#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012608.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012608 loop_ _publ_author_name 'Zhang, Yu' 'Tao, Hanbing' 'Duan, Chunying' 'Li, Yizhi' 'Zhu, Longgen' _publ_section_title ; Tetrakis[(4-aminopyridinio)acetato-\kO]diaquamanganese(II) diperchlorate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m188 _journal_page_last m189 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Mn (C7 H8 N2 O2)4 (H2 O)2] (Cl O4)2' _chemical_formula_moiety 'C28 H36 Mn N8 O10 2+ , 2Cl O4 -' _chemical_formula_sum 'C28 H36 Cl2 Mn N8 O18' _chemical_formula_weight 898.49 _chemical_name_systematic ; Tetrakis[(4-aminopyridinio)acetato-\kO]diaquamanganese(II) diperchlorate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 71.79(4) _cell_angle_beta 89.52(4) _cell_angle_gamma 76.13(4) _cell_formula_units_Z 1 _cell_length_a 9.049(2) _cell_length_b 10.507(3) _cell_length_c 10.779(3) _cell_measurement_reflns_used 2867 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.77 _cell_measurement_theta_min 1.40 _cell_volume 942.7(5) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .983 _diffrn_measured_fraction_theta_max .983 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .043 _diffrn_reflns_av_sigmaI/netI .037 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4859 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.99 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .579 _exptl_absorpt_correction_T_max .901 _exptl_absorpt_correction_T_min .870 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 463 _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _refine_diff_density_max .48 _refine_diff_density_min -.45 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 295 _refine_ls_number_reflns 3275 _refine_ls_number_restraints 160 _refine_ls_restrained_S_all 1.243 _refine_ls_R_factor_all .055 _refine_ls_R_factor_gt .049 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0923P)^2^+0.2644P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .143 _refine_ls_wR_factor_ref .148 _reflns_number_gt 2834 _reflns_number_total 3275 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ta1355.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P-1 _cod_original_cell_volume 942.7(4) _cod_database_code 2012608 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Mn .5000 .5000 .5000 .0412(2) Uani d S 1 . . Mn O1W .3803(3) .5874(3) .6475(2) .0598(6) Uani d . 1 . . O H1WA .3754 .5083 .7096 .072 Uiso d R 1 . . H H1WB .2876 .6282 .6049 .072 Uiso d R 1 . . H O1 .1171(3) .6735(3) .4687(3) .0687(7) Uani d . 1 . . O O2 .2827(3) .5108(3) .4126(3) .0620(7) Uani d . 1 . . O O3 .4198(4) .3141(3) .8073(3) .0907(10) Uani d . 1 . . O O4 .5123(3) .2935(2) .6218(2) .0597(6) Uani d . 1 . . O N1 .2135(4) .2511(3) .0093(3) .0714(9) Uani d . 