#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/00/4300003.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4300003 loop_ _publ_author_name 'Suzanne J. Brudenell' 'Leone Spiccia' 'Alan M. Bond' 'Gary D. Fallon' 'David C. R. Hockless' 'George Lazarev' 'Peter J. Mahon' 'Edward R. T. Tiekink' _publ_section_title ; Structural, Spectroscopic, and Electrochemical Studies of Binuclear Manganese(II) Complexes of Bis(pentadentate) Ligands Derived from Bis(1,4,7-triazacyclononane) Macrocycles ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 881 _journal_page_last 892 _journal_volume 39 _journal_year 2000 _chemical_formula_sum 'C18 H25 Cl2 Mn N5 O4' _chemical_formula_weight 501.27 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _audit_creation_date 'Mon Jun 30 01:41:54 1997' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.959(7) _cell_length_b 12.30(1) _cell_length_c 21.72(2) _cell_measurement_reflns_used 30 _cell_measurement_temperature 173.2 _cell_measurement_theta_max 27.8 _cell_measurement_theta_min 9.9 _cell_volume 2126(3) _computing_cell_refinement P3 _computing_data_collection P3 _computing_data_reduction XDisk _computing_publication_material teXsan _computing_structure_refinement teXsan _computing_structure_solution teXsan _diffrn_ambient_temperature 173.2 _diffrn_measurement_device 'NICOLET R3m' _diffrn_measurement_method 'omega scans' _diffrn_orient_matrix_UB_11 0.03130 _diffrn_orient_matrix_UB_12 0.02069 _diffrn_orient_matrix_UB_13 0.04303 _diffrn_orient_matrix_UB_21 0.02660 _diffrn_orient_matrix_UB_22 0.07537 _diffrn_orient_matrix_UB_23 -0.01423 _diffrn_orient_matrix_UB_31 -0.11875 _diffrn_orient_matrix_UB_32 0.02234 _diffrn_orient_matrix_UB_33 0.00815 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoKalpha _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 4.24 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 17964 _diffrn_reflns_theta_max 22.55 _diffrn_reflns_theta_min 1.5 _diffrn_standards_decay_% '< 1.0' _diffrn_standards_interval_count 297 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.907 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.566 _exptl_crystal_description tabular _exptl_crystal_F_000 1036.00 _refine_diff_density_max 0.33 _refine_diff_density_min -0.28 _refine_ls_abs_structure_Flack 0.0003(1) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.207 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 1363 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0354 _refine_ls_shift/esd_max 0.0004 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_obs 0.0304 _reflns_number_observed 1363 _reflns_number_total 1654 _reflns_observed_criterion 3.00 _[local]_cod_cif_authors_sg_H-M 'P 21 21 21 ' _[local]_cod_chemical_formula_sum_orig 'C18 H25 Cl2 N5 Mn O4 ' _cod_database_code 