# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global # Name of the journal to which the paper has been or will be submitted _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'Cif_1.cif' # Name of contact person _publ_contact_author 'Lars Eriksson' # E-mail address of contact person _publ_contact_author_email lars.eriksson@mmk.su.se _publ_contact_author_name 'Lars Eriksson' loop_ _publ_author_name 'Gustav Berggren' 'Ping Huang' 'Lars Eriksson' 'Stenbj\"on Styring' 'Magnus F. Anderlund' ; A.Thapper ; data_r _database_code_depnum_ccdc_archive 'CCDC 732737' #TrackingRef 'Cif_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H45 Cl Mn2 N8 O2, 2(Cl O4)' _chemical_formula_sum 'C38 H45 Cl3 Mn2 N8 O10' _chemical_formula_weight 990.05 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.2617(9) _cell_length_b 14.0395(7) _cell_length_c 36.5344(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.564(4) _cell_angle_gamma 90.00 _cell_volume 9860.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19027 _cell_measurement_theta_min 3.7209 _cell_measurement_theta_max 32.3242 _exptl_crystal_description block _exptl_crystal_colour colour_less _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_T_min 0.70092 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Excalibur-II with Sapphire-3 CCD' _diffrn_measurement_method '\w scans at different \f' _diffrn_detector_area_resol_mean 16.54 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 59669 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10048 _reflns_number_gt 5617 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Bergerhoff, 1996)' _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. We decided to remove disordered solvent molecules using SQUEZZE available in PLATON. The DELU restraint available in SHELXL was used in order to partly stabilize the refinement. The DELU restraint had very minor effect on the structure model. Furthermore the perchlorate ions were restrained to show the known tetrahedral conformation with all Cl-O bonds restrained to each other and all O..O contact distances equal. Furthermore a weak isotropic restraint was applied to the atoms of the perchlorate ions. ; _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^)+(0.0907P)^2^] 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 10048 _refine_ls_number_parameters 598 _refine_ls_number_restraints 303 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1537 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.982 _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 0.36080(3) 0.64720(4) 0.116968(13) 0.04241(15) Uani 1 1 d U . . Mn2 Mn 0.42695(3) 0.37791(4) 0.096698(13) 0.04489(15) Uani 1 1 d U . . Cl1 Cl 0.37699(5) 0.52968(6) 0.06478(2) 0.0509(2) Uani 1 1 d U . . O1 O 0.43758(13) 0.41784(18) 0.15068(6) 0.0587(7) Uani 1 1 d U . . C2 C 0.42839(18) 0.4891(3) 0.17047(8) 0.0447(8) Uani 1 1 d U . . O3 O 0.40246(14) 0.56553(18) 0.15963(6) 0.0600(7) Uani 1 1 d U . . C4 C 0.4529(2) 0.4824(3) 0.21004(9) 0.0787(13) Uani 1 1 d U . . H4A H 0.5008 0.5015 0.2130 0.118 Uiso 1 1 calc R . . H4B H 0.4484 0.4179 0.2183 0.118 Uiso 1 1 calc R . . H4C H 0.4252 0.5235 0.2243 0.118 Uiso 1 1 calc R . . C5 C 0.26353(19) 0.3455(3) 0.13452(11) 0.0603(10) Uani 1 1 d U . . C6 C 0.23568(18) 0.4338(3) 0.12335(11) 0.0549(9) Uani 1 1 d U . . H6 H 0.2242 0.4441 0.0986 0.066 Uiso 1 1 calc R . . C7 C 0.22472(19) 0.5062(3) 0.14814(11) 0.0588(10) Uani 1 1 d U . . C8 C 0.2419(2) 0.4917(4) 0.18456(13) 0.0798(13) Uani 1 1 d U . . H8 H 0.2365 0.5411 0.2011 0.096 Uiso 1 1 calc R . . C9 C 0.2669(3) 0.4054(4) 0.19718(13) 0.0893(15) Uani 1 1 d U . . H9 H 0.2760 0.3954 0.2222 0.107 Uiso 1 1 calc R . . C10 C 0.2787(2) 0.3325(4) 0.17219(12) 0.0786(13) Uani 1 1 d U . . H10 H 0.2968 0.2746 0.1807 0.094 Uiso 1 1 calc R . . N11 N 0.46238(14) 0.7192(2) 0.10452(7) 0.0450(7) Uani 1 1 d U . . N12 N 0.33849(15) 0.7634(2) 0.15657(8) 0.0512(7) Uani 1 1 d U . . N13 N 0.33408(14) 0.7809(2) 0.07994(7) 0.0459(7) Uani 1 1 d U . . N14 N 0.24211(15) 0.6360(2) 0.10433(8) 0.0542(8) Uani 1 1 d U . . H14 H 0.2363 0.5929 0.0858 0.065 Uiso 1 1 calc R . . C11 C 0.52261(18) 0.7114(3) 0.12463(10) 0.0560(10) Uani 1 1 d U . . H11 H 0.5244 0.6725 0.1453 0.067 Uiso 1 1 calc R . . C12 C 0.5816(2) 0.7584(3) 0.11592(11) 0.0675(11) Uani 1 1 d U . . H12 H 0.6225 0.7525 0.1306 0.081 Uiso 1 1 calc R . . C13 C 0.5793(2) 0.8141(3) 0.08539(12) 0.0708(12) Uani 1 1 d U . . H13 H 0.6193 0.8450 0.0787 0.085 Uiso 1 1 calc R . . C14 C 0.5179(2) 0.8246(3) 0.06436(11) 0.0590(10) Uani 1 1 d U . . H14B H 0.5157 0.8632 0.0436 0.071 Uiso 1 1 calc R . . C15 C 0.45965(18) 0.7766(2) 0.07472(9) 0.0471(8) Uani 1 1 d U . . C16 C 0.38929(18) 0.7843(3) 0.05307(9) 0.0533(9) Uani 1 1 d U . . H16A H 0.3865 0.8437 0.0395 0.064 Uiso 1 1 calc R . . H16B H 0.3835 0.7320 0.0358 0.064 Uiso 1 1 calc R . . C17 C 0.3345(2) 0.8672(3) 0.10272(10) 0.0538(9) Uani 1 1 d U . . H17A H 0.2972 0.9085 0.0933 0.065 Uiso 1 1 calc R . . H17B H 0.3780 0.9006 0.0999 0.065 Uiso 1 1 calc R . . C18 C 0.3266(2) 0.8515(3) 0.14272(10) 0.0545(9) Uani 1 1 d U . . C19 C 0.3100(3) 0.9250(3) 0.16584(13) 0.0924(16) Uani 1 1 d U . . H19 H 0.3023 0.9857 0.1563 0.111 Uiso 1 1 calc R . . C20 C 0.3048(3) 0.9100(4) 0.20153(13) 0.114(2) Uani 1 1 d U . . H20 H 0.2919 0.9595 0.2166 0.137 Uiso 1 1 calc R . . C21 C 0.3186(3) 0.8211(4) 0.21606(12) 0.0969(17) Uani 1 1 d U . . H21 H 0.3177 0.8098 0.2411 0.116 Uiso 1 1 calc R . . C22 C 0.3335(2) 0.7498(3) 0.19209(11) 0.0701(12) Uani 1 1 d U . . H22 H 0.3406 0.6887 0.2014 0.084 Uiso 1 1 calc R . . C23 C 0.26574(18) 0.7637(3) 0.06034(11) 0.0621(10) Uani 1 1 d U . . H23A H 0.2701 0.7165 0.0413 0.075 Uiso 1 1 calc R . . H23B H 0.2481 0.8222 0.0491 0.075 Uiso 1 1 calc R . . C24 C 0.2162(2) 0.7281(3) 0.08862(12) 0.0678(11) Uani 1 1 d U . . H24A H 0.2133 0.7748 0.1080 0.081 Uiso 1 1 calc R . . H24B H 0.1700 0.7195 0.0770 0.081 Uiso 1 1 calc R . . C25 C 0.1993(2) 0.6011(3) 0.13361(12) 0.0725(12) Uani 1 1 d U . . H25A H 0.1514 0.5950 0.1241 0.087 Uiso 1 1 calc R . . H25B H 0.2007 0.6470 0.1535 0.087 Uiso 1 1 calc R . . N21 N 0.53376(14) 0.4247(2) 0.08230(7) 0.0486(7) Uani 1 1 d U . . N22 N 0.46279(16) 0.2279(2) 0.11303(8) 0.0562(8) Uani 1 1 d U . . N23 N 0.45120(15) 0.3010(2) 0.04123(7) 0.0503(7) Uani 1 1 d U . . N24 N 0.32196(15) 0.3096(2) 0.07830(8) 0.0532(7) Uani 1 1 d U . . H24 H 0.2961 0.3581 0.0680 0.064 Uiso 1 1 calc R . . C26 C 0.2787(2) 0.2695(3) 0.10682(11) 0.0648(11) Uani 1 1 d U . . H26A H 0.3030 0.2168 0.1191 0.078 Uiso 1 1 calc R . . H26B H 0.2353 0.2454 0.0954 0.078 Uiso 1 1 calc R . . C27 C 0.3321(2) 0.2423(3) 0.04756(11) 0.0647(11) Uani 1 1 d U . . H27A H 0.2877 0.2302 0.0343 0.078 Uiso 1 1 calc R . . H27B H 0.3499 0.1822 0.0573 0.078 Uiso 1 1 calc R . . C28 C 0.3827(2) 0.2838(3) 0.02159(10) 0.0651(11) Uani 1 1 d U . . H28A H 0.3882 0.2400 0.0014 0.078 Uiso 1 1 calc R . . H28B H 0.3644 0.3433 0.0115 0.078 Uiso 1 1 calc R . . C29 C 0.4911(2) 0.2126(3) 0.04907(10) 0.0623(10) Uani 1 1 d U . . H29A H 0.5400 0.2258 0.0466 0.075 Uiso 1 1 calc R . . H29B H 0.4767 0.1655 0.0307 0.075 Uiso 1 1 calc R . . C30 C 0.48290(19) 0.1702(3) 0.08657(11) 0.0551(9) Uani 1 1 d U . . C31 C 0.4988(2) 0.0749(3) 0.09306(13) 0.0725(12) Uani 1 1 d U . . H31 H 0.5124 0.0359 0.0742 0.087 Uiso 1 1 calc R . . C32 C 0.4942(3) 0.0396(3) 0.12728(14) 0.0874(14) Uani 1 1 d U . . H32 H 0.5046 -0.0239 0.1323 0.105 Uiso 1 1 calc R . . C33 C 0.4739(3) 0.0993(3) 0.15462(13) 0.0854(14) Uani 1 1 d U . . H33 H 0.4709 0.0768 0.1784 0.102 Uiso 1 1 calc R . . C34 C 0.4584(2) 0.1920(3) 0.14627(11) 0.0740(12) Uani 1 1 d U . . H34 H 0.4442 0.2317 0.1648 0.089 Uiso 1 1 calc R . . C35 C 0.49321(19) 0.3695(3) 0.02171(9) 0.0533(9) Uani 1 1 d U . . H35A H 0.4632 0.4191 0.0111 0.064 Uiso 1 1 calc R . . H35B H 0.5147 0.3372 0.0019 0.064 Uiso 1 1 calc R . . C36 C 0.54919(19) 0.4141(3) 0.04715(9) 0.0492(9) Uani 1 1 d U . . C37 C 0.6116(2) 0.4467(3) 0.03457(10) 0.0587(10) Uani 1 1 d U . . H37 H 0.6219 0.4372 0.0103 0.070 Uiso 1 1 calc R . . C38 C 0.6585(2) 0.4941(3) 0.05891(13) 0.0710(12) Uani 1 1 d U . . H38 H 0.7001 0.5178 0.0510 0.085 Uiso 1 1 calc R . . C39 C 0.6422(2) 0.5051(3) 0.09449(11) 0.0659(11) Uani 1 1 d U . . H39 H 0.6722 0.5369 0.1112 0.079 Uiso 1 1 calc R . . C40 C 0.58046(19) 0.4681(3) 0.10498(10) 0.0604(10) Uani 1 1 d U . . H40 H 0.5706 0.4737 0.1295 0.072 Uiso 1 1 calc R . . Cl2 Cl 0.16804(7) 0.10585(10) 0.20228(3) 0.0863(4) Uani 1 1 d DU . . O201 O 0.2074(2) 0.1174(3) 0.17170(11) 0.1308(15) Uani 1 1 d DU . . O202 O 0.1321(4) 0.0211(5) 0.19735(17) 0.235(3) Uani 1 1 d DU . . O203 O 0.2109(3) 0.1033(4) 0.23341(11) 0.188(2) Uani 1 1 d DU . . O204 O 0.1219(3) 0.1835(5) 0.20499(15) 0.207(3) Uani 1 1 d DU . . Cl3 Cl 0.1682(2) 0.4926(3) 0.01213(12) 0.0464(12) Uani 0.499(6) 1 d PDU A 1 O301 O 0.2053(5) 0.4078(5) 0.0228(3) 0.093(3) Uani 0.499(6) 1 d PDU A 1 O302 O 0.2157(4) 0.5588(6) 0.0006(3) 0.112(3) Uani 0.499(6) 1 d PDU A 1 O303 O 0.1174(5) 0.4747(6) -0.0162(3) 0.137(4) Uani 0.499(6) 1 d PDU A 1 O304 O 0.1391(6) 0.5271(7) 0.0435(2) 0.145(4) Uani 0.499(6) 1 d PDU A 1 Cl4 Cl 0.1626(3) 0.4911(4) 0.00955(15) 0.0694(17) Uani 0.501(6) 1 d PDU A 2 O401 O 0.1936(6) 0.4121(7) 0.0273(3) 0.117(4) Uani 0.501(6) 1 d PDU A 2 O402 O 0.1828(5) 0.5001(6) -0.02630(19) 0.115(3) Uani 0.501(6) 1 d PDU A 2 O403 O 0.0905(4) 0.4735(8) 0.0065(3) 0.130(4) Uani 0.501(6) 1 d PDU A 2 O404 O 0.1739(6) 0.5742(6) 0.0289(3) 0.158(5) Uani 0.501(6) 1 d PDU A 2 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 0.0411(3) 0.0413(3) 0.0445(3) -0.0004(2) -0.0005(2) 0.0013(2) Mn2 0.0493(3) 0.0450(3) 0.0399(3) -0.0069(2) -0.0017(2) 0.0023(2) Cl1 0.0616(6) 0.0515(5) 0.0389(4) -0.0031(4) -0.0016(4) 0.0067(4) O1 0.0747(18) 0.0564(16) 0.0443(13) -0.0061(12) -0.0007(12) 0.0085(13) C2 0.054(2) 0.049(2) 0.0313(17) -0.0012(16) 0.0027(15) -0.0027(17) O3 