# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Zhang, Jie' _publ_contact_author_email zhangjie@fjirsm.ac.cn _publ_section_title ; Conformational and photosensitive adjustment based on the self-assembly of the photochromic 4,4'-bipyridinium and Mn(II) ions ; _publ_author_name 'Jie Zhang' # Attachment '- 1-JXH.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 765400' #TrackingRef '- 1-JXH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H70 Cl2 Mn N6 O28' _chemical_formula_sum 'C54 H70 Cl2 Mn N6 O28' _chemical_formula_weight 1377.00 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 18.076(6) _cell_length_b 18.275(6) _cell_length_c 18.908(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6246(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5147 _cell_measurement_theta_min 2.4254 _cell_measurement_theta_max 27.4217 _exptl_crystal_description flake _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1800 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_absorpt_coefficient_mu 0.388 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8094 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(R.H. Blessing, 1995&1997)' _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 'CCD area detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49522 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.45 _reflns_number_total 14232 _reflns_number_gt 10771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1748P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(3) _refine_ls_number_reflns 14232 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2647 _refine_ls_wR_factor_gt 0.2361 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _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 0.25600(4) 0.24728(3) 0.25124(3) 0.02520(17) Uani 1 1 d . . . Cl1 Cl 0.46848(10) 0.67759(12) 0.09428(10) 0.0651(5) Uani 1 1 d . . . Cl2 Cl 0.52547(10) 0.37428(9) 0.17255(9) 0.0533(4) Uani 1 1 d . . . O1 O 0.3274(2) -0.5803(2) 0.3780(3) 0.0475(11) Uani 1 1 d . . . O2 O 0.2060(2) -0.5638(2) 0.3637(2) 0.0431(9) Uani 1 1 d . . . O3 O 0.2879(2) 1.0651(2) 0.1313(3) 0.0533(12) Uani 1 1 d . . . O4 O 0.1674(3) 1.0662(2) 0.1547(2) 0.0491(11) Uani 1 1 d . . . O5 O 0.9848(3) 0.5214(3) 0.1488(2) 0.0521(11) Uani 1 1 d . . . O6 O 0.9870(3) 0.6380(2) 0.1133(2) 0.0527(11) Uani 1 1 d . . . O7 O 0.3996(3) 0.7098(3) 0.1105(3) 0.0640(13) Uani 1 1 d . . . O8 O 0.5256(4) 0.7212(4) 0.1060(6) 0.137(4) Uani 1 1 d . . . O9 O 0.4631(5) 0.6542(5) 0.0172(4) 0.119(3) Uani 1 1 d . . . O10 O 0.4779(4) 0.6098(3) 0.1295(3) 0.089(2) Uani 1 1 d . . . O11 O 0.4784(3) 0.3362(4) 0.2207(3) 0.0808(17) Uani 1 1 d . . . O12 O 0.5324(4) 0.3320(3) 0.1089(3) 0.0806(17) Uani 1 1 d . . . O13 O 0.5982(3) 0.3829(3) 0.2024(3) 0.0721(15) Uani 1 1 d . . . O14 O 0.4947(3) 0.4443(3) 0.1548(3) 0.0673(14) Uani 1 1 d . . . N1 N 0.2632(2) 0.1396(2) 0.31442(19) 0.0287(8) Uani 1 1 d . . . N2 N 0.2886(3) -0.2000(2) 0.4903(2) 0.0338(9) Uani 1 1 d . . . N3 N 0.2481(2) 0.35515(19) 0.1896(2) 0.0290(8) Uani 1 1 d . . . N4 N 0.2076(3) 0.6962(2) 0.0183(2) 0.0294(9) Uani 1 1 d . . . N5 N 1.0242(3) 0.4275(3) -0.2087(2) 0.0391(10) Uani 1 1 d . . . N6 N 1.3446(5) 0.2211(4) -0.2747(4) 0.078(2) Uani 1 1 d . . . C1 C 0.2032(3) 0.0990(3) 0.3285(3) 0.0328(11) Uani 1 1 d . . . H1 H 0.1561 0.1179 0.3157 0.039 Uiso 1 1 calc R . . C2 C 0.3288(3) 0.1126(3) 0.3337(3) 0.0315(10) Uani 1 1 d . . . H2 H 0.3717 0.1412 0.3247 0.038 Uiso 1 1 calc R . . C3 C 0.2061(3) 0.0309(3) 0.3606(3) 0.0355(11) Uani 1 1 d . . . H3 H 0.1622 0.0039 0.3692 0.043 Uiso 1 1 calc R . . C4 C 0.3378(3) 0.0450(3) 0.3660(3) 0.0341(11) Uani 1 1 d . . . H4 H 0.3858 0.0280 0.3784 0.041 Uiso 1 1 calc R . . C5 C 0.2760(3) 0.0026(2) 0.3802(2) 0.0297(10) Uani 1 1 d . . . C6 C 0.2815(3) -0.0690(2) 0.4163(3) 0.0314(10) Uani 1 1 d . . . C7 C 0.2286(4) -0.1232(3) 0.4071(3) 0.0448(13) Uani 1 1 d . . . H5 H 0.1891 -0.1154 0.3748 0.054 Uiso 1 1 calc R . . C8 C 0.3393(4) -0.0830(3) 0.4637(3) 0.0387(12) Uani 1 1 d . . . H6 H 0.3767 -0.0473 0.4714 0.046 Uiso 1 1 calc R . . C9 C 0.2323(4) -0.1882(3) 0.4442(3) 0.0476(15) Uani 1 1 d . . . H7 H 0.1955 -0.2247 0.4375 0.057 Uiso 1 1 calc R . . C10 C 0.3415(4) -0.1496(3) 0.4993(3) 0.0387(12) Uani 1 1 d . . . H8 H 0.3814 -0.1595 0.5307 0.046 Uiso 1 1 calc R . . C11 C 0.2897(4) -0.2678(2) 0.5365(3) 0.0404(13) Uani 1 1 d . . . H10 H 0.3362 -0.2684 0.5641 0.048 Uiso 1 1 calc R . . H9 H 0.2481 -0.2652 0.5704 0.048 Uiso 1 1 calc R . . C12 C 0.2839(4) -0.3376(2) 0.4952(3) 0.0350(12) Uani 1 1 d . . . C13 C 0.2150(4) -0.3657(3) 0.4763(3) 0.0412(13) Uani 1 1 d . . . H11 H 0.1712 -0.3394 0.4874 0.049 Uiso 1 1 calc R . . C14 C 0.3478(3) -0.3773(3) 0.4795(3) 0.0369(12) Uani 1 1 d . . . H12 H 0.3949 -0.3588 0.4927 0.044 Uiso 1 1 calc R . . C15 C 0.2107(3) -0.4331(3) 0.4407(3) 0.0368(11) Uani 1 1 d . . . H13 H 0.1638 -0.4522 0.4276 0.044 Uiso 1 1 calc R . . C16 C 0.3422(3) -0.4446(3) 0.4444(3) 0.0347(11) Uani 1 1 d . . . H14 H 0.3859 -0.4716 0.4344 0.042 Uiso 1 1 calc R . . C17 C 0.2750(3) -0.4722(2) 0.4243(3) 0.0310(10) Uani 1 1 d . . . C18 C 0.2694(3) -0.5451(2) 0.3860(3) 0.0333(11) Uani 1 1 d . . . C19 C 0.1807(3) 0.3873(3) 0.1794(3) 0.0322(10) Uani 1 1 d . . . H15 H 0.1378 0.3616 0.1943 0.039 Uiso 1 1 calc R . . C20 C 0.3062(3) 0.3927(3) 0.1670(3) 0.0324(11) Uani 1 1 d . . . H16 H 0.3535 0.3710 0.1731 0.039 Uiso 1 1 calc R . . C21 C 0.1720(3) 0.4545(3) 0.1488(3) 0.0323(11) Uani 1 1 d . . . H17 H 0.1239 0.4747 0.1434 0.039 Uiso 1 1 calc R . . C22 C 0.3037(3) 0.4612(3) 0.1351(3) 0.0370(12) Uani 1 1 d . . . H18 H 0.3476 0.4852 0.1202 0.044 Uiso 1 1 calc R . . C23 C 0.2337(3) 0.4937(2) 0.1256(3) 0.0296(10) Uani 1 1 d . . . C24 C 0.2264(3) 0.5665(3) 0.0914(3) 0.0311(10) Uani 1 1 d . . . C25 C 0.1634(3) 0.6075(3) 0.0997(3) 0.0423(13) Uani 1 1 d . . . H19 H 0.1255 0.5912 0.1307 0.051 Uiso 1 1 calc R . . C26 C 0.2820(3) 0.5936(3) 0.0474(3) 0.0386(12) Uani 1 1 d . . . H20 H 0.3270 0.5673 0.0417 0.046 Uiso 1 1 calc R . . C27 C 0.1549(4) 0.6729(3) 0.0630(3) 0.0439(13) Uani 1 1 d . . . H21 H 0.1114 0.7014 0.0695 0.053 Uiso 1 1 calc R . . C28 C 0.2710(3) 0.6593(3) 0.0121(3) 0.0393(12) Uani 1 1 d . . . H22 H 0.3093 0.6784 -0.0170 0.047 Uiso 1 1 calc R . . C29 C 0.1958(3) 0.7638(3) -0.0247(3) 0.0361(12) Uani 1 1 d . . . H23 H 0.1458 0.7621 -0.0460 0.043 Uiso 1 1 calc R . . H24 H 0.2322 0.7647 -0.0638 0.043 Uiso 1 1 calc R . . C30 C 0.2031(3) 0.8334(2) 0.0179(3) 0.0308(10) Uani 1 1 d . . . C31 C 0.2727(3) 0.8640(3) 0.0291(3) 0.0381(12) Uani 1 1 d . . . H26 H 0.3156 0.8399 0.0117 0.046 Uiso 1 1 calc R . . C32 C 0.1405(3) 0.8686(3) 0.0433(3) 0.0382(12) Uani 1 1 d . . . H25 H 0.0930 0.8478 0.0358 0.046 Uiso 1 1 calc R . . C33 C 0.1473(3) 0.9343(3) 0.0799(3) 0.0358(11) Uani 1 1 d . . . H27 H 0.1045 0.9582 0.0977 0.043 Uiso 1 1 calc R . . C34 C 0.2796(3) 0.9296(3) 0.0655(3) 0.0389(12) Uani 1 1 d . . . H28 H 0.3273 0.9498 0.0732 0.047 Uiso 1 1 calc R . . C35 C 0.2184(3) 0.9657(3) 