#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/00/4300000.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_4300000 loop_ _publ_author_name 'Hitoshi Masui' 'Assunta L. Freda' 'Michael C. Zerner' 'A. B. P. Lever' _publ_section_title ; Binuclear 1,2,4,5-Tetraimino-3,6-diketocyclohexane Bis[bis(Bipyridine)ruthenium(II)] Redox Series ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 141 _journal_page_last 152 _journal_volume 39 _journal_year 2000 _chemical_formula_sum 'C46 H42 Cl4 N12 O21 Ru2' _chemical_formula_weight 1442.86 _chemical_name_systematic ; Bis[bis(bipyridine)ruthenium(II)]1,2,4,5-Tetramino 3,6-Diketocyclohexane ; _space_group_IT_number 2 _symmetry_cell_setting monoclinic _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 SHELXL _cell_angle_alpha 105.17(3) _cell_angle_beta 99.62(3) _cell_angle_gamma 100.51(3) _cell_formula_units_Z 1 _cell_length_a 8.484(2) _cell_length_b 10.910(2) _cell_length_c 16.026(3) _cell_measurement_temperature 293(2) _cell_volume 1371.1(6) _computing_cell_refinement 'Siemens xscans' _computing_data_collection 'Siemens xscans' _computing_data_reduction 'Siemens xscans' _computing_molecular_graphics 'Shelxtl XP' _computing_publication_material 'Shelxtl xtext' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens R3m/v' _diffrn_measurement_method '2\q/\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 4649 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.99 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type None _exptl_crystal_colour Bronze _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_meas 0.05 _exptl_crystal_description Plate _exptl_crystal_F_000 726 _exptl_crystal_size_max 0.8 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.805 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.105 _refine_ls_hydrogen_treatment 'Riding model' _refine_ls_matrix_type full _refine_ls_number_parameters 415 _refine_ls_number_reflns 3566 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.105 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_obs 0.0496 _refine_ls_shift/esd_max -0.104 _refine_ls_shift/esd_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+1.1919P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1389 _refine_ls_wR_factor_obs 0.1264 _reflns_number_observed 2935 _reflns_number_total 3588 _reflns_observed_criterion >2sigma(I) _cod_original_cell_volume 1371.1(5) _cod_database_code 4300000 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0320(5) 0.0377(3) 0.0323(2) 0.0043(2) 0.0104(2) 0.0157(2) C1 0.030(5) 0.037(3) 0.036(3) 0.012(2) 0.006(3) 0.016(3) C2 0.024(5) 0.035(3) 0.035(3) 0.011(2) 0.010(3) 0.013(3) C3 0.026(5) 0.034(3) 0.033(3) 0.010(2) 0.010(3) 0.012(3) O1 0.047(4) 0.067(3) 