# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Laurence K. Thompson' _publ_contact_author_address ; Department of Chemistry Memorial University of St John's Newfoundland A1B 3X7 CANADA ; _publ_contact_author_email LTHOMP@MUN.CA _publ_section_title ; Self-assembled polymetallic square grids ([2x2] M4, [3x3] M9) and trigonal bipyramidal clusters (M5) - structural and magnetic properties ; loop_ _publ_author_name 'Louise N. Dawe' 'Tareque S.M. Abedin' 'Timothy L. Kelly' 'Laurence K. Thompson' 'David O. Miller' ; L.Zhao ; 'Claire Wilson' 'Michael A. Leech' 'Judith A.K. Howard' #===END data_l3m(3) _database_code_depnum_ccdc_archive 'CCDC 258937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H48 Cl4 Cu4 N20 O28.13' _chemical_formula_weight 1799.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.9608(10) _cell_length_b 17.0907(9) _cell_length_c 21.2188(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.9830(10) _cell_angle_gamma 90.00 _cell_volume 7185.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 21.25 _cell_measurement_theta_max 26.52 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3636 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART-CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88214 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 27.52 _reflns_number_total 16521 _reflns_number_gt 14833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0516P)^2^+14.1854P] 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 16521 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.90391(15) 0.47019(16) 0.91523(12) 0.0278(5) Uani 1 1 d . . . H2 H 0.9038 0.4610 0.8720 0.033 Uiso 1 1 calc R . . C3 C 0.91866(16) 0.54540(16) 0.93868(13) 0.0316(6) Uani 1 1 d . . . H3 H 0.9289 0.5854 0.9117 0.038 Uiso 1 1 calc R . . C4 C 0.91779(15) 0.55930(16) 1.00251(14) 0.0307(6) Uani 1 1 d . . . H4 H 0.9269 0.6091 1.0191 0.037 Uiso 1 1 calc R . . C5 C 0.90320(14) 0.49812(15) 1.04215(12) 0.0248(5) Uani 1 1 d . . . H5 H 0.9021 0.5065 1.0853 0.030 Uiso 1 1 calc R . . C6 C 0.89031(12) 0.42463(14) 1.01591(11) 0.0198(4) Uani 1 1 d . . . C7 C 0.87379(12) 0.35443(14) 1.05236(11) 0.0185(4) Uani 1 1 d . . . C11 C 0.82758(11) 0.17361(14) 0.99675(11) 0.0174(4) Uani 1 1 d . . . C13 C 0.80910(12) 0.09223(14) 1.01320(11) 0.0186(4) Uani 1 1 d . . . C14 C 0.80383(13) 0.06858(15) 1.07482(12) 0.0234(5) Uani 1 1 d . . . H14 H 0.8106 0.1039 1.1083 0.028 Uiso 1 1 calc R . . C15 C 0.78818(14) -0.00903(16) 1.08555(13) 0.0279(5) Uani 1 1 d . . . H15 H 0.7862 -0.0268 1.1267 0.033 Uiso 1 1 calc R . . C16 C 0.77553(15) -0.05988(16) 1.03475(13) 0.0291(6) Uani 1 1 d . . . H16 H 0.7650 -0.1120 1.0415 0.035 Uiso 1 1 calc R . . C17 C 0.77876(13) -0.03228(15) 0.97346(13) 0.0245(5) Uani 1 1 d . . . C19 C 0.76094(17) -0.08252(16) 0.91573(14) 0.0342(6) Uani 1 1 d . . . H19A H 0.7246 -0.0587 0.8886 0.051 Uiso 1 1 calc R . . H19B H 0.7472 -0.1333 0.9286 0.051 Uiso 1 1 calc R . . H19C H 0.7996 -0.0876 0.8932 0.051 Uiso 1 1 calc R . . C21 C 0.55815(13) -0.00797(15) 0.89308(11) 0.0224(5) Uani 1 1 d . . . H21 H 0.5502 0.0078 0.8509 0.027 Uiso 1 1 calc R . . C22 C 0.54008(13) -0.08352(14) 0.90895(12) 0.0230(5) Uani 1 1 d . . . H22 H 0.5193 -0.1171 0.8781 0.028 Uiso 1 1 calc R . . C23 C 0.55373(13) -0.10778(15) 0.97169(12) 0.0239(5) Uani 1 1 d . . . H23 H 0.5428 -0.1582 0.9833 0.029 Uiso 1 1 calc R . . C24 C 0.58394(13) -0.05576(15) 1.01691(12) 0.0224(5) Uani 1 1 d . . . H24 H 0.5937 -0.0710 1.0591 0.027 Uiso 1 1 calc R . . C25 C 0.59920(12) 0.01916(14) 0.99817(11) 0.0183(4) Uani 1 1 d . . . C27 C 0.62912(12) 0.08145(14) 1.04201(11) 0.0189(4) Uani 1 1 d . . . C31 C 0.66675(12) 0.26864(14) 1.00703(11) 0.0178(4) Uani 1 1 d . . . C33 C 0.69046(12) 0.34558(14) 1.03376(11) 0.0180(4) Uani 1 1 d . . . C34 C 0.70966(13) 0.35661(15) 1.09833(12) 0.0225(5) Uani 1 1 d . . . H34 H 0.7092 0.3153 1.1268 0.027 Uiso 1 1 calc R . . C35 C 0.72953(14) 0.43093(16) 1.11905(12) 0.0256(5) Uani 1 1 d . . . H35 H 0.7418 0.4403 1.1621 0.031 Uiso 1 1 calc R . . C36 C 0.73110(13) 0.49137(15) 1.07564(13) 0.0250(5) Uani 1 1 d . . . H36 H 0.7443 0.5413 1.0893 0.030 Uiso 1 1 calc R . . C37 C 0.71262(13) 0.47648(14) 1.01108(12) 0.0217(5) Uani 1 1 d . . . C39 C 0.71472(16) 0.53834(15) 0.96134(13) 0.0301(6) Uani 1 1 d . . . H39A H 0.7387 0.5189 0.9280 0.045 Uiso 1 1 calc R . . H39B H 0.7372 0.5839 0.9800 0.045 Uiso 1 1 calc R . . H39C H 0.6695 0.5519 0.9441 0.045 Uiso 1 1 calc R . . C41 C 0.52572(13) 0.42560(15) 0.93083(12) 0.0233(5) Uani 1 1 d . . . H41 H 0.5442 0.4275 0.9732 0.028 Uiso 1 1 calc R . . C42 C 0.45709(14) 0.43915(15) 0.91552(13) 0.0265(5) Uani 1 1 d . . . H42 H 0.4301 0.4499 0.9472 0.032 Uiso 1 1 calc R . . C43 C 0.42945(14) 0.43645(16) 0.85252(13) 0.0272(5) Uani 1 1 d . . . H43 H 0.3837 0.4459 0.8413 0.033 Uiso 1 1 calc R . . C44 C 0.47093(13) 0.41936(15) 0.80605(12) 0.0235(5) Uani 1 1 d . . . H44 H 0.4533 0.4166 0.7635 0.028 Uiso 1 1 calc R . . C45 C 0.53886(12) 0.40663(13) 0.82457(11) 0.0196(4) Uani 1 1 d . . . C46 C 0.58886(12) 0.38606(13) 0.78034(11) 0.0189(4) Uani 1 1 d . . . C50 C 0.75474(12) 0.34182(13) 0.81684(11) 0.0185(4) Uani 1 1 d . . . C52 C 0.81824(12) 0.31830(14) 0.79207(11) 0.0189(4) Uani 1 1 d . . . C53 C 0.82441(13) 0.31524(15) 0.72770(11) 0.0221(5) Uani 1 1 d . . . H53 H 0.7880 0.3273 0.6976 0.027 Uiso 1 1 calc R . . C54 C 0.88605(14) 0.29380(15) 0.70935(12) 0.0242(5) Uani 1 1 d . . . H54 H 0.8918 0.2920 0.6665 0.029 Uiso 1 1 calc R . . C55 C 0.93930(13) 0.27494(15) 0.75526(12) 0.0232(5) Uani 1 1 d . . . H55 H 0.9810 0.2611 0.7433 0.028 Uiso 1 1 calc R . . C56 C 0.92994(12) 0.27690(14) 0.81932(12) 0.0206(5) Uani 1 1 d . . . C58 C 0.98376(13) 0.25417(15) 0.87153(12) 0.0241(5) Uani 1 1 d . . . H58A H 0.9943 0.2981 0.8992 0.036 Uiso 1 1 calc R . . H58B H 1.0235 0.2383 0.8536 0.036 Uiso 1 1 calc R . . H58C H 0.9680 0.2115 0.8952 0.036 Uiso 1 1 calc R . . C60 C 0.94641(14) 0.04083(16) 0.89864(13) 0.0275(5) Uani 1 1 d . . . H60 H 0.9399 0.0285 0.9402 0.033 Uiso 1 1 calc R . . C61 C 1.01140(14) 0.03810(17) 0.88129(14) 0.0310(6) Uani 1 1 d . . . H61 H 1.0478 0.0246 0.9109 0.037 Uiso 1 1 calc R . . C62 C 1.02104(14) 0.05572(16) 0.81968(14) 0.0301(6) Uani 1 1 d . . . H62 H 1.0641 0.0542 0.8072 0.036 Uiso 1 1 calc R . . C63 C 0.96542(14) 0.07591(15) 0.77615(13) 0.0267(5) Uani 1 1 d . . . H63 H 0.9709 0.0879 0.7343 0.032 Uiso 1 1 calc R . . C64 C 0.90209(13) 0.07768(14) 0.79647(12) 0.0216(5) Uani 1 1 d . . . C65 C 0.83863(13) 0.10190(14) 0.75622(11) 0.0206(5) Uani 1 1 d . . . C69 C 0.68496(12) 0.13599(14) 0.80435(11) 0.0187(4) Uani 1 1 d . . . C71 C 0.61491(12) 0.16323(13) 0.78562(11) 0.0182(4) Uani 1 1 d . . . C72 C 0.58966(13) 0.17611(15) 0.72260(11) 0.0216(5) Uani 1 1 d . . . H72 H 0.6166 0.1681 0.6903 0.026 Uiso 1 1 calc R . . C73 C 0.52362(13) 0.20107(15) 0.70893(12) 0.0244(5) Uani 1 1 d . . . H73 H 0.5051 0.2092 0.6671 0.029 Uiso 1 1 calc R . . C74 C 0.48503(13) 0.21388(15) 0.75844(12) 0.0231(5) Uani 1 1 d . . . H74 H 0.4405 0.2306 0.7498 0.028 Uiso 1 1 calc R . . C75 C 0.51356(12) 0.20150(14) 0.82092(11) 0.0199(5) Uani 1 1 d . . . C77 C 0.47526(13) 0.21675(15) 0.87613(12) 0.0237(5) Uani 1 1 d . . . H77A H 0.4667 0.1681 0.8963 0.036 Uiso 1 1 calc R . . H77B H 0.4331 0.2416 0.8614 0.036 Uiso 1 1 calc R . . H77C H 0.5013 0.2503 0.9060 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.52910(6) 0.03714(5) 0.27992(3) 0.0517(3) Uani 1 1 d . . . Cl2 Cl 0.78948(3) 0.16394(4) 0.23646(3) 0.03037(14) Uani 1 1 d . . . Cl3 Cl 0.06166(4) 0.20333(4) 0.04099(3) 0.03105(14) Uani 1 1 d . . . Cl4 Cl -0.00438(4) 0.16724(4) 0.59069(4) 0.03515(15) Uani 1 1 d . . . Cu1 Cu 0.619970(14) 0.154577(16) 0.922277(13) 0.01672(7) Uani 1 1 d . . . Cu2 Cu 0.665279(14) 0.377444(16) 0.900042(13) 0.01685(7) Uani 1 1 d . . . Cu3 Cu 0.853798(14) 0.302256(16) 0.926804(13) 0.01695(7) Uani 1 1 d . . . Cu4 Cu 0.798378(15) 0.087197(17) 0.877505(13) 0.01828(7) Uani 1 1 d . . . N1 N 0.88997(11) 0.41105(12) 0.95268(10) 0.0214(4) Uani 1 1 d . . . N8 N 0.88023(11) 0.35273(13) 1.11570(10) 0.0226(4) Uani 1 1 d . . . H8A H 0.8706 0.3108 1.1351 0.027 Uiso 1 1 calc R . . H8B H 0.8940 0.3936 1.1371 0.027 Uiso 1 1 calc R . . N9 N 0.85325(10) 0.29530(12) 1.01615(9) 0.0183(4) Uani 1 1 d . . . N10 N 0.83928(10) 0.22418(12) 1.04315(9) 0.0185(4) Uani 1 1 d . . . N18 N 0.79666(10) 0.04253(12) 0.96351(10) 0.0195(4) Uani 1 1 d . . . N26 N 0.58670(10) 0.04286(12) 0.93656(9) 0.0196(4) Uani 1 1 d . . . N28 N 0.63897(11) 0.07283(13) 1.10440(10) 0.0231(4) Uani 1 1 d . . . H28A H 0.6552 0.1108 1.1281 0.028 Uiso 1 1 calc R . . H28B H 0.6292 0.0292 1.1213 0.028 Uiso 1 1 calc R . . N29 N 0.64232(10) 0.14519(12) 1.01162(9) 0.0190(4) Uani 1 1 d . . . N30 N 0.66612(10) 0.21032(12) 1.04658(9) 0.0194(4) Uani 1 1 d . . . N38 N 0.69182(10) 0.40417(12) 0.99111(9) 0.0183(4) Uani 1 1 d . . . N40 N 0.56601(10) 0.40994(12) 0.88652(10) 0.0198(4) Uani 1 1 d . . . N47 N 0.57259(11) 0.38258(13) 0.71767(10) 0.0220(4) Uani 1 1 d . . . H47A H 0.6029 0.3712 0.6936 0.026 Uiso 1 1 calc R . . H47B H 0.5318 0.3917 0.7013 0.026 Uiso 1 1 calc R . . N48 N 0.64878(10) 0.37338(12) 0.80986(9) 0.0194(4) Uani 1 1 d . . . N49 N 0.70133(10) 0.35302(12) 0.77568(10) 0.0204(4) Uani 1 1 d . . . N57 N 0.86990(10) 0.29916(11) 0.83667(9) 0.0177(4) Uani 1 1 d . . . N59 N 0.89301(11) 0.06061(12) 0.85738(10) 0.0225(4) Uani 1 1 d . . . N66 N 0.83574(11) 0.11309(13) 0.69376(10) 0.0242(4) Uani 1 1 d . . . H66A H 0.7984 0.1269 0.6721 0.029 Uiso 1 1 calc R . . H66B H 0.8712 0.1065 0.6751 0.029 Uiso 1 1 calc R . . N67 N 0.78846(10) 0.11003(12) 0.78947(9) 0.0203(4) Uani 1 1 d . . . N68 N 0.72543(10) 0.13421(12) 0.76059(9) 0.0204(4) Uani 1 1 d . . . N76 N 0.57758(10) 0.17538(11) 0.83385(9) 0.0176(4) Uani 1 1 d . . . O12 O 0.83063(9) 0.18917(10) 0.93683(8) 0.0193(3) Uani 1 1 d . . . O32 O 0.64805(9) 0.26449(10) 0.94556(8) 0.0192(3) Uani 1 1 d . . . O51 O 0.75710(8) 0.34974(10) 0.87857(8) 0.0193(3) Uani 1 1 d . . . O70 O 0.70113(9) 0.11679(10) 0.86436(8) 0.0193(3) Uani 1 1 d . . . O80 O 0.53717(19) 0.08749(16) 0.33463(11) 0.0696(10) Uani 1 1 d . . . O81 O 0.4599(2) 0.00889(19) 0.26881(14) 0.0693(9) Uani 1 1 d . . . O82 O 0.54554(14) 0.07864(13) 0.22504(10) 0.0450(6) Uani 1 1 d . . . O83 O 0.5762(2) -0.02833(15) 0.29141(11) 0.0704(10) Uani 1 1 d . . . O84 O 0.79720(15) 0.18912(17) 0.30169(11) 0.0531(7) Uani 1 1 d . . . O85 O 0.72065(12) 0.17360(18) 0.20921(13) 0.0544(7) Uani 1 1 d . . . O86 O 0.83096(13) 0.21190(16) 0.20112(12) 0.0489(6) Uani 1 1 d . . . O87 O 0.80960(14) 0.08385(15) 0.23226(11) 0.0477(6) Uani 1 1 d . . . O88 O 0.10614(12) 0.20411(17) 0.10029(10) 0.0456(6) Uani 1 1 d . . . O89 O 0.01937(13) 0.27103(15) 0.03916(12) 0.0475(6) Uani 1 1 d . . . O90 O 0.01976(19) 0.13515(16) 0.03762(14) 0.0675(9) Uani 1 1 d . . . O91 O 0.09988(15) 0.2060(2) -0.01125(12) 0.0737(11) Uani 1 1 d . . . O92 O -0.05639(13) 0.1162(2) 0.60916(15) 0.0645(9) Uani 1 1 d . . . O93 O 0.00451(16) 0.23303(16) 0.63159(13) 0.0581(7) Uani 1 1 d . . . O94 O 0.05475(12) 0.12302(14) 0.58994(15) 0.0535(7) Uani 1 1 d . . . O95 O -0.0212(3) 0.1968(2) 0.52695(14) 0.0942(15) Uani 1 1 d . . . O96 O 0.1223(2) 0.1424(4) 0.7303(2) 0.121(3) Uani 0.984(13) 1 d P . . O97 O 0.2485(2) 0.1431(3) 0.8000(2) 0.0654(18) Uani 0.712(11) 1 d P . . O98 O 0.37083(12) 0.06918(12) 0.82555(9) 0.0344(5) Uani 1 1 d . . . O99 O 0.73847(12) 0.20330(13) 0.60721(10) 0.0375(5) Uani 1 1 d . . . O100 O 0.94462(10) 0.13811(13) 0.14620(11) 0.0370(5) Uani 1 1 d . . . O101 O 0.6196(2) 0.2099(3) 0.2790(2) 0.0473(16) Uani 0.544(9) 1 d P . . O102 O 0.6605(4) 0.1949(4) 0.4104(3) 0.072(3) Uani 0.498(14) 1 d P . . O103 O 0.7614(2) 0.23771(19) 0.48245(15) 0.0517(14) Uani 0.823(11) 1 d P . . O104 O 0.6791(4) 0.1764(6) 0.3701(4) 0.089(4) Uani 0.493(14) 1 d P . . O105 O 0.8245(3) 0.2315(3) 0.4598(2) 0.0586(19) Uani 0.591(11) 1 d P . . O106 O 0.8150(6) 0.2506(6) 0.5114(5) 0.047(4) Uani 0.249(11) 1 d P . . O107 O 0.3145(9) 0.1075(9) 0.8038(8) 0.084(7) Uani 0.240(12) 1 d P . . 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 C2 0.0383(14) 0.0255(13) 0.0194(12) -0.0001(10) 0.0031(10) -0.0045(11) C3 0.0459(16) 0.0223(13) 0.0260(13) 0.0031(10) 0.0025(11) -0.0079(11) C4 0.0422(16) 0.0192(12) 0.0294(14) -0.0028(10) -0.0008(11) -0.0053(11) C5 0.0328(13) 0.0209(12) 0.0197(11) -0.0034(9) 0.0000(10) -0.0027(10) C6 0.0207(11) 0.0217(11) 0.0163(11) -0.0019(9) -0.0007(8) -0.0006(9) C7 0.0189(10) 0.0196(11) 0.0165(10) -0.0026(9) -0.0002(8) 0.0011(8) C11 0.0179(10) 0.0185(11) 0.0152(10) -0.0004(8) -0.0005(8) 0.0009(8) C13 0.0192(11) 0.0180(11) 0.0178(11) 0.0007(8) -0.0012(8) 0.0007(8) C14 0.0265(12) 0.0252(12) 0.0177(11) 0.0007(9) -0.0009(9) -0.0041(10) C15 0.0328(13) 0.0273(13) 0.0223(12) 0.0080(10) -0.0015(10) -0.0043(11) C16 0.0371(14) 0.0184(12) 0.0309(14) 0.0058(10) 0.0007(11) -0.0030(10) C17 0.0283(12) 0.0177(11) 0.0265(13) -0.0006(9) -0.0005(10) 0.0001(9) C19 0.0523(18) 0.0185(12) 0.0307(14) -0.0054(11) 0.0006(13) -0.0037(12) C21 0.0306(12) 0.0203(12) 0.0160(11) 0.0002(9) 0.0019(9) -0.0003(9) C22 0.0297(13) 0.0184(11) 0.0204(12) -0.0019(9) 0.0018(9) -0.0009(9) C23 0.0315(13) 0.0168(11) 0.0234(12) 0.0038(9) 0.0034(10) -0.0021(9) C24 0.0280(12) 0.0207(12) 0.0179(11) 0.0043(9) 0.0006(9) -0.0011(9) C25 0.0213(11) 0.0183(11) 0.0155(10) 0.0028(8) 0.0024(8) 0.0011(8) C27 0.0210(11) 0.0178(11) 0.0178(11) 0.0029(8) 0.0015(8) 0.0007(8) C31 0.0211(11) 0.0181(11) 0.0144(10) 0.0008(8) 0.0034(8) 0.0001(8) C33 0.0190(10) 0.0191(11) 0.0160(10) 0.0003(8) 0.0032(8) 0.0003(8) C34 0.0269(12) 0.0236(12) 0.0169(11) 0.0001(9) 0.0018(9) -0.0021(9) C35 0.0303(13) 0.0293(13) 0.0165(11) -0.0053(10) 0.0006(9) -0.0027(10) C36 0.0289(12) 0.0198(12) 0.0258(13) -0.0063(10) 0.0011(10) -0.0019(10) C37 0.0245(11) 0.0188(11) 0.0220(12) -0.0026(9) 0.0037(9) 0.0002(9) C39 0.0458(16) 0.0180(12) 0.0258(13) 0.0006(10) 0.0013(11) -0.0035(11) C41 0.0304(13) 0.0193(11) 0.0210(11) -0.0017(9) 0.0056(10) -0.0018(9) C42 0.0295(13) 0.0222(12) 0.0300(13) -0.0040(10) 0.0120(10) -0.0003(10) C43 0.0240(12) 0.0250(13) 0.0329(14) -0.0002(10) 0.0050(10) 0.0016(10) C44 0.0252(12) 0.0216(12) 0.0236(12) 0.0015(9) 0.0026(9) 0.0015(9) C45 0.0248(12) 0.0143(10) 0.0200(11) 0.0020(8) 0.0036(9) -0.0006(8) C46 0.0236(11) 0.0144(10) 0.0184(11) 0.0017(8) 0.0022(9) -0.0010(8) C50 0.0248(11) 0.0161(10) 0.0146(10) 0.0008(8) 0.0029(8) -0.0007(8) C52 0.0248(11) 0.0154(10) 0.0163(11) -0.0001(8) 0.0016(9) -0.0007(9) C53 0.0274(12) 0.0234(12) 0.0152(11) 0.0001(9) 0.0008(9) 0.0007(9) C54 0.0335(13) 0.0239(12) 0.0159(11) -0.0013(9) 0.0063(9) 0.0004(10) C55 0.0274(12) 0.0219(12) 0.0211(12) -0.0022(9) 0.0063(9) 0.0016(9) C56 0.0243(11) 0.0164(11) 0.0211(11) -0.0014(9) 0.0028(9) -0.0002(9) C58 0.0262(12) 0.0246(12) 0.0212(12) 0.0011(9) 0.0015(9) 0.0026(10) C60 0.0312(13) 0.0250(13) 0.0252(13) -0.0025(10) -0.0009(10) 0.0059(10) C61 0.0280(13) 0.0282(14) 0.0348(15) -0.0028(11) -0.0044(11) 0.0072(11) C62 0.0261(13) 0.0252(13) 0.0391(15) -0.0057(11) 0.0038(11) 0.0039(10) C63 0.0301(13) 0.0212(12) 0.0291(13) -0.0047(10) 0.0046(10) 0.0009(10) C64 0.0259(12) 0.0167(11) 0.0218(12) -0.0035(9) 0.0012(9) 0.0021(9) C65 0.0259(12) 0.0163(11) 0.0197(11) -0.0034(9) 0.0026(9) -0.0006(9) C69 0.0246(11) 0.0154(10) 0.0155(10) -0.0016(8) 0.0005(8) -0.0001(9) C71 0.0239(11) 0.0157(10) 0.0146(10) 0.0010(8) 0.0006(8) -0.0010(8) C72 0.0261(12) 0.0239(12) 0.0147(11) 0.0023(9) 0.0030(9) 0.0001(9) C73 0.0294(13) 0.0266(13) 0.0158(11) 0.0061(9) -0.0029(9) -0.0006(10) C74 0.0225(11) 0.0242(12) 0.0222(12) 0.0050(9) 0.0007(9) 0.0000(9) C75 0.0243(11) 0.0156(10) 0.0194(11) 0.0022(8) 0.0014(9) -0.0021(9) C77 0.0253(12) 0.0252(12) 0.0209(12) 0.0018(9) 0.0041(9) 0.0013(10) Cl1 0.1095(8) 0.0288(4) 0.0156(3) 0.0035(3) 0.0021(4) 0.0263(4) Cl2 0.0276(3) 0.0436(4) 0.0195(3) -0.0084(3) 0.0014(2) -0.0007(3) Cl3 0.0374(3) 0.0352(3) 0.0208(3) 0.0036(2) 0.0047(2) 0.0052(3) Cl4 0.0388(4) 0.0344(4) 0.0346(4) -0.0041(3) 0.0140(3) 0.0085(3) Cu1 0.02358(14) 0.01487(13) 0.01142(13) 0.00178(10) 0.00098(10) -0.00102(10) Cu2 0.02205(14) 0.01626(14) 0.01223(13) 0.00087(10) 0.00201(10) 0.00016(10) Cu3 0.02297(14) 0.01607(14) 0.01147(13) -0.00118(10) 0.00076(10) -0.00105(10) Cu4 0.02323(15) 0.01718(14) 0.01382(13) -0.00142(10) -0.00025(10) 0.00253(10) N1 0.0265(10) 0.0204(10) 0.0169(9) -0.0015(8) 0.0009(8) -0.0022(8) N8 0.0323(11) 0.0193(10) 0.0154(9) -0.0019(8) -0.0002(8) -0.0029(8) N9 0.0228(10) 0.0175(9) 0.0141(9) -0.0008(7) 0.0004(7) -0.0008(7) N10 0.0218(9) 0.0174(9) 0.0158(9) 0.0011(7) 0.0011(7) -0.0011(7) N18 0.0225(10) 0.0166(9) 0.0184(9) 0.0004(7) -0.0009(7) 0.0019(7) N26 0.0259(10) 0.0176(9) 0.0155(9) 0.0024(7) 0.0028(8) -0.0009(8) N28 0.0330(11) 0.0197(10) 0.0157(9) 0.0031(8) -0.0007(8) -0.0047(8) N29 0.0263(10) 0.0173(9) 0.0128(9) 0.0009(7) 0.0001(7) -0.0030(8) N30 0.0259(10) 0.0176(9) 0.0143(9) 0.0012(7) 0.0009(7) -0.0027(8) N38 0.0219(9) 0.0166(9) 0.0163(9) -0.0007(7) 0.0026(7) 0.0000(7) N40 0.0242(10) 0.0167(9) 0.0186(10) 0.0011(7) 0.0032(8) -0.0010(7) N47 0.0228(10) 0.0258(11) 0.0168(9) 0.0005(8) -0.0001(8) 0.0017(8) N48 0.0220(10) 0.0218(10) 0.0145(9) 0.0013(7) 0.0024(7) 0.0012(8) N49 0.0220(10) 0.0233(10) 0.0159(9) -0.0002(8) 0.0029(7) 0.0016(8) N57 0.0235(10) 0.0152(9) 0.0138(9) -0.0012(7) 0.0007(7) -0.0009(7) N59 0.0282(11) 0.0184(10) 0.0205(10) -0.0039(8) 0.0006(8) 0.0037(8) N66 0.0261(11) 0.0289(11) 0.0181(10) -0.0017(8) 0.0040(8) 0.0030(9) N67 0.0224(10) 0.0224(10) 0.0153(9) -0.0019(8) -0.0005(7) 0.0031(8) N68 0.0234(10) 0.0220(10) 0.0151(9) -0.0005(8) 0.0001(7) 0.0023(8) N76 0.0229(10) 0.0149(9) 0.0150(9) 0.0019(7) 0.0019(7) -0.0013(7) O12 0.0277(9) 0.0161(8) 0.0136(7) -0.0004(6) 0.0009(6) -0.0014(6) O32 0.0280(9) 0.0164(8) 0.0131(7) 0.0012(6) 0.0015(6) -0.0018(6) O51 0.0230(8) 0.0218(8) 0.0129(7) 0.0002(6) 0.0013(6) 0.0015(6) O70 0.0241(8) 0.0211(8) 0.0123(7) 0.0013(6) 0.0000(6) 0.0026(6) O80 0.132(3) 0.0480(15) 0.0229(11) -0.0086(10) -0.0141(14) 0.0514(17) O81 0.106(3) 0.0621(19) 0.0435(15) 0.0015(14) 0.0234(16) -0.0087(18) O82 0.0769(17) 0.0329(11) 0.0230(10) 0.0102(9) -0.0029(10) 0.0091(11) O83 0.150(3) 0.0399(14) 0.0236(11) 0.0112(10) 0.0196(15) 0.0510(17) O84 0.0702(17) 0.0657(17) 0.0213(11) -0.0147(11) -0.0033(11) 0.0061(14) O85 0.0303(12) 0.0773(19) 0.0530(15) -0.0196(14) -0.0052(11) 0.0007(12) O86 0.0533(15) 0.0484(14) 0.0483(14) -0.0091(11) 0.0200(12) -0.0120(11) O87 0.0647(16) 0.0424(13) 0.0341(12) -0.0022(10) -0.0016(11) 0.0012(12) O88 0.0407(12) 0.0698(17) 0.0254(11) 0.0097(11) 0.0009(9) 0.0052(11) O89 0.0527(14) 0.0390(13) 0.0493(14) 0.0037(11) 0.0007(11) 0.0089(11) O90 0.120(3) 0.0363(14) 0.0449(15) -0.0069(12) 0.0068(16) -0.0199(16) O91 0.0515(16) 0.146(3) 0.0261(12) 0.0173(16) 0.0148(11) 0.0255(18) O92 0.0369(13) 0.089(2) 0.073(2) -0.0242(17) 0.0268(13) -0.0177(14) O93 0.084(2) 0.0426(14) 0.0528(16) -0.0126(12) 0.0299(15) 0.0114(13) O94 0.0381(13) 0.0333(12) 0.093(2) -0.0123(13) 0.0251(13) 0.0023(10) O95 0.186(4) 0.062(2) 0.0329(14) 0.0017(13) 0.007(2) 0.059(2) O96 0.070(3) 0.228(7) 0.070(3) 0.057(3) 0.030(2) 0.033(3) O97 0.055(3) 0.053(3) 0.086(4) 0.030(2) 0.000(2) 0.0053(19) O98 0.0545(13) 0.0273(10) 0.0207(9) 0.0050(8) 0.0016(9) -0.0005(9) O99 0.0532(13) 0.0364(11) 0.0231(10) 0.0028(8) 0.0054(9) 0.0119(10) O100 0.0273(10) 0.0360(11) 0.0448(12) 0.0004(9) -0.0075(9) 0.0001(8) O101 0.044(3) 0.040(3) 0.062(3) 0.004(2) 0.021(2) -0.0019(19) O102 0.084(5) 0.084(5) 0.047(4) 0.003(3) 0.007(3) -0.004(4) O103 0.081(3) 0.0419(18) 0.0359(18) 0.0077(13) 0.0215(17) 0.0128(16) O104 0.072(5) 0.141(8) 0.060(5) -0.018(5) 0.031(4) -0.023(5) O105 0.064(3) 0.059(3) 0.055(3) -0.008(2) 0.012(2) -0.005(2) O106 0.058(8) 0.036(6) 0.048(7) -0.001(4) 0.008(5) 0.005(4) O107 0.110(15) 0.072(11) 0.076(11) -0.008(8) 0.035(9) -0.032(10) _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 C2 N1 1.336(3) . ? C2 C3 1.397(4) . ? C3 C4 1.377(4) . ? C4 C5 1.395(4) . ? C5 C6 1.385(3) . ? C6 N1 1.361(3) . ? C6 C7 1.486(3) . ? C7 N9 1.305(3) . ? C7 N8 1.335(3) . ? C11 O12 1.307(3) . ? C11 N10 1.310(3) . ? C11 C13 1.491(3) . ? C13 N18 1.353(3) . ? C13 C14 1.385(3) . ? C14 C15 1.388(4) . ? C15 C16 1.384(4) . ? C16 C17 1.392(4) . ? C17 N18 1.351(3) . ? C17 C19 1.503(4) . ? C21 N26 1.343(3) . ? C21 C22 1.393(3) . ? C22 C23 1.389(3) . ? C23 C24 1.391(4) . ? C24 C25 1.386(3) . ? C25 N26 1.362(3) . ? C25 C27 1.490(3) . ? C27 N29 1.309(3) . ? C27 N28 1.323(3) . ? C31 N30 1.304(3) . ? C31 O32 1.314(3) . ? C31 C33 1.487(3) . ? C33 N38 1.352(3) . ? C33 C34 1.390(3) . ? C34 C35 1.386(4) . ? C35 C36 1.387(4) . ? C36 C37 1.398(4) . ? C37 N38 1.355(3) . ? C37 C39 1.498(4) . ? C41 N40 1.336(3) . ? C41 C42 1.388(4) . ? C42 C43 1.384(4) . ? C43 C44 1.393(4) . ? C44 C45 1.382(4) . ? C45 N40 1.361(3) . ? C45 C46 1.493(3) . ? C46 N48 1.299(3) . ? C46 N47 1.331(3) . ? C50 N49 1.308(3) . ? C50 O51 1.312(3) . ? C50 C52 1.485(3) . ? C52 N57 1.352(3) . ? C52 C53 1.387(3) . ? C53 C54 1.384(4) . ? C54 C55 1.390(4) . ? C55 C56 1.395(3) . ? C56 N57 1.350(3) . ? C56 C58 1.498(3) . ? C60 N59 1.338(3) . ? C60 C61 1.392(4) . ? C61 C62 1.378(4) . ? C62 C63 1.398(4) . ? C63 C64 1.385(4) . ? C64 N59 1.359(3) . ? C64 C65 1.497(3) . ? C65 N67 1.301(3) . ? C65 N66 1.333(3) . ? C69 N68 1.303(3) . ? C69 O70 1.316(3) . ? C69 C71 1.481(3) . ? C71 N76 1.353(3) . ? C71 C72 1.388(3) . ? C72 C73 1.382(4) . ? C73 C74 1.393(4) . ? C74 C75 1.394(3) . ? C75 N76 1.350(3) . ? C75 C77 1.498(3) . ? Cl1 O82 1.435(2) . ? Cl1 O80 1.438(2) . ? Cl1 O81 1.455(4) . ? Cl1 O83 1.463(3) . ? Cl2 O87 1.432(3) . ? Cl2 O85 1.434(2) . ? Cl2 O86 1.439(3) . ? Cl2 O84 1.440(2) . ? Cl3 O91 1.421(3) . ? Cl3 O89 1.430(2) . ? Cl3 O90 1.431(3) . ? Cl3 O88 1.449(2) . ? Cl4 O94 1.403(2) . ? Cl4 O93 1.418(3) . ? Cl4 O95 1.445(3) . ? Cl4 O92 1.446(3) . ? Cu1 N29 1.9008(19) . ? Cu1 N76 1.9942(19) . ? Cu1 O32 2.0050(17) . ? Cu1 N26 2.056(2) . ? Cu1 O70 2.2441(17) . ? Cu2 N48 1.903(2) . ? Cu2 N38 1.994(2) . ? Cu2 O51 1.9985(17) . ? Cu2 N40 2.044(2) . ? Cu2 O32 2.2042(17) . ? Cu3 N9 1.901(2) . ? Cu3 N57 1.978(2) . ? Cu3 O12 2.0047(17) . ? Cu3 N1 2.045(2) . ? Cu3 O51 2.2252(17) . ? Cu4 N67 1.895(2) . ? Cu4 N18 1.982(2) . ? Cu4 O70 1.9925(17) . ? Cu4 N59 2.038(2) . ? Cu4 O12 2.1999(17) . ? N9 N10 1.387(3) . ? N29 N30 1.389(3) . ? N48 N49 1.390(3) . ? N67 N68 1.394(3) . ? O97 O107 1.444(19) . ? O98 O107 1.33(2) . ? O102 O104 1.022(9) . ? O103 O106 1.188(12) . ? O103 O105 1.405(6) . ? O105 O106 1.181(11) . ? 