0.0906(3) 0.0320(10) Uani 1 1 d . . . C36 C 0.2250(3) 1.0378(3) 0.1283(3) 0.0363(12) Uani 1 1 d . . . C37 C 1.2775(5) 0.1963(5) -0.2922(4) 0.072(2) Uani 1 1 d . . . H29 H 1.2732 0.1499 -0.3145 0.087 Uiso 1 1 calc R . . C38 C 1.3490(4) 0.2848(5) -0.2397(4) 0.068(2) Uani 1 1 d . . . H30 H 1.3961 0.3013 -0.2239 0.081 Uiso 1 1 calc R . . C39 C 1.2147(5) 0.2360(5) -0.2788(3) 0.0633(19) Uani 1 1 d . . . H31 H 1.1677 0.2170 -0.2917 0.076 Uiso 1 1 calc R . . C40 C 1.2863(4) 0.3280(5) -0.2255(4) 0.066(2) Uani 1 1 d . . . H32 H 1.2910 0.3735 -0.2016 0.079 Uiso 1 1 calc R . . C41 C 1.2200(4) 0.3040(4) -0.2464(3) 0.0574(17) Uani 1 1 d . . . C42 C 1.1509(4) 0.3491(4) -0.2323(3) 0.0499(15) Uani 1 1 d . . . C43 C 1.0840(4) 0.3142(4) -0.2199(4) 0.0548(16) Uani 1 1 d . . . H33 H 1.0819 0.2623 -0.2180 0.066 Uiso 1 1 calc R . . C44 C 1.1516(4) 0.4243(4) -0.2327(3) 0.0457(14) Uani 1 1 d . . . H34 H 1.1966 0.4497 -0.2411 0.055 Uiso 1 1 calc R . . C45 C 1.0885(3) 0.4623(3) -0.2212(3) 0.0383(12) Uani 1 1 d . . . H36 H 1.0896 0.5142 -0.2220 0.046 Uiso 1 1 calc R . . C46 C 1.0196(5) 0.3554(4) -0.2103(4) 0.0567(17) Uani 1 1 d . . . H35 H 0.9731 0.3318 -0.2048 0.068 Uiso 1 1 calc R . . C47 C 0.9580(3) 0.4702(4) -0.1899(3) 0.0452(13) Uani 1 1 d . . . H37 H 0.9134 0.4391 -0.1953 0.054 Uiso 1 1 calc R . . H38 H 0.9531 0.5123 -0.2225 0.054 Uiso 1 1 calc R . . C48 C 0.9627(3) 0.4975(3) -0.1147(3) 0.0380(11) Uani 1 1 d . . . C49 C 0.9521(3) 0.4501(3) -0.0604(3) 0.0423(13) Uani 1 1 d . . . H39 H 0.9403 0.4005 -0.0702 0.051 Uiso 1 1 calc R . . C50 C 0.9804(3) 0.5710(3) -0.1008(3) 0.0420(13) Uani 1 1 d . . . H40 H 0.9888 0.6044 -0.1384 0.050 Uiso 1 1 calc R . . C51 C 0.9584(3) 0.4732(3) 0.0101(3) 0.0408(12) Uani 1 1 d . . . H41 H 0.9508 0.4392 0.0474 0.049 Uiso 1 1 calc R . . C52 C 0.9853(4) 0.5936(3) -0.0309(3) 0.0442(13) Uani 1 1 d . . . H42 H 0.9956 0.6435 -0.0212 0.053 Uiso 1 1 calc R . . C53 C 0.9756(3) 0.5455(3) 0.0255(3) 0.0414(12) Uani 1 1 d . . . C54 C 0.9823(3) 0.5700(3) 0.1012(3) 0.0450(13) Uani 1 1 d . . . O1W O 0.3304(2) 0.19260(18) 0.17770(18) 0.0312(7) Uani 1 1 d . . . O2W O 0.3472(2) 0.29593(18) 0.31037(18) 0.0316(7) Uani 1 1 d . . . O3W O 0.1624(2) 0.20336(17) 0.19288(18) 0.0309(7) Uani 1 1 d . . . O4W O 0.1839(2) 0.29845(19) 0.3260(2) 0.0361(8) Uani 1 1 d . . . O5W O 0.0326(3) 0.2043(3) 0.2561(3) 0.0651(13) Uani 1 1 d . . . O6W O 0.0169(3) 0.8385(4) 0.2022(3) 0.0774(16) Uani 1 1 d . . . O7W O 0.0273(3) 1.0386(3) 0.2063(3) 0.0692(15) Uani 1 1 d . . . O8W O 0.4113(3) 0.2457(3) 0.0679(2) 0.0608(12) Uani 1 1 d . . . O9W O 0.4357(5) 0.2290(4) -0.0706(3) 0.104(3) Uani 1 1 d . . . O10W O 0.9910(6) 0.3732(4) 0.1554(4) 0.130(4) Uani 1 1 d . . . O11W O 0.8980(3) 0.7441(3) 0.0695(2) 0.0562(11) Uani 1 1 d . . . O12W O 0.9492(3) 0.9425(3) 0.1246(3) 0.0720(14) Uani 1 1 d . . . O13W O 0.9976(4) 1.1372(4) 0.0876(3) 0.089(2) Uani 1 1 d . . . O14W O 0.9755(5) 1.0163(4) -0.0053(3) 0.0891(19) Uani 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 0.0310(4) 0.0182(3) 0.0263(3) -0.0001(2) 0.0007(3) -0.0017(2) Cl1 0.0485(9) 0.0841(12) 0.0627(10) 0.0307(9) 0.0098(8) 0.0209(9) Cl2 0.0490(9) 0.0535(8) 0.0572(8) 0.0008(7) 0.0034(7) -0.0025(7) O1 0.034(2) 0.0294(18) 0.079(3) -0.0252(19) -0.001(2) 0.0028(16) O2 0.038(2) 0.0344(19) 0.057(2) -0.0106(18) -0.0037(19) 0.0015(17) O3 0.039(2) 0.036(2) 0.085(3) -0.032(2) 0.007(2) -0.0060(19) O4 0.046(2) 0.036(2) 0.066(3) -0.0219(19) 0.007(2) -0.0002(19) O5 0.064(3) 0.055(2) 0.037(2) 0.0048(19) 0.002(2) 0.006(2) O6 0.052(3) 0.051(3) 0.055(2) -0.013(2) 0.003(2) 0.004(2) O7 0.038(2) 0.089(4) 0.065(3) -0.005(3) -0.006(2) 0.014(3) O8 0.060(4) 0.076(4) 0.275(12) 0.026(6) -0.026(6) -0.005(4) O9 0.123(7) 0.162(7) 0.071(4) 0.017(4) 0.005(4) 0.065(6) O10 0.132(6) 0.060(3) 0.075(4) 0.007(3) 0.003(4) 0.034(4) O11 0.048(3) 0.110(5) 0.084(4) 0.030(3) 0.023(3) 0.006(3) O12 0.086(4) 0.069(3) 0.086(4) -0.025(3) 0.011(3) -0.017(3) O13 0.056(3) 0.071(3) 0.089(4) -0.010(3) -0.015(3) 0.002(3) O14 0.071(4) 0.060(3) 0.070(3) -0.001(2) -0.013(3) 0.009(3) N1 0.033(2) 0.0243(17) 0.0292(18) 0.0063(14) 0.0045(17) 0.0021(16) N2 0.048(3) 0.0246(18) 0.0290(19) -0.0001(15) 0.0010(19) 0.0039(19) N3 0.035(2) 0.0169(16) 0.0346(19) 0.0027(14) -0.0006(18) -0.0022(16) N4 0.037(2) 0.0166(16) 0.034(2) 0.0006(15) 0.0018(18) -0.0004(17) N5 0.041(3) 0.041(2) 0.035(2) -0.0035(18) 0.009(2) 0.000(2) N6 0.088(5) 0.086(5) 0.059(4) -0.023(3) 0.003(4) 0.024(4) C1 0.038(3) 0.022(2) 0.038(2) 0.0109(19) 0.006(2) 0.000(2) C2 0.034(3) 0.026(2) 0.034(2) -0.0002(18) 0.004(2) 0.000(2) C3 0.042(3) 0.027(2) 0.037(3) 0.004(2) 0.004(2) -0.004(2) C4 0.033(3) 0.028(2) 0.042(3) 0.003(2) 0.003(2) 0.003(2) C5 0.038(3) 0.0199(19) 0.031(2) 0.0021(17) 0.004(2) -0.0007(19) C6 0.036(3) 0.020(2) 0.039(2) 0.0001(18) 0.006(2) 0.003(2) C7 0.050(4) 0.033(2) 0.052(3) 0.002(2) -0.010(3) -0.004(3) C8 0.045(3) 0.027(2) 0.044(3) 0.003(2) 0.004(2) 0.000(2) C9 0.067(4) 0.034(3) 0.042(3) 0.000(2) 0.000(3) -0.009(3) C10 0.051(3) 0.032(2) 0.033(2) 0.003(2) -0.005(2) 0.007(2) C11 0.075(4) 0.019(2) 0.027(2) -0.0012(17) 0.003(3) 0.002(2) C12 0.056(3) 0.019(2) 0.031(2) 0.0019(17) 0.002(2) 0.000(2) C13 0.050(3) 0.031(3) 0.043(3) -0.004(2) 0.006(3) 0.011(2) C14 0.048(3) 0.023(2) 0.040(3) -0.005(2) -0.006(2) -0.001(2) C15 0.039(3) 0.027(2) 0.045(3) 0.004(2) 0.003(2) 0.000(2) C16 0.038(3) 0.027(2) 0.039(3) -0.008(2) 0.004(2) 0.007(2) C17 0.040(3) 0.0174(19) 0.035(2) -0.0004(17) 0.003(2) 0.0068(19) C18 0.041(3) 0.020(2) 0.039(2) -0.0061(18) -0.003(2) -0.004(2) C19 0.031(3) 0.024(2) 0.041(3) 0.009(2) -0.001(2) -0.0040(19) C20 0.029(3) 0.028(2) 0.040(3) 0.004(2) 0.004(2) -0.0043(19) C21 0.034(3) 0.023(2) 0.040(3) 0.0066(19) 0.001(2) -0.003(2) C22 0.040(3) 0.023(2) 0.047(3) 0.006(2) 0.004(2) -0.005(2) C23 0.030(3) 0.025(2) 0.034(2) -0.0038(18) 0.002(2) 0.0016(19) C24 0.034(3) 0.025(2) 0.035(2) 0.0001(18) 0.000(2) -0.004(2) C25 0.042(3) 0.029(2) 0.055(3) 0.010(2) 0.004(3) 0.000(2) C26 0.036(3) 0.036(3) 0.043(3) 0.013(2) -0.001(2) 0.002(2) C27 0.043(3) 0.028(2) 0.061(3) 0.004(2) 0.005(3) 0.002(2) C28 0.038(3) 0.034(3) 0.045(3) 0.012(2) 0.003(2) 0.000(2) C29 0.051(3) 0.021(2) 0.037(2) 0.0028(19) -0.008(2) -0.002(2) C30 0.040(3) 0.019(2) 0.033(2) 0.0001(17) -0.005(2) 0.0011(19) C31 0.038(3) 0.027(2) 0.049(3) -0.006(2) 0.005(2) 0.001(2) C32 0.038(3) 0.030(2) 0.047(3) -0.001(2) -0.009(2) -0.002(2) C33 0.030(3) 0.034(2) 0.043(3) -0.009(2) -0.008(2) -0.001(2) C34 0.034(3) 0.028(2) 0.055(3) -0.011(2) 0.000(3) -0.006(2) C35 0.031(3) 0.026(2) 0.039(2) -0.0062(19) -0.006(2) -0.003(2) C36 0.036(3) 0.027(2) 0.046(3) -0.010(2) -0.001(2) -0.004(2) C37 0.075(6) 0.078(5) 0.064(4) -0.016(4) -0.013(4) 0.018(5) C38 0.051(4) 0.094(6) 0.058(4) -0.018(4) -0.011(3) 0.008(4) C39 0.063(5) 0.083(5) 0.044(3) -0.017(3) -0.004(3) 0.019(4) C40 0.061(5) 0.092(5) 0.046(3) -0.021(3) -0.006(3) 0.028(4) C41 0.058(4) 0.073(4) 0.042(3) -0.005(3) 0.009(3) 0.022(4) C42 0.058(4) 0.056(3) 