0.0751(18) 0.0543(16) 0.0496(14) 0.0061(12) -0.0053(12) 0.0068(14) C4 0.112(4) 0.081(3) 0.040(2) -0.002(2) -0.014(2) 0.020(3) C5 0.047(2) 0.067(3) 0.067(2) 0.003(2) 0.0074(18) -0.0204(19) C6 0.042(2) 0.061(2) 0.061(2) -0.0035(19) 0.0023(17) -0.0163(18) C7 0.047(2) 0.067(2) 0.064(2) -0.012(2) 0.0135(18) -0.0178(19) C8 0.084(3) 0.088(3) 0.071(3) -0.010(2) 0.028(2) -0.021(3) C9 0.093(4) 0.119(4) 0.058(3) 0.004(3) 0.021(2) -0.023(3) C10 0.077(3) 0.082(3) 0.077(3) 0.023(2) 0.015(2) -0.011(3) N11 0.0445(16) 0.0454(17) 0.0450(16) 0.0061(13) 0.0023(13) 0.0000(13) N12 0.0503(18) 0.0518(18) 0.0516(17) -0.0038(14) 0.0028(13) 0.0062(14) N13 0.0455(16) 0.0476(17) 0.0435(15) 0.0029(13) -0.0051(12) -0.0029(13) N14 0.0446(17) 0.0573(19) 0.0608(19) -0.0078(15) 0.0039(14) -0.0004(14) C11 0.049(2) 0.060(2) 0.058(2) 0.0092(19) -0.0034(17) -0.0096(18) C12 0.045(2) 0.085(3) 0.072(3) 0.005(2) -0.0005(19) -0.013(2) C13 0.052(2) 0.079(3) 0.082(3) 0.004(2) 0.010(2) -0.013(2) C14 0.066(2) 0.050(2) 0.064(2) 0.0070(19) 0.0234(19) -0.0015(19) C15 0.049(2) 0.0383(19) 0.055(2) 0.0001(16) 0.0079(16) 0.0049(16) C16 0.058(2) 0.057(2) 0.044(2) 0.0070(17) 0.0003(16) 0.0000(19) C17 0.055(2) 0.046(2) 0.059(2) -0.0021(17) -0.0009(18) 0.0072(18) C18 0.055(2) 0.051(2) 0.058(2) -0.0082(18) 0.0030(17) 0.0094(18) C19 0.127(4) 0.063(3) 0.088(3) -0.006(2) 0.019(3) 0.037(3) C20 0.191(6) 0.092(4) 0.063(3) -0.025(3) 0.026(3) 0.049(4) C21 0.148(5) 0.092(4) 0.053(3) -0.012(2) 0.025(3) 0.036(4) C22 0.087(3) 0.070(3) 0.053(2) 0.000(2) 0.007(2) 0.016(2) C23 0.046(2) 0.059(2) 0.079(3) 0.006(2) -0.0176(18) 0.0094(18) C24 0.041(2) 0.063(3) 0.097(3) -0.011(2) -0.009(2) 0.0064(19) C25 0.052(2) 0.073(3) 0.095(3) -0.014(2) 0.022(2) -0.003(2) N21 0.0476(17) 0.0586(19) 0.0390(15) -0.0053(14) -0.0029(12) 0.0041(14) N22 0.064(2) 0.0491(18) 0.0544(18) -0.0036(15) -0.0021(15) 0.0086(15) N23 0.0502(17) 0.0559(18) 0.0437(16) -0.0100(14) -0.0057(13) 0.0099(14) N24 0.0522(18) 0.0494(18) 0.0573(18) -0.0072(15) -0.0019(14) -0.0011(15) C26 0.054(2) 0.055(2) 0.085(3) -0.001(2) 0.005(2) -0.0127(19) C27 0.058(2) 0.056(2) 0.078(3) -0.020(2) -0.0107(19) -0.0025(19) C28 0.059(2) 0.072(3) 0.062(2) -0.022(2) -0.0140(18) 0.006(2) C29 0.065(3) 0.060(2) 0.062(2) -0.0147(19) 0.0037(19) 0.009(2) C30 0.050(2) 0.048(2) 0.066(2) -0.0015(18) -0.0110(18) -0.0002(18) C31 0.069(3) 0.051(2) 0.096(3) -0.007(2) -0.007(2) 0.004(2) C32 0.104(4) 0.050(3) 0.107(4) 0.017(3) -0.007(3) 0.009(3) C33 0.111(4) 0.071(3) 0.074(3) 0.017(2) -0.002(3) 0.003(3) C34 0.105(4) 0.058(3) 0.059(2) 0.002(2) 0.004(2) 0.008(3) C35 0.064(2) 0.062(2) 0.0337(17) -0.0007(17) 0.0017(16) 0.0097(19) C36 0.053(2) 0.050(2) 0.0448(19) 0.0011(17) 0.0033(16) 0.0130(17) C37 0.058(2) 0.072(3) 0.047(2) 0.0109(19) 0.0103(17) 0.016(2) C38 0.049(2) 0.076(3) 0.088(3) 0.016(2) 0.006(2) 0.005(2) C39 0.047(2) 0.079(3) 0.070(3) -0.006(2) -0.0068(19) 0.001(2) C40 0.050(2) 0.083(3) 0.048(2) -0.015(2) -0.0011(17) 0.004(2) Cl2 0.0976(9) 0.0936(9) 0.0669(7) -0.0053(6) -0.0012(6) 0.0069(8) O201 0.194(4) 0.096(3) 0.110(3) -0.010(2) 0.066(3) -0.003(3) O202 0.279(7) 0.212(5) 0.225(6) -0.076(5) 0.102(5) -0.151(5) O203 0.232(5) 0.242(6) 0.081(3) -0.038(3) -0.073(3) 0.107(4) O204 0.191(5) 0.242(6) 0.186(5) -0.008(4) -0.003(4) 0.147(5) Cl3 0.0378(16) 0.057(3) 0.044(2) 0.0032(17) -0.0035(14) -0.0064(15) O301 0.104(6) 0.051(4) 0.113(7) -0.028(4) -0.070(5) 0.025(4) O302 0.092(5) 0.102(6) 0.146(8) 0.046(6) 0.030(5) -0.016(4) O303 0.152(8) 0.084(5) 0.160(8) -0.031(6) -0.127(7) 0.013(6) O304 0.183(10) 0.128(8) 0.132(6) -0.019(6) 0.081(6) 0.027(7) Cl4 0.097(3) 0.049(3) 0.061(3) -0.001(2) -0.006(2) -0.013(2) O401 0.172(8) 0.091(6) 0.089(6) 0.054(5) 0.029(6) 0.014(6) O402 0.159(8) 0.119(7) 0.073(4) 0.039(4) 0.056(5) 0.052(6) O403 0.086(5) 0.175(9) 0.130(8) 0.019(7) 0.004(5) -0.056(5) O404 0.201(11) 0.078(5) 0.180(9) -0.069(6) -0.113(8) 0.017(6) _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 O3 2.057(2) . ? Mn1 N12 2.239(3) . ? Mn1 N11 2.273(3) . ? Mn1 N14 2.309(3) . ? Mn1 N13 2.352(3) . ? Mn1 Cl1 2.5551(10) . ? Mn2 O1 2.048(2) . ? Mn2 N21 2.253(3) . ? Mn2 N22 2.284(3) . ? Mn2 N24 2.300(3) . ? Mn2 N23 2.368(3) . ? Mn2 Cl1 2.5857(10) . ? O1 C2 1.253(4) . ? C2 O3 1.239(4) . ? C2 C4 1.496(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.401(6) . ? C5 C6 1.401(5) . ? C5 C26 1.511(5) . ? C6 C7 1.386(5) . ? C6 H6 0.9300 . ? C7 C8 1.366(6) . ? C7 C25 1.505(6) . ? C8 C9 1.373(7) . ? C8 H8 0.9300 . ? C9 C10 1.399(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? N11 C11 1.339(4) . ? N11 C15 1.353(4) . ? N12 C22 1.321(4) . ? N12 C18 1.351(5) . ? N13 C17 1.470(4) . ? N13 C23 1.478(4) . ? N13 C16 1.492(4) . ? N14 C25 1.475(5) . ? N14 C24 1.488(5) . ? N14 H14 0.9100 . ? C11 C12 1.368(5) . ? C11 H11 0.9300 . ? C12 C13 1.360(6) . ? C12 H12 0.9300 . ? C13 C14 1.378(6) . ? C13 H13 0.9300 . ? C14 C15 1.381(5) . ? C14 H14B 0.9300 . ? C15 C16 1.530(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.495(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.383(5) . ? C19 C20 1.331(6) . ? C19 H19 0.9300 . ? C20 C21 1.375(7) . ? C20 H20 0.9300 . ? C21 C22 1.372(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.533(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? N21 C40 1.332(4) . ? N21 C36 1.344(4) . ? N22 C34 1.322(5) . ? N22 C30 1.337(5) . ? N23 C35 1.469(5) . ? N23 C29 1.478(5) . ? N23 C28 1.482(5) . ? N24 C26 1.486(4) . ? N24 C27 1.490(4) . ? N24 H24 0.9100 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.519(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.511(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.390(6) . ? C31 C32 1.352(6) . ? C31 H31 0.9300 . ? C32 C33 1.379(6) . ? C32 H32 0.9300 . ? C33 C34 1.365(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.514(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.391(5) . ? C37 C38 1.396(6) . ? C37 H37 0.9300 . ? C38 C39 1.364(5) . ? C38 H38 0.9300 . ? C39 C40 1.374(5) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? Cl2 O203 1.364(4) . ? Cl2 O202 1.383(5) . ? Cl2 O201 1.398(3) . ? Cl2 O204 1.413(5) . ? Cl3 O302 1.387(7) . ? Cl3 O304 1.395(8) . ? Cl3 O303 1.403(7) . ? Cl3 O301 1.430(8) . ? Cl4 O404 1.374(8) . ? Cl4 O402 1.395(7) . ? Cl4 O401 1.400(9) . ? Cl4 O403 1.408(9) . ? 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 O3 Mn1 N12 89.88(10) . . ? O3 Mn1 N11 95.71(10) . . ? N12 Mn1 N11 90.43(10) . . ? O3 Mn1 N14 116.63(11) . . ? N12 Mn1 N14 87.20(11) . . ? N11 Mn1 N14 147.55(10) . . ? O3 Mn1 N13 160.34(10) . . ? N12 Mn1 N13 75.32(10) . . ? N11 Mn1 N13 71.97(10) . . ? N14 Mn1 N13 76.15(10) . . ? O3 Mn1 Cl1 98.36(7) . . ? N12 Mn1 Cl1 171.72(8) . . ? N11 Mn1 Cl1 89.51(7) . . ? N14 Mn1 Cl1 88.41(8) . . ? N13 Mn1 Cl1 96.81(7) . . ? O1 Mn2 N21 96.13(10) . . ? O1 Mn2 N22 89.44(11) . . ? N21 Mn2 N22 93.70(11) . . ? O1 Mn2 N24 115.39(10) . . ? N21 Mn2 N24 148.47(10) . . ? N22 Mn2 N24 86.45(11) . . ? O1 Mn2 N23 159.30(10) . . ? N21 Mn2 N23 72.64(10) . . ? N22 Mn2 N23 74.38(11) . . ? N24 Mn2 N23 77.09(10) . . ? O1 Mn2 Cl1 102.76(8) . . ? N21 Mn2 Cl1 88.50(8) . . ? N22 Mn2 Cl1 167.32(8) . . ? N24 Mn2 Cl1 85.18(8) . . ? N23 Mn2 Cl1 94.44(8) . . ? Mn1 Cl1 Mn2 104.77(3) . . ? C2 O1 Mn2 139.9(2) . . ? O3 C2 O1 125.2(3) . . ? O3 C2 C4 117.4(3) . . ? O1 C2 C4 117.4(3) . . ? C2 O3 Mn1 148.9(2) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 117.0(4) . . ? C10 C5 C26 121.9(4) . . ? C6 C5 C26 121.1(4) . . ? C7 C6 C5 122.0(4) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C8 C7 C6 119.3(4) . . ? C8 C7 C25 122.0(4) . . ? C6 C7 C25 118.6(4) . . ? C7 C8 C9 121.1(5) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C5 120.9(5) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? C11 N11 C15 118.7(3) . . ? C11 N11 Mn1 125.5(2) . . ? C15 N11 Mn1 115.8(2) . . ? C22 N12 C18 118.6(3) . . ? C22 N12 Mn1 123.9(3) . . ? C18 N12 Mn1 117.4(2) . . ? C17 N13 C23 112.5(3) . . ? C17 N13 C16 111.5(3) . . ? C23 N13 C16 109.7(3) . . ? C17 N13 Mn1 109.81(19) . . ? C23 N13 Mn1 107.8(2) . . ? C16 N13 Mn1 105.3(2) . . ? C25 N14 C24 112.3(3) . . ? C25 N14 Mn1 118.0(2) . . ? C24 N14 Mn1 108.8(2) . . ? C25 N14 H14 105.6 . . ? C24 N14 H14 105.6 . . ? Mn1 N14 H14 105.6 . . ? N11 C11 C12 122.4(4) . . ? N11 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 118.9(4) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 120.0(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 118.6(4) . . ? C13 C14 H14B 120.7 . . ? C15 C14 H14B 120.7 . . ? N11 C15 C14 121.3(3) . . ? N11 C15 C16 116.6(3) . . ? C14 C15 C16 122.2(3) . . ? N13 C16 C15 107.6(3) . . ? N13 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? N13 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? N13 C17 C18 115.8(3) . . ? N13 C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? N13 C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? N12 C18 C19 119.6(4) . . ? N12 C18 C17 118.4(3) . . ? C19 C18 C17 121.9(4) . . ? C20 C19 C18 121.0(5) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.8(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 117.3(4) . . ? C22 C21 H21 121.3 . . ? C20 C21 H21 121.3 . . ? N12 C22 C21 123.5(4) . . ? N12 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N13 C23 C24 107.4(3) . . ? N13 C23 H23A 110.2 . . ? C24 C23 H23A 110.2 . . ? N13 C23 H23B 110.2 . . ? C24 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? N14 C24 C23 109.6(3) . . ? N14 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? N14 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? N14 C25 C7 111.5(3) . . ? N14 C25 H25A 109.3 . . ? C7 C25 H25A 109.3 . . ? N14 C25 H25B 109.3 . . ? C7 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C40 N21 C36 117.7(3) . . ? C40 N21 Mn2 125.4(2) . . ? C36 N21 Mn2 116.7(2) . . ? C34 N22 C30 118.1(3) . . ? C34 N22 Mn2 123.8(3) . . ? C30 N22 Mn2 117.8(2) . . ? C35 N23 C29 