1 . . N H1A .2863 .2524 -.0426 .086 Uiso calc R 1 . . H H1B .1615 .1903 .0197 .086 Uiso calc R 1 . . H N2 .7765(4) -.2212(4) .4847(4) .0727(9) Uani d . 1 . . N H2A .7329 -.2831 .4777 .087 Uiso calc R 1 . . H H2B .8570 -.2099 .4441 .087 Uiso calc R 1 . . H C1 .1638(3) .6040(4) .3959(4) .0533(8) Uani d . 1 . . C C2 .0659(5) .6423(5) .2688(4) .0766(12) Uani d . 1 . . C H2C -.0404 .6533 .2883 .092 Uiso calc R 1 . . H H2D .0769 .7306 .2109 .092 Uiso calc R 1 . . H C3 .2240(4) .5378(4) .1233(4) .0653(9) Uani d . 1 . . C H3A .2801 .6034 .1134 .078 Uiso calc R 1 . . H N3 .1065(3) .5386(3) .2009(3) .0614(8) Uani d . 1 . . N C4 .2618(4) .4441(4) .0600(3) .0626(9) Uani d . 1 . . C H4A .3429 .4466 .0065 .075 Uiso calc R 1 . . H N4 .6079(3) .0138(3) .7186(3) .0554(7) Uani d . 1 . . N C5 .1812(4) .3429(4) .0731(3) .0565(8) Uani d . 1 . . C C6 .0625(4) .3438(4) .1588(4) .0629(9) Uani d . 1 . . C H6A .0064 .2777 .1735 .075 Uiso calc R 1 . . H C7 .0306(4) .4403(5) .2192(4) .0685(10) Uani d . 1 . . C H7A -.0473 .4387 .2760 .082 Uiso calc R 1 . . H C8 .4889(4) .2472(3) .7390(3) .0556(8) Uani d . 1 . . C C9 .5523(6) .0927(4) .8068(4) .0725(11) Uani d . 1 . . C H9A .6354 .0795 .8695 .087 Uiso calc R 1 . . H H9B .4730 .0556 .8554 .087 Uiso calc R 1 . . H C10 .5385(4) -.0810(3) .7033(3) .0552(8) Uani d . 1 . . C H10A .4522 -.0935 .7483 .066 Uiso calc R 1 . . H C11 .5887(4) -.1583(3) .6257(3) .0507(7) Uani d . 1 . . C H11A .5366 -.2216 .6169 .061 Uiso calc R 1 . . H C12 .7198(4) -.1434(3) .5578(3) .0516(8) Uani d . 1 . . C C13 .7874(4) -.0408(4) .5720(4) .0671(10) Uani d . 1 . . C H13A .8717 -.0238 .5258 .081 Uiso calc R 1 . . H C14 .7316(4) .0328(4) .6515(4) .0646(10) Uani d . 1 . . C H14A .7796 .0988 .6604 .078 Uiso calc R 1 . . H Cl1 -.14846(13) .06845(12) .13633(11) .0775(4) Uani d DU 1 . . Cl O11 .0057(6) .0542(11) .1141(9) .115(3) Uani d PDU .50 A 1 O O12 -.1681(10) .0976(11) .2535(6) .111(3) Uani d PDU .50 A 1 O O13 -.1814(10) -.0588(6) .1530(9) .107(3) Uani d PDU .50 A 1 O O14 -.2431(12) .1661(8) .0364(9) .178(4) Uani d PDU .50 A 1 O O11' -.2394(11) .1683(8) .1829(11) .137(3) Uani d PDU .50 A 2 O O12' -.0392(11) -.0201(9) .2325(9) .181(4) Uani d PDU .50 A 2 O O13' -.2372(10) -.0073(9) .1018(9) .116(3) Uani d PDU .50 A 2 O O14' -.0830(12) .1400(7) .0290(8) .130(3) Uani d PDU .50 A 2 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn .0416(4) .0427(4) .0447(4) -.0139(3) .0052(3) -.0190(3) O1W .0635(14) .0626(14) .0642(15) -.0184(11) .0153(11) -.0338(12) O1 .0516(13) .0903(19) .0774(17) -.0095(12) .0060(12) -.0513(15) O2 .0474(13) .0650(15) .0821(17) -.0062(11) -.0113(11) -.0409(13) O3 .151(3) .0582(16) .0636(17) -.0189(17) .0401(18) -.0266(13) O4 .0833(16) .0448(13) .0518(14) -.0169(11) .0145(12) -.0162(10) N1 .095(2) .0628(19) .0570(18) -.0136(17) .0041(16) -.0252(15) N2 .0645(19) .081(2) .099(3) -.0339(17) .0286(18) -.054(2) C1 .0429(17) .060(2) .069(2) -.0177(15) .0054(15) -.0324(17) C2 .068(2) .084(3) .081(3) .006(2) -.013(2) -.050(2) C3 .071(2) .063(2) .064(2) -.0197(18) -.0004(18) -.0215(18) N3 .0565(17) .0682(19) .0621(18) -.0040(14) -.0070(14) -.0330(15) C4 .072(2) .065(2) .0524(19) -.0186(18) .0130(17) -.0210(17) N4 .0691(18) .0438(15) .0511(16) -.0110(13) .0022(13) -.0143(12) C5 .068(2) .0540(19) .0410(17) -.0038(16) -.0059(15) -.0143(14) C6 .066(2) .072(2) .058(2) -.0240(18) .0016(17) -.0258(18) C7 .054(2) .095(3) .064(2) -.018(2) .0057(17) -.036(2) C8 .072(2) .0477(18) .0519(19) -.0184(16) .0094(16) -.0206(15) C9 .114(3) .050(2) .051(2) -.014(2) .008(2) -.0184(16) C10 .0573(19) .0491(18) .0568(19) -.0167(15) .0108(15) -.0113(15) C11 .0472(16) .0478(17) .0613(19) -.0182(14) .0040(14) -.0184(15) C12 .0447(16) .0513(18) .063(2) -.0154(14) .0044(14) -.0219(16) C13 .0510(19) .066(2) .101(3) -.0287(17) .0200(19) -.040(2) C14 .057(2) .058(2) .090(3) -.0242(17) .0010(19) -.033(2) Cl1 .12867(7) .1431(7) .1156(7) -.0481(6) .0266(6) -.0394(6) O11 .091(4) .184(8) .132(6) -.077(5) .044(4) -.105(6) O12 .116(6) .171(8) .084(5) -.067(5) .029(4) -.071(5) O13 .134(7) .065(4) .126(7) -.045(4) .040(5) -.026(4) O14 .214(9) .129(7) .158(8) -.034(7) -.040(8) -.006(7) O11' .144(7) .105(6) .187(9) -.047(5) .065(7) -.070(6) O12' .170(8) .174(8) .166(8) -.014(7) -.071(7) -.026(7) O13' .123(6) .151(8) .116(7) -.078(6) .004(5) -.069(6) O14' .191(8) .079(5) .117(6) -.053(5) .080(6) -.014(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn .3368 .7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 Mn O4 2_666 . 180.00 ? O4 Mn O2 2_666 2_666 90.15(11) ? O4 Mn O2 . 2_666 89.85(11) ? O4 Mn O2 2_666 . 89.85(11) ? O4 Mn O2 . . 90.15(11) y O2 Mn O2 2_666 . 180.0 n O4 Mn O1W 2_666 2_666 91.80(10) ? O4 Mn O1W . 2_666 88.20(10) ? O2 Mn O1W 2_666 2_666 89.49(9) ? O2 Mn O1W . 2_666 90.51(9) ? O4 Mn O1W 2_666 . 88.20(10) ? O4 Mn O1W . . 91.80(10) y O2 Mn O1W 2_666 . 90.51(9) ? O2 Mn O1W . . 89.49(9) y O1W Mn O1W 2_666 . 180.0 ? Mn O1W H1WA . . 99.4 ? Mn O1W H1WB . . 100.1 ? H1WA O1W H1WB . . 108.7 ? C1 O2 Mn . . 127.5(2) y C8 O4 Mn . . 130.8(2) y C5 N1 H1A . . 120.0 ? C5 N1 H1B . . 120.0 ? H1A N1 H1B . . 120.0 ? C12 N2 H2A . . 120.0 ? C12 N2 H2B . . 120.0 ? H2A N2 H2B . . 120.0 ? O1 C1 O2 . . 127.5(3) y O1 C1 C2 . . 115.6(3) y O1 O1W O3 . . 111.15(13) y O2 C1 C2 . . 116.9(3) ? N3 C2 C1 . . 113.1(3) y N3 C2 H2C . . 109.0 ? C1 C2 H2C . . 109.0 ? N3 C2 H2D . . 109.0 ? C1 C2 H2D . . 109.0 ? H2C C2 H2D . . 107.8 ? C4 C3 N3 . . 121.4(4) ? C4 C3 H3A . . 119.3 ? N3 C3 H3A . . 119.3 ? C7 N3 C3 . . 118.9(3) ? C7 N3 C2 . . 120.3(3) y C3 N3 C2 . . 120.7(4) ? C3 C4 C5 . . 121.1(3) ? C3 C4 H4A . . 119.4 ? C5 C4 H4A . . 119.4 ? C10 N4 C14 . . 118.3(3) ? C10 N4 C9 . . 121.0(3) ? C14 N4 C9 . . 120.6(3) ? N1 C5 C4 . . 122.5(3) y N1 C5 C6 . . 121.5(4) ? C4 C5 C6 . . 