0.035(3) -0.002(2) -0.004(3) 0.005(3) C43 0.064(5) 0.046(3) 0.054(3) -0.003(3) 0.013(3) 0.007(3) C44 0.046(3) 0.053(3) 0.038(3) 0.001(2) 0.009(2) -0.003(3) C45 0.041(3) 0.038(3) 0.036(3) -0.001(2) 0.008(2) -0.002(2) C46 0.069(5) 0.046(3) 0.055(4) -0.014(3) 0.012(3) -0.015(3) C47 0.038(3) 0.056(3) 0.042(3) 0.000(3) 0.000(2) 0.000(3) C48 0.035(3) 0.039(3) 0.040(3) -0.003(2) 0.000(2) 0.004(2) C49 0.039(3) 0.046(3) 0.041(3) 0.000(2) 0.012(2) 0.005(3) C50 0.045(3) 0.036(3) 0.045(3) -0.003(2) 0.006(3) 0.002(2) C51 0.045(3) 0.038(3) 0.040(3) 0.005(2) 0.007(2) 0.003(2) C52 0.045(3) 0.037(3) 0.051(3) -0.003(2) 0.001(3) 0.002(2) C53 0.039(3) 0.048(3) 0.037(3) -0.006(2) 0.002(2) 0.007(3) C54 0.035(3) 0.050(3) 0.050(3) -0.008(3) 0.004(3) 0.004(3) O1W 0.0318(18) 0.0292(16) 0.0327(16) -0.0078(14) 0.0081(15) -0.0007(14) O2W 0.0334(19) 0.0252(16) 0.0361(17) -0.0049(13) -0.0033(15) 0.0001(14) O3W 0.0342(19) 0.0206(14) 0.0378(17) -0.0001(13) -0.0047(15) -0.0037(14) O4W 0.0328(19) 0.0289(16) 0.047(2) -0.0073(15) 0.0103(16) -0.0027(15) O5W 0.052(3) 0.084(3) 0.060(3) 0.014(3) 0.006(2) -0.002(3) O6W 0.065(3) 0.085(4) 0.082(4) -0.011(3) -0.003(3) 0.008(3) O7W 0.063(3) 0.087(4) 0.057(3) -0.004(3) 0.002(3) -0.026(3) O8W 0.071(3) 0.060(3) 0.051(2) 0.005(2) 0.017(2) -0.011(3) O9W 0.157(7) 0.084(4) 0.071(4) -0.007(3) 0.033(4) -0.021(5) O10W 0.231(11) 0.079(4) 0.079(4) 0.014(3) -0.050(6) -0.029(6) O11W 0.060(3) 0.055(3) 0.053(2) -0.002(2) 0.007(2) 0.018(2) O12W 0.054(3) 0.082(4) 0.080(4) 0.004(3) 0.000(3) 0.002(3) O13W 0.090(5) 0.097(5) 0.078(4) 0.022(3) 0.009(3) 0.019(4) O14W 0.105(5) 0.096(4) 0.066(4) 0.013(3) 0.015(3) -0.001(4) _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 O4W 2.138(4) . ? Mn1 O3W 2.173(3) . ? Mn1 O1W 2.177(3) . ? Mn1 O2W 2.181(4) . ? Mn1 N3 2.295(4) . ? Mn1 N1 2.305(4) . ? Cl1 O8 1.322(8) . ? Cl1 O7 1.410(5) . ? Cl1 O10 1.418(6) . ? Cl1 O9 1.522(8) . ? Cl2 O11 1.428(6) . ? Cl2 O14 1.435(6) . ? Cl2 O12 1.436(6) . ? Cl2 O13 1.440(6) . ? O1 C18 1.239(7) . ? O2 C18 1.269(7) . ? O3 C36 1.243(7) . ? O4 C36 1.266(7) . ? O5 C54 1.266(8) . ? O6 C54 1.268(8) . ? N1 C2 1.336(7) . ? N1 C1 1.340(7) . ? N2 C10 1.339(8) . ? N2 C9 1.356(8) . ? N2 C11 1.515(6) . ? N3 C20 1.325(6) . ? N3 C19 1.365(7) . ? N4 C28 1.336(7) . ? N4 C27 1.342(7) . ? N4 C29 1.495(6) . ? N5 C46 1.322(8) . ? N5 C45 1.346(7) . ? N5 C47 1.472(8) . ? N6 C37 1.337(12) . ? N6 C38 1.342(12) . ? C1 C3 1.384(7) . ? C1 H1 0.9500 . ? C2 C4 1.388(7) . ? C2 H2 0.9500 . ? C3 C5 1.414(8) . ? C3 H3 0.9500 . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 C6 1.481(6) . ? C6 C7 1.387(8) . ? C6 C8 1.400(8) . ? C7 C9 1.382(8) . ? C7 H5 0.9500 . ? C8 C10 1.392(7) . ? C8 H6 0.9500 . ? C9 H7 0.9500 . ? C10 H8 0.9500 . ? C11 C12 1.500(6) . ? C11 H10 0.9900 . ? C11 H9 0.9900 . ? C12 C13 1.393(9) . ? C12 C14 1.396(8) . ? C13 C15 1.407(7) . ? C13 H11 0.9500 . ? C14 C16 1.401(7) . ? C14 H12 0.9500 . ? C15 C17 1.398(7) . ? C15 H13 0.9500 . ? C16 C17 1.369(8) . ? C16 H14 0.9500 . ? C17 C18 1.520(6) . ? C19 C21 1.368(7) . ? C19 H15 0.9500 . ? C20 C22 1.390(7) . ? C20 H16 0.9500 . ? C21 C23 1.396(7) . ? C21 H17 0.9500 . ? C22 C23 1.409(8) . ? C22 H18 0.9500 . ? C23 C24 1.485(6) . ? C24 C25 1.372(8) . ? C24 C26 1.396(8) . ? C25 C27 1.392(7) . ? C25 H19 0.9500 . ? C26 C28 1.388(7) . ? C26 H20 0.9500 . ? C27 H21 0.9500 . ? C28 H22 0.9500 . ? C29 C30 1.510(6) . ? C29 H23 0.9900 . ? C29 H24 0.9900 . ? C30 C32 1.389(8) . ? C30 C31 1.392(8) . ? C31 C34 1.389(7) . ? C31 H26 0.9500 . ? C32 C33 1.392(7) . ? C32 H25 0.9500 . ? C33 C35 1.422(7) . ? C33 H27 0.9500 . ? C34 C35 1.371(8) . ? C34 H28 0.9500 . ? C35 C36 1.503(6) . ? C37 C39 1.370(11) . ? C37 H29 0.9500 . ? C38 C40 1.407(10) . ? C38 H30 0.9500 . ? C39 C41 1.390(10) . ? C39 H31 0.9500 . ? C40 C41 1.336(11) . ? C40 H32 0.9500 . ? C41 C42 1.518(9) . ? C42 C44 1.375(9) . ? C42 C43 1.388(10) . ? C43 C46 1.398(10) . ? C43 H33 0.9500 . ? C44 C45 1.353(9) . ? C44 H34 0.9500 . ? C45 H36 0.9500 . ? C46 H35 0.9500 . ? C47 C48 1.509(8) . ? C47 H37 0.9900 . ? C47 H38 0.9900 . ? C48 C49 1.357(8) . ? C48 C50 1.406(8) . ? C49 C51 1.401(8) . ? C49 H39 0.9500 . ? C50 C52 1.387(8) . ? C50 H40 0.9500 . ? C51 C53 1.388(8) . ? C51 H41 0.9500 . ? C52 C53 1.394(8) . ? C52 H42 0.9500 . ? C53 C54 1.504(8) . ? 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 O4W Mn1 O3W 91.32(14) . . ? O4W Mn1 O1W 178.16(15) . . ? O3W Mn1 O1W 89.24(14) . . ? O4W Mn1 O2W 86.76(14) . . ? O3W Mn1 O2W 177.44(14) . . ? O1W Mn1 O2W 92.74(14) . . ? O4W Mn1 N3 85.54(15) . . ? O3W Mn1 N3 90.62(14) . . ? O1W Mn1 N3 96.20(14) . . ? O2W Mn1 N3 87.55(14) . . ? O4W Mn1 N1 93.72(14) . . ? O3W Mn1 N1 89.52(14) . . ? O1W Mn1 N1 84.53(14) . . ? O2W Mn1 N1 92.28(14) . . ? N3 Mn1 N1 179.25(15) . . ? O8 Cl1 O7 113.6(5) . . ? O8 Cl1 O10 110.7(5) . . ? O7 Cl1 O10 111.6(4) . . ? O8 Cl1 O9 112.3(7) . . ? O7 Cl1 O9 105.6(4) . . ? O10 Cl1 O9 102.3(4) . . ? O11 Cl2 O14 110.7(4) . . ? O11 Cl2 O12 108.9(4) . . ? O14 Cl2 O12 108.5(4) . . ? O11 Cl2 O13 110.3(4) . . ? O14 Cl2 O13 110.4(3) . . ? O12 Cl2 O13 108.0(4) . . ? C2 N1 C1 117.3(4) . . ? C2 N1 Mn1 120.4(3) . . ? C1 N1 Mn1 122.1(3) . . ? C10 N2 C9 120.6(5) . . ? C10 N2 C11 118.7(5) . . ? C9 N2 C11 120.6(5) . . ? C20 N3 C19 116.0(4) . . ? C20 N3 Mn1 124.0(3) . . ? C19 N3 Mn1 119.7(3) . . ? C28 N4 C27 120.3(4) . . ? C28 N4 C29 119.5(4) . . ? C27 N4 C29 120.2(5) . . ? C46 N5 C45 121.4(6) . . ? C46 N5 C47 118.8(6) . . ? C45 N5 C47 119.7(5) . . ? C37 N6 C38 118.0(7) . . ? N1 C1 C3 123.7(5) . . ? N1 C1 H1 118.1 . . ? C3 C1 H1 118.1 . . ? N1 C2 C4 123.5(5) . . ? N1 C2 H2 118.2 . . ? C4 C2 H2 118.2 . . ? C1 C3 C5 118.5(5) . . ? C1 C3 H3 120.8 . . ? C5 C3 H3 120.8 . . ? C5 C4 C2 119.2(5) . . ? C5 C4 H4 120.4 . . ? C2 C4 H4 120.4 . . ? C4 C5 C3 117.7(4) . . ? C4 C5 C6 122.0(5) . . ? C3 C5 C6 120.3(4) . . ? C7 C6 C8 117.7(5) . . ? C7 C6 C5 121.8(5) . . ? C8 C6 C5 120.4(5) . . ? C9 C7 C6 121.1(6) . . ? C9 C7 H5 119.5 . . ? C6 C7 H5 119.5 . . ? C10 C8 C6 119.4(5) . . ? C10 C8 H6 120.3 . . ? C6 C8 H6 120.3 . . ? N2 C9 C7 120.0(6) . . ? N2 C9 H7 120.0 . . ? C7 C9 H7 120.0 . . ? N2 C10 C8 121.3(5) . . ? N2 C10 H8 119.4 . . ? C8 C10 H8 119.4 . . ? C12 C11 N2 113.3(4) . . ? C12 C11 H10 108.9 . . ? N2 C11 H10 108.9 . . ? C12 C11 H9 108.9 . . ? N2 C11 H9 108.9 . . ? H10 C11 H9 107.7 . . ? C13 C12 C14 119.6(4) . . ? C13 C12 C11 120.6(5) . . ? C14 C12 C11 119.7(5) . . ? C12 C13 C15 119.6(5) . . ? C12 C13 H11 120.2 . . ? C15 C13 H11 120.2 . . ? C12 C14 C16 119.8(5) . . ? C12 C14 H12 120.1 . . ? C16 C14 H12 120.1 . . ? C17 C15 C13 120.5(5) . . ? C17 C15 H13 119.8 . . ? C13 C15 H13 119.8 . . ? C17 C16 C14 121.2(5) . . ? C17 C16 H14 119.4 . . ? C14 C16 H14 119.4 . . ? C16 C17 C15 119.2(4) . . ? C16 C17 C18 120.9(5) . . ? C15 C17 C18 119.9(5) . . ? O1 C18 O2 125.7(4) . . ? O1 C18 C17 117.2(5) . . ? O2 C18 C17 117.1(5) . . ? N3 C19 C21 123.3(5) . . ? N3 C19 H15 118.4 . . ? C21 C19 H15 118.4 . . ? N3 C20 C22 125.5(5) . . ? N3 C20 H16 117.3 . . ? C22 C20 H16 117.3 . . ? C19 C21 C23 120.1(5) . . ? C19 C21 H17 119.9 . . ? C23 C21 H17 119.9 . . ? C20 C22 C23 117.6(5) . . ? C20 C22 H18 121.2 . . ? C23 C22 H18 121.2 . . ? C21 C23 C22 117.5(4) . . ? C21 C23 C24 121.7(5) . . ? C22 C23 C24 120.9(4) . . ? C25 C24 C26 118.2(5) . . ? C25 C24 C23 120.9(5) . . ? C26 C24 C23 120.9(5) . . ? C24 C25 C27 120.3(5) . . ? C24 C25 H19 119.9 . . ? C27 C25 H19 119.9 . . ? C28 C26 C24 119.4(5) . . ? C28 C26 H20 120.3 . . ? C24 C26 H20 120.3 . . ? N4 C27 C25 120.5(6) . . ? N4 C27 H21 119.8 . . ? C25 C27 H21 119.8 . . ? N4 C28 C26 121.2(5) . . ? N4 C28 H22 119.4 . . ? C26 C28 H22 119.4 . . ? N4 C29 C30 113.1(4) . . ? N4 C29 H23 109.0 . . ? C30 C29 H23 109.0 . . ? N4 C29 H24 109.0 . . ? C30 C29 H24 109.0 . . ? H23 C29 H24 107.8 . . ? C32 C30 C31 119.8(4) . . ? C32 C30 C29 120.2(5) . . ? C31 C30 C29 120.0(5) . . ? C34 C31 C30 120.3(5) . . ? C34 C31 H26 119.9 . . ? C30 C31 H26 119.9 . . ? C30 C32 C33 120.0(5) . . ? C30 C32 H25 120.0 . . ? C33 C32 H25 120.0 . . ? C32 C33 C35 119.9(5) . . ? C32 C33 H27 120.1 . . ? C35 C33 H27 120.1 . . ? C35 C34 C31 120.9(5) . . ? C35 C34 H28 119.5 . . ? C31 C34 H28 119.5 . . ? C34 C35 C33 119.1(4) . . ? C34 C35 C36 121.4(5) . . ? C33 C35 C36 119.5(5) . . ? O3 C36 O4 124.7(5) . . ? O3 C36 C35 116.5(5) . . ? O4 C36 C35 118.7(5) . . ? N6 C37 C39 121.8(8) . . ? N6 C37 H29 119.1 . . ? C39 C37 H29 119.1 . . ? N6 C38 C40 122.2(8) . . ? N6 C38 H30 118.9 . . ? C40 C38 H30 118.9 . . ? C37 C39 C41 119.9(8) . . ? C37 C39 H31 120.0 . . ? C41 C39 H31 120.0 . . ? C41 C40 C38 118.9(7) . . ? C41 C40 H32 120.6 . . ? C38 C40 H32 120.6 . . ? C40 C41 C39 119.0(7) . . ? C40 C41 C42 120.5(6) . . ? C39 C41 C42 120.4(7) . . ? C44 C42 C43 117.9(7) . . ? C44 C42 C41 122.2(7) . . ? C43 C42 C41 119.8(6) . . ? C42 C43 C46 120.0(6) . . ? C42 C43 H33 120.0 . . ? C46 C43 H33 120.0 . . ? C45 C44 C42 120.3(6) . . ? C45 C44 H34 119.8 . . ? C42 C44 H34 119.8 . . ? N5 C45 C44 121.0(5) . . ? N5 C45 H36 119.5 . . ? C44 C45 H36 119.5 . . ? N5 C46 C43 119.2(7) . . ? N5 C46 H35 120.4 . . ? C43 C46 H35 120.4 . . ? N5 C47 C48 110.9(5) . . ? N5 C47 H37 109.5 . . ? C48 C47 H37 109.5 . . ? N5 C47 H38 109.5 . . ? C48 C47 H38 109.5 . . ? H37 C47 H38 108.0 . . ? C49 C48 C50 120.0(5) . . ? C49 C48 C47 119.7(5) . . ? C50 C48 C47 120.4(5) . . ? C48 C49 C51 121.1(6) . . ? C48 C49 H39 119.4 . . ? C51 C49 H39 119.4 . . ? C52 C50 C48 118.5(5) . . ? C52 C50 H40 120.7 . . ? C48 C50 H40 120.7 . . ? C53 C51 C49 120.3(5) . . ? C53 C51 H41 119.8 . . ? C49 C51 H41 119.8 . . ? C50 C52 C53 122.3(6) . . ? C50 C52 H42 118.9 . . ? C53 C52 H42 118.9 . . ? C51 C53 C52 117.8(5) . . ? C51 C53 C54 120.1(5) . . ? C52 C53 C54 122.0(5) . . ? O5 C54 O6 123.9(6) . . ? O5 C54 C53 118.1(5) . . ? O6 C54 C53 118.0(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.053 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.134 # Attachment '- 2-JXH.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 765401' #TrackingRef '- 2-JXH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H68 Cl4 Mn2 N8 O30' _chemical_formula_sum 'C72 H68 Cl4 Mn2 N8 O30' _chemical_formula_weight 1777.03 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' 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.820(5) _cell_length_b 27.140(9) _cell_length_c 23.236(6) _cell_angle_alpha 90.00 _cell_angle_beta 129.027(15) _cell_angle_gamma 90.00 _cell_volume 7750(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6641 _cell_measurement_theta_min 2.2356 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8308 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(R.H. Blessing, 1995&1997)' _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 'CCD area detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60103 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17735 _reflns_number_gt 12643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.1326P)^2^+5.0354P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17735 _refine_ls_number_parameters 1039 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2614 _refine_ls_wR_factor_gt 0.2345 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.002 _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 Mn2 Mn 0.12495(5) -0.05758(2) 0.59519(3) 0.04354(17) Uani 1 1 d . . . Cl1 Cl -0.33234(15) -0.43528(6) 0.14342(9) 0.0863(5) Uani 1 1 d . . . Cl2 Cl -0.17483(11) -0.20581(5) 0.35355(7) 0.0761(4) Uani 1 1 d . . . Cl3 Cl 0.1893(3) -0.29324(7) 0.36179(12) 0.1623(14) Uani 1 1 d . . . Cl4 Cl 0.03949(13) -0.10435(6) 0.06021(9) 0.0816(4) Uani 1 1 d . . . O1 O 0.0138(2) -0.05680(11) 0.47777(16) 0.0514(7) Uani 1 1 d . . . O2 O -0.0784(2) -0.00922(11) 0.37781(17) 0.0541(7) Uani 1 1 d . . . O3 O -0.6778(3) -0.14903(12) 0.71969(19) 0.0658(9) Uani 1 1 d . . . O4 O -0.7913(2) -0.12404(12) 0.60136(18) 0.0590(8) Uani 1 1 d . . . O5 O -1.2919(2) -0.13615(11) 0.12090(17) 0.0540(7) Uani 1 1 d . . . O6 O -1.3946(3) -0.16043(13) 0.00329(19) 0.0685(9) Uani 1 1 d . . . O7 O 0.6173(3) -0.00847(12) 0.1991(2) 0.0651(9) Uani 1 1 d . . . O9 O -0.3000(8) -0.4462(4) 0.1022(5) 0.205(4) Uani 1 1 d . . . O10 O -0.2785(9) -0.3966(3) 0.1853(4) 0.275(7) Uani 1 1 d . . . O11 O -0.3288(6) -0.4721(2) 0.1862(3) 0.166(3) Uani 1 1 d . . . O12 O -0.4391(6) -0.4186(4) 0.0892(5) 0.200(4) Uani 1 1 d . . . O13 O -0.2155(8) -0.2518(3) 0.3422(5) 0.237(5) Uani 1 1 d . . . O14 O -0.2469(8) -0.1739(4) 0.3567(5) 0.225(5) Uani 1 1 d . . . O15 O -0.0774(4) -0.1999(3) 0.4221(3) 0.148(2) Uani 1 1 d . . . O16 O -0.1835(5) -0.1887(2) 0.2934(3) 0.1222(18) Uani 1 1 d . . . O17 O 0.1276(10) -0.3188(3) 0.3002(4) 0.261(6) Uani 1 1 d . . . O18 O 0.131(2) -0.2806(6) 0.3879(14) 0.458(16) Uani 1 1 d . . . O19 O 0.2127(7) -0.24757(18) 0.3526(4) 0.173(3) Uani 1 1 d . . . O20 O 0.2626(15) -0.3183(3) 0.4186(5) 0.386(13) Uani 1 1 d . . . O21 O -0.0136(7) -0.1441(2) 0.0094(4) 0.170(3) Uani 1 1 d . . . O22 O 0.1352(7) -0.0904(4) 0.0768(7) 0.246(6) Uani 1 1 d . . . O23 O -0.0314(4) -0.06499(18) 0.0283(3) 0.125(2) Uani 1 1 d . . . O24 O 0.0667(6) -0.1215(3) 0.1246(3) 0.183(4) Uani 1 1 d . . . N1 N 0.2981(3) -0.10413(13) 0.3297(2) 0.0480(8) Uani 1 1 d . . . N2 N 0.7538(3) 0.01168(14) 0.4052(2) 0.0501(8) Uani 1 1 d . . . N3 N -0.0086(3) -0.09460(12) 0.59047(19) 0.0464(7) Uani 1 1 d . . . N4 N -0.3847(3) -0.23102(13) 0.5927(2) 0.0552(9) Uani 1 1 d . . . N5 N -0.4882(2) -0.10940(12) 0.13030(18) 0.0436(7) Uani 1 1 d . . . N6 N -0.8652(3) -0.24720(12) 0.1295(2) 0.0478(8) Uani 1 1 d . . . N7 N -0.2460(3) -0.01986(14) 0.1286(2) 0.0521(8) Uani 1 1 d . . . N8 N 0.1623(3) 0.10554(12) 0.1496(2) 0.0471(8) Uani 1 1 d . . . C1 C -0.0082(3) -0.04111(14) 0.4194(2) 0.0404(8) Uani 1 1 d . . . C2 C 0.0490(3) -0.06382(13) 0.3930(2) 0.0398(8) Uani 1 1 d . . . C3 C 0.0767(4) -0.03530(16) 0.3582(3) 0.0622(12) Uani 1 1 d . . . H1 H 0.0596 -0.0012 0.3508 0.075 Uiso 1 1 calc R . . C4 C 0.0717(3) -0.11388(15) 0.4016(3) 0.0507(10) Uani 1 1 d . . . H2 H 0.0538 -0.1340 0.4259 0.061 Uiso 1 1 calc R . . C5 C 0.1297(5) -0.05589(17) 0.3338(3) 0.0671(14) Uani 1 1 d . . . H3 H 0.1522 -0.0355 0.3125 0.080 Uiso 1 1 calc R . . C6 C 0.1204(4) -0.13429(15) 0.3747(3) 0.0524(10) Uani 1 1 d . . . H4 H 0.1343 -0.1687 0.3798 0.063 Uiso 1 1 calc R . . C7 C 0.1494(3) -0.10563(16) 0.3404(3) 0.0502(9) Uani 1 1 d . . . C8 C 0.1989(4) -0.12975(17) 0.3094(3) 0.0590(12) Uani 1 1 d . . . H6 H 0.2182 -0.1642 0.3274 0.071 Uiso 1 1 calc R . . H5 H 0.1437 -0.1308 0.2547 0.071 Uiso 1 1 calc R . . C9 C 0.3049(3) -0.09454(16) 0.2757(2) 0.0516(10) Uani 1 1 d . . . H7 H 0.2452 -0.1019 0.2256 0.062 Uiso 1 1 calc R . . C10 C 0.3801(4) -0.09256(19) 0.3999(3) 0.0590(11) Uani 1 1 d . . . H8 H 0.3740 -0.0997 0.4372 0.071 Uiso 1 1 calc R . . C11 C 0.3970(3) -0.07430(16) 0.2929(2) 0.0504(9) Uani 1 1 d . . . H9 H 0.4028 -0.0693 0.2550 0.060 Uiso 1 1 calc R . . C12 C 0.4724(4) -0.07075(17) 0.4194(2) 0.0534(10) Uani 1 1 d . . . H10 H 0.5295 -0.0623 0.4696 0.064 Uiso 1 1 calc R . . C13 C 0.4824(3) -0.06089(15) 0.3651(2) 0.0451(9) Uani 1 1 d . . . C14 C 0.5808(3) -0.03742(15) 0.3836(2) 0.0446(8) Uani 1 1 d . . . C15 C 0.6332(4) -0.05742(16) 0.3584(3) 0.0528(10) Uani 1 1 d . . . H11 H 0.6103 -0.0881 0.3329 0.063 Uiso 1 1 calc R . . C16 C 0.6198(4) 0.00620(18) 0.4221(3) 0.0601(12) Uani 1 1 d . . . H12 H 0.5888 0.0200 0.4426 0.072 Uiso 1 1 calc R . . C17 C 0.7189(4) -0.03185(17) 0.3710(3) 0.0569(11) Uani 1 1 d . . . H13 H 0.7550 -0.0460 0.3543 0.068 Uiso 1 1 calc R . . C18 C 0.7050(4) 0.02997(19) 0.4307(3) 0.0605(12) Uani 1 1 d . . . H14 H 0.7294 0.0607 0.4558 0.073 Uiso 1 1 calc R . . C19 C -0.0984(4) -0.11317(16) 0.5287(3) 0.0522(10) Uani 1 1 d . . . H16 H -0.1092 -0.1090 0.4839 0.063 Uiso 1 1 calc R . . C20 C 0.0040(4) -0.09961(17) 0.6533(3) 0.0538(10) Uani 1 1 d . . . H15 H 0.0669 -0.0860 0.6980 0.065 Uiso 1 1 calc R . . C21 C -0.1771(3) -0.13821(16) 0.5259(3) 0.0515(10) Uani 1 1 d . . . H18 H -0.2397 -0.1510 0.4803 0.062 Uiso 1 1 calc R . . C22 C -0.0714(4) -0.12385(17) 0.6550(3) 0.0533(10) Uani 1 1 d . . . H17 H -0.0603 -0.1264 0.7001 0.064 Uiso 1 1 calc R . . C23 C -0.1631(3) -0.14430(14) 0.5908(2) 0.0434(8) Uani 1 1 d . . . C24 C -0.2409(3) -0.17383(14) 0.5922(2) 0.0464(9) Uani 1 1 d . . . C25 C -0.3482(4) -0.1798(2) 0.5287(3) 0.0654(13) Uani 1 1 d . . . H20 H -0.3730 -0.1639 0.4840 0.078 Uiso 1 1 calc R . . C26 C -0.2091(4) -0.19769(16) 0.6554(3) 0.0521(10) Uani 1 1 d . . . H19 H -0.1362 -0.1946 0.6998 0.062 Uiso 1 1 calc R . . C27 C -0.4182(4) -0.2083(2) 0.5299(3) 0.0685(13) Uani 1 1 d . . . H22 H -0.4913 -0.2122 0.4860 0.082 Uiso 1 1 calc R . . C28 C -0.2819(4) -0.22581(16) 0.6544(3) 0.0550(10) Uani 1 1 d . . . H21 H -0.2588 -0.2419 0.6984 0.066 Uiso 1 1 calc R . . C29 C -0.4646(4) -0.26098(17) 0.5910(3) 0.0619(12) Uani 1 1 d . . . H23 H -0.4260 -0.2878 0.6280 0.074 Uiso 1 1 calc R . . H24 H -0.5166 -0.2762 0.5415 0.074 Uiso 1 1 calc R . . C30 C -0.5268(4) -0.22995(14) 0.6077(3) 0.0497(10) Uani 1 1 d . . . C31 C -0.6264(4) -0.21117(19) 0.5515(3) 0.0629(12) Uani 1 1 d . . . H26 H -0.6560 -0.2169 0.5017 0.075 Uiso 1 1 calc R . . C32 C -0.4854(4) -0.22202(17) 0.6795(3) 0.0581(11) Uani 1 1 d . . . H25 H -0.4161 -0.2352 0.7189 0.070 Uiso 1 1 calc R . . C33 C -0.6854(4) -0.18373(18) 0.5659(3) 0.0604(11) Uani 1 1 d . . . H28 H -0.7542 -0.1705 0.5260 0.073 Uiso 1 1 calc R . . C34 C -0.5434(3) -0.19489(15) 0.6956(3) 0.0504(9) Uani 1 1 d . . . H27 H -0.5137 -0.1897 0.7456 0.060 Uiso 1 1 calc R . . C35 C -0.6442(3) -0.17564(14) 0.6384(2) 0.0446(8) Uani 1 1 d . . . C36 C -0.7101(4) -0.14752(15) 0.6547(3) 0.0506(10) Uani 1 1 d . . . C37 C -0.5924(3) -0.1120(2) 0.0713(3) 0.0631(13) Uani 1 1 d . . . H30 H -0.6162 -0.0951 0.0276 0.076 Uiso 1 1 calc R . . C38 C -0.4586(3) -0.13254(15) 0.1912(2) 0.0460(9) Uani 1 1 d . . . H29 H -0.3847 -0.1306 0.2346 0.055 Uiso 1 1 calc R . . C39 C -0.6680(3) -0.1379(2) 0.0705(3) 0.0650(13) Uani 1 1 d . . . H32 H -0.7420 -0.1384 0.0269 0.078 Uiso 1 1 calc R . . C40 C -0.5294(3) -0.15896(15) 0.1945(2) 0.0460(9) Uani 1 1 d . . . H31 H -0.5046 -0.1744 0.2394 0.055 Uiso 1 1 calc R . . C41 C -0.6375(3) -0.16300(14) 0.1317(2) 0.0404(8) Uani 1 1 d . . . C42 C -0.7151(3) -0.19333(13) 0.1320(2) 0.0406(8) Uani 1 1 d . . . C43 C -0.8099(3) -0.21219(16) 0.0662(3) 0.0521(10) Uani 1 1 d . . . H34 H -0.8232 -0.2069 0.0207 0.063 Uiso 1 1 calc R . . C44 C -0.6984(3) -0.20468(15) 0.1968(2) 0.0490(9) Uani 1 1 d . . . H33 H -0.6341 -0.1938 0.2431 0.059 Uiso 1 1 calc R . . C45 C -0.8828(3) -0.23784(16) 0.0668(3) 0.0542(10) Uani 1 1 d . . . H36 H -0.9477 -0.2493 0.0213 0.065 Uiso 1 1 calc R . . C46 C -0.7744(3) -0.23162(16) 0.1944(3) 0.0529(10) Uani 1 1 d . . . H35 H -0.7621 -0.2392 0.2390 0.063 Uiso 1 1 calc R . . C47 C -0.9481(3) -0.27465(15) 0.1286(3) 0.0564(11) Uani 1 1 d . . . H37 H -0.9113 -0.2910 0.1772 0.068 Uiso 1 1 calc R . . H38 H -0.9809 -0.3007 0.0903 0.068 Uiso 1 1 calc R . . C48 C -1.0378(3) -0.24167(14) 0.1131(3) 0.0499(10) Uani 1 1 d . . . C49 C -1.1338(4) -0.23557(16) 0.0405(3) 0.0547(10) Uani 1 1 d . . . H40 H -1.1408 -0.2504 0.0006 0.066 Uiso 1 1 calc R . . C50 C -1.0285(3) -0.21952(16) 0.1706(3) 0.0541(10) Uani 1 1 d . . . H39 H -0.9637 -0.2237 0.2202 0.065 Uiso 1 1 calc R . . C51 C -1.2192(4) -0.20784(16) 0.0263(3) 0.0535(10) Uani 1 1 d . . . H42 H -1.2839 -0.2036 -0.0233 0.064 Uiso 1 1 calc R . . C52 C -1.1134(3) -0.19120(16) 0.1563(3) 0.0527(10) Uani 1 1 d . . . H41 H -1.1053 -0.1751 0.1959 0.063 Uiso 1 1 calc R . . C53 C -1.2110(3) -0.18644(14) 0.0835(2) 0.0458(9) Uani 1 1 d . . . C54 C -1.3056(3) -0.15873(14) 0.0684(2) 0.0465(9) Uani 1 1 d . . . C55 C -0.2497(4) 0.02827(18) 0.1208(3) 0.0676(14) Uani 1 1 d . . . H44 H -0.3088 0.0456 0.1124 0.081 Uiso 1 1 calc R . . C56 C -0.1624(5) -0.04261(19) 0.1391(4) 0.0841(19) Uani 1 1 d . . . H43 H -0.1574 -0.0774 0.1448 0.101 Uiso 1 1 calc R . . C57 C -0.1719(4) 0.05527(18) 0.1243(4) 0.0724(15) Uani 1 1 d . . . H46 H -0.1773 0.0902 0.1201 0.087 Uiso 1 1 calc R . . C58 C -0.0842(5) -0.01882(19) 0.1422(4) 0.0832(19) Uani 1 1 d . . . H45 H -0.0263 -0.0371 0.1502 0.100 Uiso 1 1 calc R . . C59 C -0.0878(3) 0.03161(16) 0.1337(2) 0.0476(9) Uani 1 1 d . . . C60 C -0.0024(3) 0.05786(15) 0.1376(2) 0.0462(9) Uani 1 1 d . . . C61 C 0.0089(4) 0.10901(16) 0.1445(3) 0.0550(11) Uani 1 1 d . . . H48 H -0.0407 0.1281 0.1452 0.066 Uiso 1 1 calc R . . C62 C 0.0714(4) 0.03256(17) 0.1362(3) 0.0625(12) Uani 1 1 d . . . H47 H 0.0657 -0.0022 0.1304 0.075 Uiso 1 1 calc R . . C63 C 0.0911(4) 0.13170(16) 0.1502(3) 0.0558(11) Uani 1 1 d . . . H50 H 0.0977 0.1666 0.1545 0.067 Uiso 1 1 calc R . . C64 C 0.1532(4) 0.05678(16) 0.1431(3) 0.0637(13) Uani 1 1 d . . . H49 H 0.2045 0.0384 0.1432 0.076 Uiso 1 1 calc R . . C65 C 0.2519(4) 0.13327(17) 0.1590(4) 0.0733(16) Uani 1 1 d . . . H52 H 0.2958 0.1504 0.2074 0.088 Uiso 1 1 calc R . . H51 H 0.2195 0.1587 0.1198 0.088 Uiso 1 1 calc R . . C66 C 0.3258(4) 0.10103(15) 0.1552(3) 0.0573(12) Uani 