110.4(3) . . ? C35 N23 C28 111.8(3) . . ? C29 N23 C28 113.1(3) . . ? C35 N23 Mn2 105.1(2) . . ? C29 N23 Mn2 110.2(2) . . ? C28 N23 Mn2 105.8(2) . . ? C26 N24 C27 113.1(3) . . ? C26 N24 Mn2 118.4(2) . . ? C27 N24 Mn2 109.3(2) . . ? C26 N24 H24 104.9 . . ? C27 N24 H24 104.9 . . ? Mn2 N24 H24 104.9 . . ? N24 C26 C5 110.0(3) . . ? N24 C26 H26A 109.7 . . ? C5 C26 H26A 109.7 . . ? N24 C26 H26B 109.7 . . ? C5 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N24 C27 C28 110.3(3) . . ? N24 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N24 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N23 C28 C27 110.3(3) . . ? N23 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? N23 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? N23 C29 C30 115.1(3) . . ? N23 C29 H29A 108.5 . . ? C30 C29 H29A 108.5 . . ? N23 C29 H29B 108.5 . . ? C30 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? N22 C30 C31 122.1(4) . . ? N22 C30 C29 117.9(3) . . ? C31 C30 C29 120.0(4) . . ? C32 C31 C30 118.9(4) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 119.0(4) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 119.0(4) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? N22 C34 C33 122.9(4) . . ? N22 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? N23 C35 C36 111.4(3) . . ? N23 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? N23 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? N21 C36 C37 121.7(3) . . ? N21 C36 C35 116.2(3) . . ? C37 C36 C35 122.0(3) . . ? C36 C37 C38 119.0(3) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C39 C38 C37 118.9(4) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C38 C39 C40 118.5(4) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N21 C40 C39 124.2(3) . . ? N21 C40 H40 117.9 . . ? C39 C40 H40 117.9 . . ? O203 Cl2 O202 111.0(4) . . ? O203 Cl2 O201 109.8(3) . . ? O202 Cl2 O201 106.7(3) . . ? O203 Cl2 O204 108.2(3) . . ? O202 Cl2 O204 111.2(4) . . ? O201 Cl2 O204 110.0(3) . . ? O302 Cl3 O304 108.9(6) . . ? O302 Cl3 O303 109.7(6) . . ? O304 Cl3 O303 111.8(7) . . ? O302 Cl3 O301 108.3(6) . . ? O304 Cl3 O301 106.5(6) . . ? O303 Cl3 O301 111.5(5) . . ? O404 Cl4 O402 111.3(7) . . ? O404 Cl4 O401 112.6(7) . . ? O402 Cl4 O401 111.7(6) . . ? O404 Cl4 O403 108.3(7) . . ? O402 Cl4 O403 105.8(7) . . ? O401 Cl4 O403 106.7(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn1 Cl1 Mn2 3.71(8) . . . . ? N12 Mn1 Cl1 Mn2 -171.0(6) . . . . ? N11 Mn1 Cl1 Mn2 99.41(8) . . . . ? N14 Mn1 Cl1 Mn2 -112.98(8) . . . . ? N13 Mn1 Cl1 Mn2 171.18(7) . . . . ? O1 Mn2 Cl1 Mn1 -2.86(8) . . . . ? N21 Mn2 Cl1 Mn1 -98.81(8) . . . . ? N22 Mn2 Cl1 Mn1 161.0(4) . . . . ? N24 Mn2 Cl1 Mn1 112.11(8) . . . . ? N23 Mn2 Cl1 Mn1 -171.27(8) . . . . ? N21 Mn2 O1 C2 88.6(4) . . . . ? N22 Mn2 O1 C2 -177.8(4) . . . . ? N24 Mn2 O1 C2 -92.0(4) . . . . ? N23 Mn2 O1 C2 144.2(4) . . . . ? Cl1 Mn2 O1 C2 -1.3(4) . . . . ? Mn2 O1 C2 O3 4.4(6) . . . . ? Mn2 O1 C2 C4 -173.4(3) . . . . ? O1 C2 O3 Mn1 -1.5(7) . . . . ? C4 C2 O3 Mn1 176.2(4) . . . . ? N12 Mn1 O3 C2 176.3(5) . . . . ? N11 Mn1 O3 C2 -93.3(5) . . . . ? N14 Mn1 O3 C2 89.5(5) . . . . ? N13 Mn1 O3 C2 -143.1(4) . . . . ? Cl1 Mn1 O3 C2 -2.9(5) . . . . ? C10 C5 C6 C7 1.3(5) . . . . ? C26 C5 C6 C7 -176.7(3) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? C5 C6 C7 C25 175.8(3) . . . . ? C6 C7 C8 C9 -2.8(6) . . . . ? C25 C7 C8 C9 -178.1(4) . . . . ? C7 C8 C9 C10 3.5(7) . . . . ? C8 C9 C10 C5 -1.7(7) . . . . ? C6 C5 C10 C9 -0.6(6) . . . . ? C26 C5 C10 C9 177.3(4) . . . . ? O3 Mn1 N11 C11 -7.3(3) . . . . ? N12 Mn1 N11 C11 82.6(3) . . . . ? N14 Mn1 N11 C11 168.1(3) . . . . ? N13 Mn1 N11 C11 157.0(3) . . . . ? Cl1 Mn1 N11 C11 -105.7(3) . . . . ? O3 Mn1 N11 C15 174.7(2) . . . . ? N12 Mn1 N11 C15 -95.3(2) . . . . ? N14 Mn1 N11 C15 -9.9(3) . . . . ? N13 Mn1 N11 C15 -20.9(2) . . . . ? Cl1 Mn1 N11 C15 76.4(2) . . . . ? O3 Mn1 N12 C22 -20.9(3) . . . . ? N11 Mn1 N12 C22 -116.7(3) . . . . ? N14 Mn1 N12 C22 95.7(3) . . . . ? N13 Mn1 N12 C22 172.1(3) . . . . ? Cl1 Mn1 N12 C22 153.8(5) . . . . ? O3 Mn1 N12 C18 161.9(3) . . . . ? N11 Mn1 N12 C18 66.2(3) . . . . ? N14 Mn1 N12 C18 -81.4(3) . . . . ? N13 Mn1 N12 C18 -5.0(3) . . . . ? Cl1 Mn1 N12 C18 -23.3(7) . . . . ? O3 Mn1 N13 C17 -29.0(4) . . . . ? N12 Mn1 N13 C17 13.3(2) . . . . ? N11 Mn1 N13 C17 -82.1(2) . . . . ? N14 Mn1 N13 C17 104.0(2) . . . . ? Cl1 Mn1 N13 C17 -169.3(2) . . . . ? O3 Mn1 N13 C23 -151.8(3) . . . . ? N12 Mn1 N13 C23 -109.5(2) . . . . ? N11 Mn1 N13 C23 155.1(2) . . . . ? N14 Mn1 N13 C23 -18.8(2) . . . . ? Cl1 Mn1 N13 C23 67.9(2) . . . . ? O3 Mn1 N13 C16 91.2(3) . . . . ? N12 Mn1 N13 C16 133.5(2) . . . . ? N11 Mn1 N13 C16 38.1(2) . . . . ? N14 Mn1 N13 C16 -135.8(2) . . . . ? Cl1 Mn1 N13 C16 -49.1(2) . . . . ? O3 Mn1 N14 C25 21.2(3) . . . . ? N12 Mn1 N14 C25 -67.2(3) . . . . ? N11 Mn1 N14 C25 -153.6(2) . . . . ? N13 Mn1 N14 C25 -142.8(3) . . . . ? Cl1 Mn1 N14 C25 119.8(3) . . . . ? O3 Mn1 N14 C24 150.7(2) . . . . ? N12 Mn1 N14 C24 62.2(2) . . . . ? N11 Mn1 N14 C24 -24.2(3) . . . . ? N13 Mn1 N14 C24 -13.4(2) . . . . ? Cl1 Mn1 N14 C24 -110.8(2) . . . . ? C15 N11 C11 C12 -0.7(6) . . . . ? Mn1 N11 C11 C12 -178.6(3) . . . . ? N11 C11 C12 C13 -1.1(6) . . . . ? C11 C12 C13 C14 1.9(6) . . . . ? C12 C13 C14 C15 -0.9(6) . . . . ? C11 N11 C15 C14 1.7(5) . . . . ? Mn1 N11 C15 C14 179.8(3) . . . . ? C11 N11 C15 C16 -179.0(3) . . . . ? Mn1 N11 C15 C16 -0.9(4) . . . . ? C13 C14 C15 N11 -0.9(5) . . . . ? C13 C14 C15 C16 179.8(4) . . . . ? C17 N13 C16 C15 68.9(4) . . . . ? C23 N13 C16 C15 -165.9(3) . . . . ? Mn1 N13 C16 C15 -50.1(3) . . . . ? N11 C15 C16 N13 35.9(4) . . . . ? C14 C15 C16 N13 -144.8(3) . . . . ? C23 N13 C17 C18 99.8(4) . . . . ? C16 N13 C17 C18 -136.6(3) . . . . ? Mn1 N13 C17 C18 -20.2(4) . . . . ? C22 N12 C18 C19 0.2(6) . . . . ? Mn1 N12 C18 C19 177.5(3) . . . . ? C22 N12 C18 C17 178.1(3) . . . . ? Mn1 N12 C18 C17 -4.7(4) . . . . ? N13 C17 C18 N12 17.6(5) . . . . ? N13 C17 C18 C19 -164.6(4) . . . . ? N12 C18 C19 C20 -0.6(8) . . . . ? C17 C18 C19 C20 -178.4(5) . . . . ? C18 C19 C20 C21 2.3(9) . . . . ? C19 C20 C21 C22 -3.5(9) . . . . ? C18 N12 C22 C21 -1.6(6) . . . . ? Mn1 N12 C22 C21 -178.7(4) . . . . ? C20 C21 C22 N12 3.3(8) . . . . ? C17 N13 C23 C24 -73.9(4) . . . . ? C16 N13 C23 C24 161.5(3) . . . . ? Mn1 N13 C23 C24 47.3(3) . . . . ? C25 N14 C24 C23 176.1(3) . . . . ? Mn1 N14 C24 C23 43.6(3) . . . . ? N13 C23 C24 N14 -62.6(4) . . . . ? C24 N14 C25 C7 177.8(3) . . . . ? Mn1 N14 C25 C7 -54.4(4) . . . . ? C8 C7 C25 N14 124.7(4) . . . . ? C6 C7 C25 N14 -50.5(5) . . . . ? O1 Mn2 N21 C40 -3.0(3) . . . . ? N22 Mn2 N21 C40 -92.8(3) . . . . ? N24 Mn2 N21 C40 177.9(3) . . . . ? N23 Mn2 N21 C40 -165.2(3) . . . . ? Cl1 Mn2 N21 C40 99.7(3) . . . . ? O1 Mn2 N21 C36 -177.8(2) . . . . ? N22 Mn2 N21 C36 92.4(3) . . . . ? N24 Mn2 N21 C36 3.1(4) . . . . ? N23 Mn2 N21 C36 20.0(2) . . . . ? Cl1 Mn2 N21 C36 -75.1(2) . . . . ? O1 Mn2 N22 C34 22.8(3) . . . . ? N21 Mn2 N22 C34 118.9(3) . . . . ? N24 Mn2 N22 C34 -92.7(3) . . . . ? N23 Mn2 N22 C34 -170.3(3) . . . . ? Cl1 Mn2 N22 C34 -141.5(4) . . . . ? O1 Mn2 N22 C30 -164.0(3) . . . . ? N21 Mn2 N22 C30 -67.9(3) . . . . ? N24 Mn2 N22 C30 80.5(3) . . . . ? N23 Mn2 N22 C30 2.9(3) . . . . ? Cl1 Mn2 N22 C30 31.7(6) . . . . ? O1 Mn2 N23 C35 -93.2(4) . . . . ? N21 Mn2 N23 C35 -33.9(2) . . . . ? N22 Mn2 N23 C35 -133.0(2) . . . . ? N24 Mn2 N23 C35 137.2(2) . . . . ? Cl1 Mn2 N23 C35 53.1(2) . . . . ? O1 Mn2 N23 C29 25.8(4) . . . . ? N21 Mn2 N23 C29 85.0(2) . . . . ? N22 Mn2 N23 C29 -14.0(2) . . . . ? N24 Mn2 N23 C29 -103.9(3) . . . . ? Cl1 Mn2 N23 C29 172.1(2) . . . . ? O1 Mn2 N23 C28 148.3(3) . . . . ? N21 Mn2 N23 C28 -152.4(3) . . . . ? N22 Mn2 N23 C28 108.6(3) . . . . ? N24 Mn2 N23 C28 18.7(2) . . . . ? Cl1 Mn2 N23 C28 -65.4(2) . . . . ? O1 Mn2 N24 C26 -19.8(3) . . . . ? N21 Mn2 N24 C26 159.2(2) . . . . ? N22 Mn2 N24 C26 67.9(3) . . . . ? N23 Mn2 N24 C26 142.7(3) . . . . ? Cl1 Mn2 N24 C26 -121.6(3) . . . . ? O1 Mn2 N24 C27 -151.3(2) . . . . ? N21 Mn2 N24 C27 27.7(4) . . . . ? N22 Mn2 N24 C27 -63.6(2) . . . . ? N23 Mn2 N24 C27 11.2(2) . . . . ? Cl1 Mn2 N24 C27 106.9(2) . . . . ? C27 N24 C26 C5 -173.1(3) . . . . ? Mn2 N24 C26 C5 57.1(4) . . . . ? C10 C5 C26 N24 -125.8(4) . . . . ? C6 C5 C26 N24 52.1(5) . . . . ? C26 N24 C27 C28 -174.1(3) . . . . ? Mn2 N24 C27 C28 -39.9(4) . . . . ? C35 N23 C28 C27 -160.3(3) . . . . ? C29 N23 C28 C27 74.3(4) . . . . ? Mn2 N23 C28 C27 -46.4(3) . . . . ? N24 C27 C28 N23 60.4(4) . . . . ? C35 N23 C29 C30 139.1(3) . . . . ? C28 N23 C29 C30 -94.7(4) . . . . ? Mn2 N23 C29 C30 23.4(4) . . . . ? C34 N22 C30 C31 0.3(6) . . . . ? Mn2 N22 C30 C31 -173.3(3) . . . . ? C34 N22 C30 C29 -177.2(4) . . . . ? Mn2 N22 C30 C29 9.2(4) . . . . ? N23 C29 C30 N22 -22.8(5) . . . . ? N23 C29 C30 C31 159.8(4) . . . . ? N22 C30 C31 C32 -0.4(6) . . . . ? C29 C30 C31 C32 176.9(4) . . . . ? C30 C31 C32 C33 0.0(7) . . . . ? C31 C32 C33 C34 0.6(8) . . . . ? C30 N22 C34 C33 0.4(7) . . . . ? Mn2 N22 C34 C33 173.6(4) . . . . ? C32 C33 C34 N22 -0.8(8) . . . . ? C29 N23 C35 C36 -74.0(4) . . . . ? C28 N23 C35 C36 159.1(3) . . . . ? Mn2 N23 C35 C36 44.8(3) . . . . ? C40 N21 C36 C37 0.1(5) . . . . ? Mn2 N21 C36 C37 175.3(3) . . . . ? C40 N21 C36 C35 -176.7(3) . . . . ? Mn2 N21 C36 C35 -1.4(4) . . . . ? N23 C35 C36 N21 -31.4(4) . . . . ? N23 C35 C36 C37 151.8(3) . . . . ? N21 C36 C37 C38 -1.8(6) . . . . ? C35 C36 C37 C38 174.8(4) . . . . ? C36 C37 C38 C39 1.3(6) . . . . ? C37 C38 C39 C40 0.6(6) . . . . ? C36 N21 C40 C39 2.1(6) . . . . ? Mn2 N21 C40 C39 -172.7(3) . . . . ? C38 C39 C40 N21 -2.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.964 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.081 #=== END of CIF data_asq _database_code_depnum_ccdc_archive 'CCDC 746219' _audit_creation_method 'Manual editing of the cif produced by SHELXL-97' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C120 H132 Mn6 N24 O12, 6(Cl O4)' _chemical_formula_sum 'C120 H132 Cl6 Mn6 N24 O36' _chemical_formula_weight 3028.