0.042(2) 0.008(2) 0.003(2) 0.039(2) N1A 0.034(5) 0.039(3) 0.045(3) 0.007(2) 0.011(3) 0.013(2) C10A 0.034(6) 0.047(3) 0.053(4) 0.014(3) 0.016(3) 0.012(3) C11A 0.065(7) 0.060(4) 0.064(4) 0.024(3) 0.024(4) 0.014(4) C12A 0.086(9) 0.063(5) 0.066(5) 0.031(4) 0.012(5) 0.015(5) C13A 0.064(8) 0.051(4) 0.066(4) 0.016(3) 0.003(4) 0.023(4) C14A 0.040(6) 0.040(3) 0.051(4) 0.004(3) 0.002(3) 0.022(3) N2A 0.021(5) 0.051(3) 0.043(3) -0.001(2) 0.010(3) 0.019(3) C20A 0.025(6) 0.073(4) 0.052(4) -0.004(3) 0.015(4) 0.021(4) C21A 0.034(7) 0.102(7) 0.059(4) -0.004(4) 0.023(4) 0.031(5) C22A 0.067(9) 0.067(5) 0.082(6) -0.012(4) -0.005(5) 0.046(5) C23A 0.056(8) 0.065(5) 0.088(6) 0.009(4) 0.018(5) 0.033(5) C24A 0.031(6) 0.044(3) 0.053(4) -0.001(3) -0.001(3) 0.019(3) N3A 0.040(4) 0.059(3) 0.034(2) 0.000(2) 0.011(2) 0.019(3) C30A 0.045(6) 0.072(5) 0.051(4) -0.009(3) 0.012(4) 0.010(4) C31A 0.053(7) 0.105(7) 0.057(5) -0.009(4) -0.001(4) -0.001(5) C32A 0.079(9) 0.161(10) 0.042(4) -0.002(6) -0.005(5) 0.019(7) C33A 0.088(9) 0.126(8) 0.044(4) 0.016(5) 0.003(5) 0.019(7) C34A 0.054(6) 0.079(5) 0.042(3) 0.013(3) 0.015(3) 0.026(4) N4A 0.051(5) 0.046(3) 0.039(3) 0.007(2) 0.018(3) 0.016(3) C40A 0.066(7) 0.048(4) 0.052(4) 0.006(3) 0.026(4) 0.008(4) C41A 0.094(8) 0.061(5) 0.076(5) 0.019(4) 0.029(5) 0.000(5) C42A 0.131(11) 0.090(7) 0.088(7) 0.045(6) 0.040(7) 0.014(7) C43A 0.106(9) 0.104(7) 0.060(5) 0.040(5) 0.017(5) 0.007(6) C44A 0.063(7) 0.069(4) 0.046(4) 0.018(3) 0.024(4) 0.025(4) N5A 0.027(4) 0.035(2) 0.038(2) 0.009(2) 0.012(2) 0.015(2) N6A 0.022(4) 0.041(2) 0.036(2) 0.008(2) 0.007(2) 0.016(2) Cl1 0.164(4) 0.149(3) 0.068(2) 0.016(2) 0.022(2) -0.058(3) O10 0.377(21) 0.231(13) 0.087(6) -0.029(7) 0.030(9) -0.125(14) O11 0.143(14) 0.272(19) 0.535(35) 0.129(21) 0.107(17) 0.066(13) O12 0.528(26) 0.141(8) 0.088(6) 0.036(6) 0.086(10) -0.059(12) O13 0.157(9) 0.188(9) 0.132(7) 0.065(6) 0.048(6) -0.044(7) Cl2 0.046(2) 0.0557(10) 0.0634(10) 0.0130(8) 0.0163(10) 0.0125(9) O20 0.074(13) 0.107(11) 0.147(15) 0.054(11) 0.006(11) 0.037(9) O21 0.048(5) 0.092(4) 0.129(5) 0.039(4) -0.014(4) 0.016(3) O22 0.169(26) 0.143(18) 0.190(22) 0.059(16) 0.116(20) -0.009(16) O23 0.102(15) 0.136(19) 0.081(10) -0.064(12) -0.018(11) 0.050(14) O60 0.103(6) 0.114(5) 0.125(6) 0.057(5) 0.013(5) 0.033(4) O50 0.388(28) 0.239(17) 0.555(36) 0.214(22) 0.253(27) 0.112(18) O20A 0.050(12) 0.135(14) 0.067(8) -0.011(8) 0.020(7) 0.056(10) O23A 0.103(15) 0.213(21) 0.104(12) 0.087(14) 0.015(10) -0.037(15) O22A 0.115(21) 0.049(8) 0.335(37) 0.017(17) 0.087(24) 0.005(10) 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru -0.08657(7) 0.27366(4) 0.19607(3) 0.0338(2) Uani 1 d . . C1 C 0.1493(8) -0.0086(5) 0.0636(4) 0.033(2) Uani 1 d . . C2 C 0.0458(8) 0.0839(5) 0.0902(3) 