4300003 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' 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(1) 0.0195(5) 0.0190(6) 0.0190(6) -0.0015(6) -0.0011(6) 0.0013(6) Cl(1) 0.0216(10) 0.033(1) 0.040(1) -0.005(1) -0.0010(9) 0.006(1) Cl(2) 0.032(1) 0.035(1) 0.034(1) 0.001(1) 0.000(1) 0.001(1) O(1) 0.042(4) 0.092(5) 0.056(4) -0.035(4) -0.021(4) 0.008(4) O(2) 0.062(5) 0.190(9) 0.078(5) -0.060(6) 0.033(4) -0.016(6) O(3) 0.117(6) 0.078(5) 0.047(4) -0.015(5) -0.035(5) 0.003(4) O(4) 0.186(9) 0.054(5) 0.195(9) 0.061(6) -0.062(8) -0.047(6) N(1) 0.018(3) 0.016(3) 0.027(3) -0.001(3) -0.013(3) -0.002(3) N(2) 0.021(3) 0.020(3) 0.022(3) 0.000(3) -0.003(3) 0.005(3) N(3) 0.038(4) 0.017(4) 0.025(3) -0.010(3) 0.000(3) 0.004(3) N(4) 0.022(3) 0.020(4) 0.019(3) 0.000(3) 0.003(3) 0.006(3) N(5) 0.017(4) 0.022(4) 0.017(3) 0.002(3) -0.003(3) 0.005(3) C(1) 0.020(4) 0.029(5) 0.030(4) -0.011(4) -0.003(4) -0.004(4) C(2) 0.036(5) 0.009(4) 0.041(5) -0.003(4) 0.004(5) -0.004(4) C(3) 0.022(4) 0.019(4) 0.040(5) 0.003(4) 0.003(4) 0.006(4) C(4) 0.024(4) 0.020(4) 0.032(5) 0.004(4) 0.003(4) 0.009(4) C(5) 0.018(4) 0.020(5) 0.036(5) -0.003(4) -0.001(4) 0.006(4) C(6) 0.036(5) 0.029(5) 0.025(4) 0.010(4) 0.000(4) 0.003(4) C(7) 0.033(5) 0.029(4) 0.022(4) 0.006(4) -0.001(4) 0.002(4) C(8) 0.033(5) 0.029(4) 0.033(5) -0.004(4) -0.011(4) -0.008(4) C(9) 0.033(5) 0.019(5) 0.035(5) 0.015(4) 0.008(4) 0.001(4) C(10) 0.027(4) 0.025(5) 0.033(5) 0.011(4) -0.004(4) -0.004(4) C(11) 0.039(5) 0.024(5) 0.019(4) 0.001(4) 0.004(4) -0.003(4) C(12) 0.022(5) 0.024(5) 0.028(5) -0.005(4) 0.001(4) 0.001(4) C(13) 0.016(4) 0.022(4) 0.030(5) -0.006(4) -0.004(4) -0.006(4) C(14) 0.019(4) 0.011(4) 0.026(4) 0.007(4) -0.005(4) -0.002(4) C(15) 0.020(4) 0.024(5) 0.030(5) 0.002(4) -0.006(4) 0.003(4) C(16) 0.044(5) 0.029(5) 0.030(5) -0.003(5) -0.015(5) -0.004(4) C(17) 0.040(5) 0.025(5) 0.020(4) -0.007(5) 0.007(4) 0.005(3) C(18) 0.036(4) 0.029(5) 0.020(4) -0.004(4) 0.009(4) -0.004(4) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Mn(1) 0.3423(1) 0.57800(8) 0.07409(5) 0.0192(3) Uij ? ? Cl(1) 0.5879(2) 0.6620(2) 0.02806(9) 0.0314(6) Uij ? ? Cl(2) 0.6226(2) 0.3500(2) -0.17635(9) 0.0340(6) Uij ? ? O(1) 0.4941(7) 0.2873(5) -0.2048(3) 0.063(2) Uij ? ? O(2) 0.7617(8) 0.3521(7) -0.2150(3) 0.110(3) Uij ? ? O(3) 0.666(1) 0.3036(5) -0.1193(3) 0.081(3) Uij ? ? O(4) 0.569(1) 0.4559(6) -0.1679(4) 0.145(4) Uij ? ? N(1) 0.4850(6) 0.4192(5) 0.0773(3) 0.021(2) Uij ? ? N(2) 0.3635(7) 0.5293(4) 0.1773(2) 0.021(2) Uij ? ? N(3) 0.2844(7) 0.7339(5) 0.1242(3) 0.027(2) Uij ? ? N(4) 0.0588(7) 0.5587(4) 0.1064(2) 0.021(2) Uij ? ? N(5) 0.1956(7) 0.5417(5) -0.0101(2) 0.019(2) Uij ? ? C(1) 0.5276(9) 0.3604(6) 0.0278(3) 0.026(2) Uij ? ? C(2) 0.637(1) 0.2737(5) 0.0302(3) 0.029(2) Uij ? ? C(3) 0.7063(9) 0.2458(6) 0.0874(4) 