . ? O3 C8 1.266(4) . ? O3 Zn1 1.958(2) 2_666 ? O4 C8 1.237(4) . ? O5 C9 1.277(4) . ? O5 Zn1 1.981(2) 2_756 ? O6 C9 1.246(4) . ? O7 C15 1.287(4) . ? O7 Zn2 2.004(3) 2_767 ? N2 C15 1.300(4) . ? N2 N2 1.430(5) 2_867 ? N2 Zn2 2.102(3) 1_655 ? O8 H8B 0.877(10) . ? O8 H8A 0.878(10) . ? O9 H9A 0.881(10) . ? O9 H5B 0.88(6) . ? N1 C14 1.338(4) . ? N1 C10 1.339(5) . ? C1 C6 1.391(5) . ? C1 C2 1.394(5) . ? C1 C7 1.507(5) . ? C2 C3 1.388(5) . ? C2 H2 0.9300 . ? C3 C4 1.395(5) . ? C3 C8 1.510(5) . ? C4 C5 1.395(4) . ? C4 H4 0.9300 . ? C5 C6 1.399(5) . ? C5 C9 1.501(5) . ? C6 H6 0.9300 . ? C10 C11 1.380(5) . ? C10 H10 0.9300 . ? C11 C12 1.385(5) . ? C11 H11 0.9300 . ? C12 C13 1.387(5) . ? C12 C15 1.499(5) . ? C13 C14 1.385(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O10 H10A 0.881(10) . ? O10 H10B 0.881(10) . ? 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 O3 Zn1 O5 105.34(10) 2_666 2_756 ? O3 Zn1 O1 108.55(12) 2_666 . ? O5 Zn1 O1 110.59(11) 2_756 . ? O3 Zn1 N1 114.29(12) 2_666 . ? O5 Zn1 N1 111.64(11) 2_756 . ? O1 Zn1 N1 106.44(11) . . ? O7 Zn2 O2 140.71(11) 2_767 . ? O7 Zn2 O9 108.94(12) 2_767 . ? O2 Zn2 O9 109.38(11) . . ? O7 Zn2 N2 78.24(10) 2_767 1_455 ? O2 Zn2 N2 103.62(11) . 1_455 ? O9 Zn2 N2 99.45(12) . 1_455 ? O7 Zn2 O8 86.46(11) 2_767 . ? O2 Zn2 O8 87.48(12) . . ? O9 Zn2 O8 86.49(13) . . ? N2 Zn2 O8 164.66(11) 1_455 . ? C7 O1 Zn1 129.4(2) . . ? C7 O2 Zn2 113.1(2) . . ? C8 O3 Zn1 113.4(2) . 2_666 ? C9 O5 Zn1 109.9(2) . 2_756 ? C15 O7 Zn2 113.4(2) . 2_767 ? C15 N2 N2 111.8(3) . 2_867 ? C15 N2 Zn2 137.0(2) . 1_655 ? N2 N2 Zn2 111.2(3) 2_867 1_655 ? Zn2 O8 H8B 108(3) . . ? Zn2 O8 H8A 109(3) . . ? H8B O8 H8A 97.8(14) . . ? Zn2 O9 H9A 113(3) . . ? Zn2 O9 H5B 121(4) . . ? H9A O9 H5B 112(5) . . ? C14 N1 C10 118.4(3) . . ? C14 N1 Zn1 120.9(2) . . ? C10 N1 Zn1 120.5(2) . . ? C6 C1 C2 120.8(3) . . ? C6 C1 C7 121.2(3) . . ? C2 C1 C7 118.0(3) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 C8 121.0(3) . . ? C4 C3 C8 119.5(3) . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.3(3) . . ? C4 C5 C9 118.8(3) . . ? C6 C5 C9 121.8(3) . . ? C1 C6 C5 119.6(3) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? O1 C7 O2 121.5(3) . . ? O1 C7 C1 121.3(3) . . ? O2 C7 C1 117.2(3) . . ? O4 C8 O3 123.5(3) . . ? O4 C8 C3 120.0(3) . . ? O3 C8 C3 116.5(3) . . ? O6 C9 O5 122.9(3) . . ? O6 C9 C5 119.3(3) . . ? O5 C9 C5 117.8(3) . . ? N1 C10 C11 122.2(3) . . ? N1 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C12 119.4(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 118.6(3) . . ? C11 C12 C15 118.5(3) . . ? C13 C12 C15 122.8(3) . . ? C14 C13 C12 118.6(3) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? N1 C14 C13 122.8(3) . . ? N1 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? O7 C15 N2 125.4(3) . . ? O7 C15 C12 114.9(3) . . ? N2 C15 C12 119.7(3) . . ? H10A O10 H10B 97.0(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O4 0.881(10) 1.745(15) 2.608(4) 166(4) 1_556 O8 H8B O10 0.877(10) 2.90(4) 3.411(5) 119(3) 2_667 O8 H8A O6 0.878(10) 2.133(18) 2.982(4) 162(4) 1_556 O10 H10A O7 0.881(10) 1.98(2) 2.816(4) 159(6) 1_455 O10 H10B O6 0.881(10) 2.02(3) 2.834(5) 153(6) 2_666 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.908 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.101