0.0299(15) Uani 1 d . . C3 C -0.1007(8) 0.0888(5) 0.0311(3) 0.0298(15) Uani 1 d . . O1 O 0.2623(6) -0.0204(4) 0.1155(3) 0.0512(13) Uani 1 d . . N1A N 0.0110(8) 0.4294(4) 0.1552(3) 0.0396(15) Uani 1 d . . C10A C 0.1416(10) 0.4392(6) 0.1190(4) 0.044(2) Uani 1 d . . H10B H 0.1984(10) 0.3700(6) 0.1106(4) 0.080 Uiso 1 d R . C11A C 0.2052(11) 0.5464(7) 0.0949(5) 0.061(2) Uani 1 d . . H11B H 0.3000(11) 0.5536(7) 0.0695(5) 0.080 Uiso 1 d R . C12A C 0.1253(13) 0.6457(7) 0.1048(5) 0.070(3) Uani 1 d . . H12B H 0.1634(13) 0.7220(7) 0.0878(5) 0.080 Uiso 1 d R . C13A C -0.0144(12) 0.6351(7) 0.1372(5) 0.061(2) Uani 1 d . . H13B H -0.0712(12) 0.7043(7) 0.1456(5) 0.080 Uiso 1 d R . C14A C -0.0706(10) 0.5270(6) 0.1632(4) 0.045(2) Uani 1 d . . N2A N -0.2556(7) 0.3893(5) 0.2160(3) 0.0394(15) Uani 1 d . . C20A C -0.3866(10) 0.3636(7) 0.2495(4) 0.052(2) Uani 1 d . . H20B H -0.4170(10) 0.2822(7) 0.2619(4) 0.080 Uiso 1 d R . C21A C -0.4800(11) 0.4538(9) 0.2703(5) 0.067(2) Uani 1 d . . H21B H -0.5737(11) 0.4367(9) 0.2954(5) 0.080 Uiso 1 d R . C22A C -0.4369(14) 0.5721(8) 0.2569(6) 0.078(3) Uani 1 d . . H22B H -0.5001(14) 0.6364(8) 0.2697(6) 0.080 Uiso 1 d R . C23A C -0.3031(13) 0.6003(8) 0.2217(6) 0.070(3) Uani 1 d . . H23B H -0.2727(13) 0.6818(8) 0.2092(6) 0.080 Uiso 1 d R . C24A C -0.2163(10) 0.5070(6) 0.2009(4) 0.046(2) Uani 1 d . . N3A N 0.0355(7) 0.3613(5) 0.3287(3) 0.0458(15) Uani 1 d . . C30A C 0.1450(10) 0.4761(7) 0.3616(5) 0.062(2) Uani 1 d . . H30B H 0.1663(10) 0.5257(7) 0.3215(5) 0.080 Uiso 1 d R . C31A C 0.2358(11) 0.5197(9) 0.4486(5) 0.082(3) Uani 1 d . . H31B H 0.3145(11) 0.6025(9) 0.4697(5) 0.080 Uiso 1 d R . C32A C 0.2030(13) 0.4456(12) 0.5021(6) 0.104(4) Uani 1 d . . H32B H 0.2605(13) 0.4788(12) 0.5633(6) 0.080 Uiso 1 d R . C33A C 0.0861(13) 0.3248(10) 0.4702(5) 0.090(3) Uani 1 d . . H33B H 0.0649(13) 0.2752(10) 0.5103(5) 0.080 Uiso 1 d R . C34A C 0.0028(10) 0.2855(7) 0.3826(4) 0.058(2) Uani 1 d . . N4A N -0.1953(7) 0.1441(5) 0.2550(3) 0.0446(15) Uani 1 d . . C40A C -0.3238(10) 0.0409(6) 0.2142(4) 0.057(2) Uani 1 d . . H40B H -0.3746(10) 0.0212(6) 0.1526(4) 0.080 Uiso 1 d R . C41A C -0.3904(13) -0.0430(8) 0.2576(6) 0.078(3) Uani 1 d . . H41B H -0.4754(13) -0.1212(8) 0.2284(6) 0.080 Uiso 1 d R . C42A C -0.3219(15) -0.0209(10) 0.3446(7) 0.100(4) Uani 1 d . . H42B H -0.3562(15) -0.0794(10) 0.3771(7) 0.080 Uiso 1 d R . C43A C -0.1915(14) 0.0842(10) 0.3881(6) 0.089(3) Uani 1 d . . H43B H -0.1408(14) 0.1039(10) 0.4498(6) 0.080 Uiso 1 d R . C44A C -0.1294(10) 0.1672(7) 0.3425(4) 0.056(2) Uani 1 d . . N5A N -0.1825(7) 0.1674(4) 0.0681(3) 0.0322(12) Uani 1 d . . H5AA H -0.2827(7) 0.1716(4) 0.0414(3) 0.080 Uiso 1 d R . N6A N 0.0732(6) 0.1643(4) 0.1694(3) 0.0324(13) Uani 1 d . . H6AA H 0.1658(6) 