Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_chen2b _database_code_CSD 192268 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Jie-Sheng Chen' 'Wei Chen' 'Cheng Chen' 'Suning Wang' 'Wei Xu' 'Hong-Ming Yuan' 'Qi Yue' _publ_contact_author_name 'Prof Jie-Sheng Chen' _publ_contact_author_address ; Department of Chemistry Jilin University 119 Jiefang Road Changchun Jilin 130023 CHINA ; _publ_contact_author_email 'CHEMCJ@MAIL.JLU.EDU.CN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Assembly of a Manganese(II) Pyridine-3,4-dicarboxylate Polymeric Network Based on the Infinite Mn-O-C Chains ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Mn[C5H3N(COO)2]H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H5 Mn N O5' _chemical_formula_weight 238.06 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' 'Mn' 'Mn' 0.3368 0.7283 '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(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.7055(14) _cell_length_b 14.783(3) _cell_length_c 7.9166(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.724(3) _cell_angle_gamma 90.00 _cell_volume 771.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_% 0 _diffrn_reflns_number 5260 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 28.24 _reflns_number_total 1780 _reflns_number_gt 1449 _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^)+(0.0580P)^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 1780 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _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 Mn1 Mn 0.22533(5) 0.77848(2) 0.61339(4) 0.02027(14) Uani 1 1 d . . . C1 C 0.6893(3) 0.83775(14) 0.7898(3) 0.0201(4) Uani 1 1 d . . . C2 C 0.7287(3) 0.92576(14) 0.7049(3) 0.0197(4) Uani 1 1 d . . . C3 C 0.7280(4) 1.00754(15) 0.7894(3) 0.0257(5) Uani 1 1 d . . . H3 H 0.708(4) 1.0031(19) 0.901(3) 0.038(8) Uiso 1 1 d . . . C4 C 0.7463(4) 1.08718(16) 0.7017(3) 0.0267(5) Uani 1 1 d . . . H4 H 0.752(4) 1.146(2) 0.756(4) 0.043(8) Uiso 1 1 d . . . C5 C 0.7631(3) 1.00961(15) 0.4535(3) 0.0212(4) Uani 1 1 d . . . H5 H 0.779(3) 1.0108(16) 0.346(3) 0.022(6) Uiso 1 1 d . . . C6 C 0.7524(3) 0.92712(13) 0.5324(2) 0.0182(4) Uani 1 1 d . . . C7 C 0.7840(3) 0.84107(14) 0.4403(3) 0.0199(4) Uani 1 1 d . . . N1 N 0.7604(3) 1.08958(12) 0.5341(2) 0.0224(4) Uani 1 1 d . . . O1 O 0.5458(2) 0.79024(10) 0.7168(2) 0.0259(4) Uani 1 1 d . . . O2 O 0.8037(2) 0.81871(12) 0.93154(19) 0.0277(4) Uani 1 1 d . . . O3 O 0.8942(2) 0.78109(10) 0.52759(19) 0.0216(3) Uani 1 1 d . . . O4 O 0.7021(2) 0.83464(11) 0.28473(19) 0.0272(4) Uani 1 1 d . . . O5 O 0.1956(3) 0.86147(12) 0.8545(2) 0.0279(4) Uani 1 1 d . . . H1 H 0.067(5) 0.857(2) 0.881(5) 0.071(11) Uiso 1 1 d . . . H2 H 0.279(4) 0.826(2) 0.932(4) 0.055(10) 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 Mn1 0.0220(2) 0.0196(2) 0.01892(19) -0.00010(13) 0.00316(13) -0.00001(13) C1 0.0229(11) 0.0195(10) 0.0194(9) 0.0006(8) 0.0077(8) 0.0025(9) C2 0.0180(10) 0.0214(11) 0.0188(10) 