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 N1 C2 C3 122.3(2) . . ? C4 C3 C2 118.8(3) . . ? C3 C4 C5 119.5(2) . . ? C6 C5 C4 118.7(2) . . ? N1 C6 C5 122.0(2) . . ? N1 C6 C7 113.6(2) . . ? C5 C6 C7 124.4(2) . . ? N9 C7 N8 124.1(2) . . ? N9 C7 C6 113.1(2) . . ? N8 C7 C6 122.8(2) . . ? O12 C11 N10 124.9(2) . . ? O12 C11 C13 117.3(2) . . ? N10 C11 C13 117.8(2) . . ? N18 C13 C14 121.6(2) . . ? N18 C13 C11 115.5(2) . . ? C14 C13 C11 122.9(2) . . ? C13 C14 C15 118.6(2) . . ? C16 C15 C14 119.7(2) . . ? C15 C16 C17 119.3(2) . . ? N18 C17 C16 120.7(2) . . ? N18 C17 C19 117.0(2) . . ? C16 C17 C19 122.3(2) . . ? N26 C21 C22 122.3(2) . . ? C23 C22 C21 118.8(2) . . ? C22 C23 C24 119.2(2) . . ? C25 C24 C23 119.0(2) . . ? N26 C25 C24 122.0(2) . . ? N26 C25 C27 113.5(2) . . ? C24 C25 C27 124.5(2) . . ? N29 C27 N28 124.8(2) . . ? N29 C27 C25 112.1(2) . . ? N28 C27 C25 123.0(2) . . ? N30 C31 O32 125.0(2) . . ? N30 C31 C33 117.3(2) . . ? O32 C31 C33 117.7(2) . . ? N38 C33 C34 122.3(2) . . ? N38 C33 C31 115.5(2) . . ? C34 C33 C31 122.2(2) . . ? C35 C34 C33 118.1(2) . . ? C34 C35 C36 120.0(2) . . ? C35 C36 C37 119.4(2) . . ? N38 C37 C36 120.4(2) . . ? N38 C37 C39 117.2(2) . . ? C36 C37 C39 122.4(2) . . ? N40 C41 C42 122.0(2) . . ? C43 C42 C41 119.1(2) . . ? C42 C43 C44 119.3(2) . . ? C45 C44 C43 118.6(2) . . ? N40 C45 C44 122.0(2) . . ? N40 C45 C46 113.5(2) . . ? C44 C45 C46 124.5(2) . . ? N48 C46 N47 124.9(2) . . ? N48 C46 C45 112.5(2) . . ? N47 C46 C45 122.5(2) . . ? N49 C50 O51 125.4(2) . . ? N49 C50 C52 117.7(2) . . ? O51 C50 C52 116.9(2) . . ? N57 C52 C53 121.9(2) . . ? N57 C52 C50 115.4(2) . . ? C53 C52 C50 122.7(2) . . ? C54 C53 C52 118.4(2) . . ? C53 C54 C55 119.6(2) . . ? C54 C55 C56 119.7(2) . . ? N57 C56 C55 120.1(2) . . ? N57 C56 C58 116.9(2) . . ? C55 C56 C58 123.1(2) . . ? N59 C60 C61 122.0(3) . . ? C62 C61 C60 119.1(3) . . ? C61 C62 C63 119.3(3) . . ? C64 C63 C62 118.8(3) . . ? N59 C64 C63 121.6(2) . . ? N59 C64 C65 113.6(2) . . ? C63 C64 C65 124.7(2) . . ? N67 C65 N66 125.5(2) . . ? N67 C65 C64 112.0(2) . . ? N66 C65 C64 122.5(2) . . ? N68 C69 O70 125.7(2) . . ? N68 C69 C71 117.6(2) . . ? O70 C69 C71 116.8(2) . . ? N76 C71 C72 122.4(2) . . ? N76 C71 C69 115.7(2) . . ? C72 C71 C69 121.9(2) . . ? C73 C72 C71 118.4(2) . . ? C72 C73 C74 119.4(2) . . ? C73 C74 C75 119.6(2) . . ? N76 C75 C74 120.7(2) . . ? N76 C75 C77 117.3(2) . . ? C74 C75 C77 122.0(2) . . ? O82 Cl1 O80 110.18(18) . . ? O82 Cl1 O81 109.80(17) . . ? O80 Cl1 O81 109.9(2) . . ? O82 Cl1 O83 107.92(16) . . ? O80 Cl1 O83 108.45(16) . . ? O81 Cl1 O83 110.6(2) . . ? O87 Cl2 O85 110.31(17) . . ? O87 Cl2 O86 109.19(16) . . ? O85 Cl2 O86 107.94(18) . . ? O87 Cl2 O84 110.33(16) . . ? O85 Cl2 O84 109.78(16) . . ? O86 Cl2 O84 109.24(17) . . ? O91 Cl3 O89 108.89(19) . . ? O91 Cl3 O90 110.7(2) . . ? O89 Cl3 O90 108.54(19) . . ? O91 Cl3 O88 110.29(16) . . ? O89 Cl3 O88 108.26(16) . . ? O90 Cl3 O88 110.09(17) . . ? O94 Cl4 O93 113.02(18) . . ? O94 Cl4 O95 106.1(2) . . ? O93 Cl4 O95 107.03(19) . . ? O94 Cl4 O92 108.11(18) . . ? O93 Cl4 O92 110.66(17) . . ? O95 Cl4 O92 111.9(3) . . ? N29 Cu1 N76 167.09(9) . . ? N29 Cu1 O32 78.96(8) . . ? N76 Cu1 O32 97.98(7) . . ? N29 Cu1 N26 79.36(8) . . ? N76 Cu1 N26 101.34(8) . . ? O32 Cu1 N26 156.83(7) . . ? N29 Cu1 O70 115.11(8) . . ? N76 Cu1 O70 77.76(7) . . ? O32 Cu1 O70 101.88(7) . . ? N26 Cu1 O70 94.65(7) . . ? N48 Cu2 N38 167.45(9) . . ? N48 Cu2 O51 79.25(8) . . ? N38 Cu2 O51 97.60(7) . . ? N48 Cu2 N40 79.78(8) . . ? N38 Cu2 N40 102.28(8) . . ? O51 Cu2 N40 158.83(7) . . ? N48 Cu2 O32 113.05(8) . . ? N38 Cu2 O32 79.23(7) . . ? O51 Cu2 O32 95.09(7) . . ? N40 Cu2 O32 95.69(7) . . ? N9 Cu3 N57 169.69(9) . . ? N9 Cu3 O12 78.72(8) . . ? N57 Cu3 O12 98.25(7) . . ? N9 Cu3 N1 80.43(8) . . ? N57 Cu3 N1 100.97(8) . . ? O12 Cu3 N1 157.88(7) . . ? N9 Cu3 O51 111.82(8) . . ? N57 Cu3 O51 78.40(7) . . ? O12 Cu3 O51 101.66(7) . . ? N1 Cu3 O51 92.87(7) . . ? N67 Cu4 N18 167.26(9) . . ? N67 Cu4 O70 80.01(8) . . ? N18 Cu4 O70 95.80(8) . . ? N67 Cu4 N59 80.08(9) . . ? N18 Cu4 N59 103.14(9) . . ? O70 Cu4 N59 159.94(8) . . ? N67 Cu4 O12 112.91(8) . . ? N18 Cu4 O12 79.33(7) . . ? O70 Cu4 O12 95.24(7) . . ? N59 Cu4 O12 94.72(8) . . ? C2 N1 C6 118.8(2) . . ? C2 N1 Cu3 128.35(17) . . ? C6 N1 Cu3 112.27(16) . . ? C7 N9 N10 120.00(19) . . ? C7 N9 Cu3 119.96(17) . . ? N10 N9 Cu3 119.53(15) . . ? C11 N10 N9 107.11(19) . . ? C17 N18 C13 120.0(2) . . ? C17 N18 Cu4 122.88(17) . . ? C13 N18 Cu4 116.96(16) . . ? C21 N26 C25 118.7(2) . . ? C21 N26 Cu1 128.11(16) . . ? C25 N26 Cu1 113.13(16) . . ? C27 N29 N30 118.69(19) . . ? C27 N29 Cu1 121.65(17) . . ? N30 N29 Cu1 119.25(15) . . ? C31 N30 N29 107.35(19) . . ? C33 N38 C37 119.8(2) . . ? C33 N38 Cu2 117.03(16) . . ? C37 N38 Cu2 123.17(17) . . ? C41 N40 C45 119.0(2) . . ? C41 N40 Cu2 127.70(18) . . ? C45 N40 Cu2 112.94(16) . . ? C46 N48 N49 119.9(2) . . ? C46 N48 Cu2 121.02(17) . . ? N49 N48 Cu2 118.97(15) . . ? C50 N49 N48 107.09(19) . . ? C56 N57 C52 120.3(2) . . ? C56 N57 Cu3 121.66(16) . . ? C52 N57 Cu3 118.06(16) . . ? C60 N59 C64 119.3(2) . . ? C60 N59 Cu4 127.17(18) . . ? C64 N59 Cu4 112.69(16) . . ? C65 N67 N68 120.4(2) . . ? C65 N67 Cu4 121.18(17) . . ? N68 N67 Cu4 118.37(15) . . ? C69 N68 N67 107.35(19) . . ? C75 N76 C71 119.5(2) . . ? C75 N76 Cu1 122.22(16) . . ? C71 N76 Cu1 118.33(16) . . ? C11 O12 Cu3 109.75(14) . . ? C11 O12 Cu4 110.51(14) . . ? Cu3 O12 Cu4 139.31(8) . . ? C31 O32 Cu1 109.41(14) . . ? C31 O32 Cu2 110.31(14) . . ? Cu1 O32 Cu2 140.03(8) . . ? C50 O51 Cu2 109.24(15) . . ? C50 O51 Cu3 110.21(14) . . ? Cu2 O51 Cu3 138.57(8) . . ? C69 O70 Cu4 108.60(15) . . ? C69 O70 Cu1 110.45(14) . . ? Cu4 O70 Cu1 138.78(8) . . ? O106 O103 O105 53.4(6) . . ? O106 O105 O103 53.8(6) . . ? O105 O106 O103 72.8(7) . . ? O98 O107 O97 161.9(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.860 _refine_diff_density_min -1.113 _refine_diff_density_rms 0.090 data_shelxl(1) _database_code_depnum_ccdc_archive 'CCDC 299029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 Mn4 N32 O6' _chemical_formula_weight 1384.91 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.0200(9) _cell_length_b 14.0538(10) _cell_length_c 16.5587(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.2530(10) _cell_angle_gamma 90.00 _cell_volume 2981.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6506 _exptl_absorpt_correction_T_max 0.9647 _exptl_absorpt_process_details 'SADABS (sheldric, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker P4/RA diffractometer/SMART 1000 CCD detector' _diffrn_measurement_method '\omega csans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16310 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 26.40 _reflns_number_total 10903 _reflns_number_gt 8238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _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^)+(0.1071P)^2^+2.9863P] 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 0.28(3) _refine_ls_number_reflns 10903 _refine_ls_number_parameters 811 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.008 _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 -0.91584(8) -0.84582(8) -0.21718(7) 0.0283(3) Uani 1 1 d . . . Mn2 Mn -1.19088(8) -0.88943(8) -0.36481(7) 0.0289(3) Uani 1 1 d . . . Mn3 Mn -1.13262(9) -1.16580(8) -0.33165(7) 0.0305(3) Uani 1 1 d . . . Mn4 Mn -0.89962(10) -1.11528(9) -0.15539(7) 0.0347(3) Uani 1 1 d . . . O1 O -1.0181(4) -0.8892(4) -0.3327(3) 0.0282(11) Uani 1 1 d . . . O2 O -1.2020(4) -1.0289(4) -0.3050(3) 0.0291(12) Uani 1 1 d . . . O3 O -0.9678(4) -1.1487(4) -0.2813(3) 0.0306(12) Uani 1 1 d . . . O4 O -0.9684(4) -0.9716(4) -0.1625(3) 0.0345(13) Uani 1 1 d . . . O5 O -0.4198(10) -0.1518(11) -0.0493(7) 0.138(5) Uani 1 1 d . . . O6 O -1.4975(15) -0.5574(8) -0.1886(8) 0.177(7) Uani 1 1 d . . . N1 N -0.8126(5) -0.9122(5) -0.2963(4) 0.0309(15) Uani 1 1 d . . . N2 N -1.0228(5) -0.9555(5) -0.4619(4) 0.0294(14) Uani 1 1 d . . . N3 N -1.1299(5) -0.9414(5) -0.4689(4) 0.0293(14) Uani 1 1 d . . . N4 N -1.1440(5) -0.9835(6) -0.6067(4) 0.0434(18) Uani 1 1 d . . . N5 N -1.3316(5) -0.9156(5) -0.4787(4) 0.0329(15) Uani 1 1 d . . . N6 N -1.3071(5) -0.8731(5) -0.2786(4) 0.0350(16) Uani 1 1 d . . . N7 N -1.2998(5) -1.1190(5) -0.2282(4) 0.0324(15) Uani 1 1 d . . . N8 N -1.2466(5) -1.1940(5) -0.2553(4) 0.0296(14) Uani 1 1 d . . . N9 N -1.3234(5) -1.2916(6) -0.1691(5) 0.0462(19) Uani 1 1 d . . . N10 N -1.1419(5) -1.3327(5) -0.3078(4) 0.0367(16) Uani 1 1 d . . . N11 N -1.2457(5) -1.1763(5) -0.4557(4) 0.0341(15) Uani 1 1 d . . . N12 N -1.0311(5) -1.2086(5) -0.5648(4) 0.0359(16) Uani 1 1 d . . . N13 N -1.0455(5) -1.1928(5) -0.4274(4) 0.0292(14) Uani 1 1 d . . . N14 N -0.9380(5) -1.1985(5) -0.4077(4) 0.0309(15) Uani 1 1 d . . . N15 N -0.7648(5) -1.1531(6) -0.2199(4) 0.0417(17) Uani 1 1 d . . . N16 N -0.9388(6) -1.2735(5) -0.1194(4) 0.0419(18) Uani 1 1 d . . . N17 N -1.1415(6) -1.1866(6) -0.0159(5) 0.049(2) Uani 1 1 d . . . N18 N -1.0419(5) -1.1158(5) -0.1032(4) 0.0339(14) Uani 1 1 d . . . N19 N -1.0912(5) -1.0326(5) -0.0920(4) 0.0320(15) Uani 1 1 d . . . N20 N -1.0503(5) -0.7990(5) -0.1607(4) 0.0305(15) Uani 1 1 d . . . N21 N -0.8908(6) -0.6988(5) -0.2542(4) 0.0369(16) Uani 1 1 d . . . N22 N -0.8239(6) -0.6401(6) -0.2357(4) 0.0452(19) Uani 1 1 d . . . N23 N -0.7640(8) -0.5815(7) -0.2250(6) 0.067(3) Uani 1 1 d . . . N24 N -0.7970(6) -0.8324(7) -0.1068(4) 0.050(2) Uani 1 1 d . . . N25 N -0.7075(7) -0.8208(7) -0.0838(5) 0.059(2) Uani 1 1 d . . . N26 N -0.6166(9) -0.8207(13) -0.0564(9) 0.141(7) Uani 1 1 d . . . N27 N -1.1885(5) -0.7380(5) -0.3914(4) 0.0360(16) Uani 1 1 d . . . N28 N -1.2622(5) -0.6930(5) -0.4253(4) 0.0339(16) Uani 1 1 d . . . N29 N -1.3311(6) -0.6474(6) -0.4573(5) 0.055(2) Uani 1 1 d . . . N30 N -0.7842(8) -1.0674(7) -0.0549(5) 0.071(3) Uani 1 1 d . . . N31 N -0.7440(8) -1.0273(7) 0.0026(7) 0.069(3) Uani 1 1 d . . . N32 N -0.6993(10) -0.9811(8) 0.0664(7) 0.089(3) Uani 1 1 d . . . C1 C -0.7091(6) -0.9220(7) -0.2771(5) 0.038(2) Uani 1 1 d . . . C2 C -0.6489(6) -0.9546(7) -0.3296(6) 0.046(2) Uani 1 1 d . . . C3 C -0.6976(7) -0.9866(7) -0.4075(6) 0.043(2) Uani 1 1 d . . . C4 C -0.8033(6) -0.9775(6) -0.4281(5) 0.0364(19) Uani 1 1 d . . . C5 C -0.8596(6) -0.9388(6) -0.3709(5) 0.0289(16) Uani 1 1 d . . . C6 C -0.9746(6) -0.9270(5) -0.3893(5) 0.0287(16) Uani 1 1 d . . . C7 C -1.1844(6) -0.9575(6) -0.5404(5) 0.0316(17) Uani 1 1 d . . . C8 C -1.2988(6) -0.9436(6) -0.5485(5) 0.0366(19) Uani 1 1 d . . . C9 C -1.3671(7) -0.9588(7) -0.6201(6) 0.045(2) Uani 1 1 d . . . C10 C -1.4732(7) -0.9465(8) -0.6223(6) 0.054(3) Uani 1 1 d . . . C11 C -1.5060(6) -0.9188(7) -0.5528(6) 0.049(2) Uani 1 1 d . . . C12 C -1.4322(7) -0.9010(8) -0.4825(6) 0.051(2) Uani 1 1 d . . . C13 C -1.3557(6) -0.7923(6) -0.2642(5) 0.0355(19) Uani 1 1 d . . . C14 C -1.4237(6) -0.7844(7) -0.2094(5) 0.041(2) Uani 1 1 d . . . C15 C -1.4441(6) -0.8667(7) -0.1672(5) 0.040(2) Uani 1 1 d . . . C16 C -1.3938(6) -0.9540(6) -0.1818(5) 0.0365(19) Uani 1 1 d . . . C17 C -1.3258(5) -0.9529(6) -0.2388(5) 0.0288(17) Uani 1 1 d . . . C18 C -1.2711(5) -1.0384(6) -0.2587(5) 0.0308(18) Uani 1 1 d . . . C19 C -1.2634(6) -1.2756(6) -0.2270(5) 0.0334(19) Uani 1 1 d . . . C20 C -1.2137(6) -1.3558(6) -0.2620(5) 0.0327(17) Uani 1 1 d . . . C21 C -1.2415(7) -1.4518(7) -0.2530(5) 0.041(2) Uani 1 1 d . . . C22 C -1.1921(7) -1.5222(6) -0.2915(5) 0.039(2) Uani 1 1 d . . . C23 C -1.1183(8) -1.4944(7) -0.3368(6) 0.048(2) Uani 1 1 d . . . C24 C -1.0976(8) -1.3999(7) -0.3434(6) 0.049(2) Uani 1 1 d . . . C25 C -1.3508(6) -1.1704(7) -0.4676(6) 0.041(2) Uani 1 1 d . . . C26 C -1.4132(6) -1.1837(7) -0.5411(6) 0.046(2) Uani 1 1 d . . . C27 C -1.3681(7) -1.2059(8) -0.6060(6) 0.051(2) Uani 1 1 d . . . C28 C -1.2603(6) -1.2131(6) -0.5984(5) 0.0373(19) Uani 1 1 d . . . C29 C -1.2025(6) -1.1964(5) -0.5217(5) 0.0282(16) Uani 1 1 d . . . C30 C -1.0864(6) -1.1995(5) -0.5039(5) 0.0277(16) Uani 1 1 d . . . C31 C -0.9079(5) -1.1761(5) -0.3316(4) 0.0275(16) Uani 1 1 d . . . C32 C -0.7937(6) -1.1822(6) -0.2983(5) 0.0363(19) Uani 1 1 d . . . C33 C -0.7207(6) -1.2106(6) -0.3455(6) 0.040(2) Uani 1 1 d . . . C34 C -0.6163(7) -1.2097(8) -0.3118(7) 0.055(3) Uani 1 1 d . . . C35 C -0.5870(7) -1.1822(8) -0.2319(7) 0.059(3) Uani 1 1 d . . . C36 C -0.6613(7) -1.1523(8) -0.1890(6) 0.050(2) Uani 1 1 d . . . C37 C -0.8938(8) -1.3518(7) -0.1409(6) 0.051(2) Uani 1 1 d . . . C38 C -0.9303(9) -1.4426(7) -0.1242(6) 0.050(2) Uani 1 1 d . . . C39 C -1.0118(8) -1.4487(7) -0.0839(6) 0.050(2) Uani 1 1 d . . . C40 C -1.0587(7) -1.3686(6) -0.0616(5) 0.043(2) Uani 1 1 d . . . C41 C -1.0209(6) -1.2813(6) -0.0814(5) 0.0354(19) Uani 1 1 d . . . C42 C -1.0719(6) -1.1913(6) -0.0646(5) 0.036(2) Uani 1 1 d . . . C43 C -1.0485(6) -0.9634(6) -0.1263(5) 0.0290(17) Uani 1 1 d . . . C44 C -1.0938(5) -0.8667(5) -0.1215(4) 0.0289(17) Uani 1 1 d . . . C45 C -1.1737(6) -0.8496(6) -0.0768(4) 0.0302(16) Uani 1 1 d . . . C46 C -1.2076(6) -0.7560(7) -0.0731(5) 0.042(2) Uani 1 1 d . . . C47 C -1.1644(6) -0.6860(6) -0.1140(5) 0.0379(19) Uani 1 1 d . . . C48 C -1.0867(7) -0.7098(6) -0.1559(6) 0.041(2) Uani 1 1 d . . . H1 H -1.0707 -0.9911 -0.6023 0.052 Uiso 1 1 d . . . H2 H -1.1888 -0.9943 -0.6577 0.052 Uiso 1 1 d . . . H3 H -1.3557 -1.2397 -0.1468 0.055 Uiso 1 1 d . . . H4 H -1.3325 -1.3545 -0.1509 0.055 Uiso 1 1 d . . . H5 H -0.9573 -1.2108 -0.5528 0.044 Uiso 1 1 d . . . H6 H -1.0666 -1.2135 -0.6203 0.044 Uiso 1 1 d . . . H7 H -1.1603 -1.2424 0.0106 0.058 Uiso 1 1 d . . . H8 H -1.1730 -1.1274 -0.0070 0.058 Uiso 1 1 d . . . H9 H -0.6757 -0.9045 -0.2233 0.046 Uiso 1 1 d . . . H10 H -0.5749 -0.9563 -0.3140 0.055 Uiso 1 1 d . . . H11 H -0.6579 -1.0140 -0.4444 0.052 Uiso 1 1 d . . . H12 H -0.8386 -0.9970 -0.4807 0.044 Uiso 1 1 d . . . H13 H -1.3421 -0.9774 -0.6687 0.054 Uiso 1 1 d . . . H14 H -1.5222 -0.9567 -0.6712 0.065 Uiso 1 1 d . . . H15 H -1.5784 -0.9118 -0.5520 0.058 Uiso 1 1 d . . . H16 H -1.4556 -0.8769 -0.4350 0.062 Uiso 1 1 d . . . H17 H -1.3426 -0.7373 -0.2941 0.043 Uiso 1 1 d . . . H18 H -1.4551 -0.7251 -0.2007 0.050 Uiso 1 1 d . . . H19 H -1.4909 -0.8647 -0.1295 0.048 Uiso 1 1 d . . . H20 H -1.4063 -1.0109 -0.1541 0.044 Uiso 1 1 d . . . H21 H -1.2931 -1.4683 -0.2213 0.050 Uiso 1 1 d . . . H22 H -1.2088 -1.5878 -0.2865 0.047 Uiso 1 1 d . . . H23 H -1.0827 -1.5408 -0.3634 0.059 Uiso 1 1 d . . . H24 H -1.0472 -1.3818 -0.3758 0.060 Uiso 1 1 d . . . H25 H -1.3825 -1.1558 -0.4216 0.050 Uiso 1 1 d . . . H26 H -1.4868 -1.1785 -0.5471 0.055 Uiso 1 1 d . . . H27 H -1.4107 -1.2167 -0.6582 0.061 Uiso 1 1 d . . . H28 H -1.2283 -1.2288 -0.6439 0.045 Uiso 1 1 d . . . H29 H -0.7431 -1.2303 -0.4009 0.047 Uiso 1 1 d . . . H30 H -0.5658 -1.2278 -0.3439 0.067 Uiso 1 1 d . . . H31 H -0.5156 -1.1836 -0.2065 0.071 Uiso 1 1 d . . . H32 H -0.6395 -1.1302 -0.1342 0.061 Uiso 1 1 d . . . H33 H -0.8358 -1.3468 -0.1680 0.063 Uiso 1 1 d . . . H34 H -0.8977 -1.4986 -0.1406 0.059 Uiso 1 1 d . . . H35 H -1.0365 -1.5095 -0.0711 0.061 Uiso 1 1 d . . . H36 H -1.1160 -1.3726 -0.0335 0.051 Uiso 1 1 d . . . H37 H -1.2032 -0.9002 -0.0499 0.036 Uiso 1 1 d . . . H38 H -1.2602 -0.7405 -0.0420 0.051 Uiso 1 1 d . . . H39 H -1.1876 -0.6220 -0.1133 0.045 Uiso 1 1 d . . . H40 H -1.0566 -0.6606 -0.1836 0.049 Uiso 1 1 d . . . H41 H -0.4912 -0.1510 -0.0441 0.076 Uiso 1 1 d . . . H42 H -0.3867 -0.1091 -0.0050 0.076 Uiso 1 1 d . . . H43 H -1.4676 -0.5745 -0.2361 0.076 Uiso 1 1 d . . . H44 H -1.5476 -0.6075 -0.1857 0.076 Uiso 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 0.0308(6) 0.0273(6) 0.0272(6) 0.0013(5) 0.0059(4) 0.0029(5) Mn2 0.0273(5) 0.0267(6) 0.0328(6) -0.0004(5) 0.0057(5) 0.0024(5) Mn3 0.0318(6) 0.0280(7) 0.0346(7) -0.0001(5) 0.0134(5) 0.0017(5) Mn4 0.0469(7) 0.0288(7) 0.0290(6) 0.0011(5) 0.0083(5) 0.0043(6) O1 0.032(2) 0.029(3) 0.023(2) 0.001(2) 0.004(2) 0.002(2) O2 0.033(3) 0.027(3) 0.031(3) 0.001(2) 0.014(2) 0.004(2) O3 0.033(3) 0.032(3) 0.029(3) -0.001(2) 0.010(2) 0.005(2) O4 0.045(3) 0.023(3) 0.037(3) -0.002(2) 0.011(3) 0.002(2) O5 0.143(10) 0.172(13) 0.094(8) 0.029(8) 0.006(7) 0.046(9) O6 0.35(2) 0.081(9) 0.137(11) 0.032(8) 0.132(12) 0.077(11) N1 0.033(3) 0.033(4) 0.027(3) -0.008(3) 0.006(3) -0.004(3) N2 0.026(3) 0.031(4) 0.031(3) -0.004(3) 0.004(3) -0.001(3) N3 0.032(3) 0.025(4) 0.030(3) -0.002(3) 0.003(3) -0.003(3) N4 0.042(4) 0.052(5) 0.036(4) -0.008(3) 0.005(3) -0.002(3) N5 0.028(3) 0.030(4) 0.039(4) -0.001(3) 0.003(3) -0.006(3) N6 0.032(3) 0.037(4) 0.035(4) -0.004(3) 0.003(3) 0.007(3) N7 0.030(3) 0.032(4) 0.037(4) -0.004(3) 0.010(3) -0.003(3) N8 0.035(3) 0.024(4) 0.031(3) 0.001(3) 0.008(3) 0.001(3) N9 0.037(4) 0.047(5) 0.061(5) 0.011(4) 0.027(4) 0.000(3) N10 0.040(4) 0.025(4) 0.046(4) 0.002(3) 0.010(3) 0.010(3) N11 0.032(3) 0.033(4) 0.038(4) -0.003(3) 0.010(3) 0.000(3) N12 0.034(3) 0.044(4) 0.029(4) -0.008(3) 0.003(3) 0.002(3) N13 0.027(3) 0.031(4) 0.032(4) 0.001(3) 0.014(3) 0.001(3) N14 0.035(3) 0.030(4) 0.028(3) -0.002(3) 0.003(3) -0.001(3) N15 0.044(4) 0.042(5) 0.036(4) 0.001(3) -0.002(3) 0.005(3) N16 0.056(5) 0.031(4) 0.033(4) 0.001(3) -0.008(3) 0.005(3) N17 0.049(4) 0.039(5) 0.061(5) 0.023(4) 0.021(4) 0.002(3) N18 0.042(4) 0.027(4) 0.033(3) 0.002(3) 0.007(3) -0.001(3) N19 0.040(4) 0.027(4) 0.029(4) 0.000(3) 0.008(3) 0.000(3) N20 0.033(3) 0.023(4) 0.035(4) 0.003(3) 0.005(3) -0.001(3) N21 0.047(4) 0.031(4) 0.034(4) 0.002(3) 0.011(3) 0.000(3) N22 0.054(5) 0.042(5) 0.039(4) -0.002(3) 0.007(3) -0.007(4) N23 0.079(6) 0.065(7) 0.059(6) -0.014(5) 0.018(5) -0.026(5) N24 0.036(4) 0.076(6) 0.036(4) -0.006(4) 0.001(3) 0.011(4) N25 0.054(5) 0.074(7) 0.054(5) -0.034(5) 0.023(4) 0.000(5) N26 0.055(6) 0.24(2) 0.133(11) -0.096(12) 0.042(7) -0.037(9) N27 0.032(3) 0.025(4) 0.049(4) 0.000(3) 0.002(3) 0.005(3) N28 0.036(4) 0.028(4) 0.040(4) 0.002(3) 0.014(3) -0.007(3) N29 0.043(4) 0.057(6) 0.064(5) 0.026(4) 0.012(4) 0.007(4) N30 0.108(8) 0.067(7) 0.033(5) -0.027(4) 0.000(5) -0.044(6) N31 0.071(6) 0.062(7) 0.076(7) 0.012(6) 0.018(5) 0.003(5) N32 0.115(9) 0.073(8) 0.083(8) -0.020(6) 0.027(7) -0.007(7) C1 0.027(4) 0.050(6) 0.038(5) -0.002(4) 0.006(3) 0.006(4) C2 0.028(4) 0.053(6) 0.055(6) -0.007(5) 0.007(4) 0.004(4) C3 0.038(5) 0.042(5) 0.048(5) -0.011(4) 0.010(4) 0.001(4) C4 0.041(4) 0.030(5) 0.040(4) -0.008(4) 0.012(4) -0.002(4) C5 0.030(4) 0.023(4) 0.035(4) 0.000(3) 0.010(3) 0.000(3) C6 0.030(4) 0.025(4) 0.031(4) 0.005(3) 0.004(3) 0.006(3) C7 0.031(4) 0.028(4) 0.036(4) -0.002(3) 0.005(3) -0.004(3) C8 0.039(4) 0.026(4) 0.043(5) 0.009(4) 0.003(4) 0.000(4) C9 0.038(5) 0.046(6) 0.045(5) -0.012(4) -0.007(4) 0.000(4) C10 0.037(5) 0.060(7) 0.058(6) -0.015(5) -0.007(4) -0.006(4) C11 0.026(4) 0.058(7) 0.060(6) 0.003(5) -0.001(4) -0.001(4) C12 0.037(5) 0.054(6) 0.062(6) -0.015(5) 0.009(4) 0.004(4) C13 0.031(4) 0.038(5) 0.036(5) 0.008(4) 0.001(3) 0.012(4) C14 0.030(4) 0.046(6) 0.045(5) -0.018(4) -0.002(4) 0.018(4) C15 0.028(4) 0.051(6) 0.042(5) -0.012(4) 0.007(3) 0.004(4) C16 0.029(4) 0.045(6) 0.036(4) -0.003(4) 0.006(3) -0.003(4) C17 0.017(3) 0.033(5) 0.034(4) -0.007(3) 0.001(3) 0.005(3) C18 0.016(3) 0.037(5) 0.039(5) -0.002(4) 0.005(3) 0.003(3) C19 0.022(4) 0.040(5) 0.037(5) 0.002(4) 0.004(3) 0.001(3) C20 0.031(4) 0.028(4) 0.038(4) 0.001(4) 0.004(3) -0.005(3) C21 0.045(5) 0.041(5) 0.036(5) 0.003(4) 0.005(4) -0.003(4) C22 0.051(5) 0.023(4) 0.041(5) 0.003(4) 0.001(4) -0.002(4) C23 0.066(6) 0.033(5) 0.049(5) 0.000(4) 0.017(5) 0.014(4) C24 0.065(6) 0.031(5) 0.058(6) 0.003(4) 0.030(5) 0.004(4) C25 0.031(4) 0.037(5) 0.058(6) 0.000(4) 0.013(4) 0.002(4) C26 0.031(4) 0.042(6) 0.063(6) 0.002(5) 0.008(4) -0.004(4) C27 0.046(5) 0.057(7) 0.047(6) -0.001(5) 0.003(4) -0.004(5) C28 0.042(5) 0.027(5) 0.041(5) -0.006(4) 0.002(4) -0.004(4) C29 0.032(4) 0.017(4) 0.037(4) 0.004(3) 0.008(3) 0.001(3) C30 0.036(4) 0.016(4) 0.033(4) 0.000(3) 0.012(3) -0.003(3) C31 0.029(4) 0.024(4) 0.031(4) 0.006(3) 0.009(3) 0.007(3) C32 0.042(4) 0.027(5) 0.042(5) 0.001(4) 0.012(4) 0.000(3) C33 0.040(4) 0.031(5) 0.049(5) 0.000(4) 0.012(4) 0.011(4) C34 0.038(5) 0.066(7) 0.066(7) -0.002(5) 0.022(5) 0.006(5) C35 0.040(5) 0.063(7) 0.066(7) -0.007(6) -0.016(5) 0.006(5) C36 0.036(5) 0.062(7) 0.049(5) -0.001(5) -0.005(4) 0.008(4) C37 0.066(6) 0.037(5) 0.045(5) -0.007(4) -0.006(4) 0.017(5) C38 0.080(7) 0.024(5) 0.041(5) -0.008(4) 0.000(5) 0.009(5) C39 0.067(6) 0.028(5) 0.048(6) 0.001(4) -0.009(5) 0.005(5) C40 0.046(5) 0.033(5) 0.042(5) 0.007(4) -0.011(4) -0.009(4) C41 0.039(4) 0.030(5) 0.032(4) 0.005(3) -0.009(4) -0.008(3) C42 0.038(4) 0.029(5) 0.037(5) 0.002(4) -0.003(4) -0.005(3) C43 0.031(4) 0.030(5) 0.027(4) -0.002(3) 0.007(3) 0.001(3) C44 0.029(4) 0.029(5) 0.025(4) -0.003(3) -0.003(3) 0.003(3) C45 0.035(4) 0.032(4) 0.024(4) -0.003(3) 0.007(3) 0.005(3) C46 0.036(4) 0.048(6) 0.041(5) -0.009(4) 0.006(4) 0.005(4) C47 0.034(4) 0.035(5) 0.045(5) -0.001(4) 0.007(4) 0.006(3) C48 0.041(5) 0.031(5) 0.049(5) -0.001(4) 0.009(4) 0.000(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 O4 2.152(6) . ? Mn1 N24 2.183(7) . ? Mn1 N21 2.196(7) . ? Mn1 O1 2.213(5) . ? Mn1 N20 2.227(7) . ? Mn1 N1 2.241(6) . ? Mn2 N3 2.151(6) . ? Mn2 N27 2.175(7) . ? Mn2 O2 2.212(5) . ? Mn2 O1 2.218(5) . ? Mn2 N6 2.268(7) . ? Mn2 N5 2.411(6) . ? Mn3 N13 2.141(6) . ? Mn3 N8 2.151(6) . ? Mn3 O3 2.173(5) . ? Mn3 O2 2.203(5) . ? Mn3 N11 2.310(7) . ? Mn3 N10 2.385(7) . ? Mn4 N30 2.143(8) . ? Mn4 O3 2.167(5) . ? Mn4 N18 2.179(7) . ? Mn4 O4 2.204(5) . ? Mn4 N15 2.274(7) . ? Mn4 N16 2.380(8) . ? O1 C6 1.292(9) . ? O2 C18 1.288(9) . ? O3 C31 1.297(9) . ? O4 C43 1.297(9) . ? N1 C5 1.329(10) . ? N1 C1 1.335(10) . ? N2 C6 1.316(10) . ? N2 N3 1.392(8) . ? N3 C7 1.288(10) . ? N4 C7 1.348(11) . ? N5 C12 1.317(11) . ? N5 C8 1.360(11) . ? N6 C13 1.342(11) . ? N6 C17 1.346(11) . ? N7 C18 1.320(11) . ? N7 N8 1.379(9) . ? N8 C19 1.273(10) . ? N9 C19 1.358(11) . ? N10 C24 1.302(11) . ? N10 C20 1.344(10) . ? N11 C29 1.345(10) . ? N11 C25 1.349(10) . ? N12 C30 1.345(10) . ? N13 C30 1.287(10) . ? N13 N14 1.382(9) . ? N14 C31 1.289(9) . ? N15 C32 1.350(11) . ? N15 C36 1.354(11) . ? N16 C37 1.324(12) . ? N16 C41 1.339(12) . ? N17 C42 1.319(12) . ? N18 C42 1.332(10) . ? N18 N19 1.363(10) . ? N19 C43 1.300(10) . ? N20 C44 1.334(10) . ? N20 C48 1.347(11) . ? N21 N22 1.199(10) . ? N22 N23 1.126(11) . ? N24 N25 1.171(11) . ? N25 N26 1.190(14) . ? N27 N28 1.201(9) . ? N28 N29 1.152(10) . ? N30 N31 1.148(13) . ? N31 N32 1.288(14) . ? C1 C2 1.350(12) . ? C2 C3 1.406(13) . ? C3 C4 1.364(12) . ? C4 C5 1.406(11) . ? C5 C6 1.484(10) . ? C7 C8 1.485(11) . ? C8 C9 1.367(12) . ? C9 C10 1.386(12) . ? C10 C11 1.354(14) . ? C11 C12 1.393(13) . ? C13 C14 1.380(12) . ? C14 C15 1.401(14) . ? C15 C16 1.431(12) . ? C16 C17 1.405(11) . ? C17 C18 1.465(11) . ? C19 C20 1.468(12) . ? C20 C21 1.411(12) . ? C21 C22 1.395(13) . ? C22 C23 1.376(13) . ? C23 C24 1.364(13) . ? C25 C26 1.352(13) . ? C26 C27 1.349(14) . ? C27 C28 1.390(12) . ? C28 C29 1.376(11) . ? C29 C30 1.488(10) . ? C31 C32 1.494(11) . ? C32 C33 1.391(12) . ? C33 C34 1.375(13) . ? C34 C35 1.365(15) . ? C35 C36 1.365(14) . ? C37 C38 1.406(15) . ? C38 C39 1.353(15) . ? C39 C40 1.363(13) . ? C40 C41 1.383(12) . ? C41 C42 1.478(12) . ? C43 C44 1.489(11) . ? C44 C45 1.400(10) . ? C45 C46 1.392(12) . ? C46 C47 1.371(13) . ? C47 C48 1.366(12) . ? 