1 1 d . . . C67 C 0.2989(4) 0.0909(2) 0.0868(3) 0.0672(14) Uani 1 1 d . . . H54 H 0.2343 0.1043 0.0429 0.081 Uiso 1 1 calc R . . C68 C 0.4200(4) 0.08151(18) 0.2190(3) 0.0611(11) Uani 1 1 d . . . H53 H 0.4394 0.0884 0.2661 0.073 Uiso 1 1 calc R . . C69 C 0.3669(4) 0.06101(19) 0.0824(3) 0.0604(12) Uani 1 1 d . . . H56 H 0.3484 0.0540 0.0357 0.072 Uiso 1 1 calc R . . C70 C 0.4862(3) 0.05165(17) 0.2133(3) 0.0542(10) Uani 1 1 d . . . H55 H 0.5503 0.0379 0.2570 0.065 Uiso 1 1 calc R . . C71 C 0.4612(3) 0.04169(15) 0.1465(2) 0.0448(8) Uani 1 1 d . . . C72 C 0.5330(4) 0.00942(15) 0.1418(3) 0.0503(9) Uani 1 1 d . . . O1W O 0.2334(2) -0.06465(11) 0.71719(17) 0.0557(7) Uani 1 1 d . . . O2W O -0.2263(2) -0.08252(12) 0.24694(17) 0.0573(7) Uani 1 1 d . . . O3W O -0.4807(2) -0.07725(11) 0.00555(17) 0.0540(7) Uani 1 1 d . . . O4W O -0.4200(5) -0.2106(2) 0.3614(3) 0.1136(16) Uani 1 1 d . . . O5W O -0.5154(4) -0.29909(16) 0.3587(2) 0.0903(12) Uani 1 1 d . . . O6W O -0.6110(8) -0.2161(5) 0.3696(5) 0.263(6) Uani 1 1 d . . . Mn1 Mn -0.36804(5) -0.06696(2) 0.12599(3) 0.04230(17) Uani 1 1 d . . . O8 O 0.5079(2) -0.00007(10) 0.08009(15) 0.04230(17) Uani 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 Mn2 0.0390(3) 0.0513(3) 0.0475(4) 0.0026(3) 0.0307(3) 0.0046(2) Cl1 0.0971(11) 0.0918(10) 0.0724(9) -0.0069(7) 0.0546(9) -0.0369(9) Cl2 0.0726(8) 0.0734(8) 0.0515(7) 0.0064(6) 0.0244(6) -0.0157(6) Cl3 0.291(4) 0.0648(10) 0.0764(12) -0.0033(8) 0.0892(18) -0.0423(15) Cl4 0.0887(10) 0.0767(9) 0.0852(10) 0.0117(7) 0.0575(9) 0.0208(7) O1 0.0543(16) 0.0603(17) 0.0450(16) 0.0009(13) 0.0339(14) -0.0035(13) O2 0.0537(16) 0.0591(17) 0.0598(18) 0.0064(14) 0.0406(15) 0.0145(14) O3 0.079(2) 0.067(2) 0.063(2) 0.0103(16) 0.0510(19) 0.0246(17) O4 0.0511(16) 0.0662(19) 0.0567(18) 0.0036(15) 0.0326(15) 0.0169(15) O5 0.0563(17) 0.0559(17) 0.0567(18) 0.0032(14) 0.0389(15) 0.0091(14) O6 0.0526(18) 0.075(2) 0.064(2) -0.0123(17) 0.0304(16) 0.0080(16) O7 0.0516(17) 0.0591(18) 0.079(2) 0.0050(16) 0.0387(17) 0.0115(15) O9 0.236(9) 0.261(10) 0.207(9) 0.081(7) 0.182(8) 0.092(8) O10 0.397(14) 0.229(8) 0.084(4) -0.027(5) 0.096(6) -0.220(10) O11 0.227(7) 0.138(5) 0.118(5) -0.003(4) 0.101(5) -0.094(5) O12 0.131(6) 0.323(12) 0.151(7) 0.048(7) 0.092(6) 0.025(7) O13 0.269(10) 0.130(6) 0.188(8) -0.005(5) 0.085(7) -0.122(6) O14 0.199(8) 0.342(13) 0.126(6) 0.033(7) 0.098(6) 0.135(9) O15 0.091(3) 0.220(7) 0.071(3) 0.004(4) 0.021(3) -0.041(4) O16 0.171(5) 0.119(4) 0.091(4) 0.031(3) 0.089(4) 0.031(4) O17 0.409(15) 0.129(5) 0.086(5) -0.034(4) 0.079(7) -0.077(8) O18 0.90(5) 0.235(16) 0.59(4) -0.027(19) 0.64(4) -0.10(2) O19 0.234(8) 0.067(3) 0.137(5) 0.020(3) 0.078(5) -0.031(4) O20 0.64(3) 0.100(5) 0.103(6) 0.040(4) 0.084(10) -0.040(9) O21 0.225(7) 0.108(4) 0.110(5) -0.008(3) 0.073(5) 0.055(5) O22 0.181(7) 0.262(10) 0.396(15) 0.180(10) 0.230(10) 0.079(7) O23 0.107(4) 0.095(3) 0.119(4) -0.019(3) 0.044(3) 0.024(3) O24 0.154(6) 0.264(9) 0.064(3) 0.024(4) 0.036(3) -0.073(6) N1 0.0464(18) 0.0542(19) 0.056(2) -0.0073(16) 0.0381(17) -0.0044(15) N2 0.0386(16) 0.064(2) 0.053(2) 0.0021(16) 0.0310(16) 0.0011(15) N3 0.0474(18) 0.0509(18) 0.051(2) 0.0054(15) 0.0360(16) 0.0039(15) N4 0.065(2) 0.0451(18) 0.085(3) 0.0060(18) 0.061(2) 0.0078(17) N5 0.0367(15) 0.0501(18) 0.0454(18) -0.0003(14) 0.0264(14) -0.0050(13) N6 0.0430(17) 0.0386(16) 0.071(2) -0.0033(15) 0.0407(18) -0.0027(13) N7 0.0388(17) 0.061(2) 0.063(2) 0.0017(17) 0.0348(17) -0.0059(15) N8 0.0437(17) 0.0475(18) 0.065(2) -0.0033(15) 0.0414(17) -0.0034(14) C1 0.0338(17) 0.0449(19) 0.047(2) -0.0059(16) 0.0278(16) -0.0063(15) C2 0.0346(17) 0.0455(19) 0.044(2) 0.0000(15) 0.0268(16) -0.0010(15) C3 0.088(3) 0.044(2) 0.093(4) 0.010(2) 0.076(3) 0.010(2) C4 0.054(2) 0.049(2) 0.064(3) 0.0065(19) 0.044(2) 0.0010(18) C5 0.094(4) 0.051(2) 0.106(4) 0.011(2) 0.087(4) 0.005(2) C6 0.064(3) 0.043(2) 0.066(3) 0.0002(19) 0.049(2) -0.0005(19) C7 0.047(2) 0.052(2) 0.063(3) -0.0072(19) 0.040(2) -0.0046(18) C8 0.061(3) 0.060(2) 0.084(3) -0.021(2) 0.059(3) -0.020(2) C9 0.047(2) 0.064(3) 0.050(2) -0.0116(19) 0.0334(19) -0.0064(19) C10 0.064(3) 0.074(3) 0.059(3) -0.006(2) 0.048(2) -0.006(2) C11 0.051(2) 0.062(2) 0.049(2) -0.0013(19) 0.037(2) -0.0009(19) C12 0.049(2) 0.069(3) 0.047(2) -0.005(2) 0.032(2) -0.008(2) C13 0.0410(19) 0.050(2) 0.050(2) -0.0008(17) 0.0313(18) 0.0008(16) C14 0.0405(19) 0.054(2) 0.045(2) 0.0002(17) 0.0294(17) 0.0007(17) C15 0.054(2) 0.052(2) 0.066(3) -0.003(2) 0.045(2) -0.0012(19) C16 0.054(2) 0.074(3) 0.068(3) -0.020(2) 0.047(2) -0.014(2) C17 0.055(2) 0.060(3) 0.075(3) -0.004(2) 0.051(2) 0.000(2) C18 0.052(2) 0.072(3) 0.070(3) -0.023(2) 0.044(2) -0.020(2) C19 0.055(2) 0.060(2) 0.054(2) 0.0081(19) 0.040(2) 0.001(2) C20 0.051(2) 0.065(3) 0.055(3) -0.004(2) 0.038(2) -0.006(2) C21 0.047(2) 0.056(2) 0.055(2) 0.0102(19) 0.033(2) 0.0013(18) C22 0.059(2) 0.061(2) 0.053(2) 0.000(2) 0.042(2) -0.003(2) C23 0.049(2) 0.0400(18) 0.051(2) 0.0076(16) 0.0363(19) 0.0071(16) C24 0.051(2) 0.045(2) 0.060(2) 0.0063(18) 0.043(2) 0.0069(17) C25 0.053(2) 0.083(3) 0.068(3) 0.022(3) 0.042(2) 0.007(2) C26 0.055(2) 0.054(2) 0.059(3) 0.0043(19) 0.041(2) 0.0011(19) C27 0.051(3) 0.083(3) 0.077(3) 0.017(3) 0.043(3) 0.001(2) C28 0.070(3) 0.050(2) 0.067(3) 0.011(2) 0.054(3) 0.007(2) C29 0.071(3) 0.050(2) 0.097(4) -0.001(2) 0.068(3) -0.002(2) C30 0.058(2) 0.0412(19) 0.072(3) 0.0003(19) 0.052(2) -0.0029(18) C31 0.066(3) 0.075(3) 0.062(3) -0.001(2) 0.047(3) 0.005(2) C32 0.045(2) 0.058(2) 0.072(3) 0.009(2) 0.037(2) 0.0070(19) C33 0.057(3) 0.069(3) 0.058(3) 0.007(2) 0.037(2) 0.014(2) C34 0.049(2) 0.050(2) 0.056(2) 0.0002(18) 0.035(2) 0.0039(18) C35 0.049(2) 0.0382(18) 0.056(2) 0.0009(16) 0.0375(19) 0.0015(16) C36 0.053(2) 0.045(2) 0.062(3) 0.0040(19) 0.040(2) 0.0018(18) C37 0.042(2) 0.094(3) 0.044(2) 0.015(2) 0.0226(19) -0.010(2) C38 0.0406(19) 0.057(2) 0.041(2) -0.0025(17) 0.0262(17) -0.0089(17) C39 0.035(2) 0.097(4) 0.051(3) 0.017(2) 0.0210(19) -0.007(2) C40 0.0403(19) 0.055(2) 0.042(2) 0.0035(17) 0.0252(17) -0.0048(17) C41 0.0339(17) 0.0437(19) 0.048(2) -0.0017(16) 0.0283(16) -0.0029(15) C42 0.0364(17) 0.0397(18) 0.051(2) -0.0022(16) 0.0300(17) -0.0027(15) C43 0.048(2) 0.060(2) 0.052(2) -0.0077(19) 0.034(2) -0.0116(19) C44 0.043(2) 0.056(2) 0.051(2) -0.0054(18) 0.0309(19) -0.0090(18) C45 0.044(2) 0.055(2) 0.060(3) -0.013(2) 0.031(2) -0.0111(18) C46 0.052(2) 0.056(2) 0.062(3) 0.000(2) 0.042(2) -0.0058(19) C47 0.049(2) 0.039(2) 0.093(3) 0.002(2) 0.051(2) -0.0056(17) C48 0.048(2) 0.0404(19) 0.076(3) 0.0011(19) 0.046(2) -0.0053(17) C49 0.058(2) 0.052(2) 0.069(3) -0.003(2) 0.048(2) 0.000(2) C50 0.043(2) 0.053(2) 0.062(3) -0.003(2) 0.032(2) -0.0069(18) C51 0.050(2) 0.053(2) 0.060(3) 0.001(2) 0.036(2) -0.0006(19) C52 0.047(2) 0.053(2) 0.065(3) -0.003(2) 0.038(2) -0.0054(18) C53 0.049(2) 0.0409(19) 0.057(2) -0.0004(17) 0.038(2) -0.0047(16) C54 0.046(2) 0.0431(19) 0.057(2) 0.0024(18) 0.036(2) 0.0003(16) C55 0.053(3) 0.060(3) 0.108(4) 