#Supplementary Material (ESI) for Chemical Communications #This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Li Xu' _publ_contact_author_email XLI@FJIRSM.AC.CN _publ_section_title ; Unprecedented Helix-based Microporous Metal-Organic Frameworks Constructed from Single Ligand ; loop_ _publ_author_name 'Li Xu.' 'Rui-Li Sang.' # Attachment '696180.cif' data_cdpra2bim _database_code_depnum_ccdc_archive 'CCDC 696180' _audit_creation_method SHELXL-97 _chemical_name_systematic ; aqua(1,1'-di(propionic acid)-2,2;-biimidazole)cadium(II) dihydrate ; _chemical_name_common ;aqua(1,1'-di(propionic acid)-2,2;-biimidazole)cadium(ii) dihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Cd N4 O7' _chemical_formula_weight 442.71 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 27.1286(11) _cell_length_b 27.1286(11) _cell_length_c 12.0736(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7695.2(6) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6864 _cell_measurement_theta_min 2.4188 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.6500 _exptl_crystal_size_mid 0.1800 _exptl_crystal_size_min 0.1700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3995 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7902 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 ? _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18224 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0095 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1960 _reflns_number_gt 1933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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^)+(0.0383P)^2^+135.7860P] 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_number_reflns 1960 _refine_ls_number_parameters 131 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.306 _refine_ls_restrained_S_all 1.294 _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 Cd1 Cd 1.0000 0.25698(2) 0.7500 0.0338(2) Uani 1 2 d S . . O1 O 0.9768(4) 0.1719(4) 0.6271(9) 0.121(3) Uani 1 1 d . . . O2 O 0.9767(3) 0.2416(3) 0.5559(5) 0.0782(19) Uani 1 1 d . . . O3A O 0.9920(9) 0.3372(10) 0.7166(18) 0.038(4) Uani 0.320(8) 1 d PU . 1 O3B O 1.0000 0.341(2) 0.7500 0.040(8) Uani 0.361(16) 2 d SPU . 2 H3W H 1.0138 0.3696 0.6949 0.048 Uiso 1 1 d . . . N1 N 0.7640(2) 0.1063(2) 0.5604(4) 0.0341(10) Uani 1 1 d . . . N2 N 0.8429(2) 0.1119(2) 0.4954(4) 0.0374(11) Uani 1 1 d . . . C1 C 0.7970(2) 0.1177(2) 0.4715(4) 0.0301(11) Uani 1 1 d . . . C2 C 0.7899(2) 0.0931(3) 0.6426(5) 0.0385(13) Uani 1 1 d . . . H2A H 0.7763 0.0832 0.7146 0.046 Uiso 1 1 calc R . . C3 C 0.8378(3) 0.0963(3) 0.6043(5) 0.0420(13) Uani 1 1 d . . . H3A H 0.8629 0.0893 0.6444 0.050 Uiso 1 1 calc R . . C4A C 0.9383(5) 0.1770(5) 0.4254(9) 0.049(3) Uani 0.639(16) 1 d PU . 