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 O4 Mn1 N24 87.1(3) . . ? O4 Mn1 N21 164.6(2) . . ? N24 Mn1 N21 91.9(3) . . ? O4 Mn1 O1 87.1(2) . . ? N24 Mn1 O1 167.3(3) . . ? N21 Mn1 O1 96.6(2) . . ? O4 Mn1 N20 74.5(2) . . ? N24 Mn1 N20 96.6(3) . . ? N21 Mn1 N20 90.3(2) . . ? O1 Mn1 N20 92.7(2) . . ? O4 Mn1 N1 100.0(2) . . ? N24 Mn1 N1 96.7(3) . . ? N21 Mn1 N1 95.4(2) . . ? O1 Mn1 N1 73.2(2) . . ? N20 Mn1 N1 165.3(2) . . ? N3 Mn2 N27 98.6(3) . . ? N3 Mn2 O2 96.9(2) . . ? N27 Mn2 O2 164.2(2) . . ? N3 Mn2 O1 71.9(2) . . ? N27 Mn2 O1 89.8(2) . . ? O2 Mn2 O1 92.17(19) . . ? N3 Mn2 N6 157.2(2) . . ? N27 Mn2 N6 93.6(3) . . ? O2 Mn2 N6 72.8(2) . . ? O1 Mn2 N6 127.6(2) . . ? N3 Mn2 N5 70.1(2) . . ? N27 Mn2 N5 91.5(2) . . ? O2 Mn2 N5 96.5(2) . . ? O1 Mn2 N5 141.7(2) . . ? N6 Mn2 N5 90.5(2) . . ? N13 Mn3 N8 156.2(3) . . ? N13 Mn3 O3 71.7(2) . . ? N8 Mn3 O3 122.2(2) . . ? N13 Mn3 O2 126.4(2) . . ? N8 Mn3 O2 72.1(2) . . ? O3 Mn3 O2 103.8(2) . . ? N13 Mn3 N11 70.6(2) . . ? N8 Mn3 N11 96.6(2) . . ? O3 Mn3 N11 141.1(2) . . ? O2 Mn3 N11 90.9(2) . . ? N13 Mn3 N10 89.9(2) . . ? N8 Mn3 N10 70.2(2) . . ? O3 Mn3 N10 97.0(2) . . ? O2 Mn3 N10 142.3(2) . . ? N11 Mn3 N10 92.3(2) . . ? N30 Mn4 O3 157.8(3) . . ? N30 Mn4 N18 102.8(3) . . ? O3 Mn4 N18 98.6(2) . . ? N30 Mn4 O4 88.6(3) . . ? O3 Mn4 O4 93.1(2) . . ? N18 Mn4 O4 70.0(2) . . ? N30 Mn4 N15 86.8(3) . . ? O3 Mn4 N15 73.5(2) . . ? N18 Mn4 N15 165.3(3) . . ? O4 Mn4 N15 121.9(3) . . ? N30 Mn4 N16 104.5(3) . . ? O3 Mn4 N16 88.2(2) . . ? N18 Mn4 N16 70.3(3) . . ? O4 Mn4 N16 140.0(2) . . ? N15 Mn4 N16 96.7(3) . . ? C6 O1 Mn1 117.8(4) . . ? C6 O1 Mn2 112.5(4) . . ? Mn1 O1 Mn2 129.5(2) . . ? C18 O2 Mn3 112.5(5) . . ? C18 O2 Mn2 117.8(5) . . ? Mn3 O2 Mn2 128.5(2) . . ? C31 O3 Mn4 119.5(5) . . ? C31 O3 Mn3 112.7(5) . . ? Mn4 O3 Mn3 126.9(2) . . ? C43 O4 Mn1 117.6(5) . . ? C43 O4 Mn4 114.1(5) . . ? Mn1 O4 Mn4 128.2(3) . . ? C5 N1 C1 118.0(7) . . ? C5 N1 Mn1 115.8(5) . . ? C1 N1 Mn1 126.0(5) . . ? C6 N2 N3 109.9(6) . . ? C7 N3 N2 115.6(6) . . ? C7 N3 Mn2 125.1(5) . . ? N2 N3 Mn2 119.3(4) . . ? C12 N5 C8 117.7(7) . . ? C12 N5 Mn2 128.7(6) . . ? C8 N5 Mn2 113.5(5) . . ? C13 N6 C17 119.1(7) . . ? C13 N6 Mn2 125.9(6) . . ? C17 N6 Mn2 115.0(5) . . ? C18 N7 N8 109.7(6) . . ? C19 N8 N7 116.1(7) . . ? C19 N8 Mn3 124.3(5) . . ? N7 N8 Mn3 119.3(5) . . ? C24 N10 C20 119.3(8) . . ? C24 N10 Mn3 126.8(6) . . ? C20 N10 Mn3 113.1(5) . . ? C29 N11 C25 117.1(7) . . ? C29 N11 Mn3 116.3(5) . . ? C25 N11 Mn3 126.5(5) . . ? C30 N13 N14 116.9(6) . . ? C30 N13 Mn3 124.1(5) . . ? N14 N13 Mn3 118.9(5) . . ? C31 N14 N13 109.6(6) . . ? C32 N15 C36 117.0(8) . . ? C32 N15 Mn4 114.6(5) . . ? C36 N15 Mn4 128.3(6) . . ? C37 N16 C41 119.0(8) . . ? C37 N16 Mn4 125.8(7) . . ? C41 N16 Mn4 114.8(6) . . ? C42 N18 N19 115.7(6) . . ? C42 N18 Mn4 122.4(6) . . ? N19 N18 Mn4 120.3(5) . . ? C43 N19 N18 109.5(6) . . ? C44 N20 C48 116.9(7) . . ? C44 N20 Mn1 115.3(5) . . ? C48 N20 Mn1 127.6(5) . . ? N22 N21 Mn1 135.6(6) . . ? N23 N22 N21 173.9(10) . . ? N25 N24 Mn1 143.1(7) . . ? N24 N25 N26 171.4(15) . . ? N28 N27 Mn2 124.8(5) . . ? N29 N28 N27 178.0(9) . . ? N31 N30 Mn4 161.9(10) . . ? N30 N31 N32 179.0(13) . . ? N1 C1 C2 124.0(8) . . ? C1 C2 C3 118.7(8) . . ? C4 C3 C2 118.0(8) . . ? C3 C4 C5 119.4(8) . . ? N1 C5 C4 121.7(7) . . ? N1 C5 C6 116.1(6) . . ? C4 C5 C6 122.2(7) . . ? O1 C6 N2 126.0(7) . . ? O1 C6 C5 116.9(6) . . ? N2 C6 C5 117.0(7) . . ? N3 C7 N4 124.4(7) . . ? N3 C7 C8 116.1(7) . . ? N4 C7 C8 119.5(7) . . ? N5 C8 C9 122.0(8) . . ? N5 C8 C7 115.0(7) . . ? C9 C8 C7 123.0(8) . . ? C8 C9 C10 119.6(9) . . ? C11 C10 C9 118.5(8) . . ? C10 C11 C12 119.1(8) . . ? N5 C12 C11 123.0(9) . . ? N6 C13 C14 124.2(8) . . ? C13 C14 C15 117.6(8) . . ? C14 C15 C16 119.4(7) . . ? C17 C16 C15 117.8(8) . . ? N6 C17 C16 121.9(7) . . ? N6 C17 C18 115.8(7) . . ? C16 C17 C18 122.2(8) . . ? O2 C18 N7 126.3(7) . . ? O2 C18 C17 117.9(7) . . ? N7 C18 C17 115.8(7) . . ? N8 C19 N9 124.5(8) . . ? N8 C19 C20 115.5(7) . . ? N9 C19 C20 120.0(8) . . ? N10 C20 C21 120.5(8) . . ? N10 C20 C19 115.9(7) . . ? C21 C20 C19 123.5(7) . . ? C22 C21 C20 118.8(8) . . ? C23 C22 C21 118.1(8) . . ? C24 C23 C22 119.2(8) . . ? N10 C24 C23 124.1(9) . . ? N11 C25 C26 123.6(8) . . ? C27 C26 C25 118.1(8) . . ? C26 C27 C28 121.4(9) . . ? C29 C28 C27 116.7(8) . . ? N11 C29 C28 123.1(7) . . ? N11 C29 C30 113.7(7) . . ? C28 C29 C30 123.2(7) . . ? N13 C30 N12 124.2(7) . . ? N13 C30 C29 114.8(6) . . ? N12 C30 C29 121.0(7) . . ? N14 C31 O3 126.0(7) . . ? N14 C31 C32 117.1(6) . . ? O3 C31 C32 116.9(7) . . ? N15 C32 C33 121.7(8) . . ? N15 C32 C31 115.2(7) . . ? C33 C32 C31 122.9(8) . . ? C34 C33 C32 119.6(9) . . ? C35 C34 C33 118.8(9) . . ? C34 C35 C36 119.4(8) . . ? N15 C36 C35 123.4(9) . . ? N16 C37 C38 121.4(9) . . ? C39 C38 C37 118.4(9) . . ? C38 C39 C40 120.7(9) . . ? C39 C40 C41 118.2(9) . . ? N16 C41 C40 122.2(8) . . ? N16 C41 C42 116.2(7) . . ? C40 C41 C42 121.6(8) . . ? N17 C42 N18 123.1(8) . . ? N17 C42 C41 122.6(8) . . ? N18 C42 C41 114.3(7) . . ? O4 C43 N19 125.2(7) . . ? O4 C43 C44 117.7(7) . . ? N19 C43 C44 117.0(7) . . ? N20 C44 C45 123.6(7) . . ? N20 C44 C43 114.7(6) . . ? C45 C44 C43 121.6(7) . . ? C46 C45 C44 117.2(8) . . ? C47 C46 C45 119.7(8) . . ? C48 C47 C46 118.8(8) . . ? N20 C48 C47 123.8(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.979 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.141 #===END data_shelxl(2) _database_code_depnum_ccdc_archive 'CCDC 299030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H54 F12 Mn4 N16 O20 S4' _chemical_formula_weight 1859.16 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4058(8) _cell_length_b 14.4617(10) _cell_length_c 22.1102(15) _cell_angle_alpha 72.6290(10) _cell_angle_beta 80.7470(10) _cell_angle_gamma 78.2570(10) _cell_volume 3685.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6935 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 26.32 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5799 _exptl_absorpt_correction_T_max 0.7831 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29338 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 26.41 _reflns_number_total 15043 _reflns_number_gt 12511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _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^)+(0.0659P)^2^+4.1468P] 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 15043 _refine_ls_number_parameters 1014 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Mn1 Mn 0.11838(3) 1.00280(3) 0.301558(19) 0.02843(10) Uani 1 1 d . . . Mn2 Mn -0.15405(3) 1.14917(3) 0.224576(19) 0.02952(10) Uani 1 1 d . . . Mn3 Mn -0.04578(3) 1.40353(3) 0.186241(19) 0.02970(10) Uani 1 1 d . . . Mn4 Mn 0.18826(3) 1.25822(3) 0.301029(19) 0.02919(10) Uani 1 1 d . . . S1 S 0.30541(6) 0.93074(5) 0.40723(4) 0.03820(17) Uani 1 1 d . . . S2 S 0.26620(7) 1.39440(5) 0.45614(4) 0.04097(17) Uani 1 1 d . . . S3 S 0.33887(7) 1.58768(6) 0.12833(4) 0.04608(19) Uani 1 1 d . . . S4 S 0.70980(18) 0.87245(18) 0.13445(13) 0.0544(5) Uiso 0.50 1 d P . . S5 S 0.71360(19) 0.9024(2) 0.11259(13) 0.0589(6) Uiso 0.50 1 d P . . F1 F 0.3541(3) 0.74976(19) 0.4030(2) 0.1217(13) Uani 1 1 d . . . F2 F 0.4529(4) 0.7890(2) 0.4605(2) 0.1506(19) Uani 1 1 d . . . F3 F 0.4823(2) 0.8332(3) 0.3603(2) 0.1216(13) Uani 1 1 d . . . F4 F 0.3881(2) 1.39626(19) 0.54137(11) 0.0723(7) Uani 1 1 d . . . F5 F 0.47667(19) 1.4011(2) 0.45046(13) 0.0775(7) Uani 1 1 d . . . F6 F 0.3682(2) 1.52910(16) 0.46558(13) 0.0741(7) Uani 1 1 d . . . F7 F 0.4723(2) 1.50638(19) 0.21616(13) 0.0801(8) Uani 1 1 d . . . F8 F 0.3489(3) 1.6228(3) 0.23626(14) 0.1015(10) Uani 1 1 d . . . F9 F 0.4884(2) 1.6538(2) 0.16775(15) 0.0855(8) Uani 1 1 d . . . F10 F 0.7382(3) 0.8564(3) 0.01287(15) 0.1188(12) Uani 1 1 d . . . F11 F 0.5844(3) 0.8277(4) 0.06409(18) 0.1385(17) Uani 1 1 d . . . F12 F 0.7203(5) 0.7329(5) 0.0967(3) 0.0984(18) Uiso 0.50 1 d P . . F13 F 0.5940(6) 0.9586(6) 0.0403(4) 0.118(2) Uiso 0.50 1 d P . . O1 O 0.01867(16) 1.07467(14) 0.22227(9) 0.0312(4) Uani 1 1 d . . . O2 O -0.14138(15) 1.28993(13) 0.24236(8) 0.0295(4) Uani 1 1 d . . . O3 O 0.11842(15) 1.31257(13) 0.20978(8) 0.0297(4) Uani 1 1 d . . . O4 O 0.09197(15) 1.14047(13) 0.33000(9) 0.0302(4) Uani 1 1 d . . . O5 O 0.04245(17) 1.52606(15) 0.16564(12) 0.0463(5) Uani 1 1 d . . . O6 O 0.2559(3) 1.38955(18) 0.28423(11) 0.0588(7) Uani 1 1 d . . . O7 O 0.28949(19) 1.19497(15) 0.37997(10) 0.0428(5) Uani 1 1 d . . . O8 O 0.27425(17) 0.96116(16) 0.34311(10) 0.0404(5) Uani 1 1 d . . . O9 O 0.3689(2) 0.99495(17) 0.41888(13) 0.0579(7) Uani 1 1 d . . . O10 O 0.2188(3) 0.9010(2) 0.45526(13) 0.0738(8) Uani 1 1 d . . . O11 O 0.2942(2) 1.28876(16) 0.47176(12) 0.0558(6) Uani 1 1 d . . . O12 O 0.1729(2) 1.4312(2) 0.49377(15) 0.0673(7) Uani 1 1 d . . . O13 O 0.2702(3) 1.44296(19) 0.38902(12) 0.0667(8) Uani 1 1 d . . . O14 O 0.2740(2) 1.5113(2) 0.16217(12) 0.0598(7) Uani 1 1 d . . . O15 O 0.2771(3) 1.6830(2) 0.10749(15) 0.0817(9) Uani 1 1 d . . . O16 O 0.4237(2) 1.5583(2) 0.08203(12) 0.0574(6) Uani 1 1 d . . . O17 O 0.6370(4) 0.8718(3) 0.17613(18) 0.1181(15) Uani 1 1 d . . . O18 O 0.8147(6) 0.8996(6) 0.1134(3) 0.221(4) Uani 1 1 d . . . O19 O 0.6702(6) 0.9985(5) 0.0791(4) 0.0890(19) Uiso 0.50 1 d P . . O20 O 0.7708(9) 0.7736(8) 0.1478(5) 0.136(3) Uiso 0.50 1 d P . . O21 O -0.0122(3) 0.7189(2) 0.1486(2) 0.0901(11) Uani 1 1 d . . . N1 N 0.21968(19) 0.96780(17) 0.21585(11) 0.0340(5) Uani 1 1 d . . . N2 N 0.0012(2) 1.07717(19) 0.11833(11) 0.0366(5) Uani 1 1 d . . . N3 N -0.1020(2) 1.13207(18) 0.12921(11) 0.0341(5) Uani 1 1 d . . . N4 N -0.2954(2) 1.22567(17) 0.16126(11) 0.0359(5) Uani 1 1 d . . . N5 N -0.2071(2) 1.00169(18) 0.27773(12) 0.0380(5) Uani 1 1 d . . . N6 N -0.26334(19) 1.16411(17) 0.30970(11) 0.0329(5) Uani 1 1 d . . . N7 N -0.2908(2) 1.25679(18) 0.31964(11) 0.0343(5) Uani 1 1 d . . . N8 N -0.1773(2) 1.47602(18) 0.24915(12) 0.0366(5) Uani 1 1 d . . . N9 N -0.1590(2) 1.46184(19) 0.10390(12) 0.0393(6) Uani 1 1 d . . . N10 N 0.03141(19) 1.34385(17) 0.10649(11) 0.0311(5) Uani 1 1 d . . . N11 N 0.13314(19) 1.28237(17) 0.11090(11) 0.0325(5) Uani 1 1 d . . . N12 N 0.30979(19) 1.18807(16) 0.23484(11) 0.0319(5) Uani 1 1 d . . . N13 N 0.0325(2) 1.31466(16) 0.35572(11) 0.0335(5) Uani 1 1 d . . . N14 N -0.05814(19) 1.08322(16) 0.39789(11) 0.0321(5) Uani 1 1 d . . . N15 N -0.01399(19) 0.99746(16) 0.37983(11) 0.0304(5) Uani 1 1 d . . . N16 N 0.0840(2) 0.84339(17) 0.34197(12) 0.0354(5) Uani 1 1 d . . . C1 C 0.3214(3) 0.9138(2) 0.21403(16) 0.0414(7) Uani 1 1 d . . . C2 C 0.3720(3) 0.8843(3) 0.16112(19) 0.0519(8) Uani 1 1 d . . . C3 C 0.3174(3) 0.9118(3) 0.10765(19) 0.0576(9) Uani 1 1 d . . . C4 C 0.2134(3) 0.9676(3) 0.10805(16) 0.0487(8) Uani 1 1 d . . . C5 C 0.1670(2) 0.9944(2) 0.16331(14) 0.0340(6) Uani 1 1 d . . . C6 C 0.0545(2) 1.0534(2) 0.16821(13) 0.0317(6) Uani 1 1 d . . . C7 C -0.1666(3) 1.1597(2) 0.08474(13) 0.0364(6) Uani 1 1 d . . . C8 C -0.1401(3) 1.1356(3) 0.02237(16) 0.0513(8) Uani 1 1 d . . . C9 C -0.2740(3) 1.2194(2) 0.10037(14) 0.0367(6) Uani 1 1 d . . . C10 C -0.3469(3) 1.2697(3) 0.05548(15) 0.0487(8) Uani 1 1 d . . . C11 C -0.4428(3) 1.3281(3) 0.07295(18) 0.0542(9) Uani 1 1 d . . . C12 C -0.4653(3) 1.3329(2) 0.13466(17) 0.0477(8) Uani 1 1 d . . . C13 C -0.3898(3) 1.2803(2) 0.17736(16) 0.0426(7) Uani 1 1 d . . . C14 C -0.1694(3) 0.9180(2) 0.26175(17) 0.0470(7) Uani 1 1 d . . . C15 C -0.1916(3) 0.8278(3) 0.3007(2) 0.0566(9) Uani 1 1 d . . . C16 C -0.2581(4) 0.8246(3) 0.3567(2) 0.0608(10) Uani 1 1 d . . . C17 C -0.3001(3) 0.9104(3) 0.37348(17) 0.0521(9) Uani 1 1 d . . . C18 C -0.2730(3) 0.9984(2) 0.33326(14) 0.0388(7) Uani 1 1 d . . . C19 C -0.3086(2) 1.0937(2) 0.34885(13) 0.0365(6) Uani 1 1 d . . . C20 C -0.3865(3) 1.1034(3) 0.40637(16) 0.0526(9) Uani 1 1 d . . . C21 C -0.2245(2) 1.3141(2) 0.28194(12) 0.0290(5) Uani 1 1 d . . . C22 C -0.2496(2) 1.4184(2) 0.28448(13) 0.0314(6) Uani 1 1 d . . . C23 C -0.3436(3) 1.4534(2) 0.31972(15) 0.0420(7) Uani 1 1 d . . . C24 C -0.3651(3) 1.5516(3) 0.31711(17) 0.0490(8) Uani 1 1 d . . . C25 C -0.2929(3) 1.6119(3) 0.28008(19) 0.0528(9) Uani 1 1 d . . . C26 C -0.2001(3) 1.5715(2) 0.24778(18) 0.0490(8) Uani 1 1 d . . . C27 C -0.2548(3) 1.5241(3) 0.10283(16) 0.0504(8) Uani 1 1 d . . . C28 C -0.3137(3) 1.5606(3) 0.04999(19) 0.0559(9) Uani 1 1 d . . . C29 C -0.2713(3) 1.5316(3) -0.00393(18) 0.0555(9) Uani 1 1 d . . . C30 C -0.1737(3) 1.4658(3) -0.00335(16) 0.0468(7) Uani 1 1 d . . . C31 C -0.1189(2) 1.4317(2) 0.05091(13) 0.0352(6) Uani 1 1 d . . . C32 C -0.0126(2) 1.3628(2) 0.05421(13) 0.0333(6) Uani 1 1 d . . . C33 C 0.0386(3) 1.3210(3) 0.00042(15) 0.0459(7) Uani 1 1 d . . . C34 C 0.1689(2) 1.27247(18) 0.16539(12) 0.0283(5) Uani 1 1 d . . . C35 C 0.2786(2) 1.20807(19) 0.17622(13) 0.0300(5) Uani 1 1 d . . . C36 C 0.3442(2) 1.1707(2) 0.12876(14) 0.0379(6) Uani 1 1 d . . . C37 C 0.4437(3) 1.1103(2) 0.14263(16) 0.0435(7) Uani 1 1 d . . . C38 C 0.4757(3) 1.0889(2) 0.20304(17) 0.0434(7) Uani 1 1 d . . . C39 C 0.4071(2) 1.1293(2) 0.24752(15) 0.0390(6) Uani 1 1 d . . . C40 C 0.0044(3) 1.4030(2) 0.36788(16) 0.0426(7) Uani 1 1 d . . . C41 C -0.0877(3) 1.4259(2) 0.40753(16) 0.0458(7) Uani 1 1 d . . . C42 C -0.1541(3) 1.3566(2) 0.43655(15) 0.0451(7) Uani 1 1 d . . . C43 C -0.1272(3) 1.2648(2) 0.42450(14) 0.0374(6) Uani 1 1 d . . . C44 C -0.0336(2) 1.24738(19) 0.38359(12) 0.0307(6) Uani 1 1 d . . . C45 C 0.0025(2) 1.15069(19) 0.36854(12) 0.0283(5) Uani 1 1 d . . . C46 C -0.0407(2) 0.9164(2) 0.41684(13) 0.0319(6) Uani 1 1 d . . . C47 C -0.1137(3) 0.9083(2) 0.47786(15) 0.0459(7) Uani 1 1 d . . . C48 C 0.0130(2) 0.8280(2) 0.39571(14) 0.0337(6) Uani 1 1 d . . . C49 C -0.0056(3) 0.7337(2) 0.43014(15) 0.0436(7) Uani 1 1 d . . . C50 C 0.0499(3) 0.6546(2) 0.40977(18) 0.0522(9) Uani 1 1 d . . . C51 C 0.1228(3) 0.6697(2) 0.3552(2) 0.0543(9) Uani 1 1 d . . . C52 C 0.1357(3) 0.7654(2) 0.32254(17) 0.0467(8) Uani 1 1 d . . . C53 C 0.4038(4) 0.8198(3) 0.4082(3) 0.0744(13) Uani 1 1 d . . . C54 C 0.3815(3) 1.4317(2) 0.47930(16) 0.0466(7) Uani 1 1 d . . . C55 C 0.4159(3) 1.5930(3) 0.19087(19) 0.0576(9) Uani 1 1 d . . . C56 C 0.6635(8) 0.8739(8) 0.0607(4) 0.064(2) Uiso 0.50 1 d P . . C57 C 0.6855(7) 0.8216(7) 0.0700(4) 0.061(2) Uiso 0.50 1 d P . . C58 C 0.0456(4) 0.7684(5) 0.1695(4) 0.119(3) Uani 1 1 d . . . H1 H 0.3596 0.8948 0.2509 0.049 Uiso 1 1 d . . . H2 H 0.4438 0.8457 0.1615 0.061 Uiso 1 1 d . . . H3 H 0.3511 0.8926 0.0706 0.069 Uiso 1 1 d . . . H4 H 0.1743 0.9874 0.0713 0.058 Uiso 1 1 d . . . H5 H -0.0675 1.0968 0.0204 0.083 Uiso 1 1 d . . . H6 H -0.1411 1.1940 -0.0119 0.083 Uiso 1 1 d . . . H7 H -0.1920 1.0987 0.0176 0.083 Uiso 1 1 d . . . H8 H -0.3308 1.2642 0.0130 0.058 Uiso 1 1 d . . . H9 H -0.4930 1.3642 0.0425 0.065 Uiso 1 1 d . . . H10 H -0.5315 1.3717 0.1477 0.058 Uiso 1 1 d . . . H11 H -0.4061 1.2831 0.2204 0.050 Uiso 1 1 d . . . H12 H -0.1257 0.9202 0.2221 0.057 Uiso 1 1 d . . . H13 H -0.1604 0.7690 0.2889 0.068 Uiso 1 1 d . . . H14 H -0.2757 0.7636 0.3837 0.072 Uiso 1 1 d . . . H15 H -0.3469 0.9100 0.4120 0.063 Uiso 1 1 d . . . H16 H -0.4522 1.0791 0.4065 0.083 Uiso 1 1 d . . . H17 H -0.3524 1.0666 0.4441 0.083 Uiso 1 1 d . . . H18 H -0.4050 1.1706 0.4064 0.083 Uiso 1 1 d . . . H19 H -0.3921 1.4102 0.3451 0.051 Uiso 1 1 d . . . H20 H -0.4291 1.5775 0.3407 0.059 Uiso 1 1 d . . . H21 H -0.3067 1.6802 0.2768 0.063 Uiso 1 1 d . . . H22 H -0.1500 1.6135 0.2231 0.059 Uiso 1 1 d . . . H23 H -0.2841 1.5447 0.1402 0.061 Uiso 1 1 d . . . H24 H -0.3819 1.6045 0.0511 0.067 Uiso 1 1 d . . . H25 H -0.3090 1.5556 -0.0412 0.067 Uiso 1 1 d . . . H26 H -0.1437 1.4435 -0.0400 0.056 Uiso 1 1 d . . . H27 H -0.0168 1.3066 -0.0187 0.075 Uiso 1 1 d . . . H28 H 0.0785 1.3669 -0.0308 0.075 Uiso 1 1 d . . . H29 H 0.0892 1.2620 0.0157 0.075 Uiso 1 1 d . . . H30 H 0.3206 1.1868 0.0874 0.045 Uiso 1 1 d . . . H31 H 0.4905 1.0842 0.1110 0.052 Uiso 1 1 d . . . H32 H 0.5440 1.0476 0.2136 0.052 Uiso 1 1 d . . . H33 H 0.4292 1.1148 0.2889 0.046 Uiso 1 1 d . . . H34 H 0.0504 1.4510 0.3483 0.051 Uiso 1 1 d . . . H35 H -0.1058 1.4891 0.4146 0.055 Uiso 1 1 d . . . H36 H -0.2177 1.3711 0.4645 0.054 Uiso 1 1 d . . . H37 H -0.1724 1.2157 0.4437 0.044 Uiso 1 1 d . . . H38 H -0.1525 0.9717 0.4798 0.074 Uiso 1 1 d . . . H39 H -0.0706 0.8814 0.5131 0.074 Uiso 1 1 d . . . H40 H -0.1663 0.8669 0.4812 0.074 Uiso 1 1 d . . . H41 H -0.0561 0.7245 0.4678 0.052 Uiso 1 1 d . . . H42 H 0.0385 0.5900 0.4325 0.063 Uiso 1 1 d . . . H43 H 0.1622 0.6161 0.3401 0.064 Uiso 1 1 d . . . H44 H 0.1846 0.7755 0.2843 0.056 Uiso 1 1 d . . . H45 H 0.0242 1.5796 0.1612 0.076 Uiso 1 1 d . . . H46 H 0.1003 1.5210 0.1643 0.076 Uiso 1 1 d . . . H47 H 0.2607 1.4233 0.2552 0.076 Uiso 1 1 d . . . H48 H 0.2759 1.4108 0.3124 0.076 Uiso 1 1 d . . . H49 H 0.3030 1.2227 0.4034 0.076 Uiso 1 1 d . . . H50 H 0.3146 1.1308 0.3986 0.076 Uiso 1 1 d . . . H51 H 0.0397 0.8361 0.1432 0.139 Uiso 1 1 d . . . H52 H 0.0182 0.7704 0.2121 0.139 Uiso 1 1 d . . . H53 H 0.1216 0.7403 0.1681 0.139 Uiso 1 1 d . . . H54 H -0.0835 0.7608 0.1379 0.076 Uiso 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 0.0316(2) 0.0239(2) 0.0296(2) -0.00748(16) -0.00112(16) -0.00556(15) Mn2 0.0343(2) 0.0296(2) 0.0255(2) -0.00819(16) -0.00232(16) -0.00717(16) Mn3 0.0299(2) 0.0291(2) 0.0290(2) -0.00826(16) 0.00255(16) -0.00621(16) Mn4 0.0369(2) 0.0254(2) 0.0267(2) -0.00779(16) -0.00184(16) -0.00855(16) S1 0.0446(4) 0.0316(4) 0.0369(4) -0.0065(3) -0.0091(3) -0.0037(3) S2 0.0541(5) 0.0326(4) 0.0414(4) -0.0147(3) -0.0087(3) -0.0094(3) S3 0.0390(4) 0.0444(4) 0.0436(4) 0.0058(3) -0.0047(3) -0.0082(3) F1 0.143(3) 0.0433(14) 0.194(4) -0.0468(19) -0.064(3) 0.0055(16) F2 0.214(4) 0.084(2) 0.156(3) -0.040(2) -0.136(3) 0.072(2) F3 0.0534(16) 0.154(3) 0.172(4) -0.095(3) -0.015(2) 0.0286(18) F4 0.0891(17) 0.0890(17) 0.0493(12) -0.0226(12) -0.0228(12) -0.0209(14) F5 0.0504(13) 0.0898(18) 0.0877(18) -0.0273(14) 0.0100(12) -0.0106(12) F6 0.0860(17) 0.0452(12) 0.1016(19) -0.0235(12) -0.0129(14) -0.0273(11) F7 0.0932(18) 0.0706(16) 0.0822(17) -0.0086(13) -0.0532(15) -0.0109(14) F8 0.111(2) 0.134(3) 0.0737(18) -0.0584(18) 0.0126(16) -0.024(2) F9 0.0877(18) 0.0778(17) 0.106(2) -0.0299(15) -0.0055(15) -0.0437(15) F10 0.096(2) 0.168(3) 0.0674(18) -0.026(2) 0.0249(16) -0.002(2) F11 0.099(2) 0.252(5) 0.117(3) -0.114(3) 0.016(2) -0.073(3) O1 0.0370(10) 0.0314(10) 0.0279(9) -0.0127(8) -0.0024(8) -0.0055(8) O2 0.0304(9) 0.0304(9) 0.0277(9) -0.0096(7) 0.0028(7) -0.0074(7) O3 0.0331(9) 0.0288(9) 0.0275(9) -0.0103(7) -0.0003(7) -0.0040(7) O4 0.0348(10) 0.0260(9) 0.0311(9) -0.0106(7) 0.0020(8) -0.0079(7) O5 0.0340(11) 0.0314(11) 0.0715(15) -0.0129(10) 0.0000(10) -0.0075(9) O6 0.106(2) 0.0461(13) 0.0346(12) -0.0034(10) -0.0112(12) -0.0454(14) O7 0.0610(14) 0.0328(11) 0.0385(11) -0.0102(9) -0.0179(10) -0.0058(10) O8 0.0354(11) 0.0462(12) 0.0379(11) -0.0090(9) -0.0068(9) -0.0045(9) O9 0.0732(17) 0.0371(12) 0.0714(17) -0.0134(11) -0.0381(14) -0.0054(11) O10 0.082(2) 0.085(2) 0.0458(15) -0.0079(14) 0.0092(14) -0.0240(17) O11 0.0915(19) 0.0333(12) 0.0491(14) -0.0156(10) -0.0124(13) -0.0144(12) O12 0.0513(15) 0.0690(18) 0.088(2) -0.0367(16) 0.0066(14) -0.0120(13) O13 0.114(2) 0.0466(14) 0.0444(14) -0.0134(11) -0.0305(15) -0.0056(14) O14 0.0490(14) 0.0755(18) 0.0453(13) 0.0120(12) -0.0092(11) -0.0285(13) O15 0.084(2) 0.0617(18) 0.073(2) 0.0019(15) -0.0107(16) 0.0180(16) O16 0.0519(14) 0.0669(16) 0.0481(14) -0.0110(12) 0.0018(11) -0.0107(12) O17 0.171(4) 0.131(4) 0.072(2) -0.054(2) -0.039(3) -0.011(3) O18 0.220(7) 0.350(10) 0.144(5) -0.017(6) -0.045(5) -0.218(7) O21 0.077(2) 0.0410(15) 0.159(4) -0.0240(18) -0.041(2) -0.0068(14) N1 0.0354(12) 0.0293(12) 0.0379(13) -0.0119(10) 0.0023(10) -0.0074(10) N2 0.0400(13) 0.0436(14) 0.0302(12) -0.0148(10) -0.0003(10) -0.0117(11) N3 0.0379(13) 0.0370(13) 0.0298(12) -0.0097(10) -0.0009(10) -0.0130(10) N4 0.0433(14) 0.0329(12) 0.0343(12) -0.0078(10) -0.0099(10) -0.0102(10) N5 0.0415(13) 0.0371(13) 0.0379(13) -0.0071(10) -0.0076(11) -0.0141(11) N6 0.0341(12) 0.0374(13) 0.0291(11) -0.0080(10) -0.0015(9) -0.0133(10) N7 0.0359(12) 0.0397(13) 0.0297(12) -0.0126(10) 0.0014(9) -0.0111(10) N8 0.0371(13) 0.0352(13) 0.0406(13) -0.0173(11) 0.0037(10) -0.0089(10) N9 0.0337(12) 0.0442(14) 0.0337(13) -0.0024(11) 0.0010(10) -0.0087(11) N10 0.0312(11) 0.0326(12) 0.0298(11) -0.0090(9) -0.0014(9) -0.0070(9) N11 0.0334(12) 0.0346(12) 0.0294(11) -0.0109(10) -0.0012(9) -0.0039(10) N12 0.0322(12) 0.0291(11) 0.0333(12) -0.0066(9) -0.0015(9) -0.0072(9) N13 0.0434(13) 0.0279(11) 0.0314(12) -0.0116(9) -0.0043(10) -0.0055(10) N14 0.0362(12) 0.0274(11) 0.0316(12) -0.0082(9) -0.0003(9) -0.0055(9) N15 0.0338(12) 0.0262(11) 0.0316(11) -0.0067(9) -0.0044(9) -0.0070(9) N16 0.0365(12) 0.0264(11) 0.0435(13) -0.0091(10) -0.0038(10) -0.0068(9) C1 0.0377(16) 0.0350(15) 0.0500(18) -0.0129(13) 0.0014(13) -0.0053(12) C2 0.0428(18) 0.0461(19) 0.069(2) -0.0290(17) 0.0080(16) -0.0037(14) C3 0.053(2) 0.071(2) 0.061(2) -0.045(2) 0.0108(17) -0.0107(18) C4 0.0475(18) 0.064(2) 0.0460(18) -0.0340(17) 0.0036(14) -0.0126(16) C5 0.0381(15) 0.0333(14) 0.0360(15) -0.0157(12) 0.0017(12) -0.0131(12) C6 0.0379(14) 0.0292(13) 0.0325(14) -0.0124(11) 0.0012(11) -0.0136(11) C7 0.0470(16) 0.0371(15) 0.0283(14) -0.0046(11) -0.0062(12) -0.0190(13) C8 0.061(2) 0.065(2) 0.0336(16) -0.0165(15) -0.0079(15) -0.0151(17) C9 0.0450(16) 0.0328(14) 0.0333(14) -0.0001(11) -0.0091(12) -0.0179(12) C10 0.055(2) 0.055(2) 0.0334(16) 0.0020(14) -0.0124(14) -0.0185(16) C11 0.052(2) 0.052(2) 0.051(2) 0.0046(16) -0.0190(16) -0.0077(16) C12 0.0469(18) 0.0352(16) 0.059(2) -0.0068(14) -0.0135(15) -0.0044(13) C13 0.0476(18) 0.0379(16) 0.0452(17) -0.0128(13) -0.0096(14) -0.0078(13) C14 0.0523(19) 0.0390(17) 0.0535(19) -0.0127(14) -0.0083(15) -0.0140(14) C15 0.063(2) 0.0370(17) 0.075(3) -0.0138(17) -0.017(2) -0.0167(16) C16 