0.014(3) 0.060(3) 0.004(2) C56 0.077(3) 0.053(3) 0.158(6) 0.008(3) 0.091(4) -0.001(3) C57 0.063(3) 0.054(3) 0.122(5) 0.015(3) 0.068(3) 0.004(2) C58 0.079(4) 0.056(3) 0.155(6) 0.002(3) 0.093(4) 0.001(3) C59 0.042(2) 0.055(2) 0.051(2) -0.0001(18) 0.0316(18) -0.0042(17) C60 0.0404(19) 0.053(2) 0.050(2) -0.0025(17) 0.0310(18) -0.0044(17) C61 0.050(2) 0.053(2) 0.081(3) -0.001(2) 0.050(2) 0.0015(19) C62 0.066(3) 0.046(2) 0.103(4) -0.011(2) 0.066(3) -0.009(2) C63 0.056(2) 0.043(2) 0.085(3) -0.002(2) 0.052(3) -0.0006(18) C64 0.067(3) 0.045(2) 0.109(4) -0.009(2) 0.070(3) -0.004(2) C65 0.061(3) 0.052(2) 0.138(5) -0.008(3) 0.078(3) -0.008(2) C66 0.058(3) 0.046(2) 0.097(4) 0.005(2) 0.063(3) 0.0006(19) C67 0.049(2) 0.080(3) 0.080(3) 0.030(3) 0.044(3) 0.018(2) C68 0.060(3) 0.066(3) 0.071(3) -0.010(2) 0.047(3) -0.001(2) C69 0.048(2) 0.084(3) 0.055(3) 0.016(2) 0.035(2) 0.008(2) C70 0.045(2) 0.064(3) 0.052(2) 0.002(2) 0.030(2) 0.0051(19) C71 0.0402(19) 0.048(2) 0.053(2) -0.0002(17) 0.0327(18) -0.0007(16) C72 0.053(2) 0.045(2) 0.063(3) -0.0058(19) 0.041(2) -0.0090(18) O1W 0.0477(16) 0.0659(19) 0.0496(17) 0.0011(14) 0.0288(14) 0.0082(13) O2W 0.0487(16) 0.0636(18) 0.0499(17) 0.0030(14) 0.0263(14) 0.0056(14) O3W 0.0520(16) 0.0648(18) 0.0501(17) 0.0006(14) 0.0344(14) 0.0049(14) O4W 0.131(4) 0.116(4) 0.074(3) 0.013(3) 0.054(3) -0.013(3) O5W 0.093(3) 0.096(3) 0.069(3) 0.008(2) 0.045(2) -0.020(2) O6W 0.219(9) 0.320(14) 0.120(7) -0.023(7) 0.044(6) 0.100(9) Mn1 0.0371(3) 0.0479(3) 0.0471(3) 0.0020(2) 0.0290(3) -0.0020(2) O8 0.0371(3) 0.0479(3) 0.0471(3) 0.0020(2) 0.0290(3) -0.0020(2) _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 Mn2 O1 2.120(3) . ? Mn2 O4 2.189(3) 1_655 ? Mn2 O2 2.192(3) 3_556 ? Mn2 O1W 2.212(3) . ? Mn2 N3 2.279(3) . ? Mn2 N2 2.292(3) 3_656 ? Cl1 O10 1.317(7) . ? Cl1 O9 1.373(8) . ? Cl1 O11 1.385(5) . ? Cl1 O12 1.401(8) . ? Cl2 O13 1.353(6) . ? Cl2 O15 1.359(5) . ? Cl2 O16 1.395(5) . ? Cl2 O14 1.470(8) . ? Cl3 O20 1.274(10) . ? Cl3 O17 1.313(7) . ? Cl3 O19 1.349(5) . ? Cl3 O18 1.43(2) . ? Cl4 O24 1.353(6) . ? Cl4 O22 1.359(7) . ? Cl4 O23 1.379(5) . ? Cl4 O21 1.419(6) . ? O1 C1 1.245(5) . ? O2 C1 1.251(5) . ? O2 Mn2 2.192(3) 3_556 ? O3 C36 1.254(5) . ? O4 C36 1.259(5) . ? O4 Mn2 2.189(3) 1_455 ? O5 C54 1.256(5) . ? O5 Mn1 2.274(3) 1_455 ? O6 C54 1.261(5) . ? O7 C72 1.246(5) . ? O7 Mn1 2.441(4) 1_655 ? N1 C10 1.334(6) . ? N1 C9 1.350(5) . ? N1 C8 1.495(5) . ? N2 C18 1.330(5) . ? N2 C17 1.334(6) . ? N2 Mn2 2.292(3) 3_656 ? N3 C19 1.328(6) . ? N3 C20 1.350(5) . ? N4 C28 1.336(6) . ? N4 C27 1.347(6) . ? N4 C29 1.482(5) . ? N5 C37 1.326(5) . ? N5 C38 1.336(5) . ? N5 Mn1 2.278(3) . ? N6 C45 1.326(6) . ? N6 C46 1.338(6) . ? N6 C47 1.497(5) . ? N7 C55 1.315(6) . ? N7 C56 1.335(6) . ? N7 Mn1 2.284(3) . ? N8 C64 1.329(5) . ? N8 C63 1.338(5) . ? N8 C65 1.495(5) . ? C1 C2 1.507(5) . ? C2 C3 1.376(6) . ? C2 C4 1.388(5) . ? C3 C5 1.390(6) . ? C3 H1 0.9500 . ? C4 C6 1.377(6) . ? C4 H2 0.9500 . ? C5 C7 1.372(6) . ? C5 H3 0.9500 . ? C6 C7 1.382(6) . ? C6 H4 0.9500 . ? C7 C8 1.508(6) . ? C8 H6 0.9900 . ? C8 H5 0.9900 . ? C9 C11 1.362(6) . ? C9 H7 0.9500 . ? C10 C12 1.362(6) . ? C10 H8 0.9500 . ? C11 C13 1.385(6) . ? C11 H9 0.9500 . ? C12 C13 1.393(6) . ? C12 H10 0.9500 . ? C13 C14 1.473(5) . ? C14 C16 1.373(6) . ? C14 C15 1.392(6) . ? C15 C17 1.381(6) . ? C15 H11 0.9500 . ? C16 C18 1.391(6) . ? C16 H12 0.9500 . ? C17 H13 0.9500 . ? C18 H14 0.9500 . ? C19 C21 1.384(6) . ? C19 H16 0.9500 . ? C20 C22 1.384(6) . ? C20 H15 0.9500 . ? C21 C23 1.389(6) . ? C21 H18 0.9500 . ? C22 C23 1.383(6) . ? C22 H17 0.9500 . ? C23 C24 1.487(5) . ? C24 C26 1.377(6) . ? C24 C25 1.389(6) . ? C25 C27 1.367(6) . ? C25 H20 0.9500 . ? C26 C28 1.370(6) . ? C26 H19 0.9500 . ? C27 H22 0.9500 . ? C28 H21 0.9500 . ? C29 C30 1.519(6) . ? C29 H23 0.9900 . ? C29 H24 0.9900 . ? C30 C31 1.363(7) . ? C30 C32 1.371(7) . ? C31 C33 1.390(6) . ? C31 H26 0.9500 . ? C32 C34 1.400(6) . ? C32 H25 0.9500 . ? C33 C35 1.388(6) . ? C33 H28 0.9500 . ? C34 C35 1.384(6) . ? C34 H27 0.9500 . ? C35 C36 1.519(6) . ? C37 C39 1.378(6) . ? C37 H30 0.9500 . ? C38 C40 1.371(5) . ? C38 H29 0.9500 . ? C39 C41 1.362(6) . ? C39 H32 0.9500 . ? C40 C41 1.386(5) . ? C40 H31 0.9500 . ? C41 C42 1.481(5) . ? C42 C44 1.390(6) . ? C42 C43 1.399(5) . ? C43 C45 1.354(6) . ? C43 H34 0.9500 . ? C44 C46 1.377(5) . ? C44 H33 0.9500 . ? C45 H36 0.9500 . ? C46 H35 0.9500 . ? C47 C48 1.517(6) . ? C47 H37 0.9900 . ? C47 H38 0.9900 . ? C48 C50 1.385(6) . ? C48 C49 1.398(7) . ? C49 C51 1.393(6) . ? C49 H40 0.9500 . ? C50 C52 1.394(6) . ? C50 H39 0.9500 . ? C51 C53 1.379(6) . ? C51 H42 0.9500 . ? C52 C53 1.405(6) . ? C52 H41 0.9500 . ? C53 C54 1.506(5) . ? C55 C57 1.389(6) . ? C55 H44 0.9500 . ? C56 C58 1.358(7) . ? C56 H43 0.9500 . ? C57 C59 1.366(6) . ? C57 H46 0.9500 . ? C58 C59 1.379(7) . ? C58 H45 0.9500 . ? C59 C60 1.479(5) . ? C60 C62 1.373(6) . ? C60 C61 1.396(6) . ? C61 C63 1.368(6) . ? C61 H48 0.9500 . ? C62 C64 1.368(6) . ? C62 H47 0.9500 . ? C63 H50 0.9500 . ? C64 H49 0.9500 . ? C65 C66 1.507(6) . ? C65 H52 0.9900 . ? C65 H51 0.9900 . ? C66 C68 1.385(7) . ? C66 C67 1.390(7) . ? C67 C69 1.402(7) . ? C67 H54 0.9500 . ? C68 C70 1.395(6) . ? C68 H53 0.9500 . ? C69 C71 1.385(6) . ? C69 H56 0.9500 . ? C70 C71 1.365(6) . ? C70 H55 0.9500 . ? C71 C72 1.493(6) . ? C72 O8 1.249(5) . ? O2W Mn1 2.273(3) . ? O3W Mn1 2.192(3) . ? Mn1 O5 2.274(3) 1_655 ? Mn1 O8 2.377(3) 1_455 ? Mn1 O7 2.441(4) 1_455 ? O8 Mn1 2.377(3) 1_655 ? 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 Mn2 O4 94.01(12) . 1_655 ? O1 Mn2 O2 101.77(12) . 3_556 ? O4 Mn2 O2 164.06(12) 1_655 3_556 ? O1 Mn2 O1W 174.72(12) . . ? O4 Mn2 O1W 84.01(12) 1_655 . ? O2 Mn2 O1W 80.46(11) 3_556 . ? O1 Mn2 N3 87.12(12) . . ? O4 Mn2 N3 98.31(12) 1_655 . ? O2 Mn2 N3 84.83(12) 3_556 . ? O1W Mn2 N3 88.33(12) . . ? O1 Mn2 N2 90.43(12) . 3_656 ? O4 Mn2 N2 88.53(13) 1_655 3_656 ? O2 Mn2 N2 89.12(12) 3_556 3_656 ? O1W Mn2 N2 94.40(12) . 3_656 ? N3 Mn2 N2 172.87(12) . 3_656 ? O10 Cl1 O9 109.7(7) . . ? O10 Cl1 O11 109.3(4) . . ? O9 Cl1 O11 118.7(5) . . ? O10 Cl1 O12 105.0(8) . . ? O9 Cl1 O12 102.1(5) . . ? O11 Cl1 O12 111.1(5) . . ? O13 Cl2 O15 112.7(5) . . ? O13 Cl2 O16 112.2(5) . . ? O15 Cl2 O16 117.3(4) . . ? O13 Cl2 O14 105.4(7) . . ? O15 Cl2 O14 102.4(5) . . ? O16 Cl2 O14 105.2(4) . . ? O20 Cl3 O17 114.5(6) . . ? O20 Cl3 O19 119.6(7) . . ? O17 Cl3 O19 113.7(5) . . ? O20 Cl3 O18 95.6(12) . . ? O17 Cl3 O18 110.8(13) . . ? O19 Cl3 O18 99.4(8) . . ? O24 Cl4 O22 105.1(6) . . ? O24 Cl4 O23 116.5(5) . . ? O22 Cl4 O23 108.6(5) . . ? O24 Cl4 O21 105.6(5) . . ? O22 Cl4 O21 114.7(7) . . ? O23 Cl4 O21 106.6(4) . . ? C1 O1 Mn2 147.4(3) . . ? C1 O2 Mn2 130.3(3) . 3_556 ? C36 O4 Mn2 133.0(3) . 1_455 ? C54 O5 Mn1 132.9(3) . 1_455 ? C72 O7 Mn1 90.9(3) . 1_655 ? C10 N1 C9 120.4(4) . . ? C10 N1 C8 121.0(4) . . ? C9 N1 C8 118.5(4) . . ? C18 N2 C17 117.2(4) . . ? C18 N2 Mn2 121.4(3) . 3_656 ? C17 N2 Mn2 120.8(3) . 