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0028 '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' Cl Cl 0.1742 0.2585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.1916 1.1406 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0031 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0043 0.0104 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 26.7119(3) _cell_length_b 26.7119(3) _cell_length_c 24.2013(5) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 17268.2(5) _cell_measurement_reflns_used 34001 _cell_measurement_theta_min 2.8971 _cell_measurement_theta_max 35.1991 _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6240 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SCALE3 ABSPACK - in Crysalis RED' _exptl_special_details ; Comments for referees: The high R, Wr and Gof values is partly derived from the large number of rather weak reflections before the SQUEEZE procedure. The large cavities present in the structure, are most probably filled with solvent molecules. These need not order similarly to the host structure and that may serve as a reason for that the solvent molecules cannot be modelled in the present structure model. The fact that the structure model show quite large residual electron densities (-1.5 to 1.9 e/A3) are most probably not due to erroneous assignment of atom types, but can also be explained by disordered solvent molecules. We decided to remove disordered solvent molecules using SQUEZZE available in PLATON. Several reflection data sets were collected a 100 K at the I911-5 beamline in Maxlab using a MARCCD area detector. Post-processing of images using Crysalis RED enabled a successful integration of intensities. The present crystal was the best out of three measured individual crystals, however the data showed a missing cone close to the c-direction which gave a result that several reflections were missing at high l-values. Merging with reflection data from different crystals produced considerably worse overall fit between symmetry equivalent reflections, thus it was decided to use only this very data set. Explicit absorption corrections were not done as the effects were rather weak. With the present crystal size and the my value one would have expected transmission factors in the range 0.98 for the shortest path through the crystal and 0.89 for the longest path through the crystal. Attempts to check for absorption effects with STOE XRED did not produce any noticeable improvement or change of model. The Crysalis RED data reduction program includes an empirical absorption correction program SCALE3 ABSPACK - An Oxford Diffraction program (1.0.7,gui:1.0.3) mainly operating on scale factors for different frames. The internal R-value was only affected very little, approximately 0.5 %, i.e. from 6.0 to 5.5%. It was discovered that several strong reflections were erroneously estimated initially due to saturation of the detector. However using profile fitting option available in Crysalis RED we were able to estimate more accurate intensities. Note that a process such as structure solution may run well using a few erroneously estimated strong reflections, however the process of least squares refinement will not give a good result. The resulting bond length, specially C-C and similar should thus not be expected to show a very high accuracy.. The poor quality of the present crystal result in rather bad FOM for the refinement but we have done everything we could to improve the refinement. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90769 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline 911/5, Maxlab, Lund ' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type 'MARCCD 165' _diffrn_measurement_method '\f scan' _diffrn_detector_area_resol_mean 12.4 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 29388 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 1 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 31.96 _reflns_number_total 13671 _reflns_number_gt 7708 _reflns_threshold_expression I>2\s(I) _computing_data_collection MARCCD _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SHELXD (Sheldrick, 2008)' _computing_structure_refinement 'SHELXH (Sheldrick, 2008)' _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. The reflection data were processed with the SQUEEZE procedure available in PLATON. Energy dependent correction parameters for anomalous dispersion effects was applied at the used wavelength. The values of the df1 and df2 was obtained using the program CROMER based on a method described by L.Kissel and R.H.Pratt, Acta Crsyat A46, 170(1990) Note that a few of the atoms show rather abnormal displacement ellipsoids, this should however not be interpreted as errors of the structure model but as static displacements errors for a reasonable (low quality) structure model. Most abnormal ellipsoids have sensible directions, from a chemical point of view. ; _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^)+(0.06P)^2^] 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 13671 _refine_ls_number_parameters 837 _refine_ls_number_restraints 352 _refine_ls_R_factor_all 0.1892 _refine_ls_R_factor_gt 0.1532 _refine_ls_wR_factor_ref 0.4092 _refine_ls_wR_factor_gt 0.3973 _refine_ls_goodness_of_fit_ref 3.376 _refine_ls_restrained_S_all 3.453 _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 0.94349(6) 0.28708(7) 0.21106(8) 0.0676(6) Uani 1 1 d U . . O101 O 0.9372(3) 0.2111(3) 0.2398(4) 0.086(2) Uani 1 1 d U . . O102 O 0.8947(3) 0.3205(4) 0.2685(4) 0.087(2) Uani 1 1 d U . . N121 N 0.9418(3) 0.3628(4) 0.1640(5) 0.071(2) Uani 1 1 d U . . C1 C 0.9156(5) 0.4019(5) 0.1791(7) 0.089(4) Uani 1 1 d U . . H1 H 0.8994 0.4016 0.2140 0.107 Uiso 1 1 calc R . . C2 C 0.9112(5) 0.4406(5) 0.1482(7) 0.094(4) Uani 1 1 d U . . H2 H 0.8900 0.4670 0.1603 0.113 Uiso 1 1 calc R . . C3 C 0.9349(5) 0.4461(5) 0.1000(8) 0.101(4) Uani 1 1 d U . . H3 H 0.9325 0.4759 0.0788 0.122 Uiso 1 1 calc R . . C4 C 0.9623(4) 0.4064(4) 0.0833(6) 0.072(3) Uani 1 1 d U . . H4 H 0.9783 0.4062 0.0482 0.087 Uiso 1 1 calc R . . C5 C 0.9663(4) 0.3656(4) 0.1192(6) 0.066(3) Uani 1 1 d U . . C6 C 0.9989(4) 0.3196(4) 0.1030(6) 0.082(4) Uani 1 1 d U . . H6A H 1.0023 0.3182 0.0623 0.099 Uiso 1 1 calc R . . H6B H 1.0328 0.3234 0.1190 0.099 Uiso 1 1 calc R . . N111 N 0.9770(3) 0.2738(3) 0.1225(4) 0.065(2) Uani 1 1 d U . . C7 C 1.0167(4) 0.2364(4) 0.1318(6) 0.074(3) Uani 1 1 d U . . H7A H 1.0379 0.2340 0.0984 0.089 Uiso 1 1 calc R . . H7B H 1.0012 0.2033 0.1382 0.089 Uiso 1 1 calc R . . C8 C 1.0485(4) 0.2496(4) 0.1799(6) 0.075(3) Uani 1 1 d U . . C9 C 1.0982(4) 0.2380(4) 0.1861(6) 0.077(3) Uani 1 1 d U . . H9 H 1.1148 0.2233 0.1554 0.092 Uiso 1 1 calc R . . C10 C 1.1251(5) 0.2458(5) 0.2315(7) 0.095(4) Uani 1 1 d U . . H10 H 1.1590 0.2353 0.2339 0.114 Uiso 1 1 calc R . . C11 C 1.1016(5) 0.2700(6) 0.2754(7) 0.097(4) Uani 1 1 d U . . H11 H 1.1196 0.2790 0.3078 0.116 Uiso 1 1 calc R . . C12 C 1.0503(4) 0.2808(7) 0.2698(7) 0.110(5) Uani 1 1 d U . . H12 H 1.0329 0.2944 0.3006 0.132 Uiso 1 1 calc R . . N122 N 1.0248(3) 0.2725(4) 0.2228(5) 0.083(3) Uani 1 1 d U . . C13 C 0.9393(4) 0.2563(4) 0.0858(5) 0.059(2) Uani 1 1 d U . . H13A H 0.9551 0.2359 0.0565 0.071 Uiso 1 1 calc R . . H13B H 0.9229 0.2854 0.0679 0.071 Uiso 1 1 calc R . . C14 C 0.8987(3) 0.2242(4) 0.1156(5) 0.057(2) Uani 1 1 d U . . H14A H 0.8721 0.2151 0.0888 0.068 Uiso 1 1 calc R . . H14B H 0.9141 0.1928 0.1292 0.068 Uiso 1 1 calc R . . N112 N 0.8758(3) 0.2515(3) 0.1630(3) 0.0535(18) Uani 1 1 d U . . C15 C 0.8527(4) 0.2180(4) 0.2024(5) 0.064(3) Uani 1 1 d U . . H15A H 0.8312 0.1934 0.1831 0.077 Uiso 1 1 calc R . . H15B H 0.8318 0.2371 0.2288 0.077 Uiso 1 1 calc R . . C16 C 0.8951(4) 0.1913(5) 0.2329(6) 0.075(3) Uani 1 1 d U . . C17 C 0.8369(4) 0.2892(4) 0.1436(5) 0.061(3) Uani 1 1 d U . . H17A H 0.8243 0.3075 0.1763 0.073 Uiso 1 1 calc R . . H17B H 0.8537 0.3138 0.1193 0.073 Uiso 1 1 calc R . . C18 C 0.7924(3) 0.2678(4) 0.1127(5) 0.056(2) Uani 1 1 d U . . C19 C 0.7500 0.2500 0.1437(6) 0.050(3) Uani 1 2 d SU . . H19 H 0.7500 0.2500 0.1829 0.060 Uiso 1 2 calc SR . . C20 C 0.7901(4) 0.2684(4) 0.0569(5) 0.060(3) Uani 1 1 d U . . H20 H 0.8177 0.2824 0.0375 0.073 Uiso 1 1 calc R . . C21 C 0.7500 0.2500 0.0258(7) 0.051(3) Uani 1 2 d SU . . H21 H 0.7500 0.2500 -0.0135 0.061 Uiso 1 2 calc SR . . Mn2 Mn 0.93287(6) 0.12653(7) 0.32155(9) 0.0743(6) Uani 1 1 d U . . O202 O 0.8814(3) 0.1502(3) 0.2609(3) 0.073(2) Uani 1 1 d U . . O201 O 0.9370(2) 0.1890(3) 0.3753(3) 0.0729(19) Uani 1 1 d U . . N221 N 0.9216(4) 0.0483(4) 0.2926(5) 0.088(3) Uani 1 1 d U . . C22 C 0.8921(5) 0.0350(5) 0.2514(7) 0.092(4) Uani 1 1 d U . . H22 H 0.8814 0.0611 0.2276 0.111 Uiso 1 1 calc R . . C23 C 0.8749(6) -0.0128(6) 0.2387(8) 0.115(4) Uani 1 1 d U . . H23 H 0.8553 -0.0217 0.2074 0.138 Uiso 1 1 calc R . . C24 C 0.8928(7) -0.0483(6) 0.2836(10) 0.133(6) Uani 1 1 d U . . H24 H 0.8858 -0.0829 0.2792 0.159 Uiso 1 1 calc R . . C25 C 0.9180(8) -0.0339(8) 0.3295(13) 0.192(12) Uani 1 1 d U . . H25 H 0.9221 -0.0554 0.3605 0.230 Uiso 1 1 calc R . . C26 C 0.9359(6) 0.0106(6) 0.3284(6) 0.096(3) Uani 1 1 d U . . C27 C 0.9715(6) 0.0269(6) 0.3721(8) 0.121(5) Uani 1 1 d U . . H27A H 1.0058 0.0226 0.3574 0.146 Uiso 1 1 calc R . . H27B H 0.9680 0.0035 0.4036 0.146 Uiso 1 1 calc R . . N211 N 0.9675(4) 0.0792(5) 0.3943(5) 0.099(3) Uani 1 1 d U . . C28 C 1.0141(5) 0.1001(6) 0.4074(6) 0.099(4) Uani 1 1 d U . . H28A H 1.0332 0.0766 0.4310 0.119 Uiso 1 1 calc R . . H28B H 1.0091 0.1315 0.4284 0.119 Uiso 1 1 calc R . . C29 C 1.0436(3) 0.1111(3) 0.3550(3) 0.088(3) Uani 1 1 d GU . . C30 C 1.0955(3) 0.1083(4) 0.3522(4) 0.114(5) Uani 1 1 d GU . . H30 H 