0.0015(8) 0.0011(8) 0.0010(8) C3 0.0349(13) 0.0236(12) 0.0185(9) -0.0018(9) 0.0049(9) -0.0024(10) C4 0.0321(12) 0.0210(12) 0.0268(11) -0.0017(9) 0.0048(9) -0.0007(10) C5 0.0222(11) 0.0220(11) 0.0199(10) 0.0024(8) 0.0054(8) 0.0011(8) C6 0.0167(10) 0.0186(10) 0.0186(9) -0.0006(8) 0.0015(7) -0.0009(8) C7 0.0199(10) 0.0202(10) 0.0206(9) -0.0012(8) 0.0067(8) -0.0023(8) N1 0.0243(9) 0.0185(9) 0.0236(9) 0.0008(7) 0.0026(7) -0.0008(8) O1 0.0220(8) 0.0257(9) 0.0295(8) 0.0026(6) 0.0031(7) -0.0039(6) O2 0.0320(9) 0.0293(9) 0.0201(7) 0.0073(7) 0.0008(6) -0.0044(7) O3 0.0215(8) 0.0209(8) 0.0219(7) -0.0008(6) 0.0027(6) 0.0028(6) O4 0.0358(9) 0.0259(9) 0.0186(7) -0.0019(6) 0.0016(6) 0.0057(7) O5 0.0290(9) 0.0286(9) 0.0261(8) 0.0012(7) 0.0052(7) 0.0033(7) _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 Mn1 O1 2.1593(16) . ? Mn1 O2 2.1667(15) 4_575 ? Mn1 O4 2.1770(16) 4_576 ? Mn1 O3 2.1980(16) 1_455 ? Mn1 N1 2.2845(18) 3_676 ? Mn1 O5 2.3087(17) . ? C1 O1 1.244(3) . ? C1 O2 1.267(3) . ? C1 C2 1.510(3) . ? C2 C3 1.382(3) . ? C2 C6 1.405(3) . ? C3 C4 1.384(3) . ? C3 H3 0.92(3) . ? C4 N1 1.347(3) . ? C4 H4 0.96(3) . ? C5 N1 1.345(3) . ? C5 C6 1.378(3) . ? C5 H5 0.88(2) . ? C6 C7 1.501(3) . ? C7 O4 1.255(3) . ? C7 O3 1.273(3) . ? N1 Mn1 2.2845(18) 3_676 ? O2 Mn1 2.1667(15) 4_676 ? O3 Mn1 2.1980(16) 1_655 ? O4 Mn1 2.1770(16) 4_675 ? O5 H1 0.93(4) . ? O5 H2 0.92(3) . ? 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 O1 Mn1 O2 87.60(6) . 4_575 ? O1 Mn1 O4 90.41(6) . 4_576 ? O2 Mn1 O4 87.65(7) 4_575 4_576 ? O1 Mn1 O3 172.94(6) . 1_455 ? O2 Mn1 O3 99.34(6) 4_575 1_455 ? O4 Mn1 O3 91.19(6) 4_576 1_455 ? O1 Mn1 N1 89.53(6) . 3_676 ? O2 Mn1 N1 100.84(7) 4_575 3_676 ? O4 Mn1 N1 171.50(7) 4_576 3_676 ? O3 Mn1 N1 87.87(6) 1_455 3_676 ? O1 Mn1 O5 82.91(6) . . ? O2 Mn1 O5 166.08(6) 4_575 . ? O4 Mn1 O5 82.29(6) 4_576 . ? O3 Mn1 O5 90.49(6) 1_455 . ? N1 Mn1 O5 89.27(6) 3_676 . ? O1 C1 O2 125.1(2) . . ? O1 C1 C2 117.63(18) . . ? O2 C1 C2 117.29(18) . . ? C3 C2 C6 117.98(19) . . ? C3 C2 C1 121.46(18) . . ? C6 C2 C1 120.40(18) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 114.6(18) . . ? C4 C3 H3 125.8(18) . . ? N1 C4 C3 123.1(2) . . ? N1 C4 H4 114.4(18) . . ? C3 C4 H4 122.6(18) . . ? N1 C5 C6 123.79(19) . . ? N1 C5 H5 117.2(16) . . ? C6 C5 H5 118.9(16) . . ? C5 C6 C2 118.58(18) . . ? C5 C6 C7 120.38(18) . . ? C2 C6 C7 120.82(18) . . ? O4 C7 O3 125.7(2) . . ? O4 C7 C6 117.72(18) . . ? O3 C7 C6 116.54(17) . . ? C5 N1 C4 116.97(19) . . ? C5 N1 Mn1 120.14(14) . 3_676 ? C4 N1 Mn1 122.88(15) . 3_676 ? C1 O1 Mn1 148.35(15) . . ? C1 O2 Mn1 123.64(14) . 4_676 ? C7 O3 Mn1 129.12(13) . 1_655 ? C7 O4 Mn1 126.90(14) . 4_675 ? Mn1 O5 H1 112(2) . . ? Mn1 O5 H2 96(2) . . ? H1 O5 H2 107(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 O5 H1 O2 0.93(4) 1.96(4) 2.877(2) 167(3) 1_455 O5 H2 O3 0.92(3) 1.85(3) 2.723(2) 157(3) 4_576 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.716 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.110