# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1653 data_complex1 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84112074' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir, Please consider this CIF as a supplemetary data for the paper submitted to Dalton (Paper No. 9/07111C). Sincerely, Xiao-Ming Chen ; #============================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A novel three-dimensional hydrogen-bonded framework with triangular channels. Synthesis and structure of [Mn(4,4'-bpy)2(H2O)4](ClO4)2((4,4'-bpy)4 (4,4'-bpy = 4,4'-bipyridine) ; loop_ _publ_author_name _publ_author_address 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Lee, Hung Kay' ; Department of Chemistry The Chinese University of Hong Kong New Territories, Hong Kong P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Huang, Rong-Bin' ; Department of Chemistry The Chinese University of Hong Kong New Territories, Hong Kong P. R. China ; 'Mak, Thomas C. W.' ; Department of Chemistry The Chinese University of Hong Kong New Territories, Hong Kong P. R. China ; #============================================================ data_mn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H56 Cl2 Mn N12 O12' _chemical_formula_weight 1263.01 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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.822(2) _cell_length_b 14.306(3) _cell_length_c 14.919(3) _cell_angle_alpha 63.78(3) _cell_angle_beta 87.60(3) _cell_angle_gamma 81.30(3) _cell_volume 1479.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 655 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.862 _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 'Siemens P4' _diffrn_measurement_method psi-scan _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% none _diffrn_reflns_number 5447 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1416 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5219 _reflns_number_gt 2639 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCAN _computing_cell_refinement XSCAN _computing_data_reduction XSCAN _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 w=1/[\s^2^(Fo^2^)+(0.0412P)^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 SHELXL _refine_ls_extinction_coef 0.0086(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5219 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1501 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.008 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.5000 -0.5000 0.0422(3) Uani 1 d S . . N11 N 0.4118(4) 0.3576(2) -0.3730(2) 0.0460(8) Uani 1 d . . . N12 N 