0.1760(4) 0.2102(3) 0.080 Uiso 1 d R . Cl1 Cl 0.1834(6) 0.8621(4) 0.3563(2) 0.144(2) Uani 1 d . . O10 O 0.2466(21) 0.9738(13) 0.4295(6) 0.276(9) Uani 1 d . . O11 O 0.2915(19) 0.7684(19) 0.3369(16) 0.309(11) Uani 1 d . . O12 O 0.1526(23) 0.9108(10) 0.2854(6) 0.269(9) Uani 1 d . . O13 O 0.0426(13) 0.7855(10) 0.3667(6) 0.165(4) Uani 1 d . . Cl2 Cl 0.4011(3) 0.2405(2) -0.01194(12) 0.0556(6) Uani 1 d . . O20 O 0.4653(21) 0.1329(15) 0.0038(15) 0.107(5) Uani 0.50 d P . O21 O 0.2337(8) 0.1833(6) -0.0519(5) 0.093(2) Uani 1 d . . O22 O 0.4624(34) 0.2618(22) -0.0846(16) 0.163(10) Uani 0.50 d P . O23 O 0.4500(28) 0.3469(24) 0.0605(11) 0.127(11) Uani 0.50 d P . O60 O 0.3480(10) 0.1763(7) 0.3175(5) 0.110(2) Uani 1 d . . O50 O 0.4377(27) 0.1913(16) 0.4939(16) 0.352(12) Uani 1 d . . O20A O 0.5255(20) 0.2003(19) -0.0473(9) 0.087(5) Uani 0.50 d P . O23A O 0.4119(23) 0.2186(29) 0.0719(13) 0.143(8) Uani 0.50 d P . O22A O 0.4192(30) 0.3708(16) 0.0007(24) 0.172(12) Uani 0.50 d P . 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6A Ru1 N5A 77.0(2) . . ? N6A Ru1 N1A 99.4(2) . . ? N5A Ru1 N1A 89.5(2) . . ? N6A Ru1 N4A 89.5(2) . . ? N5A Ru1 N4A 98.4(2) . . ? N1A Ru1 N4A 169.2(2) . . ? N6A Ru1 N3A 94.1(2) . . ? N5A Ru1 N3A 170.7(2) . . ? N1A Ru1 N3A 94.5(2) . . ? N4A Ru1 N3A 78.7(2) . . ? N6A Ru1 N2A 176.4(2) . . ? N5A Ru1 N2A 100.1(2) . . ? N1A Ru1 N2A 78.3(2) . . ? N4A Ru1 N2A 93.1(2) . . ? N3A Ru1 N2A 88.9(2) . . ? O1 C1 C2 122.6(5) . . ? O1 C1 C3 122.4(5) . 2 ? C2 C1 C3 115.0(5) . 2 ? N6A C2 C3 113.4(5) . . ? N6A C2 C1 123.4(5) . . ? C3 C2 C1 123.1(5) . . ? N5A C3 C2 114.2(5) . . ? N5A C3 C1 124.1(5) . 2 ? C2 C3 C1 121.7(5) . 2 ? C10A N1A C14A 118.3(6) . . ? C10A N1A Ru1 125.5(4) . . ? C14A N1A Ru1 116.2(5) . . ? N1A C10A C11A 123.6(7) . . ? C12A C11A C10A 118.0(8) . . ? C11A C12A C13A 119.7(7) . . ? C12A C13A C14A 120.1(7) . . ? N1A C14A C13A 120.2(8) . . ? N1A C14A C24A 115.1(6) . . ? C13A C14A C24A 124.7(6) . . ? C20A N2A C24A 118.3(6) . . ? C20A N2A Ru1 126.0(5) . . ? C24A N2A Ru1 115.4(5) . . ? N2A C20A C21A 121.6(8) . . ? C22A C21A C20A 119.5(9) . . ? C21A C22A C23A 119.9(8) . . ? C24A C23A C22A 118.3(8) . . ? N2A C24A C23A 122.4(8) . . ? N2A C24A C14A 114.7(6) . . ? C23A C24A C14A 122.9(7) . . ? C30A N3A C34A 120.1(6) . . ? C30A N3A Ru1 126.0(5) . . ? C34A N3A Ru1 113.8(4) . . ? N3A C30A C31A 122.1(8) . . ? C32A C31A C30A 117.9(9) . . ? C31A C32A C33A 121.6(8) . . ? C34A C33A C32A 117.7(9) . . ? N3A C34A C33A 120.6(8) . . ? N3A C34A C44A 116.0(6) . . ? C33A C34A C44A 123.4(7) . . ? C40A N4A C44A 118.5(6) . . ? C40A N4A Ru1 125.6(4) . . ? C44A N4A Ru1 115.9(5) . . ? N4A C40A C41A 122.7(7) . . ? C42A C41A C40A 118.5(8) . . ? C41A C42A C43A 120.1(8) . . ? C42A C43A C44A 119.7(8) . . ? N4A C44A