115.9(3) ? C7 C6 C5 . . 119.9(4) ? C7 C6 H6A . . 120.0 ? C5 C6 H6A . . 120.0 ? N3 C7 C6 . . 122.6(4) ? N3 C7 H7A . . 118.7 ? C6 C7 H7A . . 118.7 ? O3 C8 O4 . . 126.6(3) y O3 C8 C9 . . 116.3(3) y O4 C8 C9 . . 117.1(3) ? N4 C9 C8 . . 114.5(3) ? N4 C9 H9A . . 108.6 ? C8 C9 H9A . . 108.6 ? N4 C9 H9B . . 108.6 ? C8 C9 H9B . . 108.6 ? H9A C9 H9B . . 107.6 ? C11 C10 N4 . . 122.8(3) ? C11 C10 H10A . . 118.6 ? N4 C10 H10A . . 118.6 ? C10 C11 C12 . . 120.0(3) ? C10 C11 H11A . . 120.0 ? C12 C11 H11A . . 120.0 ? N2 C12 C11 . . 121.9(3) y N2 C12 C13 . . 121.9(3) ? C11 C12 C13 . . 116.2(3) ? C14 C13 C12 . . 120.8(3) ? C14 C13 H13A . . 119.6 ? C12 C13 H13A . . 119.6 ? C13 C14 N4 . . 121.9(3) ? C13 C14 H14A . . 119.1 ? N4 C14 H14A . . 119.1 ? O14 Cl1 O12' . . 172.6(6) ? O14 Cl1 O14' . . 62.1(5) ? O12' Cl1 O14' . . 111.3(5) ? O14 Cl1 O13' . . 77.8(5) ? O12' Cl1 O13' . . 108.6(5) ? O14' Cl1 O13' . . 111.3(5) ? O14 Cl1 O12 . . 111.9(5) ? O12' Cl1 O12 . . 68.5(5) ? O14' Cl1 O12 . . 126.0(5) ? O13' Cl1 O12 . . 119.8(6) ? O14 Cl1 O11' . . 70.4(5) ? O12' Cl1 O11' . . 109.7(5) ? O14' Cl1 O11' . . 106.0(4) ? O13' Cl1 O11' . . 109.9(5) ? O14 Cl1 O11 . . 113.5(5) ? O12' Cl1 O11 . . 60.1(5) ? O14' Cl1 O11 . . 51.3(4) ? O13' Cl1 O11 . . 123.9(6) ? O12 Cl1 O11 . . 106.6(4) ? O11' Cl1 O11 . . 126.0(5) ? O14 Cl1 O13 . . 108.4(5) ? O12' Cl1 O13 . . 78.0(5) ? O14' Cl1 O13 . . 124.9(6) ? O12 Cl1 O13 . . 108.3(4) ? O11' Cl1 O13 . . 122.1(6) ? O11 Cl1 O13 . . 108.0(4) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn O4 2_666 2.133(2) ? Mn O4 . 2.133(2) y Mn O2 2_666 2.151(2) ? Mn O2 . 2.151(2) y Mn O1W 2_666 2.225(2) ? Mn O1W . 2.225(2) y O1W H1WA . .9001 ? O1W H1WB . .9000 ? O1 C1 . 1.238(4) y O2 C1 . 1.240(4) y O3 C8 . 1.238(4) y O4 C8 . 1.240(4) y N1 C5 . 1.330(5) y N1 H1A . .8600 ? N1 H1B . .8600 ? N2 C12 . 1.322(4) y N2 H2A . .8600 ? N2 H2B . .8600 ? C1 C2 . 1.526(5) ? C2 N3 . 1.469(5) y C2 H2C . .9700 ? C2 H2D . .9700 ? C3 C4 . 1.344(5) y C3 N3 . 1.347(5) ? C3 H3A . .9300 ? N3 C7 . 1.337(5) y C4 C5 . 1.400(5) ? C4 H4A . .9300 ? N4 C10 . 1.349(5) y N4 C14 . 1.349(5) y N4 C9 . 1.459(5) y C5 C6 . 1.411(5) y C6 C7 . 1.344(5) ? C6 H6A . .9300 ? C7 H7A . .9300 ? C8 C9 . 1.523(5) ? C9 H9A . .9700 ? C9 H9B . .9700 ? C10 C11 . 1.344(5) ? C10 H10A . .9300 ? C11 C12 . 1.404(5) ? C11 H11A . .9300 ? C12 C13 . 1.406(5) ? C13 C14 . 1.345(5) ? C13 H13A . .9300 ? C14 H14A . .9300 ? Cl1 O14 . 1.360(5) ? Cl1 O12' . 1.375(5) ? Cl1 O14' . 1.383(4) ? Cl1 O13' . 1.383(4) ? Cl1 O12 . 1.390(4) ? Cl1 O11' . 1.392(4) ? Cl1 O11 . 1.394(4) ? Cl1 O13 . 1.396(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1W H1WA O3 . .90 1.925 2.787(4) 160 N1 H1A O3 1_554 .86 2.046 2.879(5) 163 O1W H1WB O1 . .90 2.003 2.856(4) 158 N2 H2A O2 2_656 .86 2.352 3.072(5) 142 N2 H2A O4 2_656 .86 2.513 3.205(5) 138 N2 H2B O1 1_645 .86 2.353 3.038(5) 137