0.2428(5) -0.0985(3) 0.0567(3) 0.0691(11) Uani 1 d . . . O1W O 0.4211(4) 0.59230(18) -0.41620(17) 0.0544(7) Uani 1 d . . . H1WA H 0.4253 0.6569 -0.4173 0.050 Uiso 1 d R . . H1WB H 0.3720 0.5702 -0.3502 0.050 Uiso 1 d R . . O2W O 0.2426(3) 0.54728(18) -0.56942(17) 0.0529(7) Uani 1 d . . . H2WA H 0.1819 0.5890 -0.5722 0.050 Uiso 1 d R . . H2WB H 0.2435 0.5445 -0.6341 0.050 Uiso 1 d R . . C10 C 0.2693(5) 0.3587(3) -0.3219(3) 0.0513(11) Uani 1 d . . . H10A H 0.1882 0.4227 -0.3458 0.080 Uiso 1 d R . . C11 C 0.2319(5) 0.2731(3) -0.2372(3) 0.0533(11) Uani 1 d . . . H11A H 0.1294 0.2786 -0.2010 0.080 Uiso 1 d R . . C12 C 0.3426(5) 0.1781(3) -0.2033(3) 0.0443(10) Uani 1 d . . . C13 C 0.4885(6) 0.1766(3) -0.2579(3) 0.0523(11) Uani 1 d . . . H13A H 0.5697 0.1130 -0.2378 0.080 Uiso 1 d R . . C14 C 0.5184(5) 0.2664(3) -0.3405(3) 0.0555(12) Uani 1 d . . . H14A H 0.6206 0.2636 -0.3777 0.080 Uiso 1 d R . . C15 C 0.3067(5) 0.0830(3) -0.1127(3) 0.0465(10) Uani 1 d . . . C16 C 0.2113(6) 0.0897(3) -0.0355(3) 0.0581(11) Uani 1 d . . . H16A H 0.1667 0.1572 -0.0382 0.080 Uiso 1 d R . . C17 C 0.1814(6) -0.0022(4) 0.0466(3) 0.0681(13) Uani 1 d . . . H17A H 0.1127 0.0031 0.0994 0.080 Uiso 1 d R . . C18 C 0.3730(6) -0.0172(3) -0.1026(3) 0.0575(11) Uani 1 d . . . H18A H 0.4428 -0.0253 -0.1539 0.080 Uiso 1 d R . . C19 C 0.3365(6) -0.1035(3) -0.0172(4) 0.0687(13) Uani 1 d . . . H19A H 0.3816 -0.1724 -0.0110 0.080 Uiso 1 d R . . N21 N 0.4098(5) 0.8015(3) -0.4315(3) 0.0675(11) Uani 1 d . . . N22 N -0.0359(5) 1.2627(3) -0.4115(3) 0.0598(10) Uani 1 d . . . C20 C 0.3329(6) 0.8848(3) -0.5111(3) 0.0707(14) Uani 1 d . . . H20A H 0.3361 0.8801 -0.5734 0.080 Uiso 1 d R . . C21 C 0.2530(6) 0.9765(3) -0.5100(3) 0.0621(12) Uani 1 d . . . H21A H 0.1986 1.0331 -0.5698 0.080 Uiso 1 d R . . C22 C 0.2470(5) 0.9874(3) -0.4228(3) 0.0475(10) Uani 1 d . . . C23 C 0.3304(6) 0.9025(3) -0.3394(3) 0.0647(13) Uani 1 d . . . H23A H 0.3334 0.9062 -0.2768 0.080 Uiso 1 d R . . C24 C 0.4071(6) 0.8137(3) -0.3481(4) 0.0699(13) Uani 1 d . . . H24A H 0.4615 0.7555 -0.2893 0.080 Uiso 1 d R . . C25 C 0.1564(5) 1.0826(3) -0.4171(3) 0.0481(10) Uani 1 d . . . C26 C 0.1405(6) 1.1813(3) -0.4999(3) 0.0657(13) Uani 1 d . . . H26A H 0.1942 1.1884 -0.5612 0.080 Uiso 1 d R . . C27 C 0.0474(6) 1.2669(3) -0.4930(3) 0.0698(14) Uani 1 d . . . H27A H 0.0413 1.3345 -0.5499 0.080 Uiso 1 d R . . C28 C 0.0717(5) 1.0782(3) -0.3324(3) 0.0546(11) Uani 1 d . . . H28A H 0.0780 1.0121 -0.2736 0.080 Uiso 1 d R . . C29 C -0.0200(5) 1.1679(3) -0.3323(3) 0.0567(11) Uani 1 d . . . H29A H -0.0774 1.1631 -0.2726 0.080 Uiso 1 d R . . N31 N 0.2184(4) 