0.078(3) 0.0415(19) 0.064(2) 0.0036(17) -0.018(2) -0.0326(18) C17 0.061(2) 0.052(2) 0.0450(18) -0.0016(15) -0.0077(16) -0.0314(17) C18 0.0414(16) 0.0426(16) 0.0360(15) -0.0044(13) -0.0099(12) -0.0202(13) C19 0.0380(15) 0.0440(16) 0.0296(14) -0.0057(12) -0.0062(11) -0.0164(13) C20 0.057(2) 0.062(2) 0.0381(17) -0.0097(15) 0.0115(15) -0.0289(17) C21 0.0287(13) 0.0356(14) 0.0249(12) -0.0114(11) -0.0020(10) -0.0068(11) C22 0.0326(14) 0.0356(14) 0.0285(13) -0.0123(11) -0.0020(11) -0.0068(11) C23 0.0385(16) 0.0502(18) 0.0409(16) -0.0218(14) 0.0050(13) -0.0089(13) C24 0.0414(17) 0.056(2) 0.056(2) -0.0335(17) 0.0025(15) -0.0012(15) C25 0.054(2) 0.0413(18) 0.070(2) -0.0312(17) -0.0006(17) -0.0042(15) C26 0.0474(18) 0.0377(17) 0.066(2) -0.0225(16) 0.0050(16) -0.0122(14) C27 0.0366(16) 0.058(2) 0.0448(18) -0.0019(15) 0.0002(14) -0.0026(15) C28 0.0343(17) 0.067(2) 0.058(2) -0.0041(18) -0.0085(15) -0.0058(16) C29 0.0438(18) 0.066(2) 0.055(2) -0.0070(18) -0.0201(16) -0.0088(17) C30 0.0464(18) 0.0532(19) 0.0435(17) -0.0096(15) -0.0125(14) -0.0137(15) C31 0.0352(14) 0.0371(15) 0.0339(14) -0.0033(12) -0.0038(11) -0.0167(12) C32 0.0389(15) 0.0328(14) 0.0303(14) -0.0067(11) -0.0026(11) -0.0146(12) C33 0.0562(19) 0.0524(19) 0.0323(15) -0.0144(14) -0.0068(14) -0.0103(15) C34 0.0323(13) 0.0238(12) 0.0288(13) -0.0077(10) 0.0025(10) -0.0084(10) C35 0.0329(14) 0.0252(12) 0.0330(14) -0.0095(11) 0.0015(11) -0.0087(10) C36 0.0396(15) 0.0375(15) 0.0372(15) -0.0158(12) 0.0053(12) -0.0069(12) C37 0.0397(16) 0.0380(16) 0.0535(19) -0.0207(14) 0.0091(14) -0.0065(13) C38 0.0332(15) 0.0338(15) 0.059(2) -0.0107(14) -0.0017(14) -0.0012(12) C39 0.0343(15) 0.0365(15) 0.0434(16) -0.0060(13) -0.0051(12) -0.0060(12) C40 0.0524(18) 0.0332(15) 0.0476(18) -0.0189(13) -0.0076(14) -0.0060(13) C41 0.059(2) 0.0365(16) 0.0479(18) -0.0244(14) -0.0090(15) 0.0014(14) C42 0.0490(18) 0.0481(18) 0.0380(16) -0.0209(14) -0.0007(13) 0.0031(14) C43 0.0422(16) 0.0380(15) 0.0306(14) -0.0111(12) 0.0004(12) -0.0040(12) C44 0.0394(15) 0.0292(13) 0.0245(12) -0.0087(10) -0.0064(11) -0.0033(11) C45 0.0338(13) 0.0268(13) 0.0246(12) -0.0068(10) -0.0059(10) -0.0038(10) C46 0.0326(14) 0.0325(14) 0.0316(14) -0.0054(11) -0.0077(11) -0.0093(11) C47 0.057(2) 0.0434(17) 0.0348(16) -0.0045(13) 0.0023(14) -0.0182(15) C48 0.0352(14) 0.0296(14) 0.0368(14) -0.0028(11) -0.0104(11) -0.0109(11) C49 0.0522(18) 0.0341(15) 0.0440(17) -0.0023(13) -0.0092(14) -0.0157(14) C50 0.066(2) 0.0276(15) 0.062(2) -0.0008(14) -0.0163(18) -0.0161(15) C51 0.057(2) 0.0276(15) 0.078(3) -0.0152(16) -0.0045(18) -0.0060(14) C52 0.0489(18) 0.0310(15) 0.059(2) -0.0137(14) 0.0023(15) -0.0082(13) C53 0.082(3) 0.049(2) 0.099(3) -0.029(2) -0.047(3) 0.017(2) C54 0.0523(19) 0.0435(18) 0.0467(18) -0.0167(15) -0.0002(15) -0.0114(15) C55 0.063(2) 0.057(2) 0.056(2) -0.0179(18) -0.0027(18) -0.0190(18) C58 0.061(3) 0.153(6) 0.185(7) -0.125(6) 0.010(4) -0.015(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 O8 2.171(2) . ? Mn1 N15 2.181(2) . ? Mn1 O1 2.1840(19) . ? Mn1 O4 2.2095(18) . ? Mn1 N1 2.230(2) . ? Mn1 N16 2.312(2) . ? Mn2 N6 2.175(2) . ? Mn2 N3 2.176(2) . ? Mn2 O1 2.1938(19) . ? Mn2 O2 2.2250(18) . ? Mn2 N5 2.278(2) . ? Mn2 N4 2.309(2) . ? Mn3 O5 2.166(2) . ? Mn3 O2 2.1791(18) . ? Mn3 N10 2.191(2) . ? Mn3 O3 2.2342(19) . ? Mn3 N8 2.267(2) . ? Mn3 N9 2.328(3) . ? Mn4 O6 2.139(2) . ? Mn4 O4 2.1605(18) . ? Mn4 O7 2.178(2) . ? Mn4 O3 2.1857(19) . ? Mn4 N12 2.236(2) . ? Mn4 N13 2.249(2) . ? S1 O10 1.420(3) . ? S1 O9 1.433(2) . ? S1 O8 1.445(2) . ? S1 C53 1.804(4) . ? S2 O12 1.421(3) . ? S2 O13 1.437(3) . ? S2 O11 1.443(2) . ? S2 C54 1.820(4) . ? S3 O15 1.416(3) . ? S3 O16 1.438(3) . ? S3 O14 1.450(2) . ? S3 C55 1.830(4) . ? S4 S5 0.547(3) . ? S4 O17 1.182(5) . ? S4 O18 1.403(6) . ? S4 O20 1.443(11) . ? S4 C56 1.808(9) . ? S4 C57 1.876(9) . ? S4 O19 1.887(8) . ? S5 O18 1.250(6) . ? S5 O19 1.407(8) . ? S5 O17 1.563(5) . ? S5 C56 1.579(9) . ? S5 C57 1.818(9) . ? S5 O20 1.831(11) . ? F1 C53 1.330(5) . ? F2 C53 1.309(5) . ? F3 C53 1.314(6) . ? F4 C54 1.324(4) . ? F5 C54 1.308(4) . ? F6 C54 1.331(4) . ? F7 C55 1.312(5) . ? F8 C55 1.315(5) . ? F9 C55 1.322(4) . ? F10 C57 1.328(9) . ? F10 C56 1.338(9) . ? F11 C57 1.264(9) . ? F11 C56 1.275(10) . ? F12 C57 1.259(11) . ? F12 O20 1.670(12) . ? F13 C56 1.346(12) . ? F13 O19 1.655(10) . ? O1 C6 1.309(3) . ? O2 C21 1.303(3) . ? O3 C34 1.299(3) . ? O4 C45 1.298(3) . ? O21 C58 1.323(6) . ? N1 C5 1.341(4) . ? N1 C1 1.344(4) . ? N2 C6 1.299(4) . ? N2 N3 1.388(3) . ? N3 C7 1.288(4) . ? N4 C13 1.335(4) . ? N4 C9 1.356(4) . ? N5 C14 1.334(4) . ? N5 C18 1.355(4) . ? N6 C19 1.285(4) . ? N6 N7 1.388(3) . ? N7 C21 1.305(3) . ? N8 C22 1.342(4) . ? N8 C26 1.344(4) . ? N9 C27 1.336(4) . ? N9 C31 1.356(4) . ? N10 C32 1.289(4) . ? N10 N11 1.387(3) . ? N11 C34 1.309(3) . ? N12 C35 1.344(4) . ? N12 C39 1.344(4) . ? N13 C44 1.342(4) . ? N13 C40 1.348(4) . ? N14 C45 1.305(3) . ? N14 N15 1.395(3) . ? N15 C46 1.285(3) . ? N16 C52 1.333(4) . ? N16 C48 1.350(4) . ? C1 C2 1.377(5) . ? C2 C3 1.372(6) . ? C3 C4 1.376(5) . ? C4 C5 1.393(4) . ? C5 C6 1.486(4) . ? C7 C9 1.483(4) . ? C7 C8 1.492(4) . ? C9 C10 1.386(4) . ? C10 C11 1.384(5) . ? C11 C12 1.368(5) . ? C12 C13 1.382(5) . ? C14 C15 1.386(5) . ? C15 C16 1.366(6) . ? C16 C17 1.378(6) . ? C17 C18 1.388(4) . ? C18 C19 1.483(4) . ? C19 C20 1.492(4) . ? C21 C22 1.493(4) . ? C22 C23 1.387(4) . ? C23 C24 1.377(5) . ? C24 C25 1.374(5) . ? C25 C26 1.374(5) . ? C27 C28 1.388(5) . ? C28 C29 1.371(6) . ? C29 C30 1.378(5) . ? C30 C31 1.385(4) . ? C31 C32 1.480(4) . ? C32 C33 1.488(4) . ? C34 C35 1.493(4) . ? C35 C36 1.393(4) . ? C36 C37 1.380(5) . ? C37 C38 1.382(5) . ? C38 C39 1.380(4) . ? C40 C41 1.372(5) . ? C41 C42 1.370(5) . ? C42 C43 1.394(4) . ? C43 C44 1.383(4) . ? C44 C45 1.497(4) . ? C46 C48 1.486(4) . ? C46 C47 1.486(4) . ? C48 C49 1.394(4) . ? C49 C50 1.368(5) . ? C50 C51 1.376(5) . ? C51 C52 1.384(5) . ? C56 C57 0.728(10) . ? 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 O8 Mn1 N15 107.26(8) . . ? O8 Mn1 O1 152.23(8) . . ? N15 Mn1 O1 98.63(8) . . ? O8 Mn1 O4 88.22(8) . . ? N15 Mn1 O4 71.00(7) . . ? O1 Mn1 O4 90.92(7) . . ? O8 Mn1 N1 84.80(9) . . ? N15 Mn1 N1 158.41(8) . . ? O1 Mn1 N1 74.10(8) . . ? O4 Mn1 N1 128.42(8) . . ? O8 Mn1 N16 90.57(8) . . ? N15 Mn1 N16 71.06(8) . . ? O1 Mn1 N16 107.50(8) . . ? O4 Mn1 N16 139.77(8) . . ? N1 Mn1 N16 91.43(9) . . ? N6 Mn2 N3 159.12(9) . . ? N6 Mn2 O1 125.81(8) . . ? N3 Mn2 O1 72.20(8) . . ? N6 Mn2 O2 71.41(8) . . ? N3 Mn2 O2 118.29(8) . . ? O1 Mn2 O2 102.38(7) . . ? N6 Mn2 N5 70.86(9) . . ? N3 Mn2 N5 101.90(9) . . ? O1 Mn2 N5 88.77(8) . . ? O2 Mn2 N5 139.81(8) . . ? N6 Mn2 N4 91.09(9) . . ? N3 Mn2 N4 71.00(9) . . ? O1 Mn2 N4 142.98(8) . . ? O2 Mn2 N4 91.47(8) . . ? N5 Mn2 N4 102.55(9) . . ? O5 Mn3 O2 158.22(8) . . ? O5 Mn3 N10 98.74(9) . . ? O2 Mn3 N10 101.41(8) . . ? O5 Mn3 O3 84.07(7) . . ? O2 Mn3 O3 94.81(7) . . ? N10 Mn3 O3 70.73(8) . . ? O5 Mn3 N8 89.52(9) . . ? O2 Mn3 N8 74.19(8) . . ? N10 Mn3 N8 159.82(9) . . ? O3 Mn3 N8 128.76(8) . . ? O5 Mn3 N9 99.45(9) . . ? O2 Mn3 N9 94.98(8) . . ? N10 Mn3 N9 70.63(9) . . ? O3 Mn3 N9 141.29(8) . . ? N8 Mn3 N9 89.93(9) . . ? O6 Mn4 O4 167.78(9) . . ? O6 Mn4 O7 86.94(9) . . ? O4 Mn4 O7 93.73(8) . . ? O6 Mn4 O3 91.68(8) . . ? O4 Mn4 O3 90.15(7) . . ? O7 Mn4 O3 167.98(8) . . ? O6 Mn4 N12 98.58(10) . . ? O4 Mn4 N12 93.56(8) . . ? O7 Mn4 N12 93.23(9) . . ? O3 Mn4 N12 75.16(8) . . ? O6 Mn4 N13 93.03(10) . . ? O4 Mn4 N13 74.79(8) . . ? O7 Mn4 N13 98.19(9) . . ? O3 Mn4 N13 93.80(8) . . ? N12 Mn4 N13 164.13(9) . . ? O10 S1 O9 116.01(19) . . ? O10 S1 O8 114.20(16) . . ? O9 S1 O8 113.28(14) . . ? O10 S1 C53 105.0(2) . . ? O9 S1 C53 103.72(19) . . ? O8 S1 C53 102.63(18) . . ? O12 S2 O13 114.79(19) . . ? O12 S2 O11 115.20(17) . . ? O13 S2 O11 114.65(15) . . ? O12 S2 C54 103.46(16) . . ? O13 S2 C54 102.59(17) . . ? O11 S2 C54 103.82(16) . . ? O15 S3 O16 115.43(17) . . ? O15 S3 O14 115.28(19) . . ? O16 S3 O14 112.81(17) . . ? O15 S3 C55 105.5(2) . . ? O16 S3 C55 103.89(17) . . ? O14 S3 C55 101.95(16) . . ? S5 S4 O17 125.3(5) . . ? S5 S4 O18 62.6(5) . . ? O17 S4 O18 142.4(4) . . ? S5 S4 O20 127.9(6) . . ? O17 S4 O20 105.7(5) . . ? O18 S4 O20 84.1(6) . . ? S5 S4 C56 57.1(5) . . ? O17 S4 C56 112.7(4) . . ? O18 S4 C56 101.7(4) . . ? O20 S4 C56 96.7(5) . . ? S5 S4 C57 75.5(5) . . ? O17 S4 C57 114.9(4) . . ? O18 S4 C57 102.7(4) . . ? O20 S4 C57 74.3(5) . . ? C56 S4 C57 22.7(3) . . ? S5 S4 O19 24.4(4) . . ? O17 S4 O19 101.0(3) . . ? O18 S4 O19 79.7(4) . . ? O20 S4 O19 152.0(5) . . ? C56 S4 O19 64.9(4) . . ? C57 S4 O19 87.1(4) . . ? S4 S5 O18 94.5(5) . . ? S4 S5 O19 146.3(6) . . ? O18 S5 O19 107.2(5) . . ? S4 S5 O17 38.1(4) . . ? O18 S5 O17 120.5(4) . . ? O19 S5 O17 108.4(4) . . ? S4 S5 C56 106.0(6) . . ? O18 S5 C56 124.1(5) . . ? O19 S5 C56 83.0(5) . . ? O17 S5 C56 106.2(4) . . ? S4 S5 C57 87.5(5) . . ? O18 S5 C57 113.0(5) . . ? O19 S5 C57 106.3(5) . . ? O17 S5 C57 100.5(3) . . ? C56 S5 C57 23.4(4) . . ? S4 S5 O20 38.4(5) . . ? O18 S5 O20 73.8(5) . . ? O19 S5 O20 173.5(5) . . ? O17 S5 O20 75.9(4) . . ? C56 S5 O20 91.1(5) . . ? C57 S5 O20 67.7(5) . . ? C57 F10 C56 31.7(5) . . ? C57 F11 C56 33.3(5) . . ? C57 F12 O20 86.7(7) . . ? C56 F13 O19 82.0(6) . . ? C6 O1 Mn1 117.04(17) . . ? C6 O1 Mn2 112.24(17) . . ? Mn1 O1 Mn2 128.80(9) . . ? C21 O2 Mn3 117.76(16) . . ? C21 O2 Mn2 110.34(16) . . ? Mn3 O2 Mn2 129.28(8) . . ? C34 O3 Mn4 115.81(16) . . ? C34 O3 Mn3 113.29(16) . . ? Mn4 O3 Mn3 129.55(8) . . ? C45 O4 Mn4 117.29(16) . . ? C45 O4 Mn1 112.80(15) . . ? Mn4 O4 Mn1 129.87(9) . . ? S1 O8 Mn1 134.97(13) . . ? S4 O17 S5 16.59(16) . . ? S5 O18 S4 22.89(16) . . ? S5 O19 F13 92.4(5) . . ? S5 O19 S4 9.25(16) . . ? F13 O19 S4 93.1(4) . . ? S4 O20 F12 99.3(7) . . ? S4 O20 S5 13.64(18) . . ? F12 O20 S5 93.9(6) . . ? C5 N1 C1 117.8(3) . . ? C5 N1 Mn1 115.18(18) . . ? C1 N1 Mn1 126.5(2) . . ? C6 N2 N3 110.2(2) . . ? C7 N3 N2 118.0(2) . . ? C7 N3 Mn2 123.4(2) . . ? N2 N3 Mn2 118.05(17) . . ? C13 N4 C9 118.2(3) . . ? C13 N4 Mn2 126.5(2) . . ? C9 N4 Mn2 115.0(2) . . ? C14 N5 C18 118.5(3) . . ? C14 N5 Mn2 125.0(2) . . ? C18 N5 Mn2 116.1(2) . . ? C19 N6 N7 118.6(2) . . ? C19 N6 Mn2 123.7(2) . . ? N7 N6 Mn2 117.56(16) . . ? C21 N7 N6 109.7(2) . . ? C22 N8 C26 117.3(3) . . ? C22 N8 Mn3 114.37(18) . . ? C26 N8 Mn3 127.6(2) . . ? C27 N9 C31 117.9(3) . . ? C27 N9 Mn3 126.9(2) . . ? C31 N9 Mn3 115.08(19) . . ? C32 N10 N11 116.7(2) . . ? C32 N10 Mn3 123.5(2) . . ? N11 N10 Mn3 119.77(16) . . ? C34 N11 N10 109.8(2) . . ? C35 N12 C39 118.2(2) . . ? C35 N12 Mn4 114.19(18) . . ? C39 N12 Mn4 127.6(2) . . ? C44 N13 C40 117.9(3) . . ? C44 N13 Mn4 114.03(17) . . ? C40 N13 Mn4 127.7(2) . . ? C45 N14 N15 109.3(2) . . ? C46 N15 N14 117.5(2) . . ? C46 N15 Mn1 122.73(19) . . ? N14 N15 Mn1 118.73(16) . . ? C52 N16 C48 117.8(3) . . ? C52 N16 Mn1 127.1(2) . . ? C48 N16 Mn1 114.60(18) . . ? N1 C1 C2 122.7(3) . . ? C3 C2 C1 119.1(3) . . ? C2 C3 C4 119.5(3) . . ? C3 C4 C5 118.4(3) . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C6 115.5(2) . . ? C4 C5 C6 121.9(3) . . ? N2 C6 O1 126.8(3) . . ? N2 C6 C5 116.2(2) . . ? O1 C6 C5 117.1(2) . . ? N3 C7 C9 114.0(3) . . ? N3 C7 C8 124.9(3) . . ? C9 C7 C8 121.0(3) . . ? N4 C9 C10 121.2(3) . . ? N4 C9 C7 115.9(2) . . ? C10 C9 C7 122.8(3) . . ? C11 C10 C9 119.4(3) . . ? C12 C11 C10 119.3(3) . . ? C11 C12 C13 118.6(3) . . ? N4 C13 C12 123.3(3) . . ? N5 C14 C15 122.6(3) . . ? C16 C15 C14 118.8(3) . . ? C15 C16 C17 119.5(3) . . ? C16 C17 C18 119.1(3) . . ? N5 C18 C17 121.4(3) . . ? N5 C18 C19 115.4(2) . . ? C17 C18 C19 123.1(3) . . ? N6 C19 C18 113.6(3) . . ? N6 C19 C20 124.4(3) . . ? C18 C19 C20 121.9(3) . . ? O2 C21 N7 126.8(2) . . ? O2 C21 C22 117.8(2) . . ? N7 C21 C22 115.4(2) . . ? N8 C22 C23 122.7(3) . . ? N8 C22 C21 115.6(2) . . ? C23 C22 C21 121.7(3) . . ? C24 C23 C22 118.8(3) . . ? C25 C24 C23 119.2(3) . . ? C24 C25 C26 118.7(3) . . ? N8 C26 C25 123.4(3) . . ? N9 C27 C28 123.3(3) . . ? C29 C28 C27 118.4(3) . . ? C28 C29 C30 119.1(3) . . ? C29 C30 C31 119.7(3) . . ? N9 C31 C30 121.4(3) . . ? N9 C31 C32 116.1(2) . . ? C30 C31 C32 122.5(3) . . ? N10 C32 C31 114.6(3) . . ? N10 C32 C33 123.7(3) . . ? C31 C32 C33 121.7(3) . . ? O3 C34 N11 126.3(2) . . ? O3 C34 C35 118.3(2) . . ? N11 C34 C35 115.4(2) . . ? N12 C35 C36 122.0(3) . . ? N12 C35 C34 115.7(2) . . ? C36 C35 C34 122.2(3) . . ? C37 C36 C35 119.0(3) . . ? C36 C37 C38 119.2(3) . . ? C39 C38 C37 118.8(3) . . ? N12 C39 C38 122.8(3) . . ? N13 C40 C41 122.7(3) . . ? C42 C41 C40 119.2(3) . . ? C41 C42 C43 119.3(3) . . ? C44 C43 C42 118.2(3) . . ? N13 C44 C43 122.7(3) . . ? N13 C44 C45 115.4(2) . . ? C43 C44 C45 122.0(3) . . ? O4 C45 N14 126.3(2) . . ? O4 C45 C44 117.8(2) . . ? N14 C45 C44 115.8(2) . . ? N15 C46 C48 114.3(2) . . ? N15 C46 C47 124.2(3) . . ? C48 C46 C47 121.4(2) . . ? N16 C48 C49 121.4(3) . . ? N16 C48 C46 116.2(2) . . ? C49 C48 C46 122.3(3) . . ? C50 C49 C48 119.7(3) . . ? C49 C50 C51 119.3(3) . . ? C50 C51 C52 118.1(3) . . ? N16 C52 C51 123.7(3) . . ? F2 C53 F3 106.8(5) . . ? F2 C53 F1 109.7(4) . . ? F3 C53 F1 106.6(4) . . ? F2 C53 S1 111.0(3) . . ? F3 C53 S1 112.0(3) . . ? F1 C53 S1 110.6(3) . . ? F5 C54 F4 107.3(3) . . ? F5 C54 F6 108.0(3) . . ? F4 C54 F6 107.4(3) . . ? F5 C54 S2 112.4(2) . . ? F4 C54 S2 111.1(2) . . ? F6 C54 S2 110.4(2) . . ? F7 C55 F8 108.7(4) . . ? F7 C55 F9 106.8(3) . . ? F8 C55 F9 108.1(3) . . ? F7 C55 S3 110.7(3) . . ? F8 C55 S3 111.1(3) . . ? F9 C55 S3 111.3(3) . . ? C57 C56 F11 72.5(11) . . ? C57 C56 F10 73.4(11) . . ? F11 C56 F10 107.5(7) . . ? C57 C56 F13 160.8(15) . . ? F11 C56 F13 88.6(7) . . ? F10 C56 F13 110.5(8) . . ? C57 C56 S5 97.1(12) . . ? F11 C56 S5 132.5(7) . . ? F10 C56 S5 113.6(6) . . ? F13 C56 S5 98.2(7) . . ? C57 C56 S4 83.9(11) . . ? F11 C56 S4 117.8(6) . . ? F10 C56 S4 119.5(6) . . ? F13 C56 S4 108.6(7) . . ? S5 C56 S4 16.92(14) . . ? C56 C57 F12 169.0(15) . . ? C56 C57 F11 74.2(11) . . ? F12 C57 F11 106.8(8) . . ? C56 C57 F10 74.9(11) . . ? F12 C57 F10 114.4(8) . . ? F11 C57 F10 108.8(7) . . ? C56 C57 S5 59.5(10) . . ? F12 C57 S5 111.4(7) . . ? F11 C57 S5 114.8(6) . . ? F10 C57 S5 100.8(6) . . ? C56 C57 S4 73.4(11) . . ? F12 C57 S4 96.6(6) . . ? F11 C57 S4 114.0(6) . . ? F10 C57 S4 115.6(6) . . ? S5 C57 S4 16.95(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.536 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.072 #===END data_shelxl(4) _database_code_depnum_ccdc_archive 'CCDC 299031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H49 Cl4 Cu4 N31 O20' _chemical_formula_weight 1752.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 22.912(9) _cell_length_b 21.105(7) _cell_length_c 18.184(7) _cell_angle_alpha 90.00 _cell_angle_beta 128.679(7) _cell_angle_gamma 90.00 _cell_volume 6864(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 14019 _cell_measurement_theta_min 1.9298 _cell_measurement_theta_max 30.8190 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3544 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6225 _exptl_absorpt_correction_T_max 0.8358 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 37116 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 31.01 _reflns_number_total 9417 _reflns_number_gt 8054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_publication_material 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.1466P)^2^+53.5329P] 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 SHELXL _refine_ls_extinction_coef 0.00010(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9417 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1217 _refine_ls_R_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.2986 _refine_ls_wR_factor_gt 0.2878 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 Cu1 Cu 0.15303(4) 0.15100(3) 0.40302(5) 0.0315(2) Uani 1 1 d . . . Cu2 Cu 0.03482(4) 0.12777(3) 0.12290(5) 0.0323(2) Uani 1 1 d . . . Cl1 Cl 0.18354(11) 0.67324(8) 0.53168(13) 0.0500(4) Uani 1 1 d . . . Cl2 Cl 0.13522(10) 0.43842(10) 0.64651(12) 0.0509(4) Uani 1 1 d . . . O1 O 0.1001(2) 0.17562(18) 0.2717(3) 0.0323(8) Uani 1 1 d . . . O2 O 0.0548(2) 0.10429(18) 0.3888(3) 0.0340(8) Uani 1 1 d . . . O3 O 0.1866(4) 0.6454(3) 0.4635(4) 0.0655(16) Uani 1 1 d . . . O4 O 0.2428(5) 0.7188(4) 0.5885(6) 0.099(3) Uani 1 1 d . . . O5 O 0.1119(4) 0.7011(4) 0.4878(6) 0.087(2) Uani 1 1 d . . . O6 O 0.1950(4) 0.6239(3) 0.5938(5) 0.0688(17) Uani 1 1 d . . . O7 O 0.1947(4) 0.3968(3) 0.6730(4) 0.0661(15) Uiso 1 1 d . . . O8 O 0.1635(6) 0.5021(5) 0.6431(7) 0.061(2) Uiso 0.60 1 d P . . O9 O 0.1443(8) 0.4827(7) 0.6999(10) 0.060(3) Uiso 0.40 1 d P . . O10 O 0.1289(5) 0.4472(5) 0.7200(6) 0.056(2) Uiso 0.60 1 d P . . O11 O 0.0921(10) 0.3804(9) 0.6469(13) 0.078(5) Uiso 0.40 1 d P . . O12 O 0.0638(5) 0.4318(4) 0.5587(6) 0.053(2) Uiso 0.60 1 d P . . O13 O 0.0929(9) 0.4420(8) 0.5463(12) 0.071(4) Uiso 0.40 1 d P . . N1 N 0.1101(3) 0.2766(2) 0.3310(3) 0.0341(9) Uani 1 1 d . . . N2 N 0.0174(3) 0.2190(2) 0.0951(4) 0.0341(10) Uani 1 1 d . . . N3 N 0.1768(3) 0.3279(2) 0.5119(4) 0.0383(11) Uani 1 1 d . . . H6 H 0.1575 0.3560 0.4664 0.046 Uiso 1 1 calc R . . H7 H 0.1974 0.3403 0.5696 0.046 Uiso 1 1 calc R . . N4 N 0.1465(3) 0.2405(2) 0.4125(3) 0.0319(9) Uani 1 1 d . . . N5 N 0.2315(3) 0.2379(3) 0.6537(4) 0.0389(11) Uani 1 1 d . . . N6 N 0.1968(3) -0.0321(2) 0.3770(4) 0.0381(10) Uani 1 1 d . . . H14 H 0.2211 -0.0624 0.3730 0.046 Uiso 1 1 calc R . . N7 N 0.2105(3) 0.1594(2) 0.5458(3) 0.0321(9) Uani 1 1 d . . . N8 N 0.1662(3) 0.0620(2) 0.3900(3) 0.0335(9) Uani 1 1 d . . . N9 N -0.0085(3) 0.0023(2) 0.1301(4) 0.0343(10) Uani 1 1 d . . . N10 N 0.0428(3) 0.0369(2) 0.1299(3) 0.0347(10) Uani 1 1 d . . . N11 N 0.0988(3) -0.0530(2) 0.1239(4) 0.0452(13) Uani 1 1 d . . . H16 H 0.0697 -0.0792 0.1253 0.054 Uiso 1 1 calc R . . H17 H 0.1332 -0.0681 0.1211 0.054 Uiso 1 1 calc R . . N12 N 0.1859(3) 0.0308(3) 0.1103(4) 0.0384(11) Uani 1 1 d . . . N13 N 0.1191(3) 0.1155(2) 0.1141(4) 0.0354(10) Uani 1 1 d . . . N14 N 0.1390(4) 0.4600(4) 0.4031(5) 0.0634(18) Uani 1 1 d . . . N15 N 0.0707(7) 0.8202(4) 0.1759(7) 0.042(3) Uani 0.50 1 d P . . N17 N -0.0112(3) 0.3145(3) 0.0367(4) 0.0402(11) Uani 1 1 d . . . H4 H -0.0299 0.3455 -0.0047 0.048 Uiso 1 1 calc R . . C1 C 0.0425(4) 0.3851(3) 0.1768(5) 0.0460(15) Uani 1 1 d . . . H1 H 0.0467 0.3805 0.2335 0.055 Uiso 1 1 calc R . . H2 H 0.0008 0.4134 0.1322 0.055 Uiso 1 1 calc R . . H3 H 0.0891 0.4028 0.1939 0.055 Uiso 1 1 calc R . . C2 C 0.0289(3) 0.3219(3) 0.1323(4) 0.0331(11) Uani 1 1 d . . . C3 C -0.0172(4) 0.2521(3) 0.0166(4) 0.0398(12) Uani 1 1 d . . . H5 H -0.0424 0.2348 -0.0446 0.048 Uiso 1 1 calc R . . C4 C 0.0465(3) 0.2617(2) 0.1673(4) 0.0310(10) Uani 1 1 d . . . C5 C 0.0880(3) 0.2369(3) 0.2622(4) 0.0297(10) Uani 1 1 d . . . C6 C 0.1747(3) 0.2664(3) 0.4932(4) 0.0325(10) Uani 1 1 d . . . C7 C 0.2079(3) 0.2188(3) 0.5704(4) 0.0343(11) Uani 1 1 d . . . C8 C 0.2590(4) 0.1932(3) 0.7189(5) 0.0454(14) Uani 1 1 d . . . H8 H 0.2741 0.2046 0.7791 0.054 Uiso 1 1 calc R . . C9 C 0.2666(4) 0.1305(3) 0.7028(5) 0.0396(12) Uani 1 1 d . . . H9 H 0.2882 0.0994 0.7510 0.047 Uiso 1 1 calc R . . C10 C 0.2411(3) 0.1158(3) 0.6136(5) 0.0390(12) Uani 1 1 d . . . H10 H 0.2455 0.0734 0.5999 0.047 Uiso 1 1 calc R . . C11 C 0.1022(4) -0.1044(3) 0.3613(5) 0.0479(15) Uani 1 1 d . . . H11 H 0.0632 -0.1127 0.2940 0.057 Uiso 1 1 calc R . . H12 H 0.0801 -0.1050 0.3932 0.057 Uiso 1 1 calc R . . H13 H 0.1409 -0.1372 0.3885 0.057 Uiso 1 1 calc R . . C12 C 0.1361(3) -0.0412(3) 0.3740(4) 0.0350(11) Uani 1 1 d . . . C13 C 0.2136(3) 0.0297(3) 0.3868(4) 0.0374(12) Uani 1 1 d . . . H15 H 0.2536 0.0475 0.3909 0.045 Uiso 1 1 calc R . . C14 C 0.1170(3) 0.0188(2) 0.3808(4) 0.0299(10) Uani 1 1 d . . . C15 C 0.0566(3) 0.0422(3) 0.3797(4) 0.0312(10) Uani 1 1 d . . . C16 C 0.0909(3) 0.0096(3) 0.1259(4) 0.0347(11) Uani 1 1 d . . . C17 C 0.1353(3) 0.0539(3) 0.1166(4) 0.0372(12) Uani 1 1 d . . . C18 C 0.2235(3) 0.0731(3) 0.1002(5) 0.0399(12) Uani 1 1 d . . . H18 H 0.2606 0.0588 0.0957 0.048 Uiso 1 1 calc R . . C19 C 0.2101(4) 0.1371(3) 0.0960(5) 0.0465(15) Uani 1 1 d . . . H19 H 0.2367 0.1669 0.0879 0.056 Uiso 1 1 calc R . . C20 C 0.1568(4) 0.1567(3) 0.1041(5) 0.0408(13) Uani 1 1 d . . . H20 H 0.1472 0.2007 0.1023 0.049 Uiso 1 1 calc R . . C21 C 0.0488(6) 0.5422(5) 0.3881(8) 0.079(3) Uiso 1 1 d . . . H21 H -0.0019 0.5340 0.3302 0.095 Uiso 1 1 calc R . . H22 H 0.0636 0.5855 0.3867 0.095 Uiso 1 1 calc R . . H23 H 0.0501 0.5372 0.4426 0.095 Uiso 1 1 calc R . . C22 C 0.1002(4) 0.4977(4) 0.3952(6) 0.0557(18) Uani 1 1 d . . . C23 C 0.0886(13) 0.7153(11) 0.2549(16) 0.084(6) Uiso 0.50 1 d P . . H24 H 0.0760 0.7202 0.2970 0.101 Uiso 0.50 1 calc PR . . H25 H 0.1404 0.7006 0.2911 0.101 Uiso 0.50 1 calc PR . . H26 H 0.0550 0.6841 0.2059 0.101 Uiso 0.50 1 calc PR . . C24 C 0.0804(7) 0.7758(5) 0.2112(7) 0.037(2) Uani 0.50 1 d P . . 