1 H4A1 H 0.9283 0.2052 0.4030 0.059 Uiso 0.639(16) 1 calc PR . 1 H4A2 H 0.9664 0.1786 0.3734 0.059 Uiso 0.639(16) 1 calc PR . 1 C4B C 0.9438(7) 0.1408(7) 0.4743(13) 0.035(4) Uani 0.361(16) 1 d PU . 2 H4B1 H 0.9720 0.1481 0.4176 0.041 Uiso 0.361(16) 1 calc PR . 2 H4B2 H 0.9402 0.1095 0.5191 0.041 Uiso 0.361(16) 1 calc PR . 2 C5 C 0.9664(3) 0.1929(4) 0.5472(7) 0.0549(18) Uani 1 1 d . . . C6 C 0.8893(3) 0.1225(4) 0.4197(5) 0.0554(18) Uani 1 1 d U . . H6A H 0.9006 0.0943 0.4340 0.066 Uiso 1 1 calc R . 1 H6B H 0.8747 0.1166 0.3446 0.066 Uiso 1 1 calc R . 1 O1W O 0.0000 0.1085(10) 0.2500 0.35(2) Uani 1 2 d S . . H1W H 0.0299 0.0986 0.2500 0.421 Uiso 1 1 d . . . O2W O 1.0000 0.0905(7) 0.7500 0.51(3) Uani 1 2 d SD . . H2W H 0.9707 0.0922 0.7399 0.607 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 Cd1 0.0353(3) 0.0369(3) 0.0285(3) 0.00120(11) 0.0024(2) 0.01766(17) O1 0.093(6) 0.102(6) 0.178(9) 0.062(6) 0.032(6) 0.057(5) O2 0.093(5) 0.090(5) 0.058(3) 0.024(3) 0.040(3) 0.051(4) O3A 0.036(7) 0.032(7) 0.041(8) 0.002(7) 0.004(6) 0.014(5) O3B 0.038(10) 0.045(10) 0.035(12) 0.000(4) 0.000(8) 0.019(5) N1 0.032(2) 0.037(2) 0.027(2) 0.0017(18) 0.0025(17) 0.013(2) N2 0.028(2) 0.045(3) 0.029(2) -0.0074(19) -0.0022(18) 0.011(2) C1 0.024(2) 0.027(2) 0.027(2) -0.005(2) 0.0005(19) 0.004(2) C2 0.036(3) 0.044(3) 0.027(3) 0.001(2) -0.003(2) 0.014(3) C3 0.037(3) 0.045(3) 0.034(3) -0.004(2) -0.008(2) 0.014(3) C4A 0.045(5) 0.048(6) 0.044(5) -0.006(4) 0.003(4) 0.014(4) C4B 0.036(7) 0.042(9) 0.031(7) -0.011(6) 0.000(5) 0.023(7) C5 0.026(3) 0.057(4) 0.067(5) -0.018(4) 0.000(3) 0.010(3) C6 0.033(3) 0.079(5) 0.043(3) -0.015(3) 0.004(3) 0.019(3) O1W 0.43(5) 0.26(2) 0.42(5) 0.09(2) 0.19(4) 0.22(3) O2W 0.39(5) 0.168(14) 1.04(10) 0.14(3) 0.27(6) 0.19(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 Cd1 O3B 2.27(5) . ? Cd1 O3A 2.33(3) . ? Cd1 O3A 2.33(3) 5_766 ? Cd1 N1 2.358(5) 35_545 ? Cd1 N1 2.358(5) 25_656 ? Cd1 O2 2.409(7) . ? Cd1 O2 2.409(7) 5_766 ? Cd1 O1 2.543(11) . ? Cd1 O1 2.543(11) 5_766 ? O1 C5 1.222(12) . ? O2 C5 1.210(10) . ? O3A O3A 0.89(5) 5_766 ? O3A H3W 0.8192 . ? O3B H3W 0.9482 . ? N1 C1 1.332(7) . ? N1 C2 1.364(7) . ? N1 Cd1 2.358(5) 25_656 ? N2 C1 1.361(7) . ? N2 C3 1.367(7) . ? N2 C6 1.463(7) . ? C1 C1 1.451(10) 10_545 ? C2 C3 1.340(9) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4A C6 1.411(12) . ? C4A C5 1.613(13) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C4B C6 1.462(16) . ? C4B C5 1.511(16) . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O1W H1W 0.9743 . ? O2W H2W 0.8294 . ? 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 O3B Cd1 O3A 11.0(6) . . ? O3B Cd1 O3A 11.0(6) . 5_766 ? O3A Cd1 O3A 22.1(11) . 5_766 ? O3B Cd1 N1 77.61(12) . 35_545 ? O3A Cd1 N1 81.2(5) . 