0.5463(3) 0.2447(2) 0.0594(9) Uani 1 d . . . N32 N 0.2728(5) 0.5301(3) -0.2241(2) 0.0638(10) Uani 1 d . . . C30 C 0.2438(6) 0.4558(3) 0.2378(3) 0.0633(12) Uani 1 d . . . H30A H 0.2572 0.3922 0.2993 0.080 Uiso 1 d R . . C31 C 0.2487(6) 0.4475(3) 0.1492(3) 0.0563(11) Uani 1 d . . . H31A H 0.2672 0.3795 0.1495 0.080 Uiso 1 d R . . C32 C 0.2264(5) 0.5381(3) 0.0593(3) 0.0423(9) Uani 1 d . . . C33 C 0.1964(5) 0.6331(3) 0.0662(3) 0.0514(11) Uani 1 d . . . H33A H 0.1768 0.6983 0.0064 0.080 Uiso 1 d R . . C34 C 0.1969(5) 0.6330(3) 0.1584(3) 0.0593(12) Uani 1 d . . . H34A H 0.1788 0.6995 0.1612 0.080 Uiso 1 d R . . C35 C 0.2379(5) 0.5333(3) -0.0378(3) 0.0448(10) Uani 1 d . . . C36 C 0.3258(6) 0.4471(3) -0.0471(3) 0.0566(11) Uani 1 d . . . H36A H 0.3750 0.3862 0.0112 0.080 Uiso 1 d R . . C37 C 0.3396(6) 0.4493(3) -0.1410(3) 0.0649(13) Uani 1 d . . . H37A H 0.4034 0.3893 -0.1465 0.080 Uiso 1 d R . . C38 C 0.1655(6) 0.6175(3) -0.1249(3) 0.0615(12) Uani 1 d . . . H38A H 0.1034 0.6795 -0.1224 0.080 Uiso 1 d R . . C39 C 0.1864(6) 0.6110(4) -0.2136(3) 0.0674(13) Uani 1 d . . . H39A H 0.1338 0.6693 -0.2728 0.080 Uiso 1 d R . . Cl1 Cl 0.21411(18) 0.15264(8) 0.19652(9) 0.0716(4) Uani 1 d . . . O1 O 0.2799(4) 0.0433(2) 0.2489(2) 0.0775(10) Uani 1 d . . . O2 O 0.3468(6) 0.2047(3) 0.1356(3) 0.1193(16) Uani 1 d . . . O3 O 0.1657(5) 0.1967(2) 0.2643(2) 0.0885(11) Uani 1 d . . . O4 O 0.0669(6) 0.1657(3) 0.1364(3) 0.1301(17) Uani 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 0.0617(6) 0.0291(4) 0.0293(5) -0.0093(4) 0.0004(4) 0.0007(4) N11 0.061(2) 0.0302(17) 0.0389(18) -0.0105(14) 0.0038(17) 0.0000(16) N12 0.075(3) 0.059(3) 0.052(2) -0.002(2) 0.001(2) -0.019(2) O1W 0.088(2) 0.0372(14) 0.0392(15) -0.0203(12) 0.0091(14) -0.0042(14) O2W 0.069(2) 0.0446(15) 0.0420(15) -0.0211(13) -0.0046(14) 0.0090(13) C10 0.053(3) 0.040(2) 0.054(3) -0.015(2) 0.004(2) -0.004(2) C11 0.057(3) 0.043(2) 0.053(3) -0.015(2) 0.009(2) -0.008(2) C12 0.056(3) 0.036(2) 0.039(2) -0.0137(18) 0.001(2) -0.0083(19) C13 0.064(3) 0.033(2) 0.046(2) -0.0076(19) 0.006(2) -0.0007(19) C14 0.068(3) 0.037(2) 0.043(2) -0.0069(19) 0.015(2) 0.004(2) C15 0.049(3) 0.042(2) 0.044(2) -0.0143(19) -0.003(2) -0.0086(19) C16 0.068(3) 0.051(3) 0.050(3) -0.015(2) 0.012(2) -0.018(2) C17 0.078(3) 0.067(3) 0.051(3) -0.015(2) 0.013(2) -0.025(3) C18 0.072(3) 0.043(2) 0.051(3) -0.014(2) 0.009(2) -0.013(2) C19 0.076(3) 0.043(3) 0.070(3) -0.009(2) -0.003(3) -0.009(2) N21 0.087(3) 0.042(2) 0.073(3) -0.029(2) 0.003(2) 0.0014(19) N22 0.067(3) 0.046(2) 0.062(2) -0.0232(19) 0.000(2) 0.0018(18) C20 0.104(4) 0.049(3) 0.060(3) -0.029(2) 0.005(3) 