3_656 ? C19 N3 C20 117.4(4) . . ? C19 N3 Mn2 123.2(3) . . ? C20 N3 Mn2 119.4(3) . . ? C28 N4 C27 119.7(4) . . ? C28 N4 C29 121.9(4) . . ? C27 N4 C29 118.4(4) . . ? C37 N5 C38 116.6(3) . . ? C37 N5 Mn1 120.7(3) . . ? C38 N5 Mn1 122.7(2) . . ? C45 N6 C46 120.7(4) . . ? C45 N6 C47 120.4(4) . . ? C46 N6 C47 118.9(4) . . ? C55 N7 C56 115.9(4) . . ? C55 N7 Mn1 126.1(3) . . ? C56 N7 Mn1 118.0(3) . . ? C64 N8 C63 119.9(4) . . ? C64 N8 C65 122.8(3) . . ? C63 N8 C65 117.3(3) . . ? O1 C1 O2 125.5(4) . . ? O1 C1 C2 118.5(3) . . ? O2 C1 C2 116.0(3) . . ? C3 C2 C4 119.0(4) . . ? C3 C2 C1 120.3(3) . . ? C4 C2 C1 120.7(3) . . ? C2 C3 C5 120.7(4) . . ? C2 C3 H1 119.7 . . ? C5 C3 H1 119.7 . . ? C6 C4 C2 119.8(4) . . ? C6 C4 H2 120.1 . . ? C2 C4 H2 120.1 . . ? C7 C5 C3 120.2(4) . . ? C7 C5 H3 119.9 . . ? C3 C5 H3 119.9 . . ? C4 C6 C7 121.2(4) . . ? C4 C6 H4 119.4 . . ? C7 C6 H4 119.4 . . ? C5 C7 C6 118.9(4) . . ? C5 C7 C8 121.6(4) . . ? C6 C7 C8 119.5(4) . . ? N1 C8 C7 113.9(3) . . ? N1 C8 H6 108.8 . . ? C7 C8 H6 108.8 . . ? N1 C8 H5 108.8 . . ? C7 C8 H5 108.8 . . ? H6 C8 H5 107.7 . . ? N1 C9 C11 120.2(4) . . ? N1 C9 H7 119.9 . . ? C11 C9 H7 119.9 . . ? N1 C10 C12 121.5(4) . . ? N1 C10 H8 119.3 . . ? C12 C10 H8 119.3 . . ? C9 C11 C13 120.6(4) . . ? C9 C11 H9 119.7 . . ? C13 C11 H9 119.7 . . ? C10 C12 C13 119.5(4) . . ? C10 C12 H10 120.2 . . ? C13 C12 H10 120.2 . . ? C11 C13 C12 117.8(4) . . ? C11 C13 C14 120.8(4) . . ? C12 C13 C14 121.3(4) . . ? C16 C14 C15 117.9(4) . . ? C16 C14 C13 121.4(4) . . ? C15 C14 C13 120.5(4) . . ? C17 C15 C14 118.7(4) . . ? C17 C15 H11 120.7 . . ? C14 C15 H11 120.7 . . ? C14 C16 C18 119.4(4) . . ? C14 C16 H12 120.3 . . ? C18 C16 H12 120.3 . . ? N2 C17 C15 123.6(4) . . ? N2 C17 H13 118.2 . . ? C15 C17 H13 118.2 . . ? N2 C18 C16 123.0(4) . . ? N2 C18 H14 118.5 . . ? C16 C18 H14 118.5 . . ? N3 C19 C21 123.8(4) . . ? N3 C19 H16 118.1 . . ? C21 C19 H16 118.1 . . ? N3 C20 C22 122.3(4) . . ? N3 C20 H15 118.9 . . ? C22 C20 H15 118.9 . . ? C19 C21 C23 118.9(4) . . ? C19 C21 H18 120.5 . . ? C23 C21 H18 120.5 . . ? C23 C22 C20 119.9(4) . . ? C23 C22 H17 120.1 . . ? C20 C22 H17 120.1 . . ? C22 C23 C21 117.7(4) . . ? C22 C23 C24 120.9(4) . . ? C21 C23 C24 121.3(4) . . ? C26 C24 C25 117.4(4) . . ? C26 C24 C23 121.7(4) . . ? C25 C24 C23 120.9(4) . . ? C27 C25 C24 120.5(5) . . ? C27 C25 H20 119.8 . . ? C24 C25 H20 119.8 . . ? C28 C26 C24 120.3(4) . . ? C28 C26 H19 119.9 . . ? C24 C26 H19 119.9 . . ? N4 C27 C25 120.7(5) . . ? N4 C27 H22 119.6 . . ? C25 C27 H22 119.6 . . ? N4 C28 C26 121.4(4) . . ? N4 C28 H21 119.3 . . ? C26 C28 H21 119.3 . . ? N4 C29 C30 111.5(3) . . ? N4 C29 H23 109.3 . . ? C30 C29 H23 109.3 . . ? N4 C29 H24 109.3 . . ? C30 C29 H24 109.3 . . ? H23 C29 H24 108.0 . . ? C31 C30 C32 119.0(4) . . ? C31 C30 C29 120.5(4) . . ? C32 C30 C29 120.5(4) . . ? C30 C31 C33 121.2(5) . . ? C30 C31 H26 119.4 . . ? C33 C31 H26 119.4 . . ? C30 C32 C34 121.1(4) . . ? C30 C32 H25 119.4 . . ? C34 C32 H25 119.4 . . ? C35 C33 C31 120.2(4) . . ? C35 C33 H28 119.9 . . ? C31 C33 H28 119.9 . . ? C35 C34 C32 119.6(4) . . ? C35 C34 H27 120.2 . . ? C32 C34 H27 120.2 . . ? C34 C35 C33 118.9(4) . . ? C34 C35 C36 120.4(4) . . ? C33 C35 C36 120.7(4) . . ? O3 C36 O4 126.3(4) . . ? O3 C36 C35 117.4(4) . . ? O4 C36 C35 116.3(4) . . ? N5 C37 C39 123.1(4) . . ? N5 C37 H30 118.5 . . ? C39 C37 H30 118.5 . . ? N5 C38 C40 123.5(4) . . ? N5 C38 H29 118.3 . . ? C40 C38 H29 118.3 . . ? C41 C39 C37 120.5(4) . . ? C41 C39 H32 119.8 . . ? C37 C39 H32 119.8 . . ? C38 C40 C41 119.5(4) . . ? C38 C40 H31 120.2 . . ? C41 C40 H31 120.2 . . ? C39 C41 C40 116.8(3) . . ? C39 C41 C42 122.2(3) . . ? C40 C41 C42 121.1(3) . . ? C44 C42 C43 116.3(3) . . ? C44 C42 C41 122.4(3) . . ? C43 C42 C41 121.3(4) . . ? C45 C43 C42 120.7(4) . . ? C45 C43 H34 119.6 . . ? C42 C43 H34 119.6 . . ? C46 C44 C42 120.6(4) . . ? C46 C44 H33 119.7 . . ? C42 C44 H33 119.7 . . ? N6 C45 C43 121.3(4) . . ? N6 C45 H36 119.4 . . ? C43 C45 H36 119.4 . . ? N6 C46 C44 120.3(4) . . ? N6 C46 H35 119.9 . . ? C44 C46 H35 119.9 . . ? N6 C47 C48 112.9(3) . . ? N6 C47 H37 109.0 . . ? C48 C47 H37 109.0 . . ? N6 C47 H38 109.0 . . ? C48 C47 H38 109.0 . . ? H37 C47 H38 107.8 . . ? C50 C48 C49 119.2(4) . . ? C50 C48 C47 120.7(4) . . ? C49 C48 C47 119.9(4) . . ? C51 C49 C48 120.2(4) . . ? C51 C49 H40 119.9 . . ? C48 C49 H40 119.9 . . ? C48 C50 C52 120.5(4) . . ? C48 C50 H39 119.7 . . ? C52 C50 H39 119.7 . . ? C53 C51 C49 120.7(4) . . ? C53 C51 H42 119.6 . . ? C49 C51 H42 119.6 . . ? C50 C52 C53 120.0(4) . . ? C50 C52 H41 120.0 . . ? C53 C52 H41 120.0 . . ? C51 C53 C52 119.2(4) . . ? C51 C53 C54 120.6(4) . . ? C52 C53 C54 120.2(4) . . ? O5 C54 O6 124.2(4) . . ? O5 C54 C53 118.6(4) . . ? O6 C54 C53 117.2(4) . . ? N7 C55 C57 123.7(4) . . ? N7 C55 H44 118.1 . . ? C57 C55 H44 118.1 . . ? N7 C56 C58 123.7(5) . . ? N7 C56 H43 118.1 . . ? C58 C56 H43 118.1 . . ? C59 C57 C55 119.9(4) . . ? C59 C57 H46 120.0 . . ? C55 C57 H46 120.0 . . ? C56 C58 C59 120.7(5) . . ? C56 C58 H45 119.7 . . ? C59 C58 H45 119.7 . . ? C57 C59 C58 116.0(4) . . ? C57 C59 C60 122.9(4) . . ? C58 C59 C60 121.0(4) . . ? C62 C60 C61 116.8(4) . . ? C62 C60 C59 121.0(4) . . ? C61 C60 C59 122.2(4) . . ? C63 C61 C60 120.3(4) . . ? C63 C61 H48 119.9 . . ? C60 C61 H48 119.9 . . ? C64 C62 C60 120.9(4) . . ? C64 C62 H47 119.6 . . ? C60 C62 H47 119.6 . . ? N8 C63 C61 121.0(4) . . ? N8 C63 H50 119.5 . . ? C61 C63 H50 119.5 . . ? N8 C64 C62 121.2(4) . . ? N8 C64 H49 119.4 . . ? C62 C64 H49 119.4 . . ? N8 C65 C66 113.5(4) . . ? N8 C65 H52 108.9 . . ? C66 C65 H52 108.9 . . ? N8 C65 H51 108.9 . . ? C66 C65 H51 108.9 . . ? H52 C65 H51 107.7 . . ? C68 C66 C67 119.8(4) . . ? C68 C66 C65 120.8(5) . . ? C67 C66 C65 119.4(5) . . ? C66 C67 C69 120.0(4) . . ? C66 C67 H54 120.0 . . ? C69 C67 H54 120.0 . . ? C66 C68 C70 119.1(4) . . ? C66 C68 H53 120.4 . . ? C70 C68 H53 120.4 . . ? C71 C69 C67 119.9(5) . . ? C71 C69 H56 120.1 . . ? C67 C69 H56 120.1 . . ? C71 C70 C68 121.7(4) . . ? C71 C70 H55 119.1 . . ? C68 C70 H55 119.1 . . ? C70 C71 C69 119.5(4) . . ? C70 C71 C72 120.7(4) . . ? C69 C71 C72 119.8(4) . . ? O7 C72 O8 120.0(4) . . ? O7 C72 C71 120.1(4) . . ? O8 C72 C71 119.9(4) . . ? O3W Mn1 O2W 158.54(12) . . ? O3W Mn1 O5 81.93(11) . 1_655 ? O2W Mn1 O5 76.62(11) . 1_655 ? O3W Mn1 N5 87.81(12) . . ? O2W Mn1 N5 93.00(12) . . ? O5 Mn1 N5 93.94(12) 1_655 . ? O3W Mn1 N7 95.69(13) . . ? O2W Mn1 N7 84.96(13) . . ? O5 Mn1 N7 89.83(12) 1_655 . ? N5 Mn1 N7 175.19(13) . . ? O3W Mn1 O8 75.33(10) . 1_455 ? O2W Mn1 O8 126.12(11) . 1_455 ? O5 Mn1 O8 157.25(11) 1_655 1_455 ? N5 Mn1 O8 85.99(11) . 1_455 ? N7 Mn1 O8 91.69(11) . 1_455 ? O3W Mn1 O7 127.92(11) . 1_455 ? O2W Mn1 O7 73.27(11) . 1_455 ? O5 Mn1 O7 149.20(12) 1_655 1_455 ? N5 Mn1 O7 81.41(12) . 1_455 ? N7 Mn1 O7 93.82(13) . 1_455 ? O8 Mn1 O7 53.28(10) 1_455 1_455 ? C72 O8 Mn1 93.8(2) . 1_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.243 _refine_diff_density_min -1.832 _refine_diff_density_rms 0.082