35_545 ? O3A Cd1 N1 74.4(5) 5_766 35_545 ? O3B Cd1 N1 77.60(12) . 25_656 ? O3A Cd1 N1 74.4(5) . 25_656 ? O3A Cd1 N1 81.2(5) 5_766 25_656 ? N1 Cd1 N1 155.2(2) 35_545 25_656 ? O3B Cd1 O2 92.41(16) . . ? O3A Cd1 O2 81.6(6) . . ? O3A Cd1 O2 103.2(6) 5_766 . ? N1 Cd1 O2 96.6(2) 35_545 . ? N1 Cd1 O2 84.42(19) 25_656 . ? O3B Cd1 O2 92.41(16) . 5_766 ? O3A Cd1 O2 103.2(6) . 5_766 ? O3A Cd1 O2 81.6(6) 5_766 5_766 ? N1 Cd1 O2 84.42(19) 35_545 5_766 ? N1 Cd1 O2 96.62(19) 25_656 5_766 ? O2 Cd1 O2 175.2(3) . 5_766 ? O3B Cd1 O1 141.6(2) . . ? O3A Cd1 O1 130.6(6) . . ? O3A Cd1 O1 152.6(6) 5_766 . ? N1 Cd1 O1 107.9(2) 35_545 . ? N1 Cd1 O1 91.7(2) 25_656 . ? O2 Cd1 O1 49.5(3) . . ? O2 Cd1 O1 125.7(3) 5_766 . ? O3B Cd1 O1 141.6(2) . 5_766 ? O3A Cd1 O1 152.6(6) . 5_766 ? O3A Cd1 O1 130.6(6) 5_766 5_766 ? N1 Cd1 O1 91.7(2) 35_545 5_766 ? N1 Cd1 O1 107.9(2) 25_656 5_766 ? O2 Cd1 O1 125.7(3) . 5_766 ? O2 Cd1 O1 49.5(3) 5_766 5_766 ? O1 Cd1 O1 76.8(4) . 5_766 ? C5 O1 Cd1 92.8(6) . . ? C5 O2 Cd1 99.8(5) . . ? O3A O3A Cd1 79.0(6) 5_766 . ? O3A O3A H3W 91.4 5_766 . ? Cd1 O3A H3W 134.7 . . ? Cd1 O3B H3W 128.7 . . ? C1 N1 C2 105.7(5) . . ? C1 N1 Cd1 133.0(4) . 25_656 ? C2 N1 Cd1 117.3(4) . 25_656 ? C1 N2 C3 106.4(5) . . ? C1 N2 C6 126.3(5) . . ? C3 N2 C6 127.3(6) . . ? N1 C1 N2 110.6(5) . . ? N1 C1 C1 125.3(6) . 10_545 ? N2 C1 C1 124.0(5) . 10_545 ? C3 C2 N1 110.0(5) . . ? C3 C2 H2A 125.0 . . ? N1 C2 H2A 125.0 . . ? C2 C3 N2 107.3(5) . . ? C2 C3 H3A 126.3 . . ? N2 C3 H3A 126.3 . . ? C6 C4A C5 113.4(8) . . ? C6 C4A H4A1 108.9 . . ? C5 C4A H4A1 108.9 . . ? C6 C4A H4A2 108.9 . . ? C5 C4A H4A2 108.9 . . ? H4A1 C4A H4A2 107.7 . . ? C6 C4B C5 116.7(11) . . ? C6 C4B H4B1 108.1 . . ? C5 C4B H4B1 108.1 . . ? C6 C4B H4B2 108.1 . . ? C5 C4B H4B2 108.1 . . ? H4B1 C4B H4B2 107.3 . . ? O2 C5 O1 117.3(9) . . ? O2 C5 C4B 146.7(11) . . ? O1 C5 C4B 96.0(10) . . ? O2 C5 C4A 101.0(8) . . ? O1 C5 C4A 141.5(9) . . ? C4B C5 C4A 45.7(8) . . ? C4A C6 C4B 50.1(8) . . ? C4A C6 N2 116.3(7) . . ? C4B C6 N2 114.2(7) . . ? C4A C6 H6A 108.2 . . ? C4B C6 H6A 61.5 . . ? N2 C6 H6A 108.2 . . ? C4A C6 H6B 108.2 . . ? C4B C6 H6B 137.5 . . ? N2 C6 H6B 108.2 . . ? H6A C6 H6B 107.4 . . ? 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 O3B Cd1 O1 C5 4.9(7) . . . . ? O3A Cd1 O1 C5 6.1(9) . . . . ? O3A Cd1 O1 C5 2.8(13) 5_766 . . . ? N1 Cd1 O1 C5 -87.7(5) 35_545 . . . ? N1 Cd1 O1 C5 76.9(5) 25_656 . . . ? O2 Cd1 O1 C5 -4.3(5) . . . . ? O2 Cd1 O1 C5 176.2(5) 5_766 . . . ? O1 Cd1 O1 C5 -175.1(7) 5_766 . . . ? O3B Cd1 O2 C5 -169.8(5) . . . . ? O3A Cd1 O2 C5 -167.5(7) . . . . ? O3A Cd1 O2 C5 -172.2(7) 5_766 . . . ? N1 Cd1 O2 C5 112.4(5) 35_545 . . . ? N1 Cd1 O2 C5 -92.6(5) 25_656 . . . ? O2 Cd1 O2 C5 10.2(5) 5_766 . . . ? O1 Cd1 O2 C5 4.4(5) . . . . ? O1 Cd1 O2 C5 15.5(6) 5_766 . . . ? O3B Cd1 O3A O3A 0.00(2) . . . 