0.002(3) C21 0.086(4) 0.044(2) 0.052(3) -0.022(2) 0.002(2) 0.003(2) C22 0.050(3) 0.037(2) 0.055(3) -0.021(2) -0.001(2) -0.0028(19) C23 0.082(3) 0.053(3) 0.058(3) -0.027(2) -0.008(2) 0.005(2) C24 0.085(4) 0.043(3) 0.070(3) -0.019(2) -0.010(3) 0.010(2) C25 0.053(3) 0.043(2) 0.050(2) -0.023(2) -0.002(2) -0.0034(19) C26 0.083(4) 0.051(3) 0.059(3) -0.023(2) 0.020(2) -0.005(2) C27 0.091(4) 0.043(2) 0.064(3) -0.019(2) 0.018(3) 0.006(2) C28 0.063(3) 0.049(2) 0.052(3) -0.023(2) -0.001(2) -0.005(2) C29 0.066(3) 0.058(3) 0.052(3) -0.032(2) 0.003(2) -0.001(2) N31 0.066(3) 0.067(2) 0.051(2) -0.032(2) -0.0016(18) -0.0030(19) N32 0.081(3) 0.068(2) 0.043(2) -0.026(2) 0.0051(19) -0.008(2) C30 0.092(4) 0.051(3) 0.040(2) -0.014(2) 0.008(2) -0.013(2) C31 0.083(3) 0.047(2) 0.043(2) -0.023(2) 0.004(2) -0.014(2) C32 0.039(2) 0.043(2) 0.043(2) -0.0178(19) 0.0005(18) -0.0051(18) C33 0.066(3) 0.047(2) 0.041(2) -0.0216(19) 0.001(2) -0.001(2) C34 0.071(3) 0.051(3) 0.059(3) -0.029(2) 0.001(2) -0.001(2) C35 0.048(3) 0.042(2) 0.042(2) -0.0159(19) 0.0065(19) -0.0087(19) C36 0.077(3) 0.048(2) 0.043(2) -0.020(2) -0.001(2) -0.003(2) C37 0.081(4) 0.063(3) 0.057(3) -0.033(3) 0.003(3) -0.004(3) C38 0.077(3) 0.055(3) 0.045(3) -0.021(2) -0.004(2) 0.009(2) C39 0.084(4) 0.067(3) 0.043(3) -0.020(2) -0.004(2) 0.000(3) Cl1 0.1070(11) 0.0384(6) 0.0557(7) -0.0150(5) -0.0016(7) 0.0107(6) O1 0.096(2) 0.0376(16) 0.079(2) -0.0139(15) 0.0091(18) 0.0088(16) O2 0.179(4) 0.055(2) 0.108(3) -0.022(2) 0.073(3) -0.033(2) O3 0.139(3) 0.0542(19) 0.064(2) -0.0281(17) -0.004(2) 0.0166(19) O4 0.152(4) 0.112(3) 0.134(3) -0.080(3) -0.079(3) 0.066(3) _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 O2W 2.174(3) . ? Mn1 O2W 2.174(3) 2_664 ? Mn1 O1W 2.199(2) 2_664 ? Mn1 O1W 2.199(2) . ? Mn1 N11 2.263(3) 2_664 ? Mn1 N11 2.263(3) . ? N11 C10 1.326(5) . ? N11 C14 1.334(4) . ? N12 C19 1.320(5) . ? N12 C17 1.331(5) . ? O1W N32 2.852(4) . ? O1W N21 2.888(4) . ? O2W N31 2.794(4) 1_554 ? O2W N22 2.847(4) 2_574 ? C10 C11 1.376(5) . ? C11 C12 1.387(5) . ? C12 C13 1.377(5) . ? C12 C15 1.489(5) . ? C13 C14 1.375(5) . ? C15 C16 1.377(5) . ? C15 C18 1.392(5) . ? C16 C17 1.389(5) . ? C18 C19 1.385(6) . ? N21 C24 1.329(5) . ? N21 C20 1.336(5) . ? N22 C27 1.338(5) . ? N22 C29 1.339(5) . ? C20 C21 1.372(5) . ? C21 C22 1.376(5) . ? C22 C23 1.393(5) . ? C22 C25 1.473(5) . ? C23 C24 1.379(5) . ? C25 C28 1.383(5) . ? C25 C26 1.397(5) . ? C26 C27 1.370(5) . ? C28 C29 1.373(5) . ? N31 C34 1.329(5) . ? N31 C30 1.329(5) . ? N32 C39 1.317(5) . ? N32 C37 1.323(5) . ? C30 C31 1.377(5) . ? C31 C32 1.387(5) . ? C32 C33 1.391(5) . ? C32 C35 1.479(5) . ? C33 C34 1.376(5) . ? C35 C36 1.378(5) . ? C35 C38 1.390(5) . ? C36 C37 1.388(5) . ? C38 C39 1.368(5) . ? Cl1 O2 1.419(4) . ? Cl1 O3 1.422(3) . ? Cl1 O1 1.425(3) . ? Cl1 O4 1.428(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 O2W Mn1 O2W 180.0 . 