1.1142 0.0992 0.3841 0.137 Uiso 1 1 calc R . . C31 C 1.1200(2) 0.1186(4) 0.3029(5) 0.135(7) Uani 1 1 d GU . . H31 H 1.1555 0.1167 0.3010 0.162 Uiso 1 1 calc R . . C32 C 1.0926(3) 0.1319(4) 0.2563(4) 0.102(4) Uani 1 1 d GU . . H32 H 1.1093 0.1389 0.2225 0.122 Uiso 1 1 calc R . . C33 C 1.0407(3) 0.1347(3) 0.2590(3) 0.108(5) Uani 1 1 d GU . . H33 H 1.0219 0.1437 0.2272 0.129 Uiso 1 1 calc R . . N222 N 1.01619(19) 0.1243(3) 0.3084(4) 0.081(3) Uani 1 1 d GU . . C34 C 0.9349(5) 0.0852(8) 0.4378(7) 0.135(6) Uani 1 1 d U . . H34A H 0.9403 0.1190 0.4535 0.162 Uiso 1 1 calc R . . H34B H 0.9441 0.0606 0.4667 0.162 Uiso 1 1 calc R . . C35 C 0.8814(5) 0.0796(6) 0.4268(5) 0.088(4) Uani 1 1 d U . . H35A H 0.8626 0.0844 0.4617 0.105 Uiso 1 1 calc R . . H35B H 0.8748 0.0453 0.4134 0.105 Uiso 1 1 calc R . . N212 N 0.8632(3) 0.1164(4) 0.3849(4) 0.076(2) Uani 1 1 d U . . C36 C 0.8536(4) 0.1689(5) 0.4086(7) 0.091(4) Uani 1 1 d U . . H36A H 0.8258 0.1847 0.3879 0.109 Uiso 1 1 calc R . . H36B H 0.8431 0.1657 0.4477 0.109 Uiso 1 1 calc R . . C37 C 0.8991(4) 0.2025(5) 0.4056(6) 0.078(3) Uani 1 1 d U . . Mn3 Mn 0.94366(6) 0.30310(8) 0.42972(9) 0.0790(7) Uani 1 1 d U . . O301 O 0.9455(3) 0.3100(4) 0.3417(4) 0.092(3) Uani 1 1 d U . . O302 O 0.8941(3) 0.2404(3) 0.4302(4) 0.077(2) Uani 1 1 d U . . N321 N 0.9293(3) 0.3078(4) 0.5200(4) 0.075(2) Uani 1 1 d U . . C38 C 0.8928(5) 0.2844(5) 0.5443(6) 0.083(3) Uani 1 1 d U . . H38 H 0.8758 0.2591 0.5243 0.100 Uiso 1 1 calc R . . C39 C 0.8770(5) 0.2945(6) 0.5990(7) 0.102(5) Uani 1 1 d U . . H39 H 0.8492 0.2770 0.6139 0.122 Uiso 1 1 calc R . . C40 C 0.9027(5) 0.3313(6) 0.6324(6) 0.099(4) Uani 1 1 d U . . H40 H 0.8953 0.3367 0.6703 0.119 Uiso 1 1 calc R . . C41 C 0.9394(5) 0.3579(5) 0.6039(7) 0.094(4) Uani 1 1 d U . . H41 H 0.9551 0.3856 0.6215 0.113 Uiso 1 1 calc R . . C42 C 0.9538(5) 0.3453(5) 0.5509(6) 0.079(3) Uani 1 1 d U . . C43 C 0.9944(4) 0.3722(5) 0.5260(6) 0.093(3) Uani 1 1 d U . . H43A H 1.0261 0.3535 0.5307 0.111 Uiso 1 1 calc R . . H43B H 0.9981 0.4055 0.5434 0.111 Uiso 1 1 calc R . . N311 N 0.9817(3) 0.3781(4) 0.4628(5) 0.085(2) Uani 1 1 d U . . C44 C 1.0276(5) 0.3827(6) 0.4262(7) 0.102(4) Uani 1 1 d U . . H44A H 1.0178 0.3907 0.3877 0.122 Uiso 1 1 calc R . . H44B H 1.0501 0.4093 0.4400 0.122 Uiso 1 1 calc R . . C45 C 1.0525(5) 0.3328(6) 0.4291(7) 0.104(5) Uani 1 1 d U . . C46 C 1.1060(5) 0.3308(7) 0.4351(7) 0.120(5) Uani 1 1 d U . . H46 H 1.1254 0.3604 0.4382 0.144 Uiso 1 1 calc R . . C47 C 1.1295(6) 0.2808(10) 0.4363(15) 0.241(17) Uani 1 1 d U . . H47 H 1.1642 0.2772 0.4438 0.289 Uiso 1 1 calc R . . C48 C 1.0998(6) 0.2394(8) 0.4261(10) 0.165(9) Uani 1 1 d U . . H48 H 1.1136 0.2074 0.4180 0.198 Uiso 1 1 calc R . . C49 C 1.0477(5) 0.2479(6) 0.4288(7) 0.106(5) Uani 1 1 d U . . H49 H 1.0271 0.2190 0.4302 0.127 Uiso 1 1 calc R . . N322 N 1.0256(4) 0.2890(5) 0.4295(5) 0.097(3) Uani 1 1 d U . . C50 C 0.9483(5) 0.4220(5) 0.4485(7) 0.098(4) Uani 1 1 d U . . H50A H 0.9294 0.4321 0.4818 0.118 Uiso 1 1 calc R . . H50B H 0.9695 0.4506 0.4372 0.118 Uiso 1 1 calc R . . C51 C 0.9134(4) 0.4107(5) 0.4046(6) 0.086(3) Uani 1 1 d U . . H51A H 0.9322 0.4103 0.3693 0.104 Uiso 1 1 calc R . . H51B H 0.8889 0.4384 0.4025 0.104 Uiso 1 1 calc R . . N312 N 0.8849(3) 0.3624(4) 0.4092(4) 0.078(2) Uani 1 1 d U . . C52 C 0.8636(4) 0.3431(6) 0.3533(5) 0.097(4) Uani 1 1 d U . . H52A H 0.8390 0.3161 0.3597 0.116 Uiso 1 1 calc R . . H52B H 0.8469 0.3707 0.3331 0.116 Uiso 1 1 calc R . . C53 C 0.9057(5) 0.3244(6) 0.3216(7) 0.098(4) Uani 1 1 d U . . C54 C 0.8417(4) 0.3663(5) 0.4497(5) 0.081(3) Uani 1 1 d U . . H54A H 0.8257 0.3330 0.4529 0.097 Uiso 1 1 calc R . . H54B H 0.8554 0.3750 0.4865 0.097 Uiso 1 1 calc R . . C55 C 0.8029(4) 0.4032(5) 0.4353(5) 0.070(3) Uani 1 1 d U . . C56 C 0.8047(5) 0.4547(5) 0.4503(5) 0.077(3) Uani 1 1 d U . . H56 H 0.8329 0.4662 0.4705 0.093 Uiso 1 1 calc R . . C57 C 0.7661(5) 0.4907(6) 0.4365(7) 0.102(4) Uani 1 1 d U . . H57 H 0.7669 0.5244 0.4490 0.122 Uiso 1 1 calc R . . C58 C 0.7291(5) 0.4727(5) 0.4048(6) 0.087(4) Uani 1 1 d U . . H58 H 0.7046 0.4955 0.3917 0.104 Uiso 1 1 calc R . . C59 C 0.7245(4) 0.4231(5) 0.3900(5) 0.073(3) Uani 1 1 d U . . C60 C 0.7615(4) 0.3889(5) 0.4043(5) 0.066(3) Uani 1 1 d U . . H60 H 0.7584 0.3551 0.3927 0.079 Uiso 1 1 calc R . . C61 C 0.6791(4) 0.4048(5) 0.3531(5) 0.074(3) Uani 1 1 d U . . H61A H 0.6667 0.4335 0.3312 0.089 Uiso 1 1 calc R . . H61B H 0.6914 0.3792 0.3269 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.98971(14) 0.09653(14) 0.1094(2) 0.1102(13) Uani 1 1 d DU . . O11 O 1.0403(3) 0.1110(3) 0.1200(4) 0.116(3) Uani 1 1 d DU . . O12 O 0.9689(4) 0.1255(3) 0.0653(3) 0.112(3) Uani 1 1 d DU . . O13 O 0.9602(3) 0.1067(4) 0.1582(4) 0.133(4) Uani 1 1 d DU . . O14 O 0.9871(4) 0.0450(3) 0.0968(5) 0.170(6) Uani 1 1 d DU . . Cl2 Cl 0.10480(15) 0.08656(17) 0.5306(2) 0.1193(16) Uani 1 1 d DU . . O21 O 0.1178(6) 0.1123(7) 0.4813(5) 0.261(10) Uani 1 1 d DU . . O22 O 0.0551(4) 0.0680(7) 0.5278(7) 0.273(11) Uani 1 1 d DU . . O23 O 0.1377(6) 0.0441(6) 0.5354(10) 0.338(14) Uani 1 1 d DU . . O24 O 0.1113(10) 0.1177(7) 0.5769(6) 0.405(18) Uani 1 1 d DU . . Cl4 Cl 0.2500 0.2500 0.3566(5) 0.254(5) Uani 1 2 d SDU . . O41 O 0.2837(4) 0.2212(5) 0.3254(6) 0.254(5) Uani 1 1 d DU . . O42 O 0.2217(4) 0.2168(4) 0.3917(6) 0.254(5) Uani 1 1 d DU . . Cl3 Cl 0.7556(4) 0.2495(3) 0.3234(2) 0.0998(16) Uani 0.50 1 d PDU . . O31 O 0.7454(3) 0.20580(19) 0.2942(3) 0.0998(16) Uani 1 1 d DU . . O32 O 0.7500 0.2500 0.3803(3) 0.0998(16) Uani 1 2 d SDU . . O33 O 0.8154(3) 0.2436(5) 0.3240(5) 0.0998(16) Uani 0.50 1 d PDU . . 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 0.0325(9) 0.0811(13) 0.0892(13) 0.0082(10) 0.0034(8) 0.0052(8) O101 0.035(4) 0.091(5) 0.131(7) 0.034(5) 0.000(4) 0.008(3) O102 0.048(4) 0.109(6) 0.104(5) -0.004(5) 0.010(4) 0.014(4) N121 0.039(5) 0.070(5) 0.103(7) -0.007(4) -0.003(4) -0.002(4) C1 0.059(7) 0.052(6) 0.157(12) -0.024(6) 0.006(7) -0.012(5) C2 0.066(9) 0.061(7) 0.156(13) -0.021(7) 0.000(8) -0.002(6) C3 0.056(8) 0.067(7) 0.182(13) 0.004(8) 0.008(8) 0.007(6) C4 0.037(6) 0.064(6) 0.116(9) -0.004(5) -0.018(6) -0.009(4) C5 0.028(5) 0.059(5) 0.111(8) 0.002(5) -0.006(5) -0.013(4) C6 0.030(6) 0.076(6) 0.140(10) 0.026(7) 0.022(6) 0.000(4) N111 0.037(4) 0.058(5) 0.100(5) 0.021(4) 0.010(4) -0.002(3) C7 0.033(5) 0.057(6) 0.133(9) -0.004(6) 0.016(5) 0.002(4) C8 0.039(5) 0.069(7) 0.116(8) 0.023(6) 0.014(5) 0.008(5) C9 0.041(5) 0.067(7) 0.123(9) 0.012(7) 0.011(5) 0.000(5) C10 0.054(7) 0.085(10) 0.146(12) 0.014(9) -0.010(6) 0.020(7) C11 0.048(6) 0.129(12) 0.114(10) 0.020(8) -0.024(7) 0.015(7) C12 0.031(5) 0.169(15) 0.131(10) -0.017(11) 0.001(6) 0.002(7) N122 0.029(4) 0.107(8) 0.113(7) 0.007(6) -0.003(4) 0.000(4) C13 0.048(5) 0.060(6) 0.069(6) 0.001(5) 0.018(4) 0.002(4) C14 0.031(5) 0.061(6) 0.079(6) 0.005(5) 0.000(4) 0.012(4) N112 0.033(4) 0.058(5) 0.069(5) 0.007(4) 0.011(3) 0.011(3) C15 0.044(5) 0.059(6) 0.088(7) 0.020(5) 0.004(5) 0.008(4) C16 0.042(6) 0.087(8) 0.095(8) 0.021(6) 0.006(6) 0.013(5) C17 0.046(5) 0.051(6) 0.086(8) 0.005(5) -0.014(5) 0.007(4) C18 0.036(5) 0.044(6) 0.087(6) 0.006(5) -0.010(4) 0.005(4) C19 0.038(6) 0.046(8) 0.065(8) 0.000 0.000 0.013(5) C20 0.050(6) 0.052(6) 0.080(6) 0.023(5) -0.003(5) 0.008(5) C21 0.034(7) 0.041(8) 0.079(9) 0.000 0.000 0.011(6) Mn2 0.0401(9) 0.0783(13) 0.1045(15) 0.0251(11) 0.0031(9) 0.0209(8) O202 0.050(4) 0.063(5) 0.106(5) 0.015(4) -0.003(4) 0.018(3) O201 0.031(4) 0.090(5) 0.097(5) 0.019(4) -0.002(3) 0.010(3) N221 0.054(6) 0.078(5) 0.132(8) 0.028(4) 0.012(5) 0.022(4) C22 0.063(8) 0.073(7) 0.141(11) 0.010(7) 0.011(7) 0.009(6) C23 0.107(12) 0.093(9) 0.145(12) -0.018(8) 0.044(9) 0.005(8) C24 0.134(16) 0.066(9) 0.198(17) 0.023(8) 0.055(11) -0.025(9) C25 0.123(15) 0.122(12) 0.33(3) 0.104(16) -0.101(19) -0.049(13) C26 0.095(10) 0.092(6) 0.100(9) 0.041(6) 0.031(6) 0.001(7) C27 0.106(12) 0.084(7) 0.174(13) 0.073(7) -0.028(8) -0.010(7) N211 0.054(5) 0.104(6) 0.140(7) 0.044(6) -0.003(5) 0.021(5) C28 0.053(6) 0.125(11) 0.118(9) 0.024(9) -0.026(5) 0.011(7) C29 0.050(5) 0.069(8) 0.145(9) 0.015(8) -0.016(5) 0.008(6) C30 0.059(6) 0.114(12) 0.171(12) 0.042(11) -0.003(7) 0.044(8) C31 0.064(8) 0.141(14) 0.200(15) 0.092(14) 0.012(7) 0.036(9) C32 0.059(6) 0.091(10) 0.156(11) 0.024(9) 0.012(7) 0.035(7) C33 0.059(6) 0.100(10) 0.163(11) 0.051(10) 0.026(7) 0.024(7) N222 0.045(4) 0.068(6) 0.129(7) 0.020(6) 0.004(4) 0.020(4) C34 0.053(6) 0.208(17) 0.145(10) 0.091(10) 0.000(7) 0.041(9) C35 0.065(6) 0.121(10) 0.077(8) 0.029(7) -0.001(6) 0.006(7) N212 0.030(4) 0.095(6) 0.105(6) 0.023(5) -0.005(4) 0.004(4) C36 0.043(6) 0.097(7) 0.133(11) 0.000(7) 0.018(6) -0.002(5) C37 0.029(5) 0.088(7) 0.117(10) -0.001(7) 0.002(6) 0.010(5) Mn3 0.0356(9) 0.1016(15) 0.0997(15) 0.0137(11) 0.0022(9) -0.0001(9) O301 0.042(4) 0.141(8) 0.093(5) -0.001(5) 0.008(4) 0.027(4) O302 0.060(5) 0.084(5) 0.087(6) 0.000(4) -0.004(4) 0.005(4) N321 0.054(5) 0.091(7) 0.081(5) 0.014(4) -0.004(4) -0.026(5) C38 0.071(8) 0.082(9) 0.097(7) 0.012(7) 0.001(6) -0.023(6) C39 0.080(9) 0.104(11) 0.121(10) -0.018(8) 0.036(8) -0.053(8) C40 0.075(9) 0.126(12) 0.096(9) -0.009(8) 0.001(7) -0.039(8) C41 0.062(8) 0.094(10) 0.126(9) -0.024(8) 0.002(7) -0.037(7) C42 0.060(7) 0.077(8) 0.099(6) 0.023(6) -0.011(6) -0.020(6) C43 0.049(7) 0.093(9) 0.136(7) 0.019(7) 0.004(6) -0.023(6) N311 0.031(4) 0.102(6) 0.122(6) 0.011(5) 0.021(4) -0.012(4) C44 0.052(6) 0.109(8) 0.144(11) 0.025(10) 0.030(7) -0.011(5) C45 0.038(5) 0.120(8) 0.153(13) 0.003(10) 0.029(8) 0.004(5) C46 0.051(6) 0.160(12) 0.148(14) 0.049(12) -0.016(9) -0.022(6) C47 0.028(7) 0.185(15) 0.51(5) 0.09(3) -0.058(16) -0.001(7) C48 0.069(8) 0.156(13) 0.27(3) -0.010(17) -0.066(14) 0.038(8) C49 0.047(6) 0.109(8) 0.162(14) -0.029(11) -0.014(9) 0.010(6) N322 0.044(4) 0.115(7) 0.132(9) 0.021(8) 0.001(5) 0.010(4) C50 0.048(7) 0.096(7) 0.149(12) 0.024(8) 