5_766 ? N1 Cd1 O3A O3A -70(2) 35_545 . . 5_766 ? N1 Cd1 O3A O3A 106(2) 25_656 . . 5_766 ? O2 Cd1 O3A O3A -168(3) . . . 5_766 ? O2 Cd1 O3A O3A 12(3) 5_766 . . 5_766 ? O1 Cd1 O3A O3A -176(2) . . . 5_766 ? O1 Cd1 O3A O3A 7(3) 5_766 . . 5_766 ? C2 N1 C1 N2 -0.1(6) . . . . ? Cd1 N1 C1 N2 -156.3(4) 25_656 . . . ? C2 N1 C1 C1 175.8(5) . . . 10_545 ? Cd1 N1 C1 C1 19.6(8) 25_656 . . 10_545 ? C3 N2 C1 N1 0.0(6) . . . . ? C6 N2 C1 N1 -178.0(6) . . . . ? C3 N2 C1 C1 -175.9(4) . . . 10_545 ? C6 N2 C1 C1 6.1(8) . . . 10_545 ? C1 N1 C2 C3 0.1(7) . . . . ? Cd1 N1 C2 C3 160.7(4) 25_656 . . . ? N1 C2 C3 N2 -0.1(7) . . . . ? C1 N2 C3 C2 0.0(7) . . . . ? C6 N2 C3 C2 178.1(6) . . . . ? Cd1 O2 C5 O1 -7.9(8) . . . . ? Cd1 O2 C5 C4B 171.4(14) . . . . ? Cd1 O2 C5 C4A 168.8(5) . . . . ? Cd1 O1 C5 O2 7.4(8) . . . . ? Cd1 O1 C5 C4B -172.2(7) . . . . ? Cd1 O1 C5 C4A -167.5(10) . . . . ? C6 C4B C5 O2 -49(2) . . . . ? C6 C4B C5 O1 130.8(12) . . . . ? C6 C4B C5 C4A -45.1(10) . . . . ? C6 C4A C5 O2 -136.4(9) . . . . ? C6 C4A C5 O1 39.0(16) . . . . ? C6 C4A C5 C4B 45.6(10) . . . . ? C5 C4A C6 C4B -43.5(10) . . . . ? C5 C4A C6 N2 57.0(11) . . . . ? C5 C4B C6 C4A 49.1(11) . . . . ? C5 C4B C6 N2 -55.8(15) . . . . ? C1 N2 C6 C4A 95.3(9) . . . . ? C3 N2 C6 C4A -82.4(10) . . . . ? C1 N2 C6 C4B 151.0(9) . . . . ? C3 N2 C6 C4B -26.6(12) . . . . ? 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 O1W H1W O2W 0.97 1.76 2.733(19) 172.3 20_566 O2W H2W O1 0.83 2.49 2.978(18) 118.7 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.843 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.124 # Attachment '696181.cif' data_PBpra2bim _database_code_depnum_ccdc_archive 'CCDC 696181' _audit_creation_method SHELXL-97 _chemical_name_systematic ; aqua(1,1'-di(propionic acid)-2,2;-biimidazole)lead(II) hydrate ; _chemical_name_common "aqua(1,1'-di(propionic acid)-2,2;-biimidazole)lead(ii) hydrate" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 N4 O6 Pb' _chemical_formula_weight 519.48 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 27.4599(8) _cell_length_b 27.4599(8) _cell_length_c 12.5722(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8209.9(5) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6942 _cell_measurement_theta_min 2.5693 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.5400 _exptl_crystal_size_mid 0.0400 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4428 _exptl_absorpt_coefficient_mu 9.279 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8098 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ???? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20059 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2005 _reflns_number_gt 1882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0244P)^2^+50.7988P] 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_number_reflns 2005 _refine_ls_number_parameters 126 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 Pb1 Pb 0.3333 0.912124(6) 0.4167 0.03070(4) Uani 1 2 d S . . O1 O 0.31277(10) 0.91694(9) 0.21833(17) 0.0430(6) Uani 1 1 d . . . O2 O 0.31147(10) 0.83694(10) 0.2407(2) 0.0553(7) Uani 1 1 d . . . O3 O 0.3333 0.99848(12) 0.4167 0.0520(9) Uani 1 2 d S . . H3A H 0.3584 1.0212 0.3752 0.062 Uiso 0.50 1 calc PR . . N1 N 0.22851(10) 0.88737(11) 0.44452(19) 0.0352(6) Uani 1 1 d . . . N2 N 0.15397(10) 0.88662(10) 0.51278(19) 0.0333(6) Uani 1 1 d . . . C1 C 0.19736(11) 0.87815(10) 0.5312(2) 0.0278(6) Uani 1 1 d . . . C2 C 0.20333(13) 0.90297(14) 0.3684(3) 0.0408(8) Uani 1 1 d . . . H2 H 0.2164 0.9128 0.2973 0.072(14) Uiso 1 1 calc R . . C3 C 0.15782(13) 0.90251(13) 0.4078(2) 0.0393(8) Uani 1 1 d . . . H3 H 0.1331 0.9114 0.3707 0.042(9) Uiso 1 1 calc R . . C4 C 0.22462(12) 0.78832(13) 0.0800(2) 0.0388(8) Uani 1 1 d . . . H4A H 0.2090 0.7776 0.0073 0.045(10) Uiso 1 1 calc R . . H4B H 0.2394 0.7634 0.1011 0.044(9) Uiso 1 1 calc R . . C5 C 0.27240(12) 0.84887(14) 0.0792(2) 0.0389(8) Uani 1 1 d . . . H5A H 0.2575 0.8735 0.0569 0.036(9) Uiso 1 1 calc R . . H5B H 0.3007 0.8527 0.0260 0.053(11) Uiso 1 1 calc R . . C6 C 0.30125(12) 0.86886(13) 0.1871(2) 0.0357(8) Uani 1 1 d . . . O4A O 0.5604(15) 0.2278(10) 0.6084(12) 0.199(16) Uani 0.220(10) 1 d PU A 1 O4B O 0.5665(14) 0.1967(7) 0.5750(16) 0.246(19) Uani 0.280(10) 1 d PU A 2 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 Pb1 0.03247(8) 0.03416(6) 0.02491(7) 0.00098(3) 0.00196(6) 0.01623(4) O1 0.0543(11) 0.0387(10) 0.0320(11) 0.0015(8) -0.0030(10) 0.0204(9) O2 0.0639(12) 0.0474(11) 0.0585(14) -0.0018(10) -0.0248(11) 0.0307(9) O3 0.0514(19) 0.0372(12) 0.072(2) 0.0156(8) 0.0312(17) 0.0257(10) N1 0.0356(11) 0.0361(11) 0.0278(11) 0.0003(9) -0.0005(10) 0.0134(9) N2 0.0312(10) 0.0326(10) 0.0307(12) -0.0013(9) -0.0029(9) 0.0120(8) C1 0.0257(11) 0.0188(10) 0.0295(13) 0.0030(10) 0.0006(10) 0.0042(9) C2 0.0391(14) 0.0455(15) 0.0295(15) 0.0046(12) -0.0021(12) 0.0150(12) C3 0.0385(13) 0.0403(14) 0.0335(15) 0.0023(12) -0.0108(12) 0.0154(11) C4 0.0337(12) 0.0432(14) 0.0376(15) -0.0091(12) -0.0032(12) 0.0178(11) C5 0.0308(12) 0.0474(15) 0.0314(14) -0.0008(12) -0.0016(12) 0.0142(11) C6 0.0280(12) 0.0371(14) 0.0326(14) 0.0000(12) -0.0014(11) 0.0093(10) O4A 0.32(3) 0.087(14) 0.046(12) -0.002(9) -0.084(14) -0.001(18) O4B 0.45(4) 0.053(9) 0.057(8) 0.018(7) -0.048(19) -0.014(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 Pb1 O3 2.371(3) . ? Pb1 O1 2.575(2) . ? Pb1 O1 2.575(2) 11 ? Pb1 N1 2.629(3) 11 ? Pb1 N1 2.629(3) . ? O1 