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 Cu1 0.0354(4) 0.0237(3) 0.0364(4) 0.0014(2) 0.0230(3) 0.0010(2) Cu2 0.0357(4) 0.0253(3) 0.0399(4) -0.0003(3) 0.0256(3) -0.0001(2) Cl1 0.0669(10) 0.0347(8) 0.0586(10) 0.0022(7) 0.0442(9) 0.0097(7) Cl2 0.0457(8) 0.0617(10) 0.0455(8) -0.0035(7) 0.0285(7) -0.0020(7) O1 0.0372(19) 0.0238(17) 0.0329(18) 0.0020(15) 0.0205(16) 0.0011(14) O2 0.0349(19) 0.0225(17) 0.046(2) -0.0004(16) 0.0257(18) 0.0005(14) O3 0.088(4) 0.067(4) 0.068(4) -0.003(3) 0.062(4) 0.005(3) O4 0.113(6) 0.053(4) 0.096(6) -0.016(4) 0.048(5) -0.018(4) O5 0.089(5) 0.080(5) 0.110(6) 0.013(4) 0.071(5) 0.035(4) O6 0.107(5) 0.050(3) 0.072(4) 0.014(3) 0.068(4) 0.025(3) N1 0.037(2) 0.026(2) 0.039(2) 0.0040(18) 0.023(2) 0.0026(17) N2 0.038(2) 0.028(2) 0.043(3) 0.0012(19) 0.029(2) -0.0001(18) N3 0.052(3) 0.024(2) 0.040(2) 0.0003(19) 0.029(2) -0.0004(19) N4 0.034(2) 0.026(2) 0.034(2) 0.0000(17) 0.0205(19) 0.0003(16) N5 0.042(3) 0.042(3) 0.035(2) 0.000(2) 0.025(2) -0.002(2) N6 0.040(2) 0.031(2) 0.045(3) -0.003(2) 0.028(2) 0.0047(19) N7 0.035(2) 0.027(2) 0.036(2) 0.0005(18) 0.023(2) -0.0023(17) N8 0.036(2) 0.024(2) 0.040(2) 0.0012(18) 0.024(2) 0.0026(17) N9 0.034(2) 0.027(2) 0.042(2) -0.0032(19) 0.023(2) -0.0034(17) N10 0.035(2) 0.029(2) 0.038(2) -0.0014(19) 0.022(2) -0.0002(17) N11 0.049(3) 0.029(2) 0.072(4) 0.002(2) 0.045(3) 0.006(2) N12 0.035(2) 0.038(3) 0.043(3) -0.003(2) 0.025(2) 0.0036(19) N13 0.037(2) 0.030(2) 0.042(3) 0.000(2) 0.027(2) 0.0002(18) N14 0.052(4) 0.059(4) 0.068(4) -0.005(3) 0.032(3) 0.000(3) N15 0.089(8) 0.016(4) 0.045(5) -0.008(4) 0.053(6) -0.005(4) N17 0.044(3) 0.035(3) 0.040(3) 0.007(2) 0.025(2) 0.003(2) C1 0.046(3) 0.027(3) 0.053(4) 0.003(3) 0.025(3) 0.003(2) C2 0.032(2) 0.027(2) 0.037(3) 0.000(2) 0.020(2) -0.0001(19) C3 0.047(3) 0.033(3) 0.036(3) 0.002(2) 0.024(3) 0.002(2) C4 0.034(2) 0.023(2) 0.037(3) -0.003(2) 0.023(2) -0.0022(18) C5 0.027(2) 0.029(2) 0.033(2) 0.003(2) 0.018(2) 0.0014(18) C6 0.037(3) 0.025(2) 0.040(3) -0.001(2) 0.027(2) -0.0006(19) C7 0.035(3) 0.032(3) 0.038(3) 0.001(2) 0.024(2) -0.002(2) C8 0.051(3) 0.045(4) 0.041(3) 0.001(3) 0.029(3) -0.005(3) C9 0.042(3) 0.037(3) 0.042(3) 0.005(2) 0.027(3) -0.001(2) C10 0.042(3) 0.035(3) 0.047(3) 0.008(2) 0.031(3) 0.004(2) C11 0.054(4) 0.029(3) 0.055(4) -0.010(3) 0.030(3) -0.004(3) C12 0.036(3) 0.030(3) 0.037(3) 0.000(2) 0.022(2) 0.003(2) C13 0.038(3) 0.033(3) 0.044(3) -0.001(2) 0.027(3) 0.000(2) C14 0.031(2) 0.023(2) 0.032(2) 0.0015(19) 0.019(2) 0.0025(18) C15 0.033(2) 0.028(2) 0.031(2) 0.003(2) 0.019(2) 0.0040(19) C16 0.038(3) 0.029(3) 0.042(3) 0.001(2) 0.027(2) 0.004(2) C17 0.036(3) 0.038(3) 0.034(3) -0.004(2) 0.021(2) 0.002(2) C18 0.038(3) 0.042(3) 0.045(3) 0.003(3) 0.029(3) 0.002(2) C19 0.047(3) 0.043(3) 0.058(4) 0.003(3) 0.036(3) -0.002(3) C20 0.044(3) 0.033(3) 0.050(3) -0.002(2) 0.032(3) -0.002(2) C22 0.040(3) 0.044(4) 0.072(5) 0.001(3) 0.029(4) -0.003(3) C24 0.057(7) 0.028(5) 0.023(4) -0.010(4) 0.023(5) -0.012(5) _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 Cu1 N4 1.912(5) . ? Cu1 N8 1.940(5) . ? Cu1 O1 1.956(4) . ? Cu1 N7 2.057(5) . ? Cu1 O2 2.318(4) . ? Cu2 N10 1.924(5) . ? Cu2 N2 1.967(5) . ? Cu2 O2 1.992(4) 2 ? Cu2 N13 2.051(5) . ? Cu2 O1 2.349(4) . ? Cl1 O3 1.412(6) . ? Cl1 O5 1.429(7) . ? Cl1 O6 1.436(6) . ? Cl1 O4 1.443(8) . ? Cl2 O9 1.268(15) . ? Cl2 O12 1.408(9) . ? Cl2 O7 1.427(7) . ? Cl2 O13 1.434(17) . ? Cl2 O10 1.443(9) . ? Cl2 O8 1.510(10) . ? Cl2 O11 1.575(19) . ? O1 C5 1.311(6) . ? O2 C15 1.325(7) . ? O2 Cu2 1.991(4) 2 ? O8 O9 1.412(17) . ? O9 O10 0.992(16) . ? O10 O11 1.75(2) . ? O11 O12 1.69(2) . ? O12 O13 0.853(17) . ? N1 C5 1.317(7) . ? N1 N4 1.388(6) . ? N2 C3 1.320(8) . ? N2 C4 1.372(7) . ? N3 C6 1.335(7) . ? N3 H6 0.8800 . ? N3 H7 0.8800 . ? N4 C6 1.297(7) . ? N5 C7 1.312(7) . ? N5 C8 1.326(8) . ? N6 C13 1.340(8) . ? N6 C12 1.370(8) . ? N6 H14 0.8800 . ? N7 C10 1.334(7) . ? N7 C7 1.346(7) . ? N8 C13 1.313(7) . ? N8 C14 1.376(7) . ? N9 C15 1.309(7) 2 ? N9 N10 1.384(7) . ? N10 C16 1.286(7) . ? N11 C16 1.337(7) . ? N11 H16 0.8800 . ? N11 H17 0.8800 . ? N12 C17 1.325(7) . ? N12 C18 1.334(8) . ? N13 C20 1.316(8) . ? N13 C17 1.346(8) . ? N14 C22 1.135(10) . ? N15 C24 1.078(15) . ? N17 C3 1.350(8) . ? N17 C2 1.377(8) . ? N17 H4 0.8800 . ? C1 C2 1.487(8) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 C4 1.365(8) . ? C3 H5 0.9500 . ? C4 C5 1.450(7) . ? C6 C7 1.492(8) . ? C8 C9 1.390(9) . ? C8 H8 0.9500 . ? C9 C10 1.372(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.488(8) . ? C11 H11 0.9800 . ? C11 H12 0.9800 . ? C11 H13 0.9800 . ? C12 C14 1.371(7) . ? C13 H15 0.9500 . ? C14 C15 1.457(7) . ? C15 N9 1.309(7) 2 ? C16 C17 1.468(8) . ? C18 C19 1.376(9) . ? C18 H18 0.9500 . ? C19 C20 1.381(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.445(13) . ? C21 H21 0.9800 . ? C21 H22 0.9800 . ? C21 H23 0.9800 . ? C23 C24 1.45(3) . ? C23 H24 0.9800 . ? C23 H25 0.9800 . ? C23 H26 0.9800 . ? 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 N4 Cu1 N8 174.1(2) . . ? N4 Cu1 O1 79.84(18) . . ? N8 Cu1 O1 97.67(19) . . ? N4 Cu1 N7 79.99(19) . . ? N8 Cu1 N7 102.2(2) . . ? O1 Cu1 N7 159.67(18) . . ? N4 Cu1 O2 107.80(17) . . ? N8 Cu1 O2 77.79(17) . . ? O1 Cu1 O2 99.15(16) . . ? N7 Cu1 O2 89.35(17) . . ? N10 Cu2 N2 171.4(2) . . ? N10 Cu2 O2 78.90(18) . 2 ? N2 Cu2 O2 100.69(18) . 2 ? N10 Cu2 N13 79.9(2) . . ? N2 Cu2 N13 98.8(2) . . ? O2 Cu2 N13 156.79(19) 2 . ? N10 Cu2 O1 112.76(17) . . ? N2 Cu2 O1 75.86(18) . . ? O2 Cu2 O1 95.86(16) 2 . ? N13 Cu2 O1 101.00(18) . . ? O3 Cl1 O5 110.5(4) . . ? O3 Cl1 O6 107.7(4) . . ? O5 Cl1 O6 108.6(4) . . ? O3 Cl1 O4 111.4(5) . . ? O5 Cl1 O4 111.4(5) . . ? O6 Cl1 O4 107.0(5) . . ? O9 Cl2 O12 117.4(8) . . ? O9 Cl2 O7 122.0(7) . . ? O12 Cl2 O7 120.6(5) . . ? O9 Cl2 O13 126.2(10) . . ? O12 Cl2 O13 34.9(7) . . ? O7 Cl2 O13 101.9(8) . . ? O9 Cl2 O10 42.3(7) . . ? O12 Cl2 O10 110.2(6) . . ? O7 Cl2 O10 113.1(5) . . ? O13 Cl2 O10 142.2(8) . . ? O9 Cl2 O8 60.4(8) . . ? O12 Cl2 O8 105.4(6) . . ? O7 Cl2 O8 102.6(5) . . ? O13 Cl2 O8 82.4(8) . . ? O10 Cl2 O8 102.6(6) . . ? O9 Cl2 O11 111.9(10) . . ? O12 Cl2 O11 68.9(8) . . ? O7 Cl2 O11 89.4(7) . . ? O13 Cl2 O11 96.8(10) . . ? O10 Cl2 O11 70.7(8) . . ? O8 Cl2 O11 167.9(8) . . ? C5 O1 Cu1 110.0(3) . . ? C5 O1 Cu2 110.0(3) . . ? Cu1 O1 Cu2 139.00(19) . . ? C15 O2 Cu2 110.0(3) . 2 ? C15 O2 Cu1 109.4(3) . . ? Cu2 O2 Cu1 140.42(19) 2 . ? O9 O8 Cl2 51.3(7) . . ? O10 O9 Cl2 78.3(12) . . ? O10 O9 O8 146.5(16) . . ? Cl2 O9 O8 68.4(8) . . ? O9 O10 Cl2 59.4(10) . . ? O9 O10 O11 116.3(13) . . ? Cl2 O10 O11 58.2(7) . . ? Cl2 O11 O12 50.9(7) . . ? Cl2 O11 O10 51.1(6) . . ? O12 O11 O10 85.5(10) . . ? O13 O12 Cl2 74.2(13) . . ? O13 O12 O11 120.7(16) . . ? Cl2 O12 O11 60.2(7) . . ? O12 O13 Cl2 70.9(13) . . ? C5 N1 N4 106.4(4) . . ? C3 N2 C4 106.9(5) . . ? C3 N2 Cu2 133.2(4) . . ? C4 N2 Cu2 119.8(4) . . ? C6 N3 H6 120.0 . . ? C6 N3 H7 120.0 . . ? H6 N3 H7 120.0 . . ? C6 N4 N1 121.3(5) . . ? C6 N4 Cu1 120.3(4) . . ? N1 N4 Cu1 118.4(3) . . ? C7 N5 C8 115.9(6) . . ? C13 N6 C12 109.9(5) . . ? C13 N6 H14 125.0 . . ? C12 N6 H14 125.0 . . ? C10 N7 C7 116.2(5) . . ? C10 N7 Cu1 131.3(4) . . ? C7 N7 Cu1 112.0(4) . . ? C13 N8 C14 106.7(5) . . ? C13 N8 Cu1 134.7(4) . . ? C14 N8 Cu1 118.6(4) . . ? C15 N9 N10 107.7(5) 2 . ? C16 N10 N9 121.4(5) . . ? C16 N10 Cu2 119.5(4) . . ? N9 N10 Cu2 118.8(4) . . ? C16 N11 H16 120.0 . . ? C16 N11 H17 120.0 . . ? H16 N11 H17 120.0 . . ? C17 N12 C18 116.2(6) . . ? C20 N13 C17 116.9(5) . . ? C20 N13 Cu2 131.2(4) . . ? C17 N13 Cu2 111.9(4) . . ? C3 N17 C2 109.1(5) . . ? C3 N17 H4 125.5 . . ? C2 N17 H4 125.5 . . ? C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C4 C2 N17 104.6(5) . . ? C4 C2 C1 133.0(6) . . ? N17 C2 C1 122.4(5) . . ? N2 C3 N17 109.5(5) . . ? N2 C3 H5 125.3 . . ? N17 C3 H5 125.3 . . ? C2 C4 N2 109.9(5) . . ? C2 C4 C5 132.3(5) . . ? N2 C4 C5 117.8(5) . . ? O1 C5 N1 125.4(5) . . ? O1 C5 C4 116.1(5) . . ? N1 C5 C4 118.5(5) . . ? N4 C6 N3 127.6(5) . . ? N4 C6 C7 112.5(5) . . ? N3 C6 C7 119.9(5) . . ? N5 C7 N7 126.7(6) . . ? N5 C7 C6 118.7(5) . . ? N7 C7 C6 114.6(5) . . ? N5 C8 C9 122.7(6) . . ? N5 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C10 C9 C8 116.6(6) . . ? C10 C9 H9 121.7 . . ? C8 C9 H9 121.7 . . ? N7 C10 C9 121.7(6) . . ? N7 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C12 C11 H11 109.5 . . ? C12 C11 H12 109.5 . . ? H11 C11 H12 109.5 . . ? C12 C11 H13 109.5 . . ? H11 C11 H13 109.5 . . ? H12 C11 H13 109.5 . . ? N6 C12 C14 104.0(5) . . ? N6 C12 C11 123.4(5) . . ? C14 C12 C11 132.6(6) . . ? N8 C13 N6 109.6(5) . . ? N8 C13 H15 125.2 . . ? N6 C13 H15 125.2 . . ? C12 C14 N8 109.8(5) . . ? C12 C14 C15 131.8(5) . . ? N8 C14 C15 118.4(5) . . ? N9 C15 O2 124.4(5) 2 . ? N9 C15 C14 119.8(5) 2 . ? O2 C15 C14 115.8(5) . . ? N10 C16 N11 125.5(6) . . ? N10 C16 C17 113.7(5) . . ? N11 C16 C17 120.6(5) . . ? N12 C17 N13 126.2(6) . . ? N12 C17 C16 118.8(6) . . ? N13 C17 C16 115.0(5) . . ? N12 C18 C19 121.5(6) . . ? N12 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C20 118.1(6) . . ? C18 C19 H19 121.0 . . ? C20 C19 H19 121.0 . . ? N13 C20 C19 121.2(6) . . ? N13 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 H21 109.5 . . ? C22 C21 H22 109.5 . . ? H21 C21 H22 109.5 . . ? C22 C21 H23 109.5 . . ? H21 C21 H23 109.5 . . ? H22 C21 H23 109.5 . . ? N14 C22 C21 175.3(10) . . ? C24 C23 H24 109.5 . . ? C24 C23 H25 109.5 . . ? H24 C23 H25 109.5 . . ? C24 C23 H26 109.5 . . ? H24 C23 H26 109.5 . . ? H25 C23 H26 109.5 . . ? N15 C24 C23 176.6(17) . . ? _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 31.01 _diffrn_measured_fraction_theta_full 0.859 _refine_diff_density_max 1.491 _refine_diff_density_min -1.880 _refine_diff_density_rms 0.196 #===END data_shelxl(5) _database_code_depnum_ccdc_archive 'CCDC 299032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81.50 H75 Cl4 Mn5 N25 O23.50' _chemical_formula_weight 2197.17 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9992(13) _cell_length_b 22.318(2) _cell_length_c 29.476(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.573(2) _cell_angle_gamma 90.00 _cell_volume 9191.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4395 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.95 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7162 _exptl_absorpt_correction_T_max 0.9577 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72073 _diffrn_reflns_av_R_equivalents 0.1198 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 26.55 _reflns_number_total 18894 _reflns_number_gt 10078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _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^)+(0.1320P)^2^+4.4984P] 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 18894 _refine_ls_number_parameters 1241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2436 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.015 _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 0.18476(7) 0.25926(4) 0.07827(3) 0.0343(2) Uani 1 1 d . . . Mn2 Mn 0.36675(7) 0.38539(4) 0.11372(3) 0.0365(2) Uani 1 1 d . . . Mn3 Mn 0.53260(7) 0.24257(4) 0.12303(3) 0.0336(2) Uani 1 1 d . . . Mn4 Mn 0.30873(7) 0.16780(4) 0.17859(3) 0.0337(2) Uani 1 1 d . . . Mn5 Mn 0.39385(7) 0.19840(4) 0.00743(3) 0.0325(2) Uani 1 1 d . . . Cl1 Cl 0.43347(13) 0.14564(8) -0.17118(6) 0.0511(4) Uani 1 1 d . . . Cl2 Cl 0.85191(15) 0.44479(10) 0.11491(7) 0.0651(5) Uani 1 1 d . . . Cl3 Cl -0.05740(17) 0.28646(11) -0.10825(8) 0.0730(6) Uani 1 1 d . . . Cl4 Cl 0.13868(19) -0.08925(11) -0.08014(13) 0.0969(9) Uani 1 1 d . . . O1 O 0.2524(3) 0.32200(17) 0.12639(13) 0.0340(9) Uani 1 1 d . . . O2 O 0.4730(3) 0.32253(17) 0.09035(13) 0.0345(9) Uani 1 1 d . . . O3 O 0.4274(3) 0.23169(18) 0.17374(13) 0.0339(9) Uani 1 1 d . . . O4 O 0.4667(3) 0.18067(17) 0.07466(13) 0.0332(9) Uani 1 1 d . . . O5 O 0.2420(3) 0.17822(17) 0.10981(13) 0.0348(9) Uani 1 1 d . . . O6 O 0.2896(3) 0.26556(17) 0.02640(13) 0.0351(9) Uani 1 1 d . . . O7 O 0.4468(4) 0.1137(3) -0.12955(19) 0.0838(18) Uani 1 1 d . . . O8 O 0.5229(4) 0.1483(3) -0.1909(2) 0.0735(16) Uani 1 1 d . . . O9 O 0.3673(5) 0.1142(3) -0.1998(2) 0.093(2) Uani 1 1 d . . . O10 O 0.4020(5) 0.2039(3) -0.1642(3) 0.121(3) Uani 1 1 d . . . O11 O 0.8330(5) 0.4282(3) 0.1581(2) 0.101(2) Uani 1 1 d . . . O12 O 0.9501(5) 0.4493(4) 0.1123(3) 0.124(3) Uani 1 1 d . . . O13 O 0.8209(13) 0.4045(8) 0.0873(5) 0.318(10) Uani 1 1 d . . . O14 O 0.8111(7) 0.4995(5) 0.1050(4) 0.206(7) Uani 1 1 d . . . O15 O -0.0409(13) 0.2976(6) -0.0643(4) 0.262(8) Uani 1 1 d . . . O16 O -0.0293(11) 0.2357(6) -0.1252(4) 0.253(8) Uani 1 1 d . . . O17 O -0.0497(14) 0.3318(6) -0.1343(4) 0.278(9) Uani 1 1 d . . . O18 O -0.1476(12) 0.2833(13) -0.1100(8) 0.437(18) Uani 1 1 d . . . O19 O 0.1208(8) -0.0503(4) -0.0441(5) 0.237(8) Uani 1 1 d . . . O20 O 0.2348(5) -0.0961(3) -0.0793(3) 0.110(3) Uani 1 1 d . . . O21 O 0.1167(9) -0.0635(8) -0.1212(4) 0.239(7) Uani 1 1 d . . . O22 O 0.0876(6) -0.1411(4) -0.0744(4) 0.159(4) Uani 1 1 d . . . O23 O 0.0144(11) -0.0193(7) 0.1568(6) 0.184(6) Uiso 0.75 1 d P . . O24 O -0.3047(10) 0.3570(7) -0.1442(5) 0.161(5) Uiso 0.75 1 d P . . N1 N 0.0767(4) 0.2768(2) 0.12994(17) 0.0379(12) Uani 1 1 d . . . N2 N 0.2330(4) 0.3764(2) 0.19192(17) 0.0396(12) Uani 1 1 d . . . N3 N 0.3211(4) 0.3988(2) 0.18247(18) 0.0422(13) Uani 1 1 d . . . N4 N 0.4789(4) 0.4430(2) 0.15361(19) 0.0456(14) Uani 1 1 d . . . N5 N 0.2582(4) 0.4574(2) 0.0855(2) 0.0475(14) Uani 1 1 d . . . N6 N 0.4079(4) 0.4151(2) 0.04750(18) 0.0399(13) Uani 1 1 d . . . N7 N 0.4885(4) 0.3888(2) 0.03012(17) 0.0378(12) Uani 1 1 d . . . N8 N 0.6382(4) 0.2705(2) 0.07323(17) 0.0364(12) Uani 1 1 d . . . N9 N 0.5890(4) 0.2964(2) 0.18238(17) 0.0389(12) Uani 1 1 d . . . N10 N 0.3837(4) 0.2679(2) 0.24318(17) 0.0420(13) Uani 1 1 d . . . N11 N 0.3019(4) 0.2330(2) 0.23295(16) 0.0386(12) Uani 1 1 d . . . N12 N 0.1612(4) 0.1625(2) 0.20943(18) 0.0416(13) Uani 1 1 d . . . N13 N 0.5921(4) 0.1523(2) 0.14370(18) 0.0417(13) Uani 1 1 d . . . N14 N 0.4530(4) 0.0796(2) 0.05543(17) 0.0367(12) Uani 1 1 d . . . N15 N 0.3962(4) 0.1020(2) 0.01926(17) 0.0355(12) Uani 1 1 d . . . N16 N 0.2869(4) 0.1524(2) -0.04495(17) 0.0406(13) Uani 1 1 d . . . N17 N 0.3954(4) 0.0992(2) 0.22249(18) 0.0432(13) Uani 1 1 d . . . N18 N 0.2968(3) 0.0796(2) 0.14671(16) 0.0351(12) Uani 1 1 d . . . N19 N 0.2401(4) 0.0743(2) 0.10604(17) 0.0371(12) Uani 1 1 d . . . N20 N 0.1138(4) 0.1848(2) 0.03923(17) 0.0371(12) Uani 1 1 d . . . N21 N 0.5332(4) 0.1935(2) -0.02915(17) 0.0371(12) Uani 1 1 d . . . N22 N 0.4014(4) 0.2742(2) -0.03846(17) 0.0386(12) Uani 1 1 d . . . N23 N 0.3247(4) 0.3153(2) -0.03970(17) 0.0389(12) Uani 1 1 d . . . N24 N 0.1339(4) 0.3339(2) 0.03266(17) 0.0403(13) Uani 1 1 d . . . N25 N 0.2623(8) 0.3576(6) -0.2159(5) 0.156(5) Uani 1 1 d . . . C1 C -0.0122(5) 0.2546(3) 0.1301(2) 0.0480(17) Uani 1 1 d . . . C2 C -0.0735(5) 0.2693(4) 0.1622(3) 0.0562(19) Uani 1 1 d . . . C3 C -0.0446(5) 0.3093(3) 0.1960(2) 0.0516(18) Uani 1 1 d . . . C4 C 0.0464(5) 0.3324(3) 0.1964(2) 0.0466(17) Uani 1 1 d . . . C5 C 0.1054(4) 0.3153(3) 0.1629(2) 0.0356(14) Uani 1 1 d . . . C6 C 0.2046(4) 0.3391(2) 0.16044(19) 0.0319(13) Uani 1 1 d . . . C7 C 0.3661(5) 0.4322(3) 0.2119(2) 0.0510(18) Uani 1 1 d . . . C8 C 0.3317(6) 0.4443(5) 0.2580(3) 0.082(3) Uani 1 1 d . . . C9 C 0.4575(5) 0.4573(3) 0.1968(2) 0.0521(18) Uani 1 1 d . . . C10 C 0.5183(6) 0.4924(4) 0.2247(3) 0.079(3) Uani 1 1 d . . . C11 C 0.5999(6) 0.5155(4) 0.2069(3) 0.079(3) Uani 1 1 d . . . C12 C 0.6194(6) 0.5023(4) 0.1640(3) 0.071(2) Uani 1 1 d . . . C13 C 0.5578(5) 0.4656(3) 0.1390(3) 0.058(2) Uani 1 1 d . . . C14 C 0.1866(5) 0.4809(3) 0.1067(3) 0.0568(19) Uani 1 1 d . . . C15 C 0.1393(6) 0.5316(4) 0.0922(3) 0.067(2) Uani 1 1 d . . . C16 C 0.1657(6) 0.5596(3) 0.0535(3) 0.066(2) Uani 1 1 d . . . C17 C 0.2366(5) 0.5344(3) 0.0296(3) 0.0562(19) Uani 1 1 d . . . C18 C 0.2831(5) 0.4836(3) 0.0464(2) 0.0472(17) Uani 1 1 d . . . C19 C 0.3636(5) 0.4553(3) 0.0234(2) 0.0420(15) Uani 1 1 d . . . C20 C 0.3880(5) 0.4757(3) -0.0220(2) 0.0557(19) Uani 1 1 d . . . C21 C 0.5168(4) 0.3435(3) 0.05574(19) 0.0326(13) Uani 1 1 d . . . C22 C 0.6068(4) 0.3133(3) 0.0444(2) 0.0353(14) Uani 1 1 d . . . C23 C 0.6565(5) 0.3290(3) 0.0074(2) 0.0468(17) Uani 1 1 d . . . C24 C 0.7417(5) 0.3005(4) 0.0000(3) 0.059(2) Uani 1 1 d . . . C25 C 0.7736(5) 0.2566(4) 0.0289(3) 0.056(2) Uani 1 1 d . . . C26 C 0.7213(5) 0.2419(3) 0.0654(2) 0.0470(17) Uani 1 1 d . . . C27 C 0.6705(5) 0.3287(3) 0.1859(2) 0.0460(17) Uani 1 1 d . . . C28 C 0.7003(6) 0.3597(4) 0.2235(3) 0.060(2) Uani 1 1 d . . . C29 C 0.6444(6) 0.3584(4) 0.2600(3) 0.074(3) Uani 1 1 d . . . C30 C 0.5595(6) 0.3266(4) 0.2574(2) 0.065(2) Uani 1 1 d . . . C31 C 0.5338(4) 0.2962(3) 0.2174(2) 0.0368(14) Uani 1 1 d . . . C32 C 0.4416(4) 0.2630(3) 0.2108(2) 0.0370(14) Uani 1 1 d . . . C33 C 0.2306(5) 0.2392(3) 0.2576(2) 0.0375(15) Uani 1 1 d . . . C34 C 0.2277(5) 0.2826(4) 0.2959(2) 0.0562(19) Uani 1 1 d . . . C35 C 0.1486(5) 0.2003(3) 0.2447(2) 0.0402(15) Uani 1 1 d . . . C36 C 0.0645(6) 0.2025(3) 0.2657(3) 0.059(2) Uani 1 1 d . . . C37 C -0.0110(6) 0.1657(4) 0.2501(3) 0.070(2) Uani 1 1 d . . . C38 C 0.0008(5) 0.1270(4) 0.2145(3) 0.062(2) Uani 1 1 d . . . C39 C 0.0885(5) 0.1273(3) 0.1957(2) 0.0536(18) Uani 1 1 d . . . C40 C 0.6521(5) 0.1402(3) 0.1795(2) 0.0534(19) Uani 1 1 d . . . C41 C 0.6743(5) 0.0815(4) 0.1921(2) 0.058(2) Uani 1 1 d . . . C42 C 0.6345(5) 0.0359(3) 0.1684(3) 0.056(2) Uani 1 1 d . . . C43 C 0.5731(5) 0.0477(3) 0.1310(2) 0.0443(16) Uani 1 1 d . . . C44 C 0.5523(4) 0.1072(3) 0.1195(2) 0.0383(15) Uani 1 1 d . . . C45 C 0.4861(4) 0.1232(3) 0.0808(2) 0.0325(13) Uani 1 1 d . . . C46 C 0.3538(4) 0.0653(3) -0.0085(2) 0.0377(14) Uani 1 1 d . . . C47 C 0.3605(5) -0.0016(3) -0.0041(3) 0.0538(18) Uani 1 1 d . . . C48 C 0.2959(4) 0.0923(3) -0.0463(2) 0.0370(14) Uani 1 1 d . . . C49 C 0.2508(5) 0.0589(3) -0.0813(2) 0.0526(18) Uani 1 1 d . . . C50 C 0.1921(6) 0.0876(3) -0.1135(2) 0.0539(19) Uani 1 1 d . . . C51 C 0.1812(6) 0.1473(4) -0.1114(2) 0.059(2) Uani 1 1 d . . . C52 C 0.2325(6) 0.1789(3) -0.0766(2) 0.0544(19) Uani 1 1 d . . . C53 C 0.4442(5) 0.1101(3) 0.2620(2) 0.0525(18) Uani 1 1 d . . . C54 C 0.4923(6) 0.0663(4) 0.2882(3) 0.059(2) Uani 1 1 d . . . C55 C 0.4896(5) 0.0091(4) 0.2720(3) 0.060(2) Uani 1 1 d . . . C56 C 0.4402(5) -0.0039(3) 0.2308(2) 0.0482(17) Uani 1 1 d . . . C57 C 0.3937(5) 0.0425(3) 0.2069(2) 0.0408(15) Uani 1 1 d . . . C58 C 0.3385(4) 0.0326(3) 0.1630(2) 0.0367(14) Uani 1 1 d . . . C59 C 0.3327(5) -0.0281(3) 0.1418(2) 0.0519(18) Uani 1 1 d . . . C60 C 0.2146(4) 0.1276(3) 0.0913(2) 0.0345(14) Uani 1 1 d . . . C61 C 0.1465(4) 0.1298(3) 0.0506(2) 0.0343(14) Uani 1 1 d . . . C62 C 0.1187(5) 0.0796(3) 0.0259(2) 0.0435(16) Uani 1 1 d . . . C63 C 0.0541(5) 0.0861(3) -0.0112(2) 0.0505(18) Uani 1 1 d . . . C64 C 0.0215(5) 0.1415(4) -0.0230(2) 0.0533(19) Uani 1 1 d . . . C65 C 0.0517(5) 0.1898(3) 0.0031(2) 0.0467(17) Uani 1 1 d . . . C66 C 0.6023(5) 0.1529(3) -0.0231(2) 0.0477(17) Uani 1 1 d . . . C67 C 0.6791(5) 0.1476(3) -0.0498(2) 0.0531(19) Uani 1 1 d . . . C68 C 0.6853(5) 0.1873(4) -0.0848(3) 0.057(2) Uani 1 1 d . . . C69 C 0.6159(5) 0.2309(3) -0.0916(2) 0.0535(19) Uani 1 1 d . . . C70 C 0.5402(5) 0.2329(3) -0.0639(2) 0.0403(15) Uani 1 1 d . . . C71 C 0.4644(5) 0.2790(3) -0.0680(2) 0.0448(16) Uani 1 1 d . . . C72 C 0.4661(6) 0.3263(3) -0.1037(3) 0.063(2) Uani 1 1 d . . . C73 C 0.2736(4) 0.3055(3) -0.0051(2) 0.0344(14) Uani 1 1 d . . . C74 C 0.1880(5) 0.3450(3) -0.0022(2) 0.0363(14) Uani 1 1 d . . . C75 C 0.1650(5) 0.3901(3) -0.0328(2) 0.0427(16) Uani 1 1 d . . . C76 C 0.0883(5) 0.4264(3) -0.0260(3) 0.0535(19) Uani 1 1 d . . . C77 C 0.0359(5) 0.4166(3) 0.0104(3) 0.0527(18) Uani 1 1 d . . . C78 C 0.0594(5) 0.3693(3) 0.0391(2) 0.0468(17) Uani 1 1 d . . . C79 C 0.0732(10) -0.0188(7) 0.1181(5) 0.096(4) Uiso 0.75 1 d P . . C80 C -0.3189(11) 0.4115(7) -0.1641(6) 0.108(5) Uiso 0.75 1 d P . . C81 C 0.2046(13) 0.2969(9) -0.1553(6) 0.198(8) Uani 1 1 d . . . C82 C 0.2347(7) 0.3290(6) -0.1884(4) 0.094(4) Uani 1 1 d . . . H1 H -0.0333 0.2275 0.1067 0.057 Uiso 1 1 d . . . H2 H -0.1355 0.2522 0.1616 0.067 Uiso 1 1 d . . . H3 H -0.0868 0.3209 0.2186 0.062 Uiso 1 1 d . . . H4 H 0.0686 0.3596 0.2196 0.056 Uiso 1 1 d . . . H5 H 0.3769 0.4293 0.2805 0.099 Uiso 1 1 d . . . H6 H 0.3248 0.4865 0.2620 0.099 Uiso 1 1 d . . . H7 H 0.2717 0.4254 0.2608 0.099 Uiso 1 1 d . . . H8 H 0.5040 0.5007 0.2552 0.095 Uiso 1 1 d . . . H9 H 0.6418 0.5407 0.2249 0.095 Uiso 1 1 d . . . H10 H 0.6747 0.5181 0.1514 0.085 Uiso 1 1 d . . . H11 H 0.5735 0.4559 0.1090 0.070 Uiso 1 1 d . . . H12 H 0.1673 0.4616 0.1334 0.068 Uiso 1 1 d . . . H13 H 0.0883 0.5469 0.1087 0.080 Uiso 1 1 d . . . H14 H 0.1353 0.5957 0.0435 0.080 Uiso 1 1 d . . . H15 H 0.2532 0.5517 0.0018 0.067 Uiso 1 1 d . . . H16 H 0.4296 0.5092 -0.0188 0.067 Uiso 1 1 d . . . H17 H 0.4189 0.4442 -0.0369 0.067 Uiso 1 1 d . . . H18 H 0.3312 0.4868 -0.0392 0.067 Uiso 1 1 d . . . H19 H 0.6320 0.3590 -0.0131 0.056 Uiso 1 1 d . . . H20 H 0.7780 0.3117 -0.0249 0.071 Uiso 1 1 d . . . H21 H 0.8317 0.2360 0.0241 0.067 Uiso 1 1 d . . . H22 H 0.7438 0.2110 0.0855 0.056 Uiso 1 1 d . . . H23 H 0.7092 0.3295 0.1606 0.055 Uiso 1 1 d . . . H24 H 0.7583 0.3818 0.2246 0.072 Uiso 1 1 d . . . H25 H 0.6638 0.3788 0.2872 0.089 Uiso 1 1 d . . . H26 H 0.5194 0.3258 0.2823 0.078 Uiso 1 1 d . . . H27 H 0.2302 0.2615 0.3239 0.067 Uiso 1 1 d . . . H28 H 0.2807 0.3091 0.2954 0.067 Uiso 1 1 d . . . H29 H 0.1699 0.3051 0.2927 0.067 Uiso 1 1 d . . . H30 H 0.0577 0.2286 0.2907 0.070 Uiso 1 1 d . . . H31 H -0.0707 0.1675 0.2640 0.083 Uiso 1 1 d . . . H32 H -0.0495 0.1013 0.2032 0.075 Uiso 1 1 d . . . H33 H 0.0977 0.1003 0.1712 0.064 Uiso 1 1 d . . . H34 H 0.6805 0.1725 0.1967 0.064 Uiso 1 1 d . . . H35 H 0.7176 0.0738 0.2174 0.071 Uiso 1 1 d . . . H36 H 0.6482 -0.0045 0.1770 0.067 Uiso 1 1 d . . . H37 H 0.5454 0.0158 0.1132 0.053 Uiso 1 1 d . . . H38 H 0.3602 -0.0124 0.0270 0.064 Uiso 1 1 d . . . H39 H 0.3070 -0.0195 -0.0205 0.064 Uiso 1 1 d . . . H40 H 0.4178 -0.0151 -0.0163 0.064 Uiso 1 1 d . . . H41 H 0.2602 0.0167 -0.0828 0.063 Uiso 1 1 d . . . H42 H 0.1593 0.0654 -0.1371 0.065 Uiso 1 1 d . . . H43 H 0.1398 0.1680 -0.1330 0.070 Uiso 1 1 d . . . H44 H 0.2276 0.2213 -0.0759 0.065 Uiso 1 1 d . . . H45 H 0.4461 0.1502 0.2728 0.063 Uiso 1 1 d . . . H46 H 0.5259 0.0761 0.3163 0.071 Uiso 1 1 d . . . H47 H 0.5213 -0.0220 0.2891 0.071 Uiso 1 1 d . . . H48 H 0.4380 -0.0437 0.2193 0.058 Uiso 1 1 d . . . H49 H 0.3285 -0.0575 0.1650 0.062 Uiso 1 1 d . . . H50 H 0.2772 -0.0303 0.1216 0.062 Uiso 1 1 d . . . H51 H 0.3880 -0.0350 0.1257 0.062 Uiso 1 1 d . . . H52 H 0.1435 0.0412 0.0342 0.052 Uiso 1 1 d . . . H53 H 0.0330 0.0518 -0.0281 0.061 Uiso 1 1 d . . . H54 H -0.0218 0.1468 -0.0488 0.064 Uiso 1 1 d . . . H55 H 0.0277 0.2284 -0.0049 0.056 Uiso 1 1 d . . . H56 H 0.5985 0.1257 0.0015 0.057 Uiso 1 1 d . . . H57 H 0.7264 0.1175 -0.0440 0.064 Uiso 1 1 d . . . H58 H 0.7369 0.1848 -0.1042 0.069 Uiso 1 1 d . . . H59 H 0.6199 0.2592 -0.1155 0.064 Uiso 1 1 d . . . H60 H 0.4689 0.3646 -0.0899 0.076 Uiso 1 1 d . . . H61 H 0.5210 0.3207 -0.1208 0.076 Uiso 1 1 d . . . H62 H 0.4101 0.3233 -0.1235 0.076 Uiso 1 1 d . . . H63 H 0.2017 0.3958 -0.0585 0.051 Uiso 1 1 d . . . H64 H 0.0721 0.4582 -0.0467 0.064 Uiso 1 1 d . . . H65 H -0.0163 0.4421 0.0162 0.063 Uiso 1 1 d . . . H66 H 0.0213 0.3617 0.0641 0.056 Uiso 1 1 d . . . H67 H 0.2208 0.3171 -0.1276 0.241 Uiso 1 1 d . . . H68 H 0.1371 0.2932 -0.1595 0.241 Uiso 1 1 d . . . H69 H 0.2338 0.2591 -0.1555 0.241 Uiso 1 1 d . . . H70 H 0.1048 -0.0565 0.1151 0.113 Uiso 0.75 1 d P . . H71 H 0.0352 -0.0115 0.0902 0.113 Uiso 0.75 1 d P . . H72 H 0.1216 0.0119 0.1208 0.113 Uiso 0.75 1 d P . . H73 H -0.3000 0.4434 -0.1439 0.127 Uiso 0.75 1 d P . . H74 H -0.2796 0.4155 -0.1905 0.127 Uiso 0.75 1 d P . . H75 H -0.3834 0.4174 -0.1750 0.127 Uiso 0.75 1 d P . . 