0.012(6) 0.001(5) C51 0.048(6) 0.101(7) 0.111(10) 0.022(7) 0.030(5) 0.015(5) N312 0.044(5) 0.099(6) 0.090(6) 0.010(5) 0.006(4) 0.011(4) C52 0.041(6) 0.160(13) 0.089(7) -0.008(8) -0.005(5) 0.031(7) C53 0.050(7) 0.136(13) 0.109(6) -0.016(9) -0.005(6) 0.016(7) C54 0.025(5) 0.120(9) 0.097(8) -0.012(7) 0.009(5) -0.004(5) C55 0.042(5) 0.112(7) 0.055(7) 0.000(6) 0.003(5) -0.001(5) C56 0.064(7) 0.095(7) 0.073(8) 0.010(6) 0.008(6) -0.025(5) C57 0.071(9) 0.103(9) 0.130(13) -0.011(9) -0.016(8) -0.008(6) C58 0.050(7) 0.084(7) 0.127(12) 0.004(7) 0.008(6) -0.004(6) C59 0.042(6) 0.104(8) 0.073(8) -0.014(7) 0.010(5) 0.005(5) C60 0.049(6) 0.077(7) 0.072(8) 0.003(6) 0.000(5) -0.008(5) C61 0.047(6) 0.113(10) 0.062(8) 0.002(6) 0.010(5) 0.003(6) Cl1 0.075(2) 0.084(2) 0.172(4) 0.002(3) -0.002(2) 0.0323(19) O11 0.064(5) 0.098(7) 0.187(10) -0.008(7) 0.009(5) 0.031(4) O12 0.116(8) 0.086(6) 0.136(7) 0.002(6) 0.002(6) 0.015(6) O13 0.084(7) 0.139(9) 0.175(8) 0.036(7) 0.039(7) 0.056(7) O14 0.104(8) 0.066(5) 0.340(18) -0.030(8) -0.015(10) 0.036(5) Cl2 0.084(3) 0.122(3) 0.152(4) 0.068(3) -0.028(3) -0.020(2) O21 0.212(17) 0.36(2) 0.210(12) 0.141(15) -0.060(13) -0.161(16) O22 0.107(8) 0.36(3) 0.35(2) 0.20(2) -0.025(13) -0.053(11) O23 0.177(14) 0.26(2) 0.57(4) 0.14(2) 0.06(2) 0.091(16) O24 0.73(5) 0.24(2) 0.247(15) -0.025(16) 0.06(3) -0.20(3) Cl4 0.124(8) 0.310(14) 0.327(15) 0.000 0.000 0.082(7) O41 0.124(8) 0.310(14) 0.327(15) 0.000 0.000 0.082(7) O42 0.124(8) 0.310(14) 0.327(15) 0.000 0.000 0.082(7) Cl3 0.079(3) 0.101(3) 0.119(4) -0.001(5) 0.028(4) 0.011(3) O31 0.079(3) 0.101(3) 0.119(4) -0.001(5) 0.028(4) 0.011(3) O32 0.079(3) 0.101(3) 0.119(4) -0.001(5) 0.028(4) 0.011(3) O33 0.079(3) 0.101(3) 0.119(4) -0.001(5) 0.028(4) 0.011(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 O102 2.104(9) . ? Mn1 O101 2.151(8) . ? Mn1 N122 2.226(9) . ? Mn1 N121 2.322(10) . ? Mn1 N111 2.350(10) . ? Mn1 N112 2.351(8) . ? O101 C16 1.257(14) . ? O102 C53 1.321(16) . ? N121 C5 1.271(15) . ? N121 C1 1.308(15) . ? C1 C2 1.283(19) . ? C1 H1 0.9500 . ? C2 C3 1.34(2) . ? C2 H2 0.9500 . ? C3 C4 1.349(17) . ? C3 H3 0.9500 . ? C4 C5 1.398(16) . ? C4 H4 0.9500 . ? C5 C6 1.557(16) . ? C6 N111 1.435(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N111 C13 1.422(14) . ? N111 C7 1.475(13) . ? C7 C8 1.482(18) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N122 1.361(16) . ? C8 C9 1.373(15) . ? C9 C10 1.328(18) . ? C9 H9 0.9500 . ? C10 C11 1.39(2) . ? C10 H10 0.9500 . ? C11 C12 1.407(16) . ? C11 H11 0.9500 . ? C12 N122 1.345(17) . ? C12 H12 0.9500 . ? C13 C14 1.560(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N112 1.491(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N112 C15 1.444(13) . ? N112 C17 1.520(12) . ? C15 C16 1.529(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O202 1.338(14) . ? C17 C18 1.514(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.351(15) . ? C18 C19 1.440(13) . ? C19 C18 1.440(13) 2_655 ? C19 H19 0.9500 . ? C20 C21 1.400(13) . ? C20 H20 0.9500 . ? C21 C20 1.400(13) 2_655 ? C21 H21 0.9500 . ? Mn2 O202 2.109(8) . ? Mn2 O201 2.119(9) . ? Mn2 N221 2.224(12) . ? Mn2 N222 2.249(5) . ? Mn2 N211 2.356(11) . ? Mn2 N212 2.427(10) . ? O201 C37 1.301(14) . ? N221 C22 1.320(18) . ? N221 C26 1.383(16) . ? C22 C23 1.39(2) . ? C22 H22 0.9500 . ? C23 C24 1.52(3) . ? C23 H23 0.9500 . ? C24 C25 1.35(3) . ? C24 H24 0.9500 . ? C25 C26 1.28(2) . ? C25 H25 0.9500 . ? C26 C27 1.49(2) . ? C27 N211 1.50(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N211 C34 1.377(19) . ? N211 C28 1.401(17) . ? C28 C29 1.522(15) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.3900 . ? C29 N222 1.3900 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 N222 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.460(18) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N212 1.493(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? N212 C61 1.479(14) 2_655 ? N212 C36 1.536(16) . ? C36 C37 1.511(17) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O302 1.181(14) . ? Mn3 O302 2.136(9) . ? Mn3 O301 2.138(10) . ? Mn3 N321 2.221(11) . ? Mn3 N322 2.222(10) . ? Mn3 N312 2.284(10) . ? Mn3 N311 2.384(11) . ? O301 C53 1.231(15) . ? N321 C38 1.299(14) . ? N321 C42 1.411(16) . ? C38 C39 1.414(19) . ? C38 H38 0.9500 . ? C39 C40 1.446(19) . ? C39 H39 0.9500 . ? C40 C41 1.394(18) . ? C40 H40 0.9500 . ? C41 C42 1.380(19) . ? C41 H41 0.9500 . ? C42 C43 1.435(16) . ? C43 N311 1.575(17) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? N311 C50 1.513(16) . ? N311 C44 1.516(15) . ? C44 C45 1.49(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 N322 1.373(18) . ? C45 C46 1.436(18) . ? C46 C47 1.47(3) . ? C46 H46 0.9500 . ? C47 C48 1.38(3) . ? C47 H47 0.9500 . ? C48 C49 1.41(2) . ? C48 H48 0.9500 . ? C49 N322 1.246(17) . ? C49 H49 0.9500 . ? C50 C51 1.44(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N312 1.503(16) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? N312 C54 1.518(14) . ? N312 C52 1.555(16) . ? C52 C53 1.448(18) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C54 C55 1.472(17) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C60 1.391(15) . ? C55 C56 1.424(17) . ? C56 C57 1.447(19) . ? C56 H56 0.9500 . ? C57 C58 1.341(18) . ? C57 H57 0.9500 . ? C58 C59 1.377(18) . ? C58 H58 0.9500 . ? C59 C60 1.389(16) . ? C59 C61 1.583(16) . ? C60 H60 0.9500 . ? C61 N212 1.479(14) 2_655 ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? Cl1 O14 1.411(7) . ? Cl1 O11 1.427(7) . ? Cl1 O12 1.430(7) . ? Cl1 O13 1.446(7) . ? Cl2 O24 1.408(9) . ? Cl2 O22 1.419(8) . ? Cl2 O21 1.421(8) . ? Cl2 O23 1.439(9) . ? Cl4 O41 1.404(8) . ? Cl4 O41 1.404(8) 2 ? Cl4 O42 1.442(8) 2 ? Cl4 O42 1.442(8) . ? Cl3 Cl3 0.30(2) 2_655 ? Cl3 O32 1.386(8) . ? Cl3 O31 1.387(9) 2_655 ? Cl3 O31 1.390(9) . ? Cl3 O33 1.605(10) . ? Cl3 O33 1.908(15) 2_655 ? O31 Cl3 1.387(9) 2_655 ? O32 Cl3 1.386(8) 2_655 ? O33 Cl3 1.908(15) 2_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 O102 Mn1 O101 97.9(4) . . ? O102 Mn1 N122 126.5(4) . . ? O101 Mn1 N122 82.5(3) . . ? O102 Mn1 N121 86.7(4) . . ? O101 Mn1 N121 168.2(4) . . ? N122 Mn1 N121 103.6(4) . . ? O102 Mn1 N111 154.5(3) . . ? O101 Mn1 N111 100.6(3) . . ? N122 Mn1 N111 73.6(4) . . ? N121 Mn1 N111 72.0(3) . . ? O102 Mn1 N112 91.2(3) . . ? O101 Mn1 N112 73.7(3) . . ? N122 Mn1 N112 138.0(4) . . ? N121 Mn1 N112 95.4(3) . . ? N111 Mn1 N112 77.4(3) . . ? C16 O101 Mn1 115.1(7) . . ? C53 O102 Mn1 122.6(8) . . ? C5 N121 C1 117.9(12) . . ? C5 N121 Mn1 117.3(8) . . ? C1 N121 Mn1 124.7(10) . . ? C2 C1 N121 122.0(16) . . ? C2 C1 H1 119.0 . . ? N121 C1 H1 119.0 . . ? C1 C2 C3 123.7(15) . . ? C1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? C2 C3 C4 115.7(15) . . ? C2 C3 H3 122.2 . . ? C4 C3 H3 122.2 . . ? C3 C4 C5 117.9(14) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N121 C5 C4 122.4(11) . . ? N121 C5 C6 117.2(11) . . ? C4 C5 C6 120.2(12) . . ? N111 C6 C5 111.2(9) . . ? N111 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N111 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C13 N111 C6 111.4(10) . . ? C13 N111 C7 112.5(9) . . ? C6 N111 C7 109.5(8) . . ? C13 N111 Mn1 110.4(6) . . ? C6 N111 Mn1 109.1(8) . . ? C7 N111 Mn1 103.6(7) . . ? N111 C7 C8 111.8(10) . . ? N111 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N111 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N122 C8 C9 117.8(13) . . ? N122 C8 C7 116.1(9) . . ? C9 C8 C7 126.0(12) . . ? C10 C9 C8 125.3(14) . . ? C10 C9 H9 117.3 . . ? C8 C9 H9 117.3 . . ? C9 C10 C11 117.4(12) . . ? C9 C10 H10 121.3 . . ? C11 C10 H10 121.3 . . ? C10 C11 C12 117.4(14) . . ? C10 C11 H11 121.3 . . ? C12 C11 H11 121.3 . . ? N122 C12 C11 122.6(14) . . ? N122 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 N122 C8 119.1(11) . . ? C12 N122 Mn1 124.9(9) . . ? C8 N122 Mn1 115.8(8) . . ? N111 C13 C14 112.7(9) . . ? N111 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N111 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N112 C14 C13 111.8(8) . . ? N112 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? N112 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C15 N112 C14 112.3(8) . . ? C15 N112 C17 108.8(7) . . ? C14 N112 C17 111.5(8) . . ? C15 N112 Mn1 104.6(6) . . ? C14 N112 Mn1 105.2(5) . . ? C17 N112 Mn1 114.3(6) . . ? N112 C15 C16 107.1(8) . . ? N112 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? N112 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.6 . . ? O101 C16 O202 121.5(10) . . ? O101 C16 C15 122.0(11) . . ? O202 C16 C15 115.2(9) . . ? C18 C17 N112 116.1(8) . . ? C18 C17 H17A 108.3 . . ? N112 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? N112 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C20 C18 C19 119.2(10) . . ? C20 C18 C17 121.6(10) . . ? C19 C18 C17 119.0(11) . . ? C18 C19 C18 117.3(14) 2_655 . ? C18 C19 H19 121.4 2_655 . ? C18 C19 H19 121.4 . . ? C18 C20 C21 124.7(11) . . ? C18 C20 H20 117.6 . . ? C21 C20 H20 117.6 . . ? C20 C21 C20 114.8(15) . 2_655 ? C20 C21 H21 122.6 . . ? C20 C21 H21 122.6 2_655 . ? O202 Mn2 O201 103.0(3) . . ? O202 Mn2 N221 88.5(4) . . ? O201 Mn2 N221 160.1(4) . . ? O202 Mn2 N222 123.7(3) . . ? O201 Mn2 N222 93.2(3) . . ? N221 Mn2 N222 93.7(3) . . ? O202 Mn2 N211 159.6(4) . . ? O201 Mn2 N211 86.8(4) . . ? N221 Mn2 N211 77.5(5) . . ? N222 Mn2 N211 72.7(3) . . ? O202 Mn2 N212 88.5(3) . . ? O201 Mn2 N212 74.9(3) . . ? N221 Mn2 N212 89.4(4) . . ? N222 Mn2 N212 147.7(3) . . ? N211 Mn2 N212 76.7(4) . . ? C16 O202 Mn2 114.9(7) . . ? C37 O201 Mn2 121.5(8) . . ? C22 N221 C26 116.2(13) . . ? C22 N221 Mn2 124.9(9) . . ? C26 N221 Mn2 116.8(11) . . ? N221 C22 C23 127.8(15) . . ? N221 C22 H22 116.1 . . ? C23 C22 H22 116.1 . . ? C22 C23 C24 108.0(17) . . ? C22 C23 H23 126.0 . . ? C24 C23 H23 126.0 . . ? C25 C24 C23 124.5(17) . . ? C25 C24 H24 117.7 . . ? C23 C24 H24 117.7 . . ? C26 C25 C24 116(2) . . ? C26 C25 H25 122.2 . . ? C24 C25 H25 122.2 . . ? C25 C26 N221 125.9(18) . . ? C25 C26 C27 119.7(16) . . ? N221 C26 C27 114.1(13) . . ? C26 C27 N211 118.7(12) . . ? C26 C27 H27A 107.6 . . ? N211 C27 H27A 107.6 . . ? C26 C27 H27B 107.6 . . ? N211 C27 H27B 107.6 . . ? H27A C27 H27B 107.1 . . ? C34 N211 C28 110.0(14) . . ? C34 N211 C27 115.3(14) . . ? C28 N211 C27 112.9(12) . . ? C34 N211 Mn2 105.1(8) . . ? C28 N211 Mn2 107.7(9) . . ? C27 N211 Mn2 105.1(9) . . ? N211 C28 C29 110.4(11) . . ? N211 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? N211 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 N222 120.0 . . ? C30 C29 C28 123.1(7) . . ? N222 C29 C28 116.9(7) . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? N222 C33 C32 120.0 . . ? N222 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 N222 C29 120.0 . . ? C33 N222 Mn2 125.6(4) . . ? C29 N222 Mn2 114.4(4) . . ? N211 C34 C35 117.9(15) . . ? N211 C34 H34A 107.8 . . ? C35 C34 H34A 107.8 . . ? N211 C34 H34B 107.8 . . ? C35 C34 H34B 107.8 . . ? H34A C34 H34B 107.2 . . ? C34 C35 N212 112.1(11) . . ? C34 C35 H35A 109.2 . . ? N212 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? N212 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C61 N212 C35 110.5(10) 2_655 . ? C61 N212 C36 114.7(9) 2_655 . ? C35 N212 C36 113.6(11) . . ? C61 N212 Mn2 107.5(7) 2_655 . ? C35 N212 Mn2 104.6(7) . . ? C36 N212 Mn2 105.1(7) . . ? C37 C36 N212 113.0(10) . . ? C37 C36 H36A 109.0 . . ? N212 C36 H36A 109.0 . . ? C37 C36 H36B 109.0 . . ? N212 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? O302 C37 O201 127.4(12) . . ? O302 C37 C36 113.2(11) . . ? O201 C37 C36 119.2(12) . . ? O302 Mn3 O301 95.0(4) . . ? O302 Mn3 N321 86.1(3) . . ? O301 Mn3 N321 168.1(4) . . ? O302 Mn3 N322 118.6(4) . . ? O301 Mn3 N322 89.4(4) . . ? N321 Mn3 N322 100.5(4) . . ? O302 Mn3 N312 96.8(3) . . ? O301 Mn3 N312 74.9(3) . . ? N321 Mn3 N312 93.2(4) . . ? N322 Mn3 N312 142.6(4) . . ? O302 Mn3 N311 157.2(4) . . ? O301 Mn3 N311 104.6(4) . . ? N321 Mn3 N311 72.3(4) . . ? N322 Mn3 N311 73.9(4) . . ? N312 Mn3 N311 77.5(4) . . ? C53 O301 Mn3 113.7(9) . . ? C37 O302 Mn3 126.9(8) . . ? C38 N321 C42 116.6(12) . . ? C38 N321 Mn3 123.3(9) . . ? C42 N321 Mn3 118.8(8) . . ? N321 C38 C39 123.8(13) . . ? N321 C38 H38 118.1 . . ? C39 C38 H38 118.1 . . ? C38 C39 C40 120.7(12) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 113.8(13) . . ? C41 C40 H40 123.1 . . ? C39 C40 H40 123.1 . . ? C42 C41 C40 122.0(13) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C41 C42 N321 122.5(11) . . ? C41 C42 C43 118.6(13) . . ? N321 C42 C43 118.9(13) . . ? C42 C43 N311 107.2(10) . . ? C42 C43 H43A 110.3 . . ? N311 C43 H43A 110.3 . . ? C42 C43 H43B 110.3 . . ? N311 C43 H43B 110.3 . . ? H43A C43 H43B 108.5 . . ? C50 N311 C44 106.2(10) . . ? C50 N311 C43 115.2(11) . . ? C44 N311 C43 113.7(10) . . ? C50 N311 Mn3 108.8(8) . . ? C44 N311 Mn3 102.6(8) . . ? C43 N311 Mn3 109.5(7) . . ? C45 C44 N311 105.1(11) . . ? C45 C44 H44A 110.7 . . ? N311 C44 H44A 110.7 . . ? C45 C44 H44B 110.7 . . ? N311 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? N322 C45 C46 119.1(14) . . ? N322 C45 C44 121.9(11) . . ? C46 C45 C44 118.9(14) . . ? C45 C46 C47 117.3(15) . . ? C45 C46 H46 121.3 . . ? C47 C46 H46 121.3 . . ? C48 C47 C46 118.5(14) . . ? C48 C47 H47 120.7 . . ? C46 C47 H47 120.7 . . ? C47 C48 C49 115.3(18) . . ? C47 C48 H48 122.4 . . ? C49 C48 H48 122.4 . . ? N322 C49 C48 127.5(17) . . ? N322 C49 H49 116.2 . . ? C48 C49 H49 116.2 . . ? C49 N322 C45 120.2(12) . . ? C49 N322 Mn3 128.0(11) . . ? C45 N322 Mn3 111.8(9) . . ? C51 C50 N311 112.8(13) . . ? C51 C50 H50A 109.0 . . ? N311 C50 H50A 109.0 . . ? C51 C50 H50B 109.0 . . ? N311 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C50 C51 N312 116.9(11) . . ? C50 C51 H51A 108.1 . . ? N312 C51 H51A 108.1 . . ? C50 C51 H51B 108.1 . . ? N312 C51 H51B 108.1 . . ? H51A C51 H51B 107.3 . . ? C51 N312 C54 111.9(10) . . ? C51 N312 C52 113.9(11) . . ? C54 N312 C52 107.9(9) . . ? C51 N312 Mn3 105.2(7) . . ? C54 N312 Mn3 115.5(8) . . ? C52 N312 Mn3 102.2(7) . . ? C53 C52 N312 107.0(10) . . ? C53 C52 H52A 110.3 . . ? N312 C52 H52A 110.3 . . ? C53 C52 H52B 110.3 . . ? N312 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? O301 C53 O102 123.5(13) . . ? O301 C53 C52 124.6(15) . . ? O102 C53 C52 111.7(11) . . ? C55 C54 N312 115.4(11) . . ? C55 C54 H54A 108.4 . . ? N312 C54 H54A 108.4 . . ? C55 C54 H54B 108.4 . . ? N312 C54 H54B 108.4 . . ? H54A C54 H54B 107.5 . . ? C60 C55 C56 115.4(11) . . ? C60 C55 C54 120.2(12) . . ? C56 C55 C54 124.3(11) . . ? C55 C56 C57 124.0(12) . . ? C55 C56 H56 118.0 . . ? C57 C56 H56 118.0 . . ? C58 C57 C56 114.7(14) . . ? C58 C57 H57 122.7 . . ? C56 C57 H57 122.7 . . ? C57 C58 C59 124.1(14) . . ? C57 C58 H58 118.0 . . ? C59 C58 H58 118.0 . . ? C58 C59 C60 120.3(12) . . ? C58 C59 C61 120.7(12) . . ? C60 C59 C61 118.9(12) . . ? C59 C60 C55 121.3(12) . . ? C59 C60 H60 119.4 . . ? C55 C60 H60 119.4 . . ? N212 C61 C59 114.3(9) 2_655 . ? N212 C61 H61A 108.7 2_655 . ? C59 C61 H61A 108.7 . . ? N212 C61 H61B 108.7 2_655 . ? C59 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? O14 Cl1 O11 110.4(5) . . ? O14 Cl1 O12 110.3(6) . . ? O11 Cl1 O12 110.8(5) . . ? O14 Cl1 O13 109.5(6) . . ? O11 Cl1 O13 108.5(6) . . ? O12 Cl1 O13 107.2(5) . . ? O24 Cl2 O22 111.0(8) . . ? O24 Cl2 O21 110.7(7) . . ? O22 Cl2 O21 111.1(7) . . ? O24 Cl2 O23 109.0(8) . . ? O22 Cl2 O23 107.4(7) . . ? O21 Cl2 O23 107.5(7) . . ? O41 Cl4 O41 115.0(10) . 2 ? O41 Cl4 O42 108.5(4) . 2 ? O41 Cl4 O42 108.4(4) 2 2 ? O41 Cl4 O42 108.4(4) . . ? O41 Cl4 O42 108.5(4) 2 . ? O42 Cl4 O42 107.8(10) 2 . ? Cl3 Cl3 O32 83.7(4) 2_655 . ? Cl3 Cl3 O31 84(3) 2_655 2_655 ? O32 Cl3 O31 119.6(6) . 2_655 ? Cl3 Cl3 O31 83(3) 2_655 . ? O32 Cl3 O31 119.4(6) . . ? O31 Cl3 O31 117.5(7) 2_655 . ? Cl3 Cl3 O33 179(3) 2_655 . ? O32 Cl3 O33 95.7(6) . . ? O31 Cl3 O33 96.3(7) 2_655 . ? O31 Cl3 O33 96.8(7) . . ? Cl3 Cl3 O33 0(2) 2_655 2_655 ? O32 Cl3 O33 83.3(5) . 2_655 ? O31 Cl3 O33 84.3(6) 2_655 2_655 ? O31 Cl3 O33 83.7(6) . 2_655 ? O33 Cl3 O33 179.0(8) . 2_655 ? Cl3 O31 Cl3 12.5(8) 2_655 . ? Cl3 O32 Cl3 12.5(8) . 2_655 ? Cl3 O33 Cl3 0.1(5) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O102 Mn1 O101 C16 67.3(10) . . . . ? N122 Mn1 O101 C16 -166.8(10) . . . . ? N121 Mn1 O101 C16 -45(2) . . . . ? N111 Mn1 O101 C16 -95.1(9) . . . . ? N112 Mn1 O101 C16 -21.7(9) . . . . ? O101 Mn1 O102 C53 69.2(11) . . . . ? N122 Mn1 O102 C53 -17.2(13) . . . . ? N121 Mn1 O102 C53 -121.7(11) . . . . ? N111 Mn1 O102 C53 -154.6(10) . . . . ? N112 Mn1 O102 C53 143.0(11) . . . . ? O102 Mn1 N121 C5 -178.1(8) . . . . ? O101 Mn1 N121 C5 -64.7(19) . . . . ? N122 Mn1 N121 C5 55.2(9) . . . . ? N111 Mn1 N121 C5 -12.3(8) . . . . ? N112 Mn1 N121 C5 -87.1(8) . . . . ? O102 Mn1 N121 C1 -1.2(10) . . . . ? O101 Mn1 N121 C1 112.1(18) . . . . ? N122 Mn1 N121 C1 -128.0(10) . . . . ? N111 Mn1 N121 C1 164.5(10) . . . . ? N112 Mn1 N121 C1 89.7(10) . . . . ? C5 N121 C1 C2 5.4(18) . . . . ? Mn1 N121 C1 C2 -171.4(10) . . . . ? N121 C1 C2 C3 -4(2) . . . . ? C1 C2 C3 C4 4(2) . . . . ? C2 C3 C4 C5 -4.6(18) . . . . ? C1 N121 C5 C4 -6.7(16) . . . . ? Mn1 N121 C5 C4 170.4(8) . . . . ? C1 N121 C5 C6 177.7(10) . . . . ? Mn1 N121 C5 C6 -5.3(13) . . . . ? C3 C4 C5 N121 6.5(17) . . . . ? C3 C4 C5 C6 -178.0(11) . . . . ? N121 C5 C6 N111 31.4(16) . . . . ? C4 C5 C6 N111 -144.3(10) . . . . ? C5 C6 N111 C13 82.7(13) . . . . ? C5 C6 N111 C7 -152.3(11) . . . . ? C5 C6 N111 Mn1 -39.5(12) . . . . ? O102 Mn1 N111 C13 -60.0(11) . . . . ? O101 Mn1 N111 C13 75.7(7) . . . . ? N122 Mn1 N111 C13 154.6(8) . . . . ? N121 Mn1 N111 C13 -94.8(7) . . . . ? N112 Mn1 N111 C13 5.2(7) . . . . ? O102 Mn1 N111 C6 62.7(11) . . . . ? O101 Mn1 N111 C6 -161.6(7) . . . . ? N122 Mn1 N111 C6 -82.7(7) . . . . ? N121 Mn1 N111 C6 27.9(7) . . . . ? N112 Mn1 N111 C6 128.0(7) . . . . ? O102 Mn1 N111 C7 179.3(7) . . . . ? O101 Mn1 N111 C7 -45.0(7) . . . . ? N122 Mn1 N111 C7 33.9(6) . . . . ? N121 Mn1 N111 C7 144.5(7) . . . . ? N112 Mn1 N111 C7 -115.4(6) . . . . ? C13 N111 C7 C8 -165.8(9) . . . . ? C6 N111 C7 C8 69.8(13) . . . . ? Mn1 N111 C7 C8 -46.5(10) . . . . ? N111 C7 C8 N122 34.8(14) . . . . ? N111 C7 C8 C9 -149.5(11) . . . . ? N122 C8 C9 C10 2.4(19) . . . . ? C7 C8 C9 C10 -173.2(13) . . . . ? C8 C9 C10 C11 -3(2) . . . . ? C9 C10 C11 C12 5(2) . . . . ? C10 C11 C12 N122 -6(2) . . . . ? C11 C12 N122 C8 5(2) . . . . ? C11 C12 N122 Mn1 178.8(11) . . . . ? C9 C8 N122 C12 -2.8(18) . . . . ? C7 C8 N122 C12 173.2(12) . . . . ? C9 C8 N122 Mn1 -177.4(8) . . . . ? C7 C8 N122 Mn1 -1.4(14) . . . . ? O102 Mn1 N122 C12 4.7(14) . . . . ? O101 Mn1 N122 C12 -89.6(12) . . . . ? N121 Mn1 N122 C12 100.7(12) . . . . ? N111 Mn1 N122 C12 167.0(13) . . . . ? N112 Mn1 N122 C12 -144.9(11) . . . . ? O102 Mn1 N122 C8 178.9(8) . . . . ? O101 Mn1 N122 C8 84.6(9) . . . . ? N121 Mn1 N122 C8 -85.1(9) . . . . ? N111 Mn1 N122 C8 -18.7(8) . . . . ? N112 Mn1 N122 C8 29.4(11) . . . . ? C6 N111 C13 C14 -152.7(9) . . . . ? C7 N111 C13 C14 83.9(11) . . . . ? Mn1 N111 C13 C14 -31.3(10) . . . . ? N111 C13 C14 N112 54.7(11) . . . . ? C13 C14 N112 C15 -158.8(9) . . . . ? C13 C14 N112 C17 78.8(10) . . . . ? C13 C14 N112 Mn1 -45.6(9) . . . . ? O102 Mn1 N112 C15 -62.7(6) . . . . ? O101 Mn1 N112 C15 35.1(6) . . . . ? N122 Mn1 N112 C15 93.2(7) . . . . ? N121 Mn1 N112 C15 -149.5(6) . . . . ? N111 Mn1 N112 C15 140.3(6) . . . . ? O102 Mn1 N112 C14 178.8(6) . . . . ? O101 Mn1 N112 C14 -83.4(6) . . . . ? N122 Mn1 N112 C14 -25.3(8) . . . . ? N121 Mn1 N112 C14 92.0(6) . . . . ? N111 Mn1 N112 C14 21.8(6) . . . . ? O102 Mn1 N112 C17 56.2(7) . . . . ? O101 Mn1 N112 C17 154.0(7) . . . . ? N122 Mn1 N112 C17 -147.9(7) . . . . ? N121 Mn1 N112 C17 -30.6(7) . . . . ? N111 Mn1 N112 C17 -100.8(7) . . . . ? C14 N112 C15 C16 72.1(11) . . . . ? C17 N112 C15 C16 -164.0(9) . . . . ? Mn1 N112 C15 C16 -41.5(10) . . . . ? Mn1 O101 C16 O202 -162.2(9) . . . . ? Mn1 O101 C16 C15 4.3(16) . . . . ? N112 C15 C16 O101 28.7(16) . . . . ? N112 C15 C16 O202 -164.0(10) . . . . ? C15 N112 C17 C18 -63.2(13) . . . . ? C14 N112 C17 C18 61.2(12) . . . . ? Mn1 N112 C17 C18 -179.7(8) . . . . ? N112 C17 C18 C20 -98.9(12) . . . . ? N112 C17 C18 C19 86.0(11) . . . . ? C20 C18 C19 C18 1.9(7) . . . 