C43A 120.5(7) . . ? N4A C44A C34A 114.7(6) . . ? C43A C44A C34A 124.8(7) . . ? C3 N5A Ru1 117.1(4) . . ? C2 N6A Ru1 118.2(4) . . ? O13 Cl1 O10 110.9(8) . . ? O13 Cl1 O12 112.6(9) . . ? O10 Cl1 O12 104.0(8) . . ? O13 Cl1 O11 103.5(9) . . ? O10 Cl1 O11 117.3(12) . . ? O12 Cl1 O11 108.8(11) . . ? O23 Cl2 O22A 46.1(13) . . ? O23 Cl2 O20A 115.0(12) . . ? O22A Cl2 O20A 109.6(14) . . ? O23 Cl2 O21 121.9(10) . . ? O22A Cl2 O21 105.6(12) . . ? O20A Cl2 O21 122.9(7) . . ? O23 Cl2 O22 112.6(15) . . ? O22A Cl2 O22 75.9(15) . . ? O20A Cl2 O22 49.1(11) . . ? O21 Cl2 O22 101.4(12) . . ? O23 Cl2 O23A 62.9(13) . . ? O22A Cl2 O23A 108.0(16) . . ? O20A Cl2 O23A 108.6(13) . . ? O21 Cl2 O23A 101.1(7) . . ? O22 Cl2 O23A 155.0(15) . . ? O23 Cl2 O20 111.5(12) . . ? O22A Cl2 O20 150.1(14) . . ? O20A Cl2 O20 56.8(10) . . ? O21 Cl2 O20 103.7(7) . . ? O22 Cl2 O20 103.8(14) . . ? O23A Cl2 O20 60.2(12) . . ? O20A O20 O23A 109.2(14) . . ? O20A O20 Cl2 58.7(8) . . ? O23A O20 Cl2 59.0(10) . . ? O20A O22 Cl2 63.6(13) . . ? O20A O22 O22A 100.9(21) . . ? Cl2 O22 O22A 50.8(11) . . ? O22A O23 Cl2 67.3(13) . . ? O22A O23 O23A 126.6(20) . . ? Cl2 O23 O23A 60.8(11) . . ? O22 O20A O20 128.3(21) . . ? O22 O20A Cl2 67.3(13) . . ? O20 O20A Cl2 64.5(11) . . ? Cl2 O23A O20 60.8(9) . . ? Cl2 O23A O23 56.4(8) . . ? O20 O23A O23 106.7(14) . . ? O23 O22A Cl2 66.6(16) . . ? O23 O22A O22 110.3(24) . . ? Cl2 O22A O22 53.4(10) . . ? 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 Ru1 N6A 1.990(5) . ? Ru1 N5A 2.016(4) . ? Ru1 N1A 2.062(5) . ? Ru1 N4A 2.063(5) . ? Ru1 N3A 2.085(5) . ? Ru1 N2A 2.087(6) . ? C1 O1 1.209(7) . ? C1 C2 1.481(8) . ? C1 C3 1.484(7) 2 ? C2 N6A 1.295(7) . ? C2 C3 1.450(8) . ? C3 N5A 1.287(7) . ? C3 C1 1.484(7) 2 ? N1A C10A 1.335(9) . ? N1A C14A 1.362(8) . ? C10A C11A 1.372(9) . ? C11A C12A 1.368(11) . ? C12A C13A 1.370(12) . ? C13A C14A 1.382(10) . ? C14A C24A 1.470(10) . ? N2A C20A 1.328(9) . ? N2A C24A 1.361(8) . ? C20A C21A 1.381(11) . ? C21A C22A 1.358(13) . ? C22A C23A 1.371(13) . ? C23A C24A 1.367(11) . ? N3A C30A 1.332(9) . ? N3A C34A 1.370(9) . ? C30A C31A 1.387(10) . ? C31A C32A 1.352(13) . ? C32A C33A 1.408(14) . ? C33A C34A 1.378(10) . ? C34A C44A 1.461(11) . ? N4A C40A 1.346(9) . ? N4A C44A 1.359(8) . ? C40A C41A 1.384(10) . ? C41A C42A 1.357(13) . ? C42A C43A 1.373(13) . ? C43A C44A 1.389(11) . ? Cl1 O13 1.389(9) . ? Cl1 O10 1.397(10) . ? Cl1 O12 1.382(11) . ? Cl1 O11 1.50(2) . ? Cl2 O23 1.352(14) . ? Cl2 O22A 1.36(2) . ? Cl2 O20A 1.366(14) . ? Cl2 O21 1.407(6) . ? Cl2 O22 1.41(2) . ? Cl2 O23A 1.417(14) . ? Cl2 O20 1.442(14) . ? O20 O20A 1.34(2) . ? O20 O23A 1.43(3) . ? O22 O20A 1.15(3) . ? O22 O22A 1.70(3) . ? O23 O22A 1.06(3) . ? O23 O23A 1.45(3) . ? _journal_paper_doi 10.1021/ic980826q