C6 1.257(4) . ? O2 C6 1.243(4) . ? O3 H3A 0.8400 . ? N1 C1 1.330(4) . ? N1 C2 1.369(5) . ? N2 C1 1.343(4) . ? N2 C3 1.378(4) . ? N2 C4 1.475(4) 31_565 ? C1 C1 1.472(6) 18_455 ? C2 C3 1.338(5) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 N2 1.475(4) 31_565 ? C4 C5 1.518(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.528(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O4A O4A 0.63(3) 18_545 ? O4B O4B 1.75(8) 18_545 ? 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 Pb1 O1 80.74(6) . . ? O3 Pb1 O1 80.73(6) . 11 ? O1 Pb1 O1 161.47(12) . 11 ? O3 Pb1 N1 73.21(6) . 11 ? O1 Pb1 N1 90.26(7) . 11 ? O1 Pb1 N1 84.40(8) 11 11 ? O3 Pb1 N1 73.21(6) . . ? O1 Pb1 N1 84.40(8) . . ? O1 Pb1 N1 90.26(7) 11 . ? N1 Pb1 N1 146.42(12) 11 . ? C6 O1 Pb1 101.2(2) . . ? Pb1 O3 H3A 109.5 . . ? C1 N1 C2 104.8(3) . . ? C1 N1 Pb1 132.5(2) . . ? C2 N1 Pb1 119.01(19) . . ? C1 N2 C3 106.6(3) . . ? C1 N2 C4 128.0(3) . 31_565 ? C3 N2 C4 125.3(3) . 31_565 ? N1 C1 N2 111.6(3) . . ? N1 C1 C1 123.4(3) . 18_455 ? N2 C1 C1 124.9(3) . 18_455 ? C3 C2 N1 110.7(3) . . ? C3 C2 H2 124.6 . . ? N1 C2 H2 124.6 . . ? C2 C3 N2 106.3(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 111.9(3) 31_565 . ? N2 C4 H4A 109.2 31_565 . ? C5 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 31_565 . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 113.4(3) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? O2 C6 O1 123.0(3) . . ? O2 C6 C5 119.1(3) . . ? O1 C6 C5 117.9(3) . . ? 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 O3 Pb1 O1 C6 -171.0(2) . . . . ? O1 Pb1 O1 C6 -171.0(2) 11 . . . ? N1 Pb1 O1 C6 116.1(2) 11 . . . ? N1 Pb1 O1 C6 -97.1(2) . . . . ? O3 Pb1 N1 C1 -95.2(3) . . . . ? O1 Pb1 N1 C1 -177.2(3) . . . . ? O1 Pb1 N1 C1 -14.9(3) 11 . . . ? N1 Pb1 N1 C1 -95.2(3) 11 . . . ? O3 Pb1 N1 C2 59.5(2) . . . . ? O1 Pb1 N1 C2 -22.5(2) . . . . ? O1 Pb1 N1 C2 139.7(2) 11 . . . ? N1 Pb1 N1 C2 59.5(2) 11 . . . ? C2 N1 C1 N2 0.6(3) . . . . ? Pb1 N1 C1 N2 157.8(2) . . . . ? C2 N1 C1 C1 -175.7(2) . . . 18_455 ? Pb1 N1 C1 C1 -18.5(4) . . . 18_455 ? C3 N2 C1 N1 -0.3(3) . . . . ? C4 N2 C1 N1 177.0(3) 31_565 . . . ? C3 N2 C1 C1 176.0(2) . . . 18_455 ? C4 N2 C1 C1 -6.7(4) 31_565 . . 18_455 ? C1 N1 C2 C3 -0.7(4) . . . . ? Pb1 N1 C2 C3 -161.7(2) . . . . ? N1 C2 C3 N2 0.6(4) . . . . ? C1 N2 C3 C2 -0.2(3) . . . . ? C4 N2 C3 C2 -177.6(3) 31_565 . . . ? N2 C4 C5 C6 61.5(4) 31_565 . . . ? Pb1 O1 C6 O2 -13.7(3) . . . . ? Pb1 O1 C6 C5 165.1(2) . . . . ? C4 C5 C6 O2 42.4(4) . . . . ? C4 C5 C6 O1 -136.5(3) . . . . ? 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 O3 H3A O1 0.84 1.89 2.690(3) 158.2 4_675 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.746 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.109