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 0.0428(6) 0.0305(5) 0.0302(5) 0.0002(4) 0.0065(4) 0.0051(4) Mn2 0.0413(6) 0.0321(5) 0.0374(5) -0.0010(4) 0.0118(4) 0.0024(4) Mn3 0.0397(5) 0.0341(5) 0.0274(5) -0.0004(4) 0.0047(4) 0.0031(4) Mn4 0.0393(5) 0.0333(5) 0.0288(5) -0.0005(4) 0.0041(4) 0.0007(4) Mn5 0.0418(5) 0.0265(5) 0.0296(5) 0.0010(4) 0.0062(4) 0.0044(4) Cl1 0.0504(10) 0.0497(10) 0.0537(11) 0.0044(8) 0.0074(8) 0.0036(8) Cl2 0.0642(13) 0.0829(15) 0.0491(11) 0.0151(10) 0.0100(9) 0.0010(11) Cl3 0.0699(14) 0.0843(16) 0.0653(14) 0.0084(12) 0.0076(11) -0.0042(12) Cl4 0.0713(17) 0.0610(15) 0.161(3) -0.0020(17) 0.0259(17) -0.0085(12) O1 0.038(2) 0.034(2) 0.031(2) -0.0055(18) 0.0118(18) 0.0023(18) O2 0.037(2) 0.031(2) 0.037(2) 0.0046(18) 0.0114(19) 0.0039(18) O3 0.037(2) 0.039(2) 0.027(2) -0.0062(18) 0.0065(18) -0.0025(18) O4 0.041(2) 0.029(2) 0.029(2) 0.0015(17) 0.0026(18) 0.0043(18) O5 0.045(2) 0.029(2) 0.030(2) 0.0011(17) -0.0007(19) 0.0039(19) O6 0.045(2) 0.030(2) 0.030(2) 0.0015(18) 0.0072(19) 0.0074(19) O7 0.088(4) 0.107(5) 0.058(4) 0.021(3) 0.013(3) -0.018(4) O8 0.065(4) 0.079(4) 0.078(4) 0.017(3) 0.023(3) -0.002(3) O9 0.083(4) 0.109(5) 0.084(4) 0.006(4) -0.025(4) -0.024(4) O10 0.118(6) 0.076(5) 0.170(8) -0.005(5) 0.017(5) 0.034(4) O11 0.101(5) 0.123(6) 0.080(5) 0.046(4) 0.027(4) 0.011(4) O12 0.081(5) 0.149(7) 0.149(7) 0.012(6) 0.054(5) 0.014(5) O13 0.37(2) 0.34(2) 0.235(16) -0.123(15) -0.094(15) -0.128(18) O14 0.178(9) 0.222(11) 0.233(11) 0.176(10) 0.141(9) 0.122(9) O15 0.46(2) 0.171(11) 0.135(10) 0.038(8) -0.141(13) 0.042(13) O16 0.345(18) 0.216(13) 0.204(12) 0.007(10) 0.059(12) 0.211(13) O17 0.52(3) 0.167(11) 0.155(10) 0.105(9) 0.118(14) 0.122(14) O18 0.207(16) 0.71(5) 0.41(3) -0.27(3) 0.125(17) -0.27(2) O19 0.223(11) 0.123(8) 0.389(18) -0.141(10) 0.217(12) -0.077(8) O20 0.069(5) 0.081(5) 0.182(8) -0.019(5) 0.028(5) -0.001(4) O21 0.225(13) 0.326(18) 0.154(11) -0.037(12) -0.076(10) -0.091(13) O22 0.140(7) 0.106(6) 0.243(11) -0.067(7) 0.086(7) -0.074(6) N1 0.041(3) 0.036(3) 0.038(3) 0.003(2) 0.009(2) 0.004(2) N2 0.037(3) 0.044(3) 0.039(3) -0.007(2) 0.007(2) -0.003(2) N3 0.040(3) 0.047(3) 0.040(3) -0.005(3) 0.011(3) 0.001(3) N4 0.042(3) 0.045(3) 0.051(4) -0.008(3) 0.010(3) -0.003(3) N5 0.052(3) 0.035(3) 0.057(4) 0.007(3) 0.014(3) 0.010(3) N6 0.049(3) 0.028(3) 0.043(3) 0.001(2) 0.009(3) 0.001(2) N7 0.043(3) 0.034(3) 0.036(3) 0.004(2) 0.008(2) 0.000(2) N8 0.037(3) 0.038(3) 0.034(3) -0.007(2) 0.007(2) 0.001(2) N9 0.040(3) 0.041(3) 0.035(3) -0.001(2) 0.001(2) -0.004(2) N10 0.047(3) 0.049(3) 0.031(3) -0.007(2) 0.008(2) -0.004(3) N11 0.049(3) 0.041(3) 0.027(3) -0.001(2) 0.007(2) 0.000(3) N12 0.041(3) 0.047(3) 0.037(3) 0.005(3) 0.006(2) -0.003(3) N13 0.045(3) 0.043(3) 0.037(3) 0.002(3) 0.003(3) 0.014(3) N14 0.042(3) 0.028(3) 0.040(3) 0.004(2) 0.005(2) 0.000(2) N15 0.042(3) 0.031(3) 0.034(3) 0.000(2) 0.007(2) 0.000(2) N16 0.049(3) 0.038(3) 0.035(3) -0.004(2) 0.002(2) 0.007(3) N17 0.047(3) 0.044(3) 0.038(3) 0.006(3) 0.003(3) 0.006(3) N18 0.037(3) 0.034(3) 0.034(3) 0.002(2) 0.002(2) 0.000(2) N19 0.046(3) 0.034(3) 0.032(3) 0.001(2) 0.001(2) 0.005(2) N20 0.038(3) 0.040(3) 0.033(3) 0.000(2) 0.004(2) 0.003(2) N21 0.047(3) 0.033(3) 0.033(3) -0.001(2) 0.011(2) 0.005(2) N22 0.050(3) 0.031(3) 0.036(3) 0.002(2) 0.010(3) 0.004(2) N23 0.053(3) 0.032(3) 0.033(3) 0.003(2) 0.009(3) 0.008(2) N24 0.051(3) 0.034(3) 0.037(3) 0.004(2) 0.010(3) 0.010(2) N25 0.092(8) 0.220(14) 0.155(11) 0.072(10) -0.013(7) -0.015(8) C1 0.041(4) 0.047(4) 0.056(4) -0.002(3) 0.004(3) -0.008(3) C2 0.042(4) 0.069(5) 0.058(5) -0.006(4) 0.005(4) -0.007(4) C3 0.040(4) 0.067(5) 0.049(4) -0.003(4) 0.016(3) 0.000(4) C4 0.050(4) 0.057(4) 0.035(4) 0.002(3) 0.011(3) 0.004(3) C5 0.045(4) 0.029(3) 0.034(3) 0.005(3) 0.011(3) 0.003(3) C6 0.039(3) 0.028(3) 0.029(3) 0.001(3) 0.006(3) 0.003(3) C7 0.046(4) 0.056(4) 0.052(4) -0.016(4) 0.006(3) -0.008(3) C8 0.070(6) 0.121(8) 0.056(5) -0.040(5) 0.016(4) -0.032(6) C9 0.048(4) 0.055(4) 0.053(5) -0.012(4) 0.006(3) -0.011(3) C10 0.065(6) 0.100(7) 0.073(6) -0.038(5) 0.008(5) -0.020(5) C11 0.053(5) 0.093(7) 0.093(7) -0.036(6) 0.007(5) -0.023(5) C12 0.049(5) 0.068(6) 0.097(7) -0.023(5) 0.022(5) -0.008(4) C13 0.045(4) 0.059(5) 0.073(5) -0.009(4) 0.017(4) -0.004(4) C14 0.054(5) 0.043(4) 0.075(5) 0.004(4) 0.013(4) 0.005(4) C15 0.057(5) 0.047(5) 0.097(7) 0.002(4) 0.015(5) 0.012(4) C16 0.062(5) 0.040(4) 0.096(7) 0.000(4) -0.007(5) 0.008(4) C17 0.053(5) 0.043(4) 0.073(5) 0.007(4) 0.000(4) -0.001(4) C18 0.047(4) 0.037(4) 0.057(4) 0.005(3) -0.002(3) 0.003(3) C19 0.048(4) 0.033(3) 0.045(4) 0.005(3) 0.000(3) -0.002(3) C20 0.063(5) 0.053(4) 0.050(4) 0.014(4) -0.001(4) -0.001(4) C21 0.038(3) 0.034(3) 0.027(3) -0.001(3) 0.010(3) -0.003(3) C22 0.039(4) 0.037(3) 0.031(3) -0.003(3) 0.005(3) -0.002(3) C23 0.052(4) 0.046(4) 0.045(4) 0.000(3) 0.021(3) -0.003(3) C24 0.053(5) 0.059(5) 0.068(5) -0.010(4) 0.033(4) -0.008(4) C25 0.047(4) 0.061(5) 0.062(5) -0.017(4) 0.019(4) 0.003(4) C26 0.040(4) 0.048(4) 0.053(4) -0.006(3) 0.006(3) 0.004(3) C27 0.042(4) 0.058(4) 0.038(4) 0.000(3) 0.004(3) -0.007(3) C28 0.059(5) 0.078(6) 0.044(4) -0.004(4) -0.001(4) -0.022(4) C29 0.078(6) 0.104(7) 0.040(4) -0.026(4) 0.004(4) -0.044(5) C30 0.064(5) 0.094(6) 0.038(4) -0.017(4) 0.008(4) -0.026(5) C31 0.038(3) 0.045(4) 0.028(3) -0.001(3) 0.005(3) -0.001(3) C32 0.039(4) 0.040(4) 0.033(3) 0.001(3) 0.002(3) -0.002(3) C33 0.047(4) 0.037(3) 0.030(3) 0.006(3) 0.011(3) 0.004(3) C34 0.055(5) 0.067(5) 0.049(4) -0.010(4) 0.023(4) -0.005(4) C35 0.040(4) 0.050(4) 0.032(3) 0.010(3) 0.007(3) 0.004(3) C36 0.058(5) 0.059(5) 0.061(5) 0.001(4) 0.023(4) 0.001(4) C37 0.049(5) 0.077(6) 0.086(6) 0.007(5) 0.022(4) -0.007(4) C38 0.050(5) 0.064(5) 0.073(6) 0.007(4) 0.007(4) -0.017(4) C39 0.057(5) 0.055(5) 0.049(4) 0.005(4) 0.007(4) -0.006(4) C40 0.054(4) 0.065(5) 0.040(4) 0.003(4) -0.006(3) 0.013(4) C41 0.057(5) 0.072(6) 0.044(4) 0.012(4) -0.012(4) 0.016(4) C42 0.054(4) 0.057(5) 0.059(5) 0.026(4) 0.010(4) 0.021(4) C43 0.045(4) 0.041(4) 0.047(4) 0.008(3) 0.009(3) 0.005(3) C44 0.041(4) 0.040(4) 0.035(3) 0.005(3) 0.013(3) 0.008(3) C45 0.032(3) 0.033(3) 0.033(3) 0.005(3) 0.009(3) 0.004(3) C46 0.044(4) 0.031(3) 0.040(4) -0.003(3) 0.013(3) 0.000(3) C47 0.063(5) 0.036(4) 0.062(5) -0.008(3) 0.001(4) -0.005(3) C48 0.041(4) 0.039(4) 0.033(3) -0.006(3) 0.012(3) -0.002(3) C49 0.066(5) 0.045(4) 0.048(4) -0.014(3) 0.011(4) -0.004(4) C50 0.070(5) 0.057(5) 0.035(4) -0.008(3) -0.002(4) -0.004(4) C51 0.071(5) 0.063(5) 0.041(4) -0.007(4) -0.006(4) 0.000(4) C52 0.075(5) 0.044(4) 0.043(4) -0.001(3) -0.004(4) 0.014(4) C53 0.065(5) 0.049(4) 0.042(4) 0.008(3) -0.006(4) 0.000(4) C54 0.069(5) 0.062(5) 0.046(4) 0.009(4) -0.002(4) 0.007(4) C55 0.062(5) 0.061(5) 0.054(5) 0.024(4) -0.007(4) 0.010(4) C56 0.051(4) 0.044(4) 0.050(4) 0.008(3) 0.005(3) 0.008(3) C57 0.040(4) 0.044(4) 0.039(4) 0.005(3) 0.007(3) 0.009(3) C58 0.040(4) 0.034(3) 0.037(3) 0.011(3) 0.005(3) 0.002(3) C59 0.069(5) 0.036(4) 0.051(4) -0.002(3) 0.006(4) 0.014(3) C60 0.037(3) 0.037(4) 0.031(3) -0.006(3) 0.009(3) -0.003(3) C61 0.036(3) 0.034(3) 0.033(3) -0.002(3) 0.006(3) -0.003(3) C62 0.048(4) 0.044(4) 0.040(4) -0.008(3) 0.005(3) 0.001(3) C63 0.054(4) 0.056(5) 0.042(4) -0.012(3) 0.006(3) -0.004(4) C64 0.061(5) 0.066(5) 0.032(4) -0.004(3) -0.011(3) -0.003(4) C65 0.053(4) 0.047(4) 0.040(4) 0.011(3) -0.003(3) 0.004(3) C66 0.054(4) 0.041(4) 0.049(4) 0.006(3) 0.009(3) 0.011(3) C67 0.058(5) 0.051(4) 0.052(4) -0.003(4) 0.019(4) 0.016(4) C68 0.058(5) 0.069(5) 0.048(4) -0.001(4) 0.025(4) 0.008(4) C69 0.063(5) 0.061(5) 0.038(4) 0.012(3) 0.020(3) 0.010(4) C70 0.050(4) 0.038(4) 0.034(3) 0.000(3) 0.009(3) 0.002(3) C71 0.062(4) 0.039(4) 0.034(4) 0.005(3) 0.014(3) 0.006(3) C72 0.084(6) 0.056(5) 0.053(5) 0.016(4) 0.030(4) 0.019(4) C73 0.045(4) 0.026(3) 0.032(3) 0.003(3) 0.001(3) 0.002(3) C74 0.048(4) 0.029(3) 0.031(3) -0.001(3) 0.001(3) 0.005(3) C75 0.050(4) 0.034(4) 0.043(4) 0.009(3) 0.002(3) 0.006(3) C76 0.059(5) 0.041(4) 0.061(5) 0.016(3) 0.005(4) 0.020(3) C77 0.054(4) 0.045(4) 0.059(5) 0.002(4) 0.005(4) 0.015(3) C78 0.052(4) 0.049(4) 0.041(4) 0.004(3) 0.012(3) 0.018(3) C81 0.188(17) 0.23(2) 0.178(16) 0.102(15) 0.039(13) -0.035(15) C82 0.070(7) 0.134(10) 0.080(7) 0.046(7) 0.004(5) -0.002(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 O5 2.165(4) . ? Mn1 O1 2.168(4) . ? Mn1 O6 2.189(4) . ? Mn1 N20 2.221(5) . ? Mn1 N24 2.230(5) . ? Mn1 N1 2.247(5) . ? Mn2 N6 2.173(5) . ? Mn2 N3 2.183(5) . ? Mn2 O1 2.186(4) . ? Mn2 O2 2.187(4) . ? Mn2 N4 2.295(5) . ? Mn2 N5 2.330(5) . ? Mn3 O4 2.151(4) . ? Mn3 O2 2.170(4) . ? Mn3 O3 2.177(4) . ? Mn3 N9 2.226(5) . ? Mn3 N8 2.236(5) . ? Mn3 N13 2.249(5) . ? Mn4 N11 2.171(5) . ? Mn4 N18 2.183(5) . ? Mn4 O5 2.191(4) . ? Mn4 O3 2.201(4) . ? Mn4 N17 2.301(5) . ? Mn4 N12 2.311(5) . ? Mn5 N22 2.173(5) . ? Mn5 N15 2.180(5) . ? Mn5 O6 2.189(4) . ? Mn5 O4 2.207(4) . ? Mn5 N21 2.290(5) . ? Mn5 N16 2.321(5) . ? Cl1 O10 1.391(7) . ? Cl1 O9 1.402(6) . ? Cl1 O8 1.414(6) . ? Cl1 O7 1.422(6) . ? Cl2 O13 1.271(12) . ? Cl2 O11 1.367(6) . ? Cl2 O14 1.373(8) . ? Cl2 O12 1.385(7) . ? Cl3 O18 1.262(15) . ? Cl3 O17 1.279(10) . ? Cl3 O16 1.309(10) . ? Cl3 O15 1.325(11) . ? Cl4 O20 1.353(7) . ? Cl4 O21 1.357(13) . ? Cl4 O22 1.376(7) . ? Cl4 O19 1.407(10) . ? O1 C6 1.297(7) . ? O2 C21 1.309(7) . ? O3 C32 1.301(7) . ? O4 C45 1.322(7) . ? O5 C60 1.302(7) . ? O6 C73 1.297(7) . ? O23 C79 1.447(19) . ? O24 C80 1.361(18) . ? N1 C5 1.340(8) . ? N1 C1 1.340(8) . ? N2 C6 1.291(7) . ? N2 N3 1.376(7) . ? N3 C7 1.279(8) . ? N4 C13 1.311(9) . ? N4 C9 1.365(8) . ? N5 C14 1.322(9) . ? N5 C18 1.357(9) . ? N6 C19 1.278(8) . ? N6 N7 1.398(7) . ? N7 C21 1.310(7) . ? N8 C22 1.335(8) . ? N8 C26 1.359(8) . ? N9 C31 1.328(8) . ? N9 C27 1.349(8) . ? N10 C32 1.296(8) . ? N10 N11 1.401(7) . ? N11 C33 1.279(8) . ? N12 C39 1.330(9) . ? N12 C35 1.359(8) . ? N13 C40 1.335(8) . ? N13 C44 1.336(8) . ? N14 C45 1.296(7) . ? N14 N15 1.383(7) . ? N15 C46 1.279(8) . ? N16 C52 1.309(8) . ? N16 C48 1.350(8) . ? N17 C53 1.334(8) . ? N17 C57 1.346(8) . ? N18 C58 1.279(7) . ? N18 N19 1.401(7) . ? N19 C60 1.310(8) . ? N20 C65 1.336(8) . ? N20 C61 1.345(8) . ? N21 C66 1.328(8) . ? N21 C70 1.359(8) . ? N22 C71 1.283(8) . ? N22 N23 1.410(7) . ? N23 C73 1.299(7) . ? N24 C78 1.331(8) . ? N24 C74 1.336(8) . ? N25 C82 1.121(13) . ? C1 C2 1.357(10) . ? C2 C3 1.380(10) . ? C3 C4 1.373(10) . ? C4 C5 1.380(9) . ? C5 C6 1.494(8) . ? C7 C9 1.490(10) . ? C7 C8 1.494(10) . ? C9 C10 1.388(10) . ? C10 C11 1.386(12) . ? C11 C12 1.341(12) . ? C12 C13 1.370(11) . ? C14 C15 1.367(10) . ? C15 C16 1.370(12) . ? C16 C17 1.372(11) . ? C17 C18 1.384(9) . ? C18 C19 1.490(9) . ? C19 C20 1.474(9) . ? C21 C22 1.485(8) . ? C22 C23 1.375(8) . ? C23 C24 1.382(10) . ? C24 C25 1.356(11) . ? C25 C26 1.378(10) . ? C27 C28 1.351(10) . ? C28 C29 1.369(11) . ? C29 C30 1.381(10) . ? C30 C31 1.387(9) . ? C31 C32 1.490(8) . ? C33 C35 1.470(9) . ? C33 C34 1.489(9) . ? C35 C36 1.365(9) . ? C36 C37 1.393(11) . ? C37 C38 1.377(12) . ? C38 C39 1.378(10) . ? C40 C41 1.393(10) . ? C41 C42 1.337(11) . ? C42 C43 1.380(10) . ? C43 C44 1.397(9) . ? C44 C45 1.467(8) . ? C46 C48 1.465(9) . ? C46 C47 1.500(9) . ? C48 C49 1.392(9) . ? C49 C50 1.375(10) . ? C50 C51 1.344(10) . ? C51 C52 1.404(10) . ? C53 C54 1.393(10) . ? C54 C55 1.363(11) . ? C55 C56 1.390(10) . ? C56 C57 1.391(9) . ? C57 C58 1.481(9) . ? C58 C59 1.494(9) . ? C60 C61 1.484(8) . ? C61 C62 1.379(8) . ? C62 C63 1.382(9) . ? C63 C64 1.357(10) . ? C64 C65 1.374(10) . ? C66 C67 1.378(9) . ? C67 C68 1.366(10) . ? C68 C69 1.381(10) . ? C69 C70 1.379(9) . ? C70 C71 1.478(9) . ? C71 C72 1.490(9) . ? C73 C74 1.496(8) . ? C74 C75 1.376(8) . ? C75 C76 1.370(9) . ? C76 C77 1.357(10) . ? C77 C78 1.378(9) . ? C81 C82 1.301(17) . ? 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 O5 Mn1 O1 97.11(15) . . ? O5 Mn1 O6 96.14(15) . . ? O1 Mn1 O6 97.53(15) . . ? O5 Mn1 N20 74.86(17) . . ? O1 Mn1 N20 170.17(17) . . ? O6 Mn1 N20 89.09(17) . . ? O5 Mn1 N24 168.29(17) . . ? O1 Mn1 N24 91.23(18) . . ? O6 Mn1 N24 74.55(17) . . ? N20 Mn1 N24 97.55(19) . . ? O5 Mn1 N1 95.85(17) . . ? O1 Mn1 N1 74.26(17) . . ? O6 Mn1 N1 166.23(17) . . ? N20 Mn1 N1 100.57(19) . . ? N24 Mn1 N1 94.30(19) . . ? N6 Mn2 N3 154.3(2) . . ? N6 Mn2 O1 126.08(17) . . ? N3 Mn2 O1 70.76(17) . . ? N6 Mn2 O2 71.91(17) . . ? N3 Mn2 O2 128.64(18) . . ? O1 Mn2 O2 99.11(15) . . ? N6 Mn2 N4 94.5(2) . . ? N3 Mn2 N4 71.2(2) . . ? O1 Mn2 N4 139.44(18) . . ? O2 Mn2 N4 93.66(17) . . ? N6 Mn2 N5 70.8(2) . . ? N3 Mn2 N5 90.9(2) . . ? O1 Mn2 N5 92.23(18) . . ? O2 Mn2 N5 140.46(18) . . ? N4 Mn2 N5 101.9(2) . . ? O4 Mn3 O2 95.55(15) . . ? O4 Mn3 O3 95.90(15) . . ? O2 Mn3 O3 97.96(15) . . ? O4 Mn3 N9 169.67(17) . . ? O2 Mn3 N9 90.73(17) . . ? O3 Mn3 N9 75.07(17) . . ? O4 Mn3 N8 91.04(16) . . ? O2 Mn3 N8 74.39(17) . . ? O3 Mn3 N8 170.18(17) . . ? N9 Mn3 N8 98.56(18) . . ? O4 Mn3 N13 74.99(17) . . ? O2 Mn3 N13 169.25(18) . . ? O3 Mn3 N13 88.23(17) . . ? N9 Mn3 N13 99.38(19) . . ? N8 Mn3 N13 100.31(19) . . ? N11 Mn4 N18 156.40(19) . . ? N11 Mn4 O5 125.17(17) . . ? N18 Mn4 O5 71.38(16) . . ? N11 Mn4 O3 71.42(17) . . ? N18 Mn4 O3 126.46(17) . . ? O5 Mn4 O3 98.68(15) . . ? N11 Mn4 N17 94.41(19) . . ? N18 Mn4 N17 70.46(19) . . ? O5 Mn4 N17 140.39(17) . . ? O3 Mn4 N17 95.40(18) . . ? N11 Mn4 N12 70.3(2) . . ? N18 Mn4 N12 94.42(19) . . ? O5 Mn4 N12 91.70(17) . . ? O3 Mn4 N12 139.04(17) . . ? N17 Mn4 N12 101.40(19) . . ? N22 Mn5 N15 150.16(19) . . ? N22 Mn5 O6 71.62(17) . . ? N15 Mn5 O6 129.72(17) . . ? N22 Mn5 O4 131.37(17) . . ? N15 Mn5 O4 71.20(17) . . ? O6 Mn5 O4 99.87(15) . . ? N22 Mn5 N21 70.65(19) . . ? N15 Mn5 N21 91.30(18) . . ? O6 Mn5 N21 138.98(17) . . ? O4 Mn5 N21 93.14(17) . . ? N22 Mn5 N16 89.10(19) . . ? N15 Mn5 N16 70.91(19) . . ? O6 Mn5 N16 93.44(17) . . ? O4 Mn5 N16 139.52(17) . . ? N21 Mn5 N16 101.44(18) . . ? O10 Cl1 O9 110.7(5) . . ? O10 Cl1 O8 108.6(4) . . ? O9 Cl1 O8 110.1(4) . . ? O10 Cl1 O7 111.5(5) . . ? O9 Cl1 O7 108.3(4) . . ? O8 Cl1 O7 107.7(4) . . ? O13 Cl2 O11 109.0(10) . . ? O13 Cl2 O14 111.9(10) . . ? O11 Cl2 O14 109.7(5) . . ? O13 Cl2 O12 108.5(10) . . ? O11 Cl2 O12 108.8(5) . . ? O14 Cl2 O12 109.0(6) . . ? O18 Cl3 O17 98.1(15) . . ? O18 Cl3 O16 105.1(13) . . ? O17 Cl3 O16 114.6(9) . . ? O18 Cl3 O15 99.4(12) . . ? O17 Cl3 O15 115.1(9) . . ? O16 Cl3 O15 119.8(8) . . ? O20 Cl4 O21 103.5(7) . . ? O20 Cl4 O22 115.2(6) . . ? O21 Cl4 O22 112.0(8) . . ? O20 Cl4 O19 106.3(7) . . ? O21 Cl4 O19 111.7(9) . . ? O22 Cl4 O19 108.0(6) . . ? C6 O1 Mn1 118.1(4) . . ? C6 O1 Mn2 111.1(3) . . ? Mn1 O1 Mn2 126.92(18) . . ? C21 O2 Mn3 116.9(4) . . ? C21 O2 Mn2 112.2(3) . . ? Mn3 O2 Mn2 129.66(18) . . ? C32 O3 Mn3 116.2(4) . . ? C32 O3 Mn4 111.8(4) . . ? Mn3 O3 Mn4 131.51(18) . . ? C45 O4 Mn3 117.1(4) . . ? C45 O4 Mn5 112.1(3) . . ? Mn3 O4 Mn5 129.41(18) . . ? C60 O5 Mn1 116.9(4) . . ? C60 O5 Mn4 113.2(4) . . ? Mn1 O5 Mn4 127.67(18) . . ? C73 O6 Mn1 116.9(4) . . ? C73 O6 Mn5 112.0(4) . . ? Mn1 O6 Mn5 128.40(18) . . ? C5 N1 C1 118.1(5) . . ? C5 N1 Mn1 114.8(4) . . ? C1 N1 Mn1 127.0(4) . . ? C6 N2 N3 109.2(5) . . ? C7 N3 N2 118.9(5) . . ? C7 N3 Mn2 123.3(5) . . ? N2 N3 Mn2 117.1(4) . . ? C13 N4 C9 117.0(6) . . ? C13 N4 Mn2 127.6(5) . . ? C9 N4 Mn2 115.3(4) . . ? C14 N5 C18 118.3(6) . . ? C14 N5 Mn2 126.9(5) . . ? C18 N5 Mn2 113.8(4) . . ? C19 N6 N7 117.7(5) . . ? C19 N6 Mn2 124.5(5) . . ? N7 N6 Mn2 117.8(4) . . ? C21 N7 N6 109.6(5) . . ? C22 N8 C26 118.6(5) . . ? C22 N8 Mn3 114.4(4) . . ? C26 N8 Mn3 126.1(4) . . ? C31 N9 C27 118.1(5) . . ? C31 N9 Mn3 114.5(4) . . ? C27 N9 Mn3 127.3(4) . . ? C32 N10 N11 109.6(5) . . ? C33 N11 N10 118.3(5) . . ? C33 N11 Mn4 124.3(4) . . ? N10 N11 Mn4 117.3(4) . . ? C39 N12 C35 117.9(6) . . ? C39 N12 Mn4 126.5(5) . . ? C35 N12 Mn4 115.5(4) . . ? C40 N13 C44 119.4(6) . . ? C40 N13 Mn3 126.8(5) . . ? C44 N13 Mn3 113.3(4) . . ? C45 N14 N15 110.0(5) . . ? C46 N15 N14 118.9(5) . . ? C46 N15 Mn5 121.9(4) . . ? N14 N15 Mn5 118.9(4) . . ? C52 N16 C48 118.6(6) . . ? C52 N16 Mn5 126.8(5) . . ? C48 N16 Mn5 113.7(4) . . ? C53 N17 C57 117.8(6) . . ? C53 N17 Mn4 126.4(5) . . ? C57 N17 Mn4 115.9(4) . . ? C58 N18 N19 118.3(5) . . ? C58 N18 Mn4 123.8(4) . . ? N19 N18 Mn4 117.9(3) . . ? C60 N19 N18 109.6(5) . . ? C65 N20 C61 118.0(5) . . ? C65 N20 Mn1 126.7(4) . . ? C61 N20 Mn1 114.8(4) . . ? C66 N21 C70 117.2(5) . . ? C66 N21 Mn5 127.1(4) . . ? C70 N21 Mn5 115.3(4) . . ? C71 N22 N23 118.9(5) . . ? C71 N22 Mn5 123.4(4) . . ? N23 N22 Mn5 117.1(4) . . ? C73 N23 N22 109.0(5) . . ? C78 N24 C74 119.1(5) . . ? C78 N24 Mn1 125.5(4) . . ? C74 N24 Mn1 115.3(4) . . ? N1 C1 C2 122.7(6) . . ? C1 C2 C3 119.4(7) . . ? C4 C3 C2 118.6(6) . . ? C3 C4 C5 119.1(6) . . ? N1 C5 C4 122.1(6) . . ? N1 C5 C6 115.4(5) . . ? C4 C5 C6 122.5(6) . . ? N2 C6 O1 126.5(6) . . ? N2 C6 C5 116.1(5) . . ? O1 C6 C5 117.3(5) . . ? N3 C7 C9 114.4(6) . . ? N3 C7 C8 123.3(7) . . ? C9 C7 C8 122.3(6) . . ? N4 C9 C10 121.5(7) . . ? N4 C9 C7 115.6(6) . . ? C10 C9 C7 122.9(7) . . ? C11 C10 C9 118.3(8) . . ? C12 C11 C10 119.8(8) . . ? C11 C12 C13 118.7(8) . . ? N4 C13 C12 124.6(7) . . ? N5 C14 C15 123.1(7) . . ? C14 C15 C16 119.2(7) . . ? C15 C16 C17 118.8(7) . . ? C16 C17 C18 119.4(7) . . ? N5 C18 C17 121.1(7) . . ? N5 C18 C19 116.4(6) . . ? C17 C18 C19 122.5(7) . . ? N6 C19 C20 126.1(6) . . ? N6 C19 C18 113.6(6) . . ? C20 C19 C18 120.3(6) . . ? N7 C21 O2 125.8(5) . . ? N7 C21 C22 116.8(5) . . ? O2 C21 C22 117.4(5) . . ? N8 C22 C23 121.7(6) . . ? N8 C22 C21 115.5(5) . . ? C23 C22 C21 122.8(6) . . ? C22 C23 C24 119.5(7) . . ? C25 C24 C23 119.1(7) . . ? C24 C25 C26 119.5(7) . . ? N8 C26 C25 121.6(7) . . ? N9 C27 C28 123.7(6) . . ? C27 C28 C29 118.1(7) . . ? C28 C29 C30 120.0(7) . . ? C29 C30 C31 118.4(7) . . ? N9 C31 C30 121.8(6) . . ? N9 C31 C32 116.1(5) . . ? C30 C31 C32 122.1(6) . . ? N10 C32 O3 126.4(6) . . ? N10 C32 C31 115.9(5) . . ? O3 C32 C31 117.6(5) . . ? N11 C33 C35 114.4(6) . . ? N11 C33 C34 124.1(6) . . ? C35 C33 C34 121.5(6) . . ? N12 C35 C36 121.6(6) . . ? N12 C35 C33 115.4(5) . . ? C36 C35 C33 123.0(6) . . ? C35 C36 C37 119.2(7) . . ? C38 C37 C36 119.8(7) . . ? C37 C38 C39 117.2(7) . . ? N12 C39 C38 124.3(7) . . ? N13 C40 C41 121.4(7) . . ? C42 C41 C40 119.9(6) . . ? C41 C42 C43 119.4(6) . . ? C42 C43 C44 119.0(7) . . ? N13 C44 C43 120.9(6) . . ? N13 C44 C45 117.1(5) . . ? C43 C44 C45 122.0(6) . . ? N14 C45 O4 125.9(5) . . ? N14 C45 C44 116.9(5) . . ? O4 C45 C44 117.2(5) . . ? N15 C46 C48 115.9(5) . . ? N15 C46 C47 123.9(6) . . ? C48 C46 C47 120.3(6) . . ? N16 C48 C49 121.1(6) . . ? N16 C48 C46 115.7(5) . . ? C49 C48 C46 123.2(6) . . ? C50 C49 C48 119.1(6) . . ? C51 C50 C49 119.7(7) . . ? C50 C51 C52 118.5(7) . . ? N16 C52 C51 122.9(7) . . ? N17 C53 C54 124.0(7) . . ? C55 C54 C53 117.5(7) . . ? C54 C55 C56 120.1(7) . . ? C55 C56 C57 118.6(7) . . ? N17 C57 C56 122.0(6) . . ? N17 C57 C58 115.8(5) . . ? C56 C57 C58 122.2(6) . . ? N18 C58 C57 114.1(6) . . ? N18 C58 C59 125.1(6) . . ? C57 C58 C59 120.8(5) . . ? O5 C60 N19 125.6(5) . . ? O5 C60 C61 117.9(5) . . ? N19 C60 C61 116.5(5) . . ? N20 C61 C62 121.9(6) . . ? N20 C61 C60 115.0(5) . . ? C62 C61 C60 123.1(6) . . ? C61 C62 C63 118.9(6) . . ? C64 C63 C62 119.4(6) . . ? C63 C64 C65 119.0(6) . . ? N20 C65 C64 122.8(6) . . ? N21 C66 C67 124.7(6) . . ? C68 C67 C66 117.7(7) . . ? C67 C68 C69 119.3(6) . . ? C70 C69 C68 119.8(6) . . ? N21 C70 C69 121.3(6) . . ? N21 C70 C71 115.4(5) . . ? C69 C70 C71 123.2(6) . . ? N22 C71 C70 114.0(6) . . ? N22 C71 C72 125.5(6) . . ? C70 C71 C72 120.5(6) . . ? O6 C73 N23 126.8(6) . . ? O6 C73 C74 117.8(5) . . ? N23 C73 C74 115.3(5) . . ? N24 C74 C75 121.3(6) . . ? N24 C74 C73 115.5(5) . . ? C75 C74 C73 123.3(6) . . ? C76 C75 C74 119.4(6) . . ? C77 C76 C75 119.1(6) . . ? C76 C77 C78 119.3(6) . . ? N24 C78 C77 121.7(6) . . ? N25 C82 C81 177.8(18) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.619 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.149 #===END data_shelxl(6) _database_code_depnum_ccdc_archive 'CCDC 299033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H74 Cl4 N42 Mn5 O29 ' _chemical_formula_weight 2264.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.8375(19) _cell_length_b 23.483(3) _cell_length_c 23.610(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.970(3) _cell_angle_gamma 90.00 _cell_volume 9266.