2_664 ? O2W Mn1 O1W 90.79(10) . 2_664 ? O2W Mn1 O1W 89.21(10) 2_664 2_664 ? O2W Mn1 O1W 89.21(10) . . ? O2W Mn1 O1W 90.79(10) 2_664 . ? O1W Mn1 O1W 180.0 2_664 . ? O2W Mn1 N11 89.61(11) . 2_664 ? O2W Mn1 N11 90.39(11) 2_664 2_664 ? O1W Mn1 N11 89.39(10) 2_664 2_664 ? O1W Mn1 N11 90.61(10) . 2_664 ? O2W Mn1 N11 90.39(11) . . ? O2W Mn1 N11 89.61(11) 2_664 . ? O1W Mn1 N11 90.61(10) 2_664 . ? O1W Mn1 N11 89.39(10) . . ? N11 Mn1 N11 180.0 2_664 . ? C10 N11 C14 116.5(3) . . ? C10 N11 Mn1 125.5(2) . . ? C14 N11 Mn1 117.7(3) . . ? C19 N12 C17 116.2(4) . . ? Mn1 O1W N32 129.88(13) . . ? Mn1 O1W N21 141.17(13) . . ? N32 O1W N21 88.95(13) . . ? Mn1 O2W N31 115.86(12) . 1_554 ? Mn1 O2W N22 120.70(12) . 2_574 ? N31 O2W N22 105.70(13) 1_554 2_574 ? N11 C10 C11 123.4(4) . . ? C10 C11 C12 120.1(4) . . ? C13 C12 C11 116.4(3) . . ? C13 C12 C15 121.6(3) . . ? C11 C12 C15 122.0(4) . . ? C12 C13 C14 120.0(3) . . ? N11 C14 C13 123.6(4) . . ? C16 C15 C18 117.5(4) . . ? C16 C15 C12 122.2(3) . . ? C18 C15 C12 120.2(4) . . ? C15 C16 C17 119.3(4) . . ? N12 C17 C16 123.7(4) . . ? C19 C18 C15 118.3(4) . . ? N12 C19 C18 124.9(4) . . ? C24 N21 C20 114.8(4) . . ? C24 N21 O1W 118.8(3) . . ? C20 N21 O1W 119.9(3) . . ? C27 N22 C29 115.9(3) . . ? N21 C20 C21 124.5(4) . . ? C20 C21 C22 120.3(4) . . ? C21 C22 C23 116.1(4) . . ? C21 C22 C25 122.2(4) . . ? C23 C22 C25 121.7(4) . . ? C24 C23 C22 119.2(4) . . ? N21 C24 C23 125.1(4) . . ? C28 C25 C26 116.4(4) . . ? C28 C25 C22 122.0(4) . . ? C26 C25 C22 121.5(4) . . ? C27 C26 C25 119.6(4) . . ? N22 C27 C26 124.1(4) . . ? C29 C28 C25 120.1(4) . . ? N22 C29 C28 123.9(4) . . ? C34 N31 C30 115.7(4) . . ? C39 N32 C37 116.0(4) . . ? C39 N32 O1W 112.0(3) . . ? C37 N32 O1W 124.9(3) . . ? N31 C30 C31 124.5(4) . . ? C30 C31 C32 119.7(4) . . ? C31 C32 C33 116.1(3) . . ? C31 C32 C35 121.6(3) . . ? C33 C32 C35 122.3(3) . . ? C34 C33 C32 119.8(4) . . ? N31 C34 C33 124.2(4) . . ? C36 C35 C38 116.8(4) . . ? C36 C35 C32 121.9(3) . . ? C38 C35 C32 121.3(3) . . ? C35 C36 C37 119.2(4) . . ? N32 C37 C36 123.9(4) . . ? C39 C38 C35 119.1(4) . . ? N32 C39 C38 124.9(4) . . ? O2 Cl1 O3 108.8(2) . . ? O2 Cl1 O1 108.1(2) . . ? O3 Cl1 O1 110.90(19) . . ? O2 Cl1 O4 110.4(3) . . ? O3 Cl1 O4 109.4(2) . . ? O1 Cl1 O4 109.3(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.052 #_eof #End of Crystallographic Information File