2_655 ? C17 C18 C19 C18 177.2(10) . . . 2_655 ? C19 C18 C20 C21 -4.1(14) . . . . ? C17 C18 C20 C21 -179.2(8) . . . . ? C18 C20 C21 C20 2.1(7) . . . 2_655 ? O101 C16 O202 Mn2 5.5(15) . . . . ? C15 C16 O202 Mn2 -161.9(8) . . . . ? O201 Mn2 O202 C16 59.9(8) . . . . ? N221 Mn2 O202 C16 -136.5(8) . . . . ? N222 Mn2 O202 C16 -43.0(9) . . . . ? N211 Mn2 O202 C16 177.0(11) . . . . ? N212 Mn2 O202 C16 134.0(8) . . . . ? O202 Mn2 O201 C37 67.7(9) . . . . ? N221 Mn2 O201 C37 -56.4(14) . . . . ? N222 Mn2 O201 C37 -166.7(9) . . . . ? N211 Mn2 O201 C37 -94.2(9) . . . . ? N212 Mn2 O201 C37 -17.1(9) . . . . ? O202 Mn2 N221 C22 1.2(11) . . . . ? O201 Mn2 N221 C22 127.4(12) . . . . ? N222 Mn2 N221 C22 -122.5(11) . . . . ? N211 Mn2 N221 C22 166.1(11) . . . . ? N212 Mn2 N221 C22 89.7(11) . . . . ? O202 Mn2 N221 C26 -161.5(9) . . . . ? O201 Mn2 N221 C26 -35.3(15) . . . . ? N222 Mn2 N221 C26 74.9(9) . . . . ? N211 Mn2 N221 C26 3.5(9) . . . . ? N212 Mn2 N221 C26 -73.0(9) . . . . ? C26 N221 C22 C23 -2(2) . . . . ? Mn2 N221 C22 C23 -164.8(11) . . . . ? N221 C22 C23 C24 4(2) . . . . ? C22 C23 C24 C25 4(3) . . . . ? C23 C24 C25 C26 -14(4) . . . . ? C24 C25 C26 N221 17(4) . . . . ? C24 C25 C26 C27 -169.3(19) . . . . ? C22 N221 C26 C25 -10(3) . . . . ? Mn2 N221 C26 C25 154(2) . . . . ? C22 N221 C26 C27 176.5(13) . . . . ? Mn2 N221 C26 C27 -19.3(16) . . . . ? C25 C26 C27 N211 -141(2) . . . . ? N221 C26 C27 N211 33(2) . . . . ? C26 C27 N211 C34 87.6(17) . . . . ? C26 C27 N211 C28 -144.7(14) . . . . ? C26 C27 N211 Mn2 -27.6(16) . . . . ? O202 Mn2 N211 C34 -61.9(19) . . . . ? O201 Mn2 N211 C34 57.8(12) . . . . ? N221 Mn2 N211 C34 -109.9(12) . . . . ? N222 Mn2 N211 C34 152.1(13) . . . . ? N212 Mn2 N211 C34 -17.5(12) . . . . ? O202 Mn2 N211 C28 -179.1(10) . . . . ? O201 Mn2 N211 C28 -59.5(10) . . . . ? N221 Mn2 N211 C28 132.9(11) . . . . ? N222 Mn2 N211 C28 34.9(10) . . . . ? N212 Mn2 N211 C28 -134.7(11) . . . . ? O202 Mn2 N211 C27 60.2(15) . . . . ? O201 Mn2 N211 C27 179.9(9) . . . . ? N221 Mn2 N211 C27 12.2(9) . . . . ? N222 Mn2 N211 C27 -85.8(9) . . . . ? N212 Mn2 N211 C27 104.6(9) . . . . ? C34 N211 C28 C29 -159.3(12) . . . . ? C27 N211 C28 C29 70.3(15) . . . . ? Mn2 N211 C28 C29 -45.3(13) . . . . ? N211 C28 C29 C30 -147.6(9) . . . . ? N211 C28 C29 N222 32.2(15) . . . . ? N222 C29 C30 C31 0.0 . . . . ? C28 C29 C30 C31 179.7(11) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 N222 0.0 . . . . ? C32 C33 N222 C29 0.0 . . . . ? C32 C33 N222 Mn2 -179.8(6) . . . . ? C30 C29 N222 C33 0.0 . . . . ? C28 C29 N222 C33 -179.7(10) . . . . ? C30 C29 N222 Mn2 179.8(5) . . . . ? C28 C29 N222 Mn2 0.1(10) . . . . ? O202 Mn2 N222 C33 -4.8(6) . . . . ? O201 Mn2 N222 C33 -112.7(5) . . . . ? N221 Mn2 N222 C33 85.9(6) . . . . ? N211 Mn2 N222 C33 161.6(6) . . . . ? N212 Mn2 N222 C33 -179.2(6) . . . . ? O202 Mn2 N222 C29 175.4(4) . . . . ? O201 Mn2 N222 C29 67.5(5) . . . . ? N221 Mn2 N222 C29 -93.9(5) . . . . ? N211 Mn2 N222 C29 -18.2(5) . . . . ? N212 Mn2 N222 C29 1.0(8) . . . . ? C28 N211 C34 C35 162.1(15) . . . . ? C27 N211 C34 C35 -68.8(18) . . . . ? Mn2 N211 C34 C35 46.5(18) . . . . ? N211 C34 C35 N212 -60(2) . . . . ? C34 C35 N212 C61 149.6(14) . . . 2_655 ? C34 C35 N212 C36 -79.9(15) . . . . ? C34 C35 N212 Mn2 34.2(15) . . . . ? O202 Mn2 N212 C61 39.4(8) . . . 2_655 ? O201 Mn2 N212 C61 143.3(8) . . . 2_655 ? N221 Mn2 N212 C61 -49.1(8) . . . 2_655 ? N222 Mn2 N212 C61 -145.2(7) . . . 2_655 ? N211 Mn2 N212 C61 -126.4(8) . . . 2_655 ? O202 Mn2 N212 C35 156.9(8) . . . . ? O201 Mn2 N212 C35 -99.2(8) . . . . ? N221 Mn2 N212 C35 68.3(9) . . . . ? N222 Mn2 N212 C35 -27.7(12) . . . . ? N211 Mn2 N212 C35 -9.0(8) . . . . ? O202 Mn2 N212 C36 -83.1(8) . . . . ? O201 Mn2 N212 C36 20.7(7) . . . . ? N221 Mn2 N212 C36 -171.7(8) . . . . ? N222 Mn2 N212 C36 92.2(9) . . . . ? N211 Mn2 N212 C36 111.0(8) . . . . ? C61 N212 C36 C37 -141.3(12) 2_655 . . . ? C35 N212 C36 C37 90.3(13) . . . . ? Mn2 N212 C36 C37 -23.5(13) . . . . ? Mn2 O201 C37 O302 -167.2(11) . . . . ? Mn2 O201 C37 C36 8.5(16) . . . . ? N212 C36 C37 O302 -170.6(12) . . . . ? N212 C36 C37 O201 13.1(18) . . . . ? O302 Mn3 O301 C53 69.3(11) . . . . ? N321 Mn3 O301 C53 -26(2) . . . . ? N322 Mn3 O301 C53 -172.1(11) . . . . ? N312 Mn3 O301 C53 -26.4(11) . . . . ? N311 Mn3 O301 C53 -98.9(11) . . . . ? O201 C37 O302 Mn3 4(2) . . . . ? C36 C37 O302 Mn3 -171.7(8) . . . . ? O301 Mn3 O302 C37 52.8(11) . . . . ? N321 Mn3 O302 C37 -139.1(11) . . . . ? N322 Mn3 O302 C37 -39.2(12) . . . . ? N312 Mn3 O302 C37 128.1(11) . . . . ? N311 Mn3 O302 C37 -157.9(11) . . . . ? O302 Mn3 N321 C38 -14.5(11) . . . . ? O301 Mn3 N321 C38 81(2) . . . . ? N322 Mn3 N321 C38 -132.8(11) . . . . ? N312 Mn3 N321 C38 82.2(11) . . . . ? N311 Mn3 N321 C38 158.0(12) . . . . ? O302 Mn3 N321 C42 178.9(9) . . . . ? O301 Mn3 N321 C42 -85(2) . . . . ? N322 Mn3 N321 C42 60.5(10) . . . . ? N312 Mn3 N321 C42 -84.5(9) . . . . ? N311 Mn3 N321 C42 -8.6(9) . . . . ? C42 N321 C38 C39 0(2) . . . . ? Mn3 N321 C38 C39 -166.9(11) . . . . ? N321 C38 C39 C40 -3(2) . . . . ? C38 C39 C40 C41 6(2) . . . . ? C39 C40 C41 C42 -8(2) . . . . ? C40 C41 C42 N321 6(2) . . . . ? C40 C41 C42 C43 -175.4(14) . . . . ? C38 N321 C42 C41 -1.6(19) . . . . ? Mn3 N321 C42 C41 165.9(11) . . . . ? C38 N321 C42 C43 179.8(13) . . . . ? Mn3 N321 C42 C43 -12.6(16) . . . . ? C41 C42 C43 N311 -143.9(13) . . . . ? N321 C42 C43 N311 34.7(16) . . . . ? C42 C43 N311 C50 84.2(14) . . . . ? C42 C43 N311 C44 -152.9(12) . . . . ? C42 C43 N311 Mn3 -38.8(13) . . . . ? O302 Mn3 N311 C50 -81.6(13) . . . . ? O301 Mn3 N311 C50 66.7(8) . . . . ? N321 Mn3 N311 C50 -101.3(8) . . . . ? N322 Mn3 N311 C50 151.7(9) . . . . ? N312 Mn3 N311 C50 -3.8(8) . . . . ? O302 Mn3 N311 C44 166.2(9) . . . . ? O301 Mn3 N311 C44 -45.5(9) . . . . ? N321 Mn3 N311 C44 146.5(9) . . . . ? N322 Mn3 N311 C44 39.5(8) . . . . ? N312 Mn3 N311 C44 -116.0(9) . . . . ? O302 Mn3 N311 C43 45.1(13) . . . . ? O301 Mn3 N311 C43 -166.6(7) . . . . ? N321 Mn3 N311 C43 25.4(7) . . . . ? N322 Mn3 N311 C43 -81.5(8) . . . . ? N312 Mn3 N311 C43 122.9(8) . . . . ? C50 N311 C44 C45 -164.6(13) . . . . ? C43 N311 C44 C45 67.7(15) . . . . ? Mn3 N311 C44 C45 -50.4(13) . . . . ? N311 C44 C45 N322 39(2) . . . . ? N311 C44 C45 C46 -136.7(14) . . . . ? N322 C45 C46 C47 5(3) . . . . ? C44 C45 C46 C47 -178(2) . . . . ? C45 C46 C47 C48 6(4) . . . . ? C46 C47 C48 C49 -15(4) . . . . ? C47 C48 C49 N322 14(4) . . . . ? C48 C49 N322 C45 -2(3) . . . . ? C48 C49 N322 Mn3 176.9(15) . . . . ? C46 C45 N322 C49 -8(2) . . . . ? C44 C45 N322 C49 175.9(16) . . . . ? C46 C45 N322 Mn3 173.1(12) . . . . ? C44 C45 N322 Mn3 -3(2) . . . . ? O302 Mn3 N322 C49 1.1(16) . . . . ? O301 Mn3 N322 C49 -94.3(15) . . . . ? N321 Mn3 N322 C49 92.4(15) . . . . ? N312 Mn3 N322 C49 -158.0(13) . . . . ? N311 Mn3 N322 C49 160.4(15) . . . . ? O302 Mn3 N322 C45 179.9(10) . . . . ? O301 Mn3 N322 C45 84.6(11) . . . . ? N321 Mn3 N322 C45 -88.7(11) . . . . ? N312 Mn3 N322 C45 20.9(15) . . . . ? N311 Mn3 N322 C45 -20.8(10) . . . . ? C44 N311 C50 C51 90.1(13) . . . . ? C43 N311 C50 C51 -143.1(11) . . . . ? Mn3 N311 C50 C51 -19.7(13) . . . . ? N311 C50 C51 N312 47.3(15) . . . . ? C50 C51 N312 C54 78.3(13) . . . . ? C50 C51 N312 C52 -158.9(11) . . . . ? C50 C51 N312 Mn3 -47.8(12) . . . . ? O302 Mn3 N312 C51 -177.8(8) . . . . ? O301 Mn3 N312 C51 -84.5(8) . . . . ? N321 Mn3 N312 C51 95.7(8) . . . . ? N322 Mn3 N312 C51 -16.2(12) . . . . ? N311 Mn3 N312 C51 24.6(8) . . . . ? O302 Mn3 N312 C54 58.3(8) . . . . ? O301 Mn3 N312 C54 151.6(9) . . . . ? N321 Mn3 N312 C54 -28.2(8) . . . . ? N322 Mn3 N312 C54 -140.2(9) . . . . ? N311 Mn3 N312 C54 -99.3(9) . . . . ? O302 Mn3 N312 C52 -58.5(8) . . . . ? O301 Mn3 N312 C52 34.8(7) . . . . ? N321 Mn3 N312 C52 -145.0(8) . . . . ? N322 Mn3 N312 C52 103.0(10) . . . . ? N311 Mn3 N312 C52 143.9(8) . . . . ? C51 N312 C52 C53 73.1(15) . . . . ? C54 N312 C52 C53 -162.0(12) . . . . ? Mn3 N312 C52 C53 -39.8(13) . . . . ? Mn3 O301 C53 O102 -164.0(12) . . . . ? Mn3 O301 C53 C52 10(2) . . . . ? Mn1 O102 C53 O301 1(2) . . . . ? Mn1 O102 C53 C52 -172.9(10) . . . . ? N312 C52 C53 O301 24(2) . . . . ? N312 C52 C53 O102 -162.1(12) . . . . ? C51 N312 C54 C55 61.9(14) . . . . ? C52 N312 C54 C55 -64.2(14) . . . . ? Mn3 N312 C54 C55 -177.8(9) . . . . ? N312 C54 C55 C60 91.5(14) . . . . ? N312 C54 C55 C56 -87.2(14) . . . . ? C60 C55 C56 C57 1.9(18) . . . . ? C54 C55 C56 C57 -179.3(12) . . . . ? C55 C56 C57 C58 -4(2) . . . . ? C56 C57 C58 C59 6(2) . . . . ? C57 C58 C59 C60 -5(2) . . . . ? C57 C58 C59 C61 178.9(13) . . . . ? C58 C59 C60 C55 2.2(18) . . . . ? C61 C59 C60 C55 178.3(10) . . . . ? C56 C55 C60 C59 -0.8(16) . . . . ? C54 C55 C60 C59 -179.6(11) . . . . ? C58 C59 C61 N212 -96.7(14) . . . 2_655 ? C60 C59 C61 N212 87.3(13) . . . 2_655 ? O32 Cl3 O31 Cl3 78.9(17) . . . 2_655 ? O31 Cl3 O31 Cl3 -79.9(17) 2_655 . . 2_655 ? O33 Cl3 O31 Cl3 179(100) . . . 2_655 ? O33 Cl3 O31 Cl3 0.3(15) 2_655 . . 2_655 ? O31 Cl3 O32 Cl3 80(3) 2_655 . . 2_655 ? O31 Cl3 O32 Cl3 -79(3) . . . 2_655 ? O33 Cl3 O32 Cl3 -180(100) . . . 2_655 ? O33 Cl3 O32 Cl3 0(3) 2_655 . . 2_655 ? O32 Cl3 O33 Cl3 26(100) . . . 2_655 ? O31 Cl3 O33 Cl3 146(100) 2_655 . . 2_655 ? O31 Cl3 O33 Cl3 -95(100) . . . 2_655 ? O33 Cl3 O33 Cl3 23(100) 2_655 . . 2_655 ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 31.99 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.861 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.148