0.027(2) Uij ? ? C(4) 0.665(1) 0.3054(6) 0.1379(3) 0.025(2) Uij ? ? C(5) 0.5547(9) 0.3936(6) 0.1323(3) 0.025(2) Uij ? ? C(6) 0.5200(9) 0.4684(6) 0.1852(4) 0.030(2) Uij ? ? C(7) 0.3575(10) 0.6291(6) 0.2179(3) 0.028(2) Uij ? ? C(8) 0.3948(9) 0.7296(6) 0.1793(3) 0.032(2) Uij ? ? C(9) 0.0998(10) 0.7500(6) 0.1380(3) 0.029(2) Uij ? ? C(10) -0.0080(9) 0.6711(6) 0.1029(3) 0.028(2) Uij ? ? C(11) 0.2146(9) 0.4585(6) 0.1881(3) 0.028(2) Uij ? ? C(12) 0.0485(9) 0.5117(6) 0.1692(3) 0.025(2) Uij ? ? C(13) -0.0244(8) 0.4891(5) 0.0600(3) 0.023(2) Uij ? ? C(14) 0.0335(9) 0.5125(6) -0.0043(3) 0.019(2) Uij ? ? C(15) -0.0705(9) 0.4976(6) -0.0543(3) 0.025(2) Uij ? ? C(16) -0.005(1) 0.5122(7) -0.1131(3) 0.035(3) Uij ? ? C(17) 0.161(1) 0.5437(6) -0.1191(3) 0.028(2) Uij ? ? C(18) 0.2579(9) 0.5574(6) -0.0663(3) 0.028(2) Uij ? ? H(1) 0.4800 0.3794 -0.0109 0.0314 Uij ? ? H(2) 0.6650 0.2339 -0.0059 0.0345 Uij ? ? H(3) 0.7812 0.1860 0.0908 0.0325 Uij ? ? H(4) 0.7107 0.2872 0.1769 0.0305 Uij ? ? H(5) 0.6102 0.5186 0.1887 0.0364 Uij ? ? H(6) 0.5124 0.4266 0.2218 0.0364 Uij ? ? H(7) 0.2490 0.6356 0.2357 0.0333 Uij ? ? H(8) 0.4391 0.6227 0.2496 0.0333 Uij ? ? H(9) 0.5088 0.7275 0.1663 0.0382 Uij ? ? H(10) 0.3764 0.7926 0.2036 0.0382 Uij ? ? H(11) 0.0819 0.7396 0.1808 0.0349 Uij ? ? H(12) 0.0687 0.8219 0.1270 0.0349 Uij ? ? H(13) -0.0121 0.6929 0.0610 0.0340 Uij ? ? H(14) -0.1182 0.6722 0.1197 0.0340 Uij ? ? H(15) 0.2284 0.3935 0.1651 0.0330 Uij ? ? H(16) 0.2094 0.4416 0.2308 0.0330 Uij ? ? H(17) 0.0224 0.5679 0.1976 0.0296 Uij ? ? H(18) -0.0378 0.4583 0.1699 0.0296 Uij ? ? H(19) -0.0007 0.4153 0.0693 0.0272 Uij ? ? H(20) -0.1423 0.5010 0.0622 0.0272 Uij ? ? H(21) -0.1848 0.4778 -0.0487 0.0295 Uij ? ? H(22) -0.0736 0.5007 -0.1484 0.0414 Uij ? ? H(23) 0.2087 0.5558 -0.1587 0.0340 Uij ? ? H(24) 0.3721 0.5786 -0.0704 0.0341 Uij ? ? H(25) 0.3188 0.7897 0.1004 0.0316 Uij ? ? loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn 0 4 0.337 0.728 'International Tables' C 0 72 0.003 0.002 'International Tables' H 0 100 0.000 0.000 'International Tables' N 0 20 0.006 0.003 'International Tables' Cl 0 8 0.148 0.159 'International Tables' O 0 16 0.011 0.006 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 0 0 4 0 0 1 -5 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Mn(1) N(1) 88.6(1) ? ? ? yes Cl(1) Mn(1) N(2) 116.6(2) ? ? ? yes Cl(1) Mn(1) N(3) 90.1(2) ? ? ? yes Cl(1) Mn(1) N(4) 158.4(1) ? ? ? yes Cl(1) Mn(1) N(5) 99.8(2) ? ? ? yes N(1) Mn(1) N(2) 73.2(2) ? ? ? yes N(1) Mn(1) N(3) 145.4(2) ? ? ? yes N(1) Mn(1) N(4) 112.5(2) ? ? ? yes N(1) Mn(1) N(5) 96.7(2) ? ? ? yes N(2) Mn(1) N(3) 76.6(2) ? ? ? yes N(2) Mn(1) N(4) 76.0(2) ? ? ? yes N(2) Mn(1) N(5) 141.4(2) ? ? ? yes N(3) Mn(1) N(4) 75.4(2) ? ? ? yes N(3) Mn(1) N(5) 117.6(2) ? ? ? yes N(4) Mn(1) N(5) 73.9(2) ? ? ? yes