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 22446 _cell_measurement_theta_min 1.7378 _cell_measurement_theta_max 27.3794 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4612 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6677 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 32353 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.38 _reflns_number_total 16107 _reflns_number_gt 13249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_publication_material 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.1745P)^2^+25.0992P] 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 16107 _refine_ls_number_parameters 1222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.2906 _refine_ls_wR_factor_gt 0.2731 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.38329(5) 0.29245(3) 0.15150(3) 0.0382(2) Uani 1 1 d . . . Mn2 Mn 0.47942(5) 0.12440(4) 0.24734(3) 0.0400(2) Uani 1 1 d . . . Mn3 Mn 0.35079(5) 0.24152(3) 0.30649(4) 0.0406(2) Uani 1 1 d . . . Mn4 Mn 0.60818(5) 0.24417(3) 0.18715(4) 0.0402(2) Uani 1 1 d . . . Mn5 Mn 0.57195(5) 0.29881(3) 0.33875(4) 0.0426(2) Uani 1 1 d . . . Cl1 Cl 0.22532(10) 0.00598(8) 0.98160(7) 0.0613(4) Uani 1 1 d . . . Cl2 Cl 0.05091(11) 0.11876(9) 0.32041(9) 0.0705(5) Uani 1 1 d . . . Cl3 Cl 0.23774(10) 0.98927(7) 0.49928(7) 0.0546(4) Uani 1 1 d . . . Cl4 Cl 0.1669(2) 0.74535(15) 0.95218(16) 0.1179(10) Uiso 1 1 d . . . O1 O 0.3749(2) 0.17634(16) 0.24424(16) 0.0402(8) Uani 1 1 d . . . O2 O 0.4839(2) 0.23509(16) 0.14554(16) 0.0411(8) Uani 1 1 d . . . O3 O 0.5816(2) 0.30956(15) 0.24786(16) 0.0429(9) Uani 1 1 d . . . O4 O 0.3727(2) 0.30499(15) 0.24251(16) 0.0417(9) Uani 1 1 d . . . O5 O 0.5834(2) 0.17853(16) 0.24916(16) 0.0406(8) Uani 1 1 d . . . O6 O 0.4763(2) 0.23818(16) 0.34611(16) 0.0412(8) Uani 1 1 d . . . O7 O 0.2833(6) -0.0328(3) 1.0027(3) 0.141(4) Uani 1 1 d . . . O8 O 0.1831(4) 0.0207(4) 1.0275(3) 0.122(3) Uani 1 1 d . . . O9 O 0.1775(5) -0.0183(6) 0.9362(4) 0.172(5) Uani 1 1 d . . . O10 O 0.2592(8) 0.0538(3) 0.9633(4) 0.170(5) Uani 1 1 d . . . O11 O 0.1313(4) 0.1172(4) 0.3139(4) 0.119(3) Uani 1 1 d . . . O12 O 0.0320(4) 0.0933(2) 0.3707(2) 0.0745(15) Uani 1 1 d . . . O13 O 0.0170(4) 0.1732(3) 0.3139(4) 0.113(3) Uani 1 1 d . . . O14 O 0.0082(6) 0.0850(5) 0.2735(4) 0.138(3) Uani 1 1 d . . . O15 O 0.3167(3) 1.0127(2) 0.5050(2) 0.0710(14) Uani 1 1 d . . . O16 O 0.1842(5) 1.0324(3) 0.4798(4) 0.123(3) Uani 1 1 d . . . O17 O 0.2204(4) 0.9712(4) 0.5534(3) 0.105(2) Uani 1 1 d . . . O18 O 0.2329(4) 0.9428(3) 0.4624(3) 0.0930(19) Uani 1 1 d . . . O19 O 0.1804(10) 0.7464(6) 0.8963(7) 0.223(6) Uiso 1 1 d . . . O20 O 0.0985(7) 0.7453(4) 0.9803(5) 0.151(3) Uiso 1 1 d . . . O21 O 0.1947(18) 0.8091(13) 0.9690(12) 0.377(13) Uiso 1 1 d . . . O22 O 0.2559(13) 0.7380(9) 0.9950(8) 0.289(10) Uiso 1 1 d . . . O23 O 0.1478(17) 0.9019(11) 0.8272(11) 0.185(9) Uiso 0.50 1 d P . . O24 O 0.0916(11) 0.8721(8) 0.8385(8) 0.122(5) Uiso 0.50 1 d P . . O25 O 0.0498(6) 0.8124(4) 0.8423(4) 0.065(2) Uiso 0.50 1 d P . . O26 O 0.0395(13) 0.7494(9) 0.8079(9) 0.151(7) Uiso 0.50 1 d P . . O27 O 0.0235(11) 0.7066(9) 0.7583(7) 0.128(6) Uiso 0.50 1 d P . . O28 O -0.0644(12) 0.7316(8) 0.6151(8) 0.134(6) Uiso 0.50 1 d P . . O29 O -0.0621(12) 0.6089(9) 0.7065(9) 0.272(8) Uiso 1 1 d . . . O30 O 0.0928(19) 0.6381(14) 0.8327(13) 0.209(11) Uiso 0.50 1 d P . . O31 O 0.1441(19) 0.5987(13) 0.8166(13) 0.205(11) Uiso 0.50 1 d P . . O32 O 0.0436(14) 0.3595(11) 0.3309(11) 0.165(8) Uiso 0.50 1 d P . . O33 O 0.1268(9) 0.2562(6) 0.4380(7) 0.205(5) Uiso 1 1 d . . . O34 O 0.197(2) 0.0014(13) 0.7776(14) 0.235(13) Uiso 0.50 1 d P . . N1 N 0.1128(3) 0.2086(3) 0.2143(3) 0.0645(16) Uani 1 1 d . . . H4 H 0.0609 0.2127 0.2047 0.077 Uiso 1 1 calc R . . N2 N 0.2330(3) 0.2228(2) 0.2587(2) 0.0490(12) Uani 1 1 d . . . N3 N 0.3166(3) 0.1133(2) 0.1761(2) 0.0469(11) Uani 1 1 d . . . N4 N 0.3957(3) 0.0946(2) 0.1783(2) 0.0458(11) Uani 1 1 d . . . N5 N 0.3551(4) 0.0350(3) 0.1014(3) 0.0743(18) Uani 1 1 d . . . H6 H 0.3052 0.0468 0.0991 0.089 Uiso 1 1 calc R . . H7 H 0.3687 0.0091 0.0774 0.089 Uiso 1 1 calc R . . N6 N 0.5113(4) -0.0005(2) 0.1059(3) 0.0660(16) Uani 1 1 d . . . N7 N 0.5435(3) 0.0579(2) 0.1879(2) 0.0559(13) Uani 1 1 d . . . N8 N 0.6345(4) 0.1197(2) 0.0529(2) 0.0577(14) Uani 1 1 d . . . H14 H 0.6588 0.0953 0.0325 0.069 Uiso 1 1 calc R . . N9 N 0.6168(3) 0.1836(2) 0.1174(2) 0.0466(11) Uani 1 1 d . . . N10 N 0.4037(3) 0.18959(19) 0.0721(2) 0.0439(11) Uani 1 1 d . . . N11 N 0.3460(3) 0.22454(19) 0.09091(19) 0.0403(10) Uani 1 1 d . . . N12 N 0.2485(3) 0.1750(2) 0.0309(2) 0.0538(13) Uani 1 1 d . . . H16 H 0.2836 0.1515 0.0190 0.065 Uiso 1 1 calc R . . H17 H 0.1974 0.1719 0.0180 0.065 Uiso 1 1 calc R . . N13 N 0.1375(3) 0.2490(2) 0.0649(2) 0.0514(12) Uani 1 1 d . . . N14 N 0.2414(3) 0.2953(2) 0.1260(2) 0.0463(11) Uani 1 1 d . . . N15 N 0.6530(4) 0.4018(2) 0.0968(3) 0.0660(16) Uani 1 1 d . . . H24 H 0.6659 0.4236 0.0690 0.079 Uiso 1 1 calc R . . N16 N 0.6310(3) 0.3246(2) 0.1441(2) 0.0450(11) Uani 1 1 d . . . N17 N 0.5814(4) 0.4065(2) 0.2647(2) 0.0538(13) Uani 1 1 d . . . N18 N 0.5611(3) 0.3882(2) 0.3173(2) 0.0486(12) Uani 1 1 d . . . N19 N 0.5331(8) 0.4827(3) 0.3381(4) 0.129(4) Uani 1 1 d . . . H26 H 0.5430 0.4951 0.3045 0.155 Uiso 1 1 calc R . . H27 H 0.5185 0.5067 0.3635 0.155 Uiso 1 1 calc R . . N20 N 0.4973(5) 0.4455(3) 0.4424(3) 0.083(2) Uani 1 1 d . . . N21 N 0.5313(3) 0.3511(2) 0.4174(2) 0.0508(12) Uani 1 1 d . . . N22 N 0.3057(5) 0.4014(3) 0.3927(2) 0.0727(18) Uani 1 1 d . . . H34 H 0.2944 0.4239 0.4204 0.087 Uiso 1 1 calc R . . N23 N 0.3275(3) 0.3233(2) 0.3474(2) 0.0462(11) Uani 1 1 d . . . N24 N 0.3685(3) 0.4017(2) 0.2221(2) 0.0481(12) Uani 1 1 d . . . N25 N 0.3910(3) 0.38186(18) 0.1704(2) 0.0421(10) Uani 1 1 d . . . N26 N 0.4141(5) 0.4767(2) 0.1475(3) 0.0734(19) Uani 1 1 d . . . H36 H 0.4013 0.4893 0.1803 0.088 Uiso 1 1 calc R . . H37 H 0.4287 0.5008 0.1222 0.088 Uiso 1 1 calc R . . N27 N 0.4624(4) 0.4384(2) 0.0473(2) 0.0604(14) Uani 1 1 d . . . N28 N 0.4231(3) 0.3449(2) 0.07105(19) 0.0429(10) Uani 1 1 d . . . N29 N 0.8472(3) 0.2061(2) 0.2733(2) 0.0537(13) Uani 1 1 d . . . H44 H 0.8996 0.2082 0.2807 0.064 Uiso 1 1 calc R . . N30 N 0.7260(3) 0.2246(2) 0.2337(2) 0.0449(11) Uani 1 1 d . . . N31 N 0.6425(3) 0.1157(2) 0.3181(2) 0.0434(11) Uani 1 1 d . . . N32 N 0.5635(3) 0.09599(19) 0.3157(2) 0.0418(10) Uani 1 1 d . . . N33 N 0.6072(4) 0.0343(3) 0.3906(3) 0.0712(17) Uani 1 1 d . . . H46 H 0.6569 0.0467 0.3937 0.085 Uiso 1 1 calc R . . H47 H 0.5938 0.0072 0.4135 0.085 Uiso 1 1 calc R . . N34 N 0.4171(3) 0.0563(2) 0.3077(2) 0.0482(11) Uani 1 1 d . . . N35 N 0.4545(3) -0.0051(2) 0.3867(2) 0.0517(12) Uani 1 1 d . . . N36 N 0.3418(3) 0.1140(2) 0.4400(2) 0.0511(12) Uani 1 1 d . . . H54 H 0.3206 0.0879 0.4603 0.061 Uiso 1 1 calc R . . N37 N 0.3502(3) 0.1797(2) 0.3764(2) 0.0445(11) Uani 1 1 d . . . N38 N 0.5630(3) 0.1956(2) 0.4186(2) 0.0441(11) Uani 1 1 d . . . N39 N 0.6169(3) 0.2329(2) 0.3985(2) 0.0430(10) Uani 1 1 d . . . N40 N 0.7192(4) 0.1855(3) 0.4569(2) 0.0607(14) Uani 1 1 d . . . H56 H 0.6859 0.1613 0.4700 0.073 Uiso 1 1 calc R . . H57 H 0.7707 0.1834 0.4686 0.073 Uiso 1 1 calc R . . N41 N 0.7157(3) 0.3063(2) 0.3620(2) 0.0514(12) Uani 1 1 d . . . N42 N 0.8252(3) 0.2593(3) 0.4164(3) 0.0619(15) Uani 1 1 d . . . C1 C 0.1285(4) 0.1293(3) 0.1456(3) 0.068(2) Uani 1 1 d . . . H1 H 0.1700 0.1208 0.1211 0.081 Uiso 1 1 calc R . . H2 H 0.0819 0.1460 0.1225 0.081 Uiso 1 1 calc R . . H3 H 0.1125 0.0942 0.1635 0.081 Uiso 1 1 calc R . . C2 C 0.1604(4) 0.1704(3) 0.1905(3) 0.0564(16) Uani 1 1 d . . . C3 C 0.1574(4) 0.2387(3) 0.2545(3) 0.0632(19) Uani 1 1 d . . . H5 H 0.1372 0.2675 0.2771 0.076 Uiso 1 1 calc R . . C4 C 0.2353(3) 0.1801(3) 0.2180(3) 0.0455(13) Uani 1 1 d . . . C5 C 0.3132(3) 0.1548(2) 0.2119(2) 0.0425(12) Uani 1 1 d . . . C6 C 0.4101(4) 0.0564(3) 0.1412(3) 0.0514(14) Uani 1 1 d . . . C7 C 0.4926(4) 0.0362(3) 0.1447(3) 0.0522(15) Uani 1 1 d . . . C8 C 0.5887(6) -0.0159(3) 0.1099(3) 0.072(2) Uani 1 1 d . . . H8 H 0.6045 -0.0415 0.0822 0.086 Uiso 1 1 calc R . . C9 C 0.6453(6) 0.0032(3) 0.1513(4) 0.076(2) Uani 1 1 d . . . H9 H 0.6998 -0.0081 0.1532 0.091 Uiso 1 1 calc R . . C10 C 0.6186(5) 0.0408(3) 0.1910(4) 0.071(2) Uani 1 1 d . . . H10 H 0.6559 0.0544 0.2214 0.085 Uiso 1 1 calc R . . C11 C 0.4981(5) 0.1016(3) 0.0013(3) 0.0661(19) Uani 1 1 d . . . H11 H 0.4455 0.0977 0.0148 0.079 Uiso 1 1 calc R . . H12 H 0.5189 0.0638 -0.0064 0.079 Uiso 1 1 calc R . . H13 H 0.4928 0.1243 -0.0337 0.079 Uiso 1 1 calc R . . C12 C 0.5547(4) 0.1307(3) 0.0463(3) 0.0492(14) Uani 1 1 d . . . C13 C 0.6711(4) 0.1525(3) 0.0961(3) 0.0548(15) Uani 1 1 d . . . H15 H 0.7268 0.1528 0.1087 0.066 Uiso 1 1 calc R . . C14 C 0.5438(4) 0.1707(2) 0.0869(2) 0.0430(12) Uani 1 1 d . . . C15 C 0.4729(4) 0.1997(2) 0.1024(2) 0.0418(12) Uani 1 1 d . . . C16 C 0.2728(4) 0.2157(2) 0.0688(2) 0.0424(12) Uani 1 1 d . . . C17 C 0.2125(4) 0.2555(2) 0.0873(2) 0.0423(12) Uani 1 1 d . . . C18 C 0.1874(4) 0.3309(3) 0.1428(3) 0.0531(15) Uani 1 1 d . . . H18 H 0.2043 0.3596 0.1700 0.064 Uiso 1 1 calc R . . C19 C 0.1083(4) 0.3273(3) 0.1219(3) 0.0619(17) Uani 1 1 d . . . H19 H 0.0703 0.3530 0.1341 0.074 Uiso 1 1 calc R . . C20 C 0.0853(4) 0.2855(3) 0.0829(3) 0.0602(17) Uani 1 1 d . . . H20 H 0.0304 0.2824 0.0682 0.072 Uiso 1 1 calc R . . C21 C 0.6280(8) 0.4819(3) 0.1604(5) 0.108(4) Uani 1 1 d . . . H21 H 0.5857 0.4892 0.1846 0.129 Uiso 1 1 calc R . . H22 H 0.6172 0.5038 0.1250 0.129 Uiso 1 1 calc R . . H23 H 0.6798 0.4934 0.1807 0.129 Uiso 1 1 calc R . . C22 C 0.6300(5) 0.4207(3) 0.1469(3) 0.0636(19) Uani 1 1 d . . . C23 C 0.6529(4) 0.3440(3) 0.0964(3) 0.0562(16) Uani 1 1 d . . . H25 H 0.6668 0.3210 0.0660 0.067 Uiso 1 1 calc R . . C24 C 0.6160(4) 0.3719(2) 0.1766(3) 0.0458(13) Uani 1 1 d . . . C25 C 0.5910(4) 0.3626(2) 0.2332(3) 0.0451(13) Uani 1 1 d . . . C26 C 0.5404(5) 0.4271(3) 0.3506(3) 0.0637(19) Uani 1 1 d . . . C27 C 0.5217(4) 0.4075(3) 0.4072(3) 0.0584(17) Uani 1 1 d . . . C28 C 0.4801(6) 0.4261(3) 0.4925(3) 0.078(2) Uani 1 1 d . . . H28 H 0.4636 0.4525 0.5193 0.094 Uiso 1 1 calc R . . C29 C 0.4854(5) 0.3693(3) 0.5069(3) 0.0618(17) Uani 1 1 d . . . H29 H 0.4711 0.3557 0.5422 0.074 Uiso 1 1 calc R . . C30 C 0.5127(4) 0.3327(3) 0.4670(3) 0.0579(16) Uani 1 1 d . . . H30 H 0.5182 0.2933 0.4758 0.070 Uiso 1 1 calc R . . C31 C 0.3217(8) 0.4792(3) 0.3239(4) 0.105(4) Uani 1 1 d . . . H31 H 0.3596 0.4854 0.2961 0.126 Uiso 1 1 calc R . . H32 H 0.3377 0.5022 0.3580 0.126 Uiso 1 1 calc R . . H33 H 0.2679 0.4904 0.3071 0.126 Uiso 1 1 calc R . . C32 C 0.3217(5) 0.4190(3) 0.3396(3) 0.0634(18) Uani 1 1 d . . . C33 C 0.3103(4) 0.3444(3) 0.3955(3) 0.0557(16) Uani 1 1 d . . . H35 H 0.3022 0.3224 0.4281 0.067 Uiso 1 1 calc R . . C34 C 0.3368(4) 0.3696(2) 0.3122(3) 0.0462(13) Uani 1 1 d . . . C35 C 0.3612(4) 0.3584(2) 0.2556(2) 0.0418(12) Uani 1 1 d . . . C36 C 0.4116(4) 0.4210(2) 0.1363(3) 0.0476(14) Uani 1 1 d . . . C37 C 0.4336(4) 0.4006(2) 0.0815(3) 0.0475(13) Uani 1 1 d . . . C38 C 0.4426(4) 0.3257(3) 0.0212(3) 0.0513(14) Uani 1 1 d . . . H38 H 0.4361 0.2864 0.0122 0.062 Uiso 1 1 calc R . . C39 C 0.4720(4) 0.3619(3) -0.0175(3) 0.0562(16) Uani 1 1 d . . . H39 H 0.4851 0.3482 -0.0531 0.067 Uiso 1 1 calc R . . C40 C 0.4818(5) 0.4187(3) -0.0028(3) 0.0617(17) Uani 1 1 d . . . H40 H 0.5027 0.4443 -0.0284 0.074 Uiso 1 1 calc R . . C41 C 0.8301(4) 0.1290(3) 0.3455(3) 0.0588(16) Uani 1 1 d . . . H41 H 0.7899 0.1231 0.3716 0.071 Uiso 1 1 calc R . . H42 H 0.8789 0.1446 0.3667 0.071 Uiso 1 1 calc R . . H43 H 0.8422 0.0926 0.3282 0.071 Uiso 1 1 calc R . . C42 C 0.7985(3) 0.1698(2) 0.3000(3) 0.0442(13) Uani 1 1 d . . . C43 C 0.8015(4) 0.2376(3) 0.2344(3) 0.0524(15) Uani 1 1 d . . . H45 H 0.8215 0.2656 0.2107 0.063 Uiso 1 1 calc R . . C44 C 0.7232(3) 0.1817(2) 0.2746(2) 0.0395(11) Uani 1 1 d . . . C45 C 0.6453(3) 0.1573(2) 0.2816(2) 0.0394(12) Uani 1 1 d . . . C46 C 0.5525(4) 0.0565(2) 0.3516(3) 0.0466(13) Uani 1 1 d . . . C47 C 0.4692(4) 0.0341(2) 0.3483(3) 0.0457(13) Uani 1 1 d . . . C48 C 0.3784(5) -0.0225(3) 0.3834(3) 0.0597(17) Uani 1 1 d . . . H48 H 0.3644 -0.0502 0.4097 0.072 Uiso 1 1 calc R . . C49 C 0.3200(4) -0.0018(3) 0.3434(3) 0.0607(17) Uani 1 1 d . . . H49 H 0.2662 -0.0144 0.3419 0.073 Uiso 1 1 calc R . . C50 C 0.3416(4) 0.0373(3) 0.3062(3) 0.0591(16) Uani 1 1 d . . . H50 H 0.3019 0.0520 0.2779 0.071 Uiso 1 1 calc R . . C51 C 0.4801(4) 0.1022(3) 0.4902(3) 0.0590(17) Uani 1 1 d . . . H51 H 0.4841 0.1250 0.5252 0.071 Uiso 1 1 calc R . . H52 H 0.5323 0.1011 0.4759 0.071 Uiso 1 1 calc R . . H53 H 0.4634 0.0634 0.4984 0.071 Uiso 1 1 calc R . . C52 C 0.4199(4) 0.1284(2) 0.4463(2) 0.0436(13) Uani 1 1 d . . . C53 C 0.3007(4) 0.1451(3) 0.3985(3) 0.0504(14) Uani 1 1 d . . . H55 H 0.2448 0.1426 0.3870 0.060 Uiso 1 1 calc R . . C54 C 0.4250(4) 0.1701(2) 0.4052(2) 0.0409(12) Uani 1 1 d . . . C55 C 0.4918(4) 0.2028(2) 0.3893(2) 0.0394(12) Uani 1 1 d . . . C56 C 0.6912(4) 0.2259(2) 0.4187(2) 0.0467(13) Uani 1 1 d . . . C57 C 0.7483(4) 0.2665(3) 0.3980(3) 0.0505(14) Uani 1 1 d . . . C58 C 0.8738(5) 0.2969(3) 0.3954(4) 0.074(2) Uani 1 1 d . . . H58 H 0.9297 0.2940 0.4068 0.089 Uiso 1 1 calc R . . C59 C 0.8471(5) 0.3390(4) 0.3587(4) 0.076(2) Uani 1 1 d . . . H59 H 0.8833 0.3650 0.3447 0.091 Uiso 1 1 calc R . . C60 C 0.7665(4) 0.3430(3) 0.3424(3) 0.0666(19) Uani 1 1 d . . . H60 H 0.7464 0.3722 0.3167 0.080 Uiso 1 1 calc R . . 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 0.0463(5) 0.0312(4) 0.0382(4) 0.0008(3) 0.0091(3) 0.0027(3) Mn2 0.0426(5) 0.0355(4) 0.0423(5) 0.0000(3) 0.0073(4) 0.0015(3) Mn3 0.0500(5) 0.0339(4) 0.0394(5) 0.0055(3) 0.0112(4) 0.0046(3) Mn4 0.0465(5) 0.0332(4) 0.0416(5) 0.0009(3) 0.0074(4) 0.0029(3) Mn5 0.0509(5) 0.0361(4) 0.0423(5) 0.0020(4) 0.0113(4) -0.0031(3) Cl1 0.0601(10) 0.0764(11) 0.0495(8) 0.0010(8) 0.0151(7) 0.0085(8) Cl2 0.0532(9) 0.0778(12) 0.0825(12) 0.0340(10) 0.0168(8) 0.0058(8) Cl3 0.0630(9) 0.0494(8) 0.0518(8) 0.0012(7) 0.0089(7) -0.0048(7) O1 0.040(2) 0.0371(19) 0.043(2) -0.0005(16) 0.0039(16) 0.0024(15) O2 0.048(2) 0.0364(19) 0.040(2) -0.0049(16) 0.0074(16) 0.0061(16) O3 0.061(2) 0.0324(18) 0.0378(19) 0.0007(16) 0.0139(17) -0.0039(17) O4 0.058(2) 0.0304(18) 0.0385(19) 0.0023(16) 0.0123(17) 0.0047(16) O5 0.041(2) 0.0381(19) 0.042(2) 0.0044(16) 0.0028(16) 0.0010(15) O6 0.046(2) 0.0372(19) 0.041(2) 0.0042(16) 0.0077(16) -0.0032(16) O7 0.211(9) 0.116(6) 0.083(4) -0.040(4) -0.034(5) 0.097(6) O8 0.083(4) 0.210(9) 0.079(4) -0.023(5) 0.036(3) 0.003(5) O9 0.109(6) 0.311(15) 0.091(5) -0.067(7) -0.006(5) -0.036(8) O10 0.345(16) 0.070(4) 0.120(6) 0.010(4) 0.133(9) -0.015(7) O11 0.054(3) 0.149(7) 0.158(7) 0.081(6) 0.027(4) 0.018(4) O12 0.105(4) 0.061(3) 0.063(3) 0.010(2) 0.034(3) 0.017(3) O13 0.064(4) 0.093(4) 0.184(7) 0.069(5) 0.023(4) 0.014(3) O14 0.147(7) 0.168(9) 0.093(5) -0.029(6) -0.009(5) -0.016(6) O15 0.074(3) 0.079(3) 0.057(3) 0.025(3) -0.001(2) -0.029(3) O16 0.109(5) 0.077(4) 0.166(7) -0.002(4) -0.054(5) 0.019(4) O17 0.085(4) 0.160(7) 0.074(4) 0.016(4) 0.031(3) -0.030(4) O18 0.102(4) 0.068(3) 0.118(5) -0.034(3) 0.047(4) -0.014(3) N1 0.041(3) 0.073(4) 0.081(4) 0.033(3) 0.012(3) 0.005(3) N2 0.046(3) 0.049(3) 0.054(3) 0.009(2) 0.012(2) 0.003(2) N3 0.049(3) 0.045(3) 0.047(3) 0.001(2) 0.003(2) -0.005(2) N4 0.055(3) 0.038(2) 0.044(3) 0.001(2) 0.006(2) -0.003(2) N5 0.086(4) 0.069(4) 0.066(4) -0.026(3) 0.002(3) -0.015(3) N6 0.098(5) 0.046(3) 0.059(3) -0.014(3) 0.026(3) -0.002(3) N7 0.066(3) 0.048(3) 0.057(3) -0.009(3) 0.019(3) 0.004(3) N8 0.069(4) 0.050(3) 0.057(3) -0.008(3) 0.019(3) 0.018(3) N9 0.055(3) 0.039(2) 0.048(3) 0.002(2) 0.015(2) 0.007(2) N10 0.050(3) 0.035(2) 0.046(3) -0.001(2) 0.006(2) 0.006(2) N11 0.047(3) 0.035(2) 0.039(2) 0.001(2) 0.0053(19) 0.0042(19) N12 0.051(3) 0.052(3) 0.057(3) -0.009(3) -0.001(2) -0.003(2) N13 0.048(3) 0.050(3) 0.056(3) 0.010(2) 0.004(2) -0.001(2) N14 0.048(3) 0.040(2) 0.051(3) 0.005(2) 0.007(2) 0.004(2) N15 0.087(4) 0.054(3) 0.065(4) 0.019(3) 0.041(3) 0.011(3) N16 0.052(3) 0.037(2) 0.048(3) 0.003(2) 0.014(2) 0.004(2) N17 0.075(4) 0.031(2) 0.059(3) -0.002(2) 0.026(3) -0.008(2) N18 0.068(3) 0.033(2) 0.047(3) -0.002(2) 0.018(2) -0.006(2) N19 0.279(14) 0.031(3) 0.097(6) -0.011(3) 0.100(7) -0.008(5) N20 0.144(7) 0.046(3) 0.066(4) -0.021(3) 0.045(4) -0.017(4) N21 0.061(3) 0.048(3) 0.045(3) -0.008(2) 0.012(2) -0.009(2) N22 0.121(6) 0.055(3) 0.046(3) -0.007(3) 0.025(3) 0.007(3) N23 0.058(3) 0.042(3) 0.040(2) 0.001(2) 0.013(2) 0.006(2) N24 0.070(3) 0.033(2) 0.044(3) -0.001(2) 0.017(2) 0.003(2) N25 0.057(3) 0.029(2) 0.042(2) 0.0016(19) 0.016(2) 0.0017(19) N26 0.134(6) 0.033(3) 0.059(3) 0.004(2) 0.036(4) -0.004(3) N27 0.088(4) 0.042(3) 0.056(3) 0.009(2) 0.028(3) 0.002(3) N28 0.052(3) 0.039(2) 0.038(2) 0.002(2) 0.006(2) 0.003(2) N29 0.040(3) 0.063(3) 0.059(3) 0.003(3) 0.010(2) -0.005(2) N30 0.043(3) 0.044(3) 0.049(3) 0.001(2) 0.010(2) 0.004(2) N31 0.044(3) 0.039(2) 0.047(3) 0.003(2) 0.004(2) 0.0023(19) N32 0.044(3) 0.035(2) 0.047(3) 0.003(2) 0.010(2) 0.0021(19) N33 0.068(4) 0.068(4) 0.075(4) 0.032(3) -0.002(3) -0.003(3) N34 0.052(3) 0.042(3) 0.052(3) 0.006(2) 0.013(2) -0.005(2) N35 0.067(3) 0.040(3) 0.051(3) 0.005(2) 0.018(2) 0.001(2) N36 0.066(3) 0.043(3) 0.046(3) 0.016(2) 0.013(2) -0.009(2) N37 0.053(3) 0.037(2) 0.044(3) 0.005(2) 0.012(2) -0.001(2) N38 0.052(3) 0.036(2) 0.045(3) 0.004(2) 0.006(2) -0.003(2) N39 0.044(3) 0.042(2) 0.043(3) 0.002(2) 0.007(2) -0.002(2) N40 0.057(3) 0.061(3) 0.061(3) 0.003(3) -0.004(3) 0.009(3) N41 0.054(3) 0.047(3) 0.055(3) -0.007(2) 0.010(2) -0.005(2) N42 0.050(3) 0.062(3) 0.073(4) -0.019(3) 0.006(3) -0.001(3) C1 0.050(4) 0.076(5) 0.074(5) 0.025(4) -0.008(3) -0.013(3) C2 0.053(4) 0.058(4) 0.058(4) 0.020(3) 0.005(3) -0.008(3) C3 0.058(4) 0.063(4) 0.072(5) 0.023(4) 0.023(4) 0.018(3) C4 0.042(3) 0.045(3) 0.049(3) 0.016(3) 0.006(2) 0.002(2) C5 0.049(3) 0.038(3) 0.040(3) 0.007(2) 0.003(2) -0.005(2) C6 0.071(4) 0.043(3) 0.042(3) -0.002(3) 0.013(3) -0.005(3) C7 0.075(4) 0.038(3) 0.046(3) -0.005(3) 0.018(3) -0.002(3) C8 0.104(6) 0.053(4) 0.064(4) -0.016(4) 0.032(4) 0.005(4) C9 0.087(6) 0.053(4) 0.094(6) -0.013(4) 0.037(5) 0.013(4) C10 0.079(5) 0.061(4) 0.074(5) -0.017(4) 0.016(4) 0.009(4) C11 0.083(5) 0.054(4) 0.059(4) -0.019(3) -0.002(3) 0.017(4) C12 0.059(4) 0.047(3) 0.042(3) -0.004(3) 0.010(3) 0.013(3) C13 0.053(4) 0.051(3) 0.062(4) 0.002(3) 0.012(3) 0.009(3) C14 0.052(3) 0.036(3) 0.040(3) 0.000(2) 0.006(2) 0.006(2) C15 0.052(3) 0.033(3) 0.041(3) 0.004(2) 0.009(2) 0.007(2) C16 0.053(3) 0.034(3) 0.040(3) 0.005(2) 0.007(2) -0.002(2) C17 0.046(3) 0.040(3) 0.041(3) 0.009(2) 0.007(2) -0.002(2) C18 0.056(4) 0.045(3) 0.060(4) 0.002(3) 0.012(3) 0.004(3) C19 0.057(4) 0.056(4) 0.075(5) 0.011(4) 0.016(3) 0.015(3) C20 0.046(3) 0.057(4) 0.078(5) 0.018(4) 0.007(3) 0.006(3) C21 0.163(10) 0.042(4) 0.137(9) 0.020(5) 0.096(8) 0.007(5) C22 0.080(5) 0.042(3) 0.076(5) 0.016(3) 0.038(4) 0.006(3) C23 0.066(4) 0.057(4) 0.049(3) 0.011(3) 0.020(3) 0.010(3) C24 0.053(3) 0.037(3) 0.051(3) 0.003(3) 0.019(3) -0.001(2) C25 0.050(3) 0.038(3) 0.050(3) 0.004(3) 0.016(3) -0.004(2) C26 0.105(6) 0.032(3) 0.060(4) -0.012(3) 0.033(4) -0.017(3) C27 0.077(4) 0.046(3) 0.055(4) -0.015(3) 0.019(3) -0.016(3) C28 0.120(7) 0.060(4) 0.061(4) -0.022(4) 0.034(5) -0.019(4) C29 0.076(5) 0.068(4) 0.043(3) -0.012(3) 0.013(3) -0.013(4) C30 0.064(4) 0.066(4) 0.045(3) 0.000(3) 0.009(3) -0.004(3) C31 0.198(12) 0.042(4) 0.085(6) -0.008(4) 0.053(7) 0.009(5) C32 0.094(5) 0.045(3) 0.052(4) -0.011(3) 0.013(3) 0.004(3) C33 0.074(4) 0.055(4) 0.041(3) 0.002(3) 0.020(3) 0.007(3) C34 0.059(4) 0.037(3) 0.044(3) -0.001(2) 0.011(3) 0.008(2) C35 0.054(3) 0.032(3) 0.041(3) 0.000(2) 0.011(2) 0.004(2) C36 0.064(4) 0.033(3) 0.047(3) 0.008(2) 0.015(3) 0.001(2) C37 0.056(3) 0.035(3) 0.051(3) 0.011(3) 0.007(3) 0.002(2) C38 0.062(4) 0.045(3) 0.048(3) 0.001(3) 0.008(3) 0.001(3) C39 0.074(4) 0.057(4) 0.038(3) 0.009(3) 0.011(3) 0.005(3) C40 0.078(5) 0.055(4) 0.054(4) 0.014(3) 0.018(3) 0.002(3) C41 0.044(3) 0.065(4) 0.068(4) 0.006(3) 0.007(3) 0.006(3) C42 0.043(3) 0.043(3) 0.046(3) -0.003(3) 0.006(2) 0.004(2) C43 0.049(4) 0.053(3) 0.057(4) 0.005(3) 0.011(3) -0.004(3) C44 0.042(3) 0.038(3) 0.039(3) 0.000(2) 0.007(2) 0.003(2) C45 0.045(3) 0.035(3) 0.039(3) -0.004(2) 0.009(2) 0.003(2) C46 0.053(3) 0.039(3) 0.049(3) 0.004(3) 0.009(3) 0.006(2) C47 0.054(3) 0.031(3) 0.053(3) 0.004(3) 0.011(3) 0.001(2) C48 0.082(5) 0.041(3) 0.062(4) 0.005(3) 0.029(4) -0.009(3) C49 0.060(4) 0.050(4) 0.075(5) 0.010(3) 0.019(3) -0.009(3) C50 0.056(4) 0.059(4) 0.063(4) 0.008(3) 0.009(3) -0.008(3) C51 0.077(5) 0.044(3) 0.053(4) 0.010(3) -0.006(3) -0.010(3) C52 0.059(4) 0.035(3) 0.037(3) 0.004(2) 0.009(2) -0.003(2) C53 0.055(4) 0.044(3) 0.054(3) 0.007(3) 0.013(3) -0.005(3) C54 0.054(3) 0.032(3) 0.037(3) 0.002(2) 0.008(2) 0.000(2) C55 0.053(3) 0.031(2) 0.034(3) 0.004(2) 0.007(2) -0.001(2) C56 0.060(4) 0.039(3) 0.041(3) -0.004(3) 0.009(3) 0.002(3) C57 0.044(3) 0.055(3) 0.052(3) -0.019(3) 0.004(3) -0.001(3) C58 0.051(4) 0.067(5) 0.105(6) -0.023(5) 0.009(4) -0.007(3) C59 0.066(5) 0.077(5) 0.091(6) -0.019(5) 0.032(4) -0.024(4) C60 0.060(4) 0.065(4) 0.077(5) -0.006(4) 0.017(3) -0.015(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 N25 2.147(4) . ? Mn1 O2 2.182(4) . ? Mn1 N11 2.183(5) . ? Mn1 O4 2.197(4) . ? Mn1 N14 2.392(5) . ? Mn1 N28 2.425(5) . ? Mn2 N32 2.121(5) . ? Mn2 O1 2.135(4) . ? Mn2 N4 2.139(5) . ? Mn2 O5 2.159(4) . ? Mn2 N7 2.438(5) . ? Mn2 N34 2.460(5) . ? Mn3 O4 2.185(4) . ? Mn3 O1 2.194(4) . ? Mn3 N37 2.200(5) . ? Mn3 N2 2.204(5) . ? Mn3 N23 2.206(5) . ? Mn3 O6 2.207(4) . ? Mn4 O3 2.184(4) . ? Mn4 N9 2.194(5) . ? Mn4 N30 2.197(5) . ? Mn4 O5 2.201(4) . ? Mn4 N16 2.201(5) . ? Mn4 O2 2.211(4) . ? Mn5 N18 2.162(5) . ? Mn5 N39 2.169(5) . ? Mn5 O6 2.172(4) . ? Mn5 O3 2.186(4) . ? Mn5 N21 2.395(5) . ? Mn5 N41 2.423(5) . ? Cl1 O10 1.354(8) . ? Cl1 O9 1.382(8) . ? Cl1 O7 1.383(7) . ? Cl1 O8 1.409(6) . ? Cl2 O11 1.382(6) . ? Cl2 O12 1.400(5) . ? Cl2 O13 1.400(7) . ? Cl2 O14 1.477(8) . ? Cl3 O18 1.391(6) . ? Cl3 O16 1.395(6) . ? Cl3 O17 1.410(6) . ? Cl3 O15 1.429(5) . ? Cl4 O19 1.365(16) . ? Cl4 O20 1.397(11) . ? Cl4 O21 1.60(3) . ? Cl4 O22 1.71(2) . ? O1 C5 1.314(7) . ? O2 C15 1.309(7) . ? O3 C25 1.309(7) . ? O4 C35 1.312(6) . ? O5 C45 1.315(7) . ? O6 C55 1.317(6) . ? O23 O24 1.23(3) . ? O24 O25 1.58(2) . ? O25 O26 1.69(2) . ? O26 O27 1.54(3) . ? O28 O33 1.56(2) 3_566 ? O29 O32 1.22(3) 3_566 ? O30 O31 1.35(3) . ? O32 O29 1.22(3) 3_566 ? O33 O28 1.56(2) 3_566 ? N1 C3 1.339(11) . ? N1 C2 1.368(10) . ? N2 C3 1.318(9) . ? N2 C4 1.394(8) . ? N3 C5 1.295(8) . ? N3 N4 1.397(7) . ? N4 C6 1.297(8) . ? N5 C6 1.337(9) . ? N6 C7 1.324(8) . ? N6 C8 1.344(11) . ? N7 C10 1.321(10) . ? N7 C7 1.349(9) . ? N8 C12 1.359(9) . ? N8 C13 1.363(9) . ? N9 C13 1.317(8) . ? N9 C14 1.382(8) . ? N10 C15 1.313(8) . ? N10 N11 1.386(7) . ? N11 C16 1.295(8) . ? N12 C16 1.338(8) . ? N13 C17 1.318(8) . ? N13 C20 1.332(9) . ? N14 C18 1.330(8) . ? N14 C17 1.355(8) . ? N15 C23 1.356(9) . ? N15 C22 1.363(9) . ? N16 C23 1.308(8) . ? N16 C24 1.391(7) . ? N17 C25 1.293(8) . ? N17 N18 1.396(7) . ? N18 C26 1.280(8) . ? N19 C26 1.342(9) . ? N20 C27 1.316(9) . ? N20 C28 1.333(10) . ? N21 C30 1.321(8) . ? N21 C27 1.351(9) . ? N22 C33 1.342(9) . ? N22 C32 1.377(9) . ? N23 C33 1.304(8) . ? N23 C34 1.387(8) . ? N24 C35 1.304(7) . ? N24 N25 1.400(7) . ? N25 C36 1.297(7) . ? N26 C36 1.333(8) . ? N27 C37 1.330(8) . ? N27 C40 1.345(9) . ? N28 C38 1.336(8) . ? N28 C37 1.339(7) . ? N29 C43 1.347(9) . ? N29 C42 1.385(8) . ? N30 C43 1.306(8) . ? N30 C44 1.401(7) . ? N31 C45 1.305(7) . ? N31 N32 1.403(7) . ? N32 C46 1.285(8) . ? N33 C46 1.328(8) . ? N34 C47 1.325(8) . ? N34 C50 1.344(8) . ? N35 C47 1.337(8) . ? N35 C48 1.338(9) . ? N36 C53 1.345(8) . ? N36 C52 1.348(8) . ? N37 C53 1.315(8) . ? N37 C54 1.375(8) . ? N38 C55 1.319(8) . ? N38 N39 1.385(7) . ? N39 C56 1.292(8) . ? N40 C56 1.354(8) . ? N41 C57 1.336(9) . ? N41 C60 1.337(9) . ? N42 C57 1.325(8) . ? N42 C58 1.340(10) . ? C1 C2 1.485(10) . ? C2 C4 1.365(9) . ? C4 C5 1.463(8) . ? C6 C7 1.459(10) . ? C8 C9 1.356(13) . ? C9 C10 1.401(10) . ? C11 C12 1.502(9) . ? C12 C14 1.370(8) . ? C14 C15 1.459(8) . ? C16 C17 1.485(8) . ? C18 C19 1.366(10) . ? C19 C20 1.369(11) . ? C21 C22 1.474(10) . ? C22 C24 1.379(8) . ? C24 C25 1.464(8) . ? C26 C27 1.484(9) . ? C28 C29 1.378(11) . ? C29 C30 1.393(10) . ? C31 C32 1.462(10) . ? C32 C34 1.366(9) . ? C34 C35 1.468(8) . ? C36 C37 1.470(9) . ? C38 C39 1.384(9) . ? C39 C40 1.383(10) . ? C41 C42 1.488(9) . ? C42 C44 1.364(8) . ? C44 C45 1.460(8) . ? C46 C47 1.491(9) . ? C48 C49 1.366(11) . ? C49 C50 1.351(9) . ? C51 C52 1.491(9) . ? C52 C54 1.389(8) . ? C54 C55 1.448(8) . ? C56 C57 1.479(9) . ? C58 C59 1.355(13) . ? C59 C60 1.368(11) . ? 