O(1) Cl(2) O(2) 108.7(4) ? ? ? yes O(1) Cl(2) O(3) 109.7(4) ? ? ? yes O(1) Cl(2) O(4) 110.2(5) ? ? ? yes O(2) Cl(2) O(3) 110.3(5) ? ? ? yes O(2) Cl(2) O(4) 108.0(6) ? ? ? yes O(3) Cl(2) O(4) 109.9(5) ? ? ? yes Mn(1) N(1) C(1) 124.7(5) ? ? ? yes Mn(1) N(1) C(5) 115.8(5) ? ? ? yes C(1) N(1) C(5) 118.6(6) ? ? ? yes Mn(1) N(2) C(6) 107.8(4) ? ? ? yes Mn(1) N(2) C(7) 110.5(4) ? ? ? yes Mn(1) N(2) C(11) 104.2(4) ? ? ? yes C(6) N(2) C(7) 112.0(6) ? ? ? yes C(6) N(2) C(11) 111.1(5) ? ? ? yes C(7) N(2) C(11) 111.0(6) ? ? ? yes Mn(1) N(3) C(8) 103.7(4) ? ? ? yes Mn(1) N(3) C(9) 113.9(5) ? ? ? yes C(8) N(3) C(9) 114.8(6) ? ? ? yes Mn(1) N(4) C(10) 103.4(4) ? ? ? yes Mn(1) N(4) C(12) 111.3(4) ? ? ? yes Mn(1) N(4) C(13) 106.4(4) ? ? ? yes C(10) N(4) C(12) 113.1(5) ? ? ? yes C(10) N(4) C(13) 110.1(5) ? ? ? yes C(12) N(4) C(13) 112.1(5) ? ? ? yes Mn(1) N(5) C(14) 118.9(5) ? ? ? yes Mn(1) N(5) C(18) 122.1(4) ? ? ? yes C(14) N(5) C(18) 118.7(6) ? ? ? yes N(1) C(1) C(2) 123.2(7) ? ? ? yes C(1) C(2) C(3) 118.1(7) ? ? ? yes C(2) C(3) C(4) 119.2(6) ? ? ? yes C(3) C(4) C(5) 119.9(7) ? ? ? yes N(1) C(5) C(4) 121.0(7) ? ? ? yes N(1) C(5) C(6) 117.2(6) ? ? ? yes C(4) C(5) C(6) 121.7(6) ? ? ? yes N(2) C(6) C(5) 112.5(6) ? ? ? yes N(2) C(7) C(8) 109.4(5) ? ? ? yes N(3) C(8) C(7) 111.0(6) ? ? ? yes N(3) C(9) C(10) 111.7(6) ? ? ? yes N(4) C(10) C(9) 111.8(6) ? ? ? yes N(2) C(11) C(12) 113.3(6) ? ? ? yes N(4) C(12) C(11) 111.5(6) ? ? ? yes N(4) C(13) C(14) 112.7(5) ? ? ? yes N(5) C(14) C(13) 115.6(6) ? ? ? yes N(5) C(14) C(15) 122.6(7) ? ? ? yes C(13) C(14) C(15) 121.7(6) ? ? ? yes C(14) C(15) C(16) 119.0(7) ? ? ? yes C(15) C(16) C(17) 118.5(7) ? ? ? yes C(16) C(17) C(18) 119.0(7) ? ? ? yes N(5) C(18) C(17) 122.2(6) ? ? ? yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) Cl(1) 2.427(3) ? ? yes Mn(1) N(1) 2.261(5) ? ? yes Mn(1) N(2) 2.326(5) ? ? yes Mn(1) N(3) 2.253(6) ? ? yes Mn(1) N(4) 2.375(6) ? ? yes Mn(1) N(5) 2.214(5) ? ? yes Cl(2) O(1) 1.422(6) ? ? yes Cl(2) O(2) 1.390(6) ? ? yes Cl(2) O(3) 1.407(6) ? ? yes Cl(2) O(4) 1.384(7) ? ? yes N(1) C(1) 1.340(8) ? ? yes N(1) C(5) 1.353(8) ? ? yes N(2) C(6) 1.463(9) ? ? yes N(2) C(7) 1.512(8) ? ? yes N(2) C(11) 1.489(9) ? ? yes N(3) C(8) 1.485(9) ? ? yes N(3) C(9) 1.513(9) ? ? yes N(4) C(10) 1.483(8) ? ? yes N(4) C(12) 1.483(8) ? ? yes N(4) C(13) 1.479(8) ? ? yes N(5) C(14) 1.345(9) ? ? yes N(5) C(18) 1.331(8) ? ? yes C(1) C(2) 1.379(9) ? ? yes C(2) C(3) 1.401(10) ? ? yes C(3) C(4) 1.360(9) ? ? yes C(4) C(5) 1.400(9) ? ? yes C(5) C(6) 1.50(1) ? ? yes C(7) C(8) 1.522(10) ? ? yes C(9) C(10) 1.50(1) ? ? yes C(11) C(12) 1.531(10) ? ? yes C(13) C(14) 1.499(9) ? ? yes C(14) C(15) 1.377(9) ? ? yes C(15) C(16) 1.389(10) ? ? yes C(16) C(17) 1.39(1) ? ? yes C(17) C(18) 1.391(10) ? ? yes _journal_paper_doi 10.1021/ic9814470