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 N25 Mn1 O2 126.08(17) . . ? N25 Mn1 N11 148.86(18) . . ? O2 Mn1 N11 70.78(16) . . ? N25 Mn1 O4 71.08(15) . . ? O2 Mn1 O4 107.53(14) . . ? N11 Mn1 O4 133.45(16) . . ? N25 Mn1 N14 93.34(18) . . ? O2 Mn1 N14 139.50(16) . . ? N11 Mn1 N14 69.91(17) . . ? O4 Mn1 N14 92.63(17) . . ? N25 Mn1 N28 69.58(16) . . ? O2 Mn1 N28 88.40(15) . . ? N11 Mn1 N28 86.70(17) . . ? O4 Mn1 N28 139.54(15) . . ? N14 Mn1 N28 98.68(17) . . ? N32 Mn2 O1 132.59(16) . . ? N32 Mn2 N4 142.55(19) . . ? O1 Mn2 N4 72.34(17) . . ? N32 Mn2 O5 72.89(16) . . ? O1 Mn2 O5 109.10(15) . . ? N4 Mn2 O5 131.72(17) . . ? N32 Mn2 N7 86.34(19) . . ? O1 Mn2 N7 140.06(18) . . ? N4 Mn2 N7 69.4(2) . . ? O5 Mn2 N7 88.52(17) . . ? N32 Mn2 N34 69.31(18) . . ? O1 Mn2 N34 89.03(16) . . ? N4 Mn2 N34 86.60(18) . . ? O5 Mn2 N34 140.60(16) . . ? N7 Mn2 N34 99.64(19) . . ? O4 Mn3 O1 87.26(14) . . ? O4 Mn3 N37 170.27(18) . . ? O1 Mn3 N37 93.45(16) . . ? O4 Mn3 N2 89.93(17) . . ? O1 Mn3 N2 75.28(17) . . ? N37 Mn3 N2 99.65(19) . . ? O4 Mn3 N23 76.25(16) . . ? O1 Mn3 N23 163.28(16) . . ? N37 Mn3 N23 103.27(18) . . ? N2 Mn3 N23 101.59(19) . . ? O4 Mn3 O6 94.79(15) . . ? O1 Mn3 O6 90.78(14) . . ? N37 Mn3 O6 75.50(16) . . ? N2 Mn3 O6 165.07(17) . . ? N23 Mn3 O6 93.29(17) . . ? O3 Mn4 N9 170.43(18) . . ? O3 Mn4 N30 93.61(17) . . ? N9 Mn4 N30 95.84(19) . . ? O3 Mn4 O5 89.15(14) . . ? N9 Mn4 O5 94.60(16) . . ? N30 Mn4 O5 75.74(16) . . ? O3 Mn4 N16 76.14(16) . . ? N9 Mn4 N16 100.32(18) . . ? N30 Mn4 N16 102.30(19) . . ? O5 Mn4 N16 165.08(16) . . ? O3 Mn4 O2 95.80(15) . . ? N9 Mn4 O2 75.50(17) . . ? N30 Mn4 O2 161.91(17) . . ? O5 Mn4 O2 88.97(14) . . ? N16 Mn4 O2 94.94(17) . . ? N18 Mn5 N39 149.14(19) . . ? N18 Mn5 O6 127.78(18) . . ? N39 Mn5 O6 71.56(16) . . ? N18 Mn5 O3 70.89(16) . . ? N39 Mn5 O3 131.26(17) . . ? O6 Mn5 O3 107.35(15) . . ? N18 Mn5 N21 70.07(18) . . ? N39 Mn5 N21 88.37(19) . . ? O6 Mn5 N21 89.43(16) . . ? O3 Mn5 N21 139.84(17) . . ? N18 Mn5 N41 92.1(2) . . ? N39 Mn5 N41 69.11(18) . . ? O6 Mn5 N41 139.39(16) . . ? O3 Mn5 N41 91.34(17) . . ? N21 Mn5 N41 99.11(18) . . ? O10 Cl1 O9 108.8(7) . . ? O10 Cl1 O7 110.8(8) . . ? O9 Cl1 O7 109.0(6) . . ? O10 Cl1 O8 108.3(5) . . ? O9 Cl1 O8 113.4(5) . . ? O7 Cl1 O8 106.6(5) . . ? O11 Cl2 O12 114.2(4) . . ? O11 Cl2 O13 113.8(4) . . ? O12 Cl2 O13 110.5(4) . . ? O11 Cl2 O14 107.3(6) . . ? O12 Cl2 O14 105.5(5) . . ? O13 Cl2 O14 104.7(6) . . ? O18 Cl3 O16 112.1(5) . . ? O18 Cl3 O17 109.1(5) . . ? O16 Cl3 O17 108.7(6) . . ? O18 Cl3 O15 110.1(4) . . ? O16 Cl3 O15 107.9(4) . . ? O17 Cl3 O15 108.8(4) . . ? O19 Cl4 O20 134.6(9) . . ? O19 Cl4 O21 98.3(12) . . ? O20 Cl4 O21 96.7(11) . . ? O19 Cl4 O22 109.7(10) . . ? O20 Cl4 O22 115.6(8) . . ? O21 Cl4 O22 74.9(11) . . ? C5 O1 Mn2 113.0(3) . . ? C5 O1 Mn3 117.5(3) . . ? Mn2 O1 Mn3 126.46(17) . . ? C15 O2 Mn1 113.8(3) . . ? C15 O2 Mn4 116.3(3) . . ? Mn1 O2 Mn4 127.73(17) . . ? C25 O3 Mn4 117.1(3) . . ? C25 O3 Mn5 113.3(3) . . ? Mn4 O3 Mn5 127.50(17) . . ? C35 O4 Mn3 116.5(3) . . ? C35 O4 Mn1 113.0(3) . . ? Mn3 O4 Mn1 128.69(17) . . ? C45 O5 Mn2 111.8(3) . . ? C45 O5 Mn4 116.9(3) . . ? Mn2 O5 Mn4 128.18(17) . . ? C55 O6 Mn5 113.4(3) . . ? C55 O6 Mn3 116.1(3) . . ? Mn5 O6 Mn3 128.61(18) . . ? O23 O24 O25 151(2) . . ? O24 O25 O26 140.7(12) . . ? O27 O26 O25 159.3(17) . . ? C3 N1 C2 109.3(6) . . ? C3 N2 C4 105.0(6) . . ? C3 N2 Mn3 141.5(5) . . ? C4 N2 Mn3 113.5(4) . . ? C5 N3 N4 109.3(5) . . ? C6 N4 N3 116.6(5) . . ? C6 N4 Mn2 125.5(4) . . ? N3 N4 Mn2 117.5(3) . . ? C7 N6 C8 115.9(7) . . ? C10 N7 C7 116.4(6) . . ? C10 N7 Mn2 130.5(5) . . ? C7 N7 Mn2 113.1(4) . . ? C12 N8 C13 109.2(5) . . ? C13 N9 C14 107.1(5) . . ? C13 N9 Mn4 139.4(5) . . ? C14 N9 Mn4 113.4(4) . . ? C15 N10 N11 109.2(4) . . ? C16 N11 N10 116.5(5) . . ? C16 N11 Mn1 124.4(4) . . ? N10 N11 Mn1 119.0(3) . . ? C17 N13 C20 115.8(6) . . ? C18 N14 C17 115.6(5) . . ? C18 N14 Mn1 129.8(4) . . ? C17 N14 Mn1 114.6(4) . . ? C23 N15 C22 109.3(5) . . ? C23 N16 C24 106.6(5) . . ? C23 N16 Mn4 141.2(4) . . ? C24 N16 Mn4 112.2(4) . . ? C25 N17 N18 109.1(5) . . ? C26 N18 N17 116.2(5) . . ? C26 N18 Mn5 124.8(4) . . ? N17 N18 Mn5 119.0(3) . . ? C27 N20 C28 116.5(7) . . ? C30 N21 C27 116.2(6) . . ? C30 N21 Mn5 129.8(5) . . ? C27 N21 Mn5 113.8(4) . . ? C33 N22 C32 109.1(6) . . ? C33 N23 C34 106.1(5) . . ? C33 N23 Mn3 141.4(4) . . ? C34 N23 Mn3 112.4(4) . . ? C35 N24 N25 109.1(4) . . ? C36 N25 N24 115.2(5) . . ? C36 N25 Mn1 125.3(4) . . ? N24 N25 Mn1 119.3(3) . . ? C37 N27 C40 116.7(6) . . ? C38 N28 C37 116.7(5) . . ? C38 N28 Mn1 129.7(4) . . ? C37 N28 Mn1 113.2(4) . . ? C43 N29 C42 109.2(5) . . ? C43 N30 C44 105.9(5) . . ? C43 N30 Mn4 140.9(4) . . ? C44 N30 Mn4 113.0(4) . . ? C45 N31 N32 109.3(4) . . ? C46 N32 N31 115.1(5) . . ? C46 N32 Mn2 126.4(4) . . ? N31 N32 Mn2 117.9(3) . . ? C47 N34 C50 115.5(5) . . ? C47 N34 Mn2 112.5(4) . . ? C50 N34 Mn2 132.0(4) . . ? C47 N35 C48 115.2(6) . . ? C53 N36 C52 110.6(5) . . ? C53 N37 C54 106.8(5) . . ? C53 N37 Mn3 139.9(4) . . ? C54 N37 Mn3 113.1(4) . . ? C55 N38 N39 109.4(4) . . ? C56 N39 N38 116.1(5) . . ? C56 N39 Mn5 125.2(4) . . ? N38 N39 Mn5 118.7(4) . . ? C57 N41 C60 116.2(6) . . ? C57 N41 Mn5 114.6(4) . . ? C60 N41 Mn5 129.2(5) . . ? C57 N42 C58 114.2(7) . . ? C4 C2 N1 104.5(6) . . ? C4 C2 C1 132.9(7) . . ? N1 C2 C1 122.7(6) . . ? N2 C3 N1 110.9(7) . . ? C2 C4 N2 110.2(6) . . ? C2 C4 C5 132.4(6) . . ? N2 C4 C5 117.4(5) . . ? N3 C5 O1 125.1(5) . . ? N3 C5 C4 118.7(5) . . ? O1 C5 C4 116.2(5) . . ? N4 C6 N5 124.4(7) . . ? N4 C6 C7 116.2(6) . . ? N5 C6 C7 119.4(6) . . ? N6 C7 N7 125.8(7) . . ? N6 C7 C6 118.5(6) . . ? N7 C7 C6 115.6(5) . . ? N6 C8 C9 123.6(7) . . ? C8 C9 C10 115.8(8) . . ? N7 C10 C9 122.4(8) . . ? N8 C12 C14 105.4(6) . . ? N8 C12 C11 121.9(6) . . ? C14 C12 C11 132.7(6) . . ? N9 C13 N8 109.2(6) . . ? C12 C14 N9 109.2(5) . . ? C12 C14 C15 132.8(6) . . ? N9 C14 C15 118.0(5) . . ? O2 C15 N10 124.9(5) . . ? O2 C15 C14 116.7(5) . . ? N10 C15 C14 118.4(5) . . ? N11 C16 N12 125.7(6) . . ? N11 C16 C17 115.6(5) . . ? N12 C16 C17 118.8(5) . . ? N13 C17 N14 126.8(6) . . ? N13 C17 C16 117.8(5) . . ? N14 C17 C16 115.5(5) . . ? N14 C18 C19 121.6(6) . . ? C18 C19 C20 118.2(6) . . ? N13 C20 C19 122.0(6) . . ? N15 C22 C24 104.8(6) . . ? N15 C22 C21 121.5(6) . . ? C24 C22 C21 133.6(7) . . ? N16 C23 N15 110.1(6) . . ? C22 C24 N16 109.2(5) . . ? C22 C24 C25 132.4(6) . . ? N16 C24 C25 118.4(5) . . ? N17 C25 O3 125.4(5) . . ? N17 C25 C24 118.4(5) . . ? O3 C25 C24 116.2(5) . . ? N18 C26 N19 125.6(7) . . ? N18 C26 C27 115.9(6) . . ? N19 C26 C27 118.5(6) . . ? N20 C27 N21 126.3(6) . . ? N20 C27 C26 118.3(6) . . ? N21 C27 C26 115.4(6) . . ? N20 C28 C29 122.3(7) . . ? C28 C29 C30 116.5(7) . . ? N21 C30 C29 122.1(7) . . ? C34 C32 N22 104.1(6) . . ? C34 C32 C31 134.0(7) . . ? N22 C32 C31 121.8(6) . . ? N23 C33 N22 110.6(6) . . ? C32 C34 N23 109.9(5) . . ? C32 C34 C35 132.2(6) . . ? N23 C34 C35 117.9(5) . . ? N24 C35 O4 125.0(5) . . ? N24 C35 C34 118.1(5) . . ? O4 C35 C34 116.9(5) . . ? N25 C36 N26 125.2(6) . . ? N25 C36 C37 115.5(5) . . ? N26 C36 C37 119.3(5) . . ? N27 C37 N28 126.1(6) . . ? N27 C37 C36 117.8(5) . . ? N28 C37 C36 116.1(5) . . ? N28 C38 C39 121.4(6) . . ? C40 C39 C38 117.9(6) . . ? N27 C40 C39 121.2(6) . . ? C44 C42 N29 104.1(5) . . ? C44 C42 C41 132.9(6) . . ? N29 C42 C41 123.0(5) . . ? N30 C43 N29 110.7(6) . . ? C42 C44 N30 110.0(5) . . ? C42 C44 C45 132.1(5) . . ? N30 C44 C45 117.9(5) . . ? N31 C45 O5 125.4(5) . . ? N31 C45 C44 118.3(5) . . ? O5 C45 C44 116.3(5) . . ? N32 C46 N33 126.7(6) . . ? N32 C46 C47 115.4(5) . . ? N33 C46 C47 117.9(6) . . ? N34 C47 N35 126.9(6) . . ? N34 C47 C46 115.8(5) . . ? N35 C47 C46 117.2(5) . . ? N35 C48 C49 122.4(6) . . ? C50 C49 C48 117.6(7) . . ? N34 C50 C49 122.4(7) . . ? N36 C52 C54 104.0(5) . . ? N36 C52 C51 123.0(5) . . ? C54 C52 C51 133.0(6) . . ? N37 C53 N36 109.2(6) . . ? N37 C54 C52 109.3(5) . . ? N37 C54 C55 118.6(5) . . ? C52 C54 C55 132.1(5) . . ? O6 C55 N38 124.6(5) . . ? O6 C55 C54 116.6(5) . . ? N38 C55 C54 118.8(5) . . ? N39 C56 N40 125.3(6) . . ? N39 C56 C57 115.9(5) . . ? N40 C56 C57 118.9(6) . . ? N42 C57 N41 127.4(6) . . ? N42 C57 C56 117.3(6) . . ? N41 C57 C56 115.3(5) . . ? N42 C58 C59 123.3(7) . . ? C58 C59 C60 118.0(7) . . ? N41 C60 C59 120.9(8) . . ? _diffrn_measured_fraction_theta_max 0.765 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.765 _refine_diff_density_max 1.477 _refine_diff_density_min -2.478 _refine_diff_density_rms 0.145 #===END data_shelxl(7) _database_code_depnum_ccdc_archive 'CCDC 299034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H134 Mn9 N72 O58' _chemical_formula_weight 3791.07 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a c d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/4, x+3/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+1/4, -x+1/4, z+3/4' '-x, y, z+1/2' 'y+3/4, x+3/4, z+3/4' 'x+1/2, -y, z' '-y+3/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+3/4, -x+3/4, z+5/4' '-x+1/2, y+1/2, z+1' 'y+5/4, x+5/4, z+5/4' 'x+1, -y+1/2, z+1/2' '-y+5/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-1/4, -x-3/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-1/4, x-1/4, -z-3/4' 'x, -y, -z-1/2' '-y-3/4, -x-3/4, -z-3/4' '-x-1/2, y, -z' 'y-3/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z+1/4' 'x, y+1/2, -z' '-y+1/4, x+1/4, -z-1/4' 'x+1/2, -y+1/2, -z' '-y-1/4, -x-1/4, -z-1/4' '-x, y+1/2, -z+1/2' 'y-1/4, x+1/4, -z+1/4' _cell_length_a 27.9255(13) _cell_length_b 27.9255(13) _cell_length_c 40.217(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 31362(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 50066 _cell_measurement_theta_min 2.3062 _cell_measurement_theta_max 30.8436 _exptl_crystal_description Chip _exptl_crystal_colour Red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15512 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8901 _exptl_absorpt_correction_T_max 0.9176 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 151450 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.93 _reflns_number_total 11887 _reflns_number_gt 11169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_publication_material 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0942P)^2^+214.6007P] 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 11887 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.1278 _refine_ls_wR_factor_ref 0.3049 _refine_ls_wR_factor_gt 0.3008 _refine_ls_goodness_of_fit_ref 1.348 _refine_ls_restrained_S_all 1.348 _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 0.35264(3) 0.12659(3) 0.14715(2) 0.0380(2) Uani 1 1 d . . . Mn2 Mn 0.36197(3) 0.26784(3) 0.138473(18) 0.0349(2) Uani 1 1 d . . . Mn3 Mn 0.5000 0.2500 0.1250 0.0326(3) Uani 1 4 d S . . O1 O 0.36562(14) 0.19923(13) 0.16633(9) 0.0378(8) Uani 1 1 d . . . O2 O 0.37283(14) 0.34553(13) 0.14270(9) 0.0384(8) Uani 1 1 d . . . O3 O 0.42516(13) 0.25675(13) 0.10868(8) 0.0350(7) Uani 1 1 d . . . O4 O 0.68526(18) 0.7797(3) 0.01949(12) 0.0795(18) Uani 1 1 d . . . O5 O 0.6444(2) 0.8228(3) 0.05267(16) 0.092(2) Uani 1 1 d . . . O6 O 0.6242(3) 0.7511(3) 0.04397(19) 0.119(3) Uani 1 1 d . . . O7 O 0.6204(13) 0.4854(15) 0.0450(9) 0.241(16) Uiso 0.50 1 d P . . O8 O 0.6275(5) 0.5491(5) 0.0630(4) 0.085(3) Uiso 0.50 1 d P . . O9 O 0.5819(9) 0.5372(9) 0.0190(6) 0.162(8) Uiso 0.50 1 d P . . O10 O 0.1884(10) 0.0528(10) -0.0083(7) 0.200(11) Uiso 0.50 1 d P . . O11 O 0.2500 0.1452(5) 0.0000 0.135(4) Uiso 1 2 d S . . O12 O 0.4064(5) 0.8612(5) 0.0400(3) 0.179(5) Uiso 1 1 d . . . O13 O 0.5457(7) 0.6937(7) 0.0832(5) 0.117(6) Uiso 0.50 1 d P . . O14 O 0.5348(9) 0.6689(9) 0.0771(6) 0.155(9) Uiso 0.50 1 d P . . O15 O 0.5198(7) 0.5013(9) -0.0067(6) 0.156(8) Uiso 0.50 1 d P . . O16 O 0.7620(5) 0.4880(5) 0.1250 0.092(6) Uiso 0.50 2 d SP . . O17 O 0.7555(7) 0.4892(7) 0.1027(5) 0.131(6) Uiso 0.50 1 d P . . O18 O 0.7469(15) 0.4937(15) 0.0714(11) 0.127(12) Uiso 0.25 1 d P . . O19 O 0.7367(15) 0.5002(15) 0.0512(10) 0.270(19) Uiso 0.50 1 d P . . O20 O 0.7046(12) 0.5368(12) -0.0018(8) 0.240(13) Uiso 0.50 1 d P . . O21 O 0.8986(9) 0.1512(9) 0.1419(5) 0.161(8) Uiso 0.50 1 d P . . O22 O 0.9422(5) 0.2950(5) 0.0909(3) 0.080(3) Uiso 0.50 1 d P . . O23 O 0.9479(4) 0.3209(4) 0.0915(3) 0.060(2) Uiso 0.50 1 d P . . N1 N 0.36728(18) 0.04804(17) 0.15885(12) 0.0426(10) Uani 1 1 d . . . N2 N 0.3941(3) -0.00349(19) 0.20203(14) 0.0630(16) Uani 1 1 d . . . N3 N 0.4060(3) 0.0757(2) 0.24204(14) 0.084(2) Uani 1 1 d . . . H1 H 0.4106 0.1007 0.2550 0.101 Uiso 1 1 calc R . . H2 H 0.4136 0.0469 0.2490 0.101 Uiso 1 1 calc R . . N4 N 0.37442(18) 0.12150(17) 0.19818(11) 0.0414(10) Uani 1 1 d . . . N5 N 0.37881(19) 0.16319(16) 0.21703(12) 0.0443(11) Uani 1 1 d . . . N6 N 0.37369(15) 0.28457(15) 0.19088(10) 0.0345(8) Uani 1 1 d . . . N7 N 0.37981(18) 0.41020(16) 0.17884(11) 0.0403(10) Uani 1 1 d . . . N8 N 0.37939(17) 0.43560(16) 0.14877(11) 0.0406(10) Uani 1 1 d . . . N9 N 0.3839(2) 0.50849(19) 0.17791(14) 0.0585(14) Uani 1 1 d . . . H3 H 0.3835 0.4948 0.1976 0.070 Uiso 1 1 calc R . . H4 H 0.3856 0.5399 0.1763 0.070 Uiso 1 1 calc R . . N10 N 0.3844(2) 0.55481(19) 0.11800(15) 0.0543(13) Uani 1 1 d . . . N11 N 0.37899(18) 0.47828(19) 0.09120(12) 0.0461(11) Uani 1 1 d . . . N12 N 0.27718(17) 0.26323(18) 0.13626(11) 0.0424(10) Uani 1 1 d . . . N13 N 0.21408(18) 0.2488(2) 0.09757(13) 0.0528(13) Uani 1 1 d . . . N14 N 0.28068(17) 0.2430(2) 0.04772(12) 0.0552(14) Uani 1 1 d . . . H5 H 0.3015 0.2413 0.0314 0.066 Uiso 1 1 calc R . . H6 H 0.2499 0.2394 0.0437 0.066 Uiso 1 1 calc R . . N15 N 0.33955(16) 0.25710(17) 0.08800(11) 0.0384(9) Uani 1 1 d . . . N16 N 0.37393(15) 0.25419(18) 0.06296(11) 0.0390(9) Uani 1 1 d . . . N17 N 0.5000 0.2500 0.07074(13) 0.0315(11) Uani 1 2 d S . . N18 N 0.65112(19) 0.7840(2) 0.03855(12) 0.0531(13) Uani 1 1 d . . . N19 N 0.6222(14) 0.5256(16) 0.0418(11) 0.200(15) Uiso 0.50 1 d P . . C1 C 0.3651(2) 0.0107(2) 0.13814(16) 0.0519(14) Uani 1 1 d . . . H7 H 0.3552 0.0159 0.1158 0.062 Uiso 1 1 calc R . . C2 C 0.3768(3) -0.0353(2) 0.14807(18) 0.0579(16) Uani 1 1 d . . . H8 H 0.3750 -0.0617 0.1332 0.070 Uiso 1 1 calc R . . C3 C 0.3911(3) -0.0408(2) 0.18068(18) 0.067(2) Uani 1 1 d . . . H9 H 0.3991 -0.0719 0.1884 0.081 Uiso 1 1 calc R . . C4 C 0.3823(2) 0.0390(2) 0.19001(14) 0.0478(13) Uani 1 1 d . . . C5 C 0.3875(3) 0.0816(2) 0.21203(14) 0.0495(14) Uani 1 1 d . . . C6 C 0.37259(19) 0.20117(18) 0.19806(12) 0.0362(10) Uani 1 1 d . . . C7 C 0.37586(19) 0.24938(19) 0.21360(12) 0.0366(10) Uani 1 1 d . . . C8 C 0.3810(2) 0.2588(2) 0.24723(13) 0.0431(12) Uani 1 1 d . . . H10 H 0.3817 0.2335 0.2631 0.052 Uiso 1 1 calc R . . C9 C 0.3850(2) 0.3064(2) 0.25701(13) 0.0482(14) Uani 1 1 d . . . H11 H 0.3888 0.3140 0.2799 0.058 Uiso 1 1 calc R . . C10 C 0.3836(2) 0.3428(2) 0.23384(14) 0.0428(12) Uani 1 1 d . . . H12 H 0.3868 0.3753 0.2404 0.051 Uiso 1 1 calc R . . C11 C 0.37752(19) 0.33049(19) 0.20067(12) 0.0365(10) Uani 1 1 d . . . C12 C 0.37652(17) 0.36470(18) 0.17228(12) 0.0327(9) Uani 1 1 d . . . C13 C 0.3820(2) 0.4819(2) 0.15077(14) 0.0415(11) Uani 1 1 d . . . C14 C 0.3819(2) 0.5072(2) 0.11778(15) 0.0443(12) Uani 1 1 d . . . C15 C 0.3821(3) 0.5760(2) 0.08802(19) 0.0608(18) Uani 1 1 d . . . H13 H 0.3830 0.6100 0.0868 0.073 Uiso 1 1 calc R . . C16 C 0.3785(3) 0.5505(3) 0.05968(18) 0.0639(19) Uani 1 1 d . . . H14 H 0.3772 0.5661 0.0387 0.077 Uiso 1 1 calc R . . C17 C 0.3769(3) 0.5011(3) 0.06168(17) 0.0563(16) Uani 1 1 d . . . H15 H 0.3742 0.4828 0.0418 0.068 Uiso 1 1 calc R . . C18 C 0.2450(2) 0.2660(3) 0.16065(16) 0.0551(15) Uani 1 1 d . . . H16 H 0.2557 0.2721 0.1827 0.066 Uiso 1 1 calc R . . C19 C 0.1963(3) 0.2603(3) 0.15478(17) 0.0610(18) Uani 1 1 d . . . H17 H 0.1737 0.2622 0.1724 0.073 Uiso 1 1 calc R . . C20 C 0.1821(2) 0.2519(3) 0.12221(18) 0.0604(17) Uani 1 1 d . . . H18 H 0.1490 0.2483 0.1174 0.073 Uiso 1 1 calc R . . C21 C 0.25940(19) 0.2546(2) 0.10552(13) 0.0415(11) Uani 1 1 d . . . C22 C 0.2956(2) 0.2512(2) 0.07856(13) 0.0423(11) Uani 1 1 d . . . C23 C 0.41611(19) 0.25485(18) 0.07680(11) 0.0339(10) Uani 1 1 d . . . C24 C 0.45842(17) 0.25248(19) 0.05427(12) 0.0351(10) Uani 1 1 d . . . C25 C 0.45652(19) 0.2525(2) 0.01975(12) 0.0402(11) Uani 1 1 d . . . H19 H 0.4268 0.2542 0.0083 0.048 Uiso 1 1 calc R . . C26 C 0.5000 0.2500 0.00250(19) 0.0433(16) Uani 1 2 d S . . H20 H 0.5000 0.2500 -0.0211 0.052 Uiso 1 2 calc SR . . 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 0.0400(4) 0.0407(4) 0.0335(4) -0.0011(3) 0.0019(3) -0.0004(3) Mn2 0.0384(4) 0.0376(4) 0.0287(4) -0.0016(3) 0.0012(3) -0.0007(3) Mn3 0.0364(5) 0.0364(5) 0.0249(6) 0.000 0.000 0.000 O1 0.047(2) 0.0365(18) 0.0300(16) 0.0008(14) 0.0018(15) 0.0002(15) O2 0.047(2) 0.0369(18) 0.0314(17) 0.0001(14) 0.0030(15) 0.0011(15) O3 0.0366(18) 0.0411(19) 0.0274(15) 0.0012(13) -0.0020(13) 0.0014(15) O4 0.053(3) 0.146(6) 0.040(2) -0.011(3) -0.003(2) 0.025(3) O5 0.083(4) 0.106(5) 0.087(4) -0.042(4) -0.043(3) 0.044(4) O6 0.090(5) 0.171(8) 0.097(5) 0.056(5) -0.040(4) -0.069(5) N1 0.048(3) 0.039(2) 0.041(2) -0.0027(19) 0.000(2) -0.0032(19) N2 0.108(5) 0.036(3) 0.046(3) 0.002(2) 0.001(3) 0.001(3) N3 0.173(8) 0.037(3) 0.042(3) 0.000(2) -0.022(4) 0.007(4) N4 0.052(3) 0.036(2) 0.036(2) 0.0009(18) 0.0017(19) -0.0008(19) N5 0.064(3) 0.033(2) 0.037(2) -0.0005(18) 0.006(2) 0.002(2) N6 0.035(2) 0.036(2) 0.033(2) -0.0013(16) 0.0027(16) 0.0022(17) N7 0.053(3) 0.035(2) 0.033(2) 0.0035(17) 0.0000(19) -0.0001(19) N8 0.046(2) 0.038(2) 0.038(2) 0.0023(18) 0.0013(19) 0.0040(19) N9 0.091(4) 0.040(3) 0.045(3) 0.002(2) 0.005(3) -0.001(3) N10 0.064(3) 0.040(3) 0.059(3) 0.011(2) 0.011(3) 0.006(2) N11 0.049(3) 0.048(3) 0.041(2) 0.006(2) 0.002(2) 0.001(2) N12 0.043(2) 0.048(3) 0.036(2) -0.0042(19) 0.0070(19) 0.004(2) N13 0.037(2) 0.073(4) 0.048(3) -0.008(3) 0.004(2) -0.008(2) N14 0.029(2) 0.095(4) 0.041(2) -0.012(3) 0.0043(19) -0.009(2) N15 0.034(2) 0.049(3) 0.032(2) -0.0071(18) 0.0035(16) -0.0044(18) N16 0.031(2) 0.053(3) 0.034(2) -0.0013(19) 0.0027(16) -0.0045(19) N17 0.034(3) 0.035(3) 0.026(2) 0.000 0.000 -0.005(2) N18 0.040(3) 0.085(4) 0.035(2) -0.002(2) -0.007(2) 0.003(3) C1 0.062(4) 0.050(3) 0.044(3) -0.006(3) -0.003(3) -0.006(3) C2 0.076(5) 0.040(3) 0.057(4) -0.009(3) 0.000(3) -0.006(3) C3 0.114(7) 0.034(3) 0.054(4) 0.002(3) -0.003(4) -0.004(4) C4 0.069(4) 0.038(3) 0.036(3) -0.001(2) 0.005(3) -0.001(3) C5 0.079(4) 0.033(3) 0.036(3) 0.001(2) 0.003(3) 0.001(3) C6 0.042(3) 0.035(2) 0.031(2) -0.0006(18) 0.0080(19) 0.000(2) C7 0.040(3) 0.036(2) 0.033(2) -0.0005(19) 0.0049(19) 0.005(2) C8 0.060(3) 0.039(3) 0.031(2) 0.001(2) 0.001(2) 0.006(2) C9 0.067(4) 0.049(3) 0.029(2) -0.003(2) -0.002(2) 0.004(3) C10 0.053(3) 0.037(3) 0.039(3) -0.004(2) -0.001(2) 0.002(2) C11 0.039(3) 0.037(2) 0.033(2) -0.0021(19) 0.0006(19) 0.005(2) C12 0.030(2) 0.039(2) 0.029(2) 0.0006(18) 0.0016(17) 0.0029(18) C13 0.048(3) 0.036(3) 0.041(3) 0.003(2) 0.002(2) 0.002(2) C14 0.046(3) 0.039(3) 0.048(3) 0.008(2) 0.005(2) 0.009(2) C15 0.074(5) 0.043(3) 0.065(4) 0.019(3) 0.012(4) 0.006(3) C16 0.080(5) 0.057(4) 0.055(4) 0.025(3) 0.004(3) 0.002(4) C17 0.069(4) 0.057(4) 0.043(3) 0.013(3) -0.002(3) -0.004(3) C18 0.054(4) 0.069(4) 0.042(3) -0.007(3) 0.010(3) 0.002(3) C19 0.049(3) 0.081(5) 0.053(4) -0.007(3) 0.013(3) -0.005(3) C20 0.042(3) 0.079(5) 0.060(4) -0.014(4) 0.012(3) -0.009(3) C21 0.037(3) 0.049(3) 0.039(3) -0.004(2) 0.002(2) -0.001(2) C22 0.041(3) 0.051(3) 0.035(2) -0.002(2) 0.001(2) -0.004(2) C23 0.042(3) 0.034(2) 0.026(2) -0.0003(17) -0.0020(18) -0.006(2) C24 0.032(2) 0.042(3) 0.031(2) -0.0023(19) -0.0003(18) -0.004(2) C25 0.037(2) 0.052(3) 0.031(2) 0.003(2) 0.0015(19) -0.005(2) C26 0.043(4) 0.057(5) 0.030(3) 0.000 0.000 -0.004(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 N8 2.135(5) 20_656 ? Mn1 N4 2.145(5) . ? Mn1 O2 2.162(4) 20_656 ? Mn1 O1 2.200(4) . ? Mn1 N1 2.280(5) . ? Mn1 N11 2.309(5) 20_656 ? Mn2 N15 2.145(4) . ? Mn2 O3 2.155(4) . ? Mn2 N6 2.183(4) . ? Mn2 O2 2.197(4) . ? Mn2 O1 2.222(4) . ? Mn2 N12 2.373(5) . ? Mn3 N17 2.182(5) . ? Mn3 N17 2.182(5) 26_565 ? Mn3 O3 2.199(3) 26_565 ? Mn3 O3 2.199(3) 11_554 ? Mn3 O3 2.199(3) . ? Mn3 O3 2.199(3) 20_656 ? O1 C6 1.292(6) . ? O2 C12 1.309(6) . ? O2 Mn1 2.162(4) 26_565 ? O3 C23 1.308(5) . ? O4 N18 1.229(7) . ? O5 N18 1.239(8) . ? O6 N18 1.205(9) . ? O7 N19 1.13(5) . ? O8 N19 1.09(4) . ? O9 N19 1.49(4) . ? O13 O14 0.79(3) . ? O15 O15 1.23(4) 17_665 ? O16 O17 0.92(2) 22_776 ? O16 O17 0.92(2) . ? O17 O18 1.29(4) . ? O17 O17 1.81(4) 22_776 ? O18 O19 0.88(5) . ? O21 O21 1.36(4) 32_645 ? O22 O23 0.742(14) . ? N1 C1 1.336(8) . ? N1 C4 1.346(7) . ? N2 C4 1.323(8) . ? N2 C3 1.352(9) . ? N3 C5 1.323(8) . ? N4 C5 1.297(7) . ? N4 N5 1.395(6) . ? N5 C6 1.318(7) . ? N6 C7 1.343(7) . ? N6 C11 1.346(7) . ? N7 C12 1.301(7) . ? N7 N8 1.402(6) . ? N8 C13 1.298(7) . ? N8 Mn1 2.135(5) 26_565 ? N9 C13 1.321(8) . ? N10 C14 1.330(8) . ? N10 C15 1.344(9) . ? N11 C14 1.343(8) . ? N11 C17 1.348(8) . ? N11 Mn1 2.309(5) 26_565 ? N12 C18 1.332(7) . ? N12 C21 1.354(7) . ? N13 C21 1.315(7) . ? N13 C20 1.337(8) . ? N14 C22 1.328(7) . ? N15 C22 1.294(7) . ? N15 N16 1.394(6) . ? N16 C23 1.303(6) . ? N17 C24 1.338(5) . ? N17 C24 1.339(5) 11_554 ? C1 C2 1.384(10) . ? C2 C3 1.379(10) . ? C4 C5 1.491(8) . ? C6 C7 1.487(7) . ? C7 C8 1.385(7) . ? C8 C9 1.393(8) . ? C9 C10 1.378(8) . ? C10 C11 1.388(7) . ? C11 C12 1.489(7) . ? C13 C14 1.503(8) . ? C15 C16 1.348(11) . ? C16 C17 1.382(10) . ? C18 C19 1.389(10) . ? C19 C20 1.390(10) . ? C21 C22 1.486(7) . ? C23 C24 1.491(7) . ? C24 C25 1.389(7) . ? C25 C26 1.400(6) . ? C26 C25 1.400(6) 11_554 ? 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 N8 Mn1 N4 166.37(18) 20_656 . ? N8 Mn1 O2 72.27(16) 20_656 20_656 ? N4 Mn1 O2 121.08(17) . 20_656 ? N8 Mn1 O1 110.61(16) 20_656 . ? N4 Mn1 O1 71.27(16) . . ? O2 Mn1 O1 101.21(14) 20_656 . ? N8 Mn1 N1 107.66(18) 20_656 . ? N4 Mn1 N1 71.82(17) . . ? O2 Mn1 N1 89.22(16) 20_656 . ? O1 Mn1 N1 141.71(16) . . ? N8 Mn1 N11 71.63(18) 20_656 20_656 ? N4 Mn1 N11 94.88(19) . 20_656 ? O2 Mn1 N11 143.82(16) 20_656 20_656 ? O1 Mn1 N11 93.63(16) . 20_656 ? N1 Mn1 N11 99.29(18) . 20_656 ? N15 Mn2 O3 72.11(15) . . ? N15 Mn2 N6 170.75(17) . . ? O3 Mn2 N6 116.40(14) . . ? N15 Mn2 O2 104.57(16) . . ? O3 Mn2 O2 94.12(14) . . ? N6 Mn2 O2 72.14(15) . . ? N15 Mn2 O1 111.71(16) . . ? O3 Mn2 O1 96.83(14) . . ? N6 Mn2 O1 71.99(15) . . ? O2 Mn2 O1 143.72(14) . . ? N15 Mn2 N12 70.47(16) . . ? O3 Mn2 N12 142.02(15) . . ? N6 Mn2 N12 101.39(16) . . ? O2 Mn2 N12 101.20(16) . . ? O1 Mn2 N12 91.03(16) . . ? N17 Mn3 N17 180.0 . 26_565 ? N17 Mn3 O3 107.37(9) . 26_565 ? N17 Mn3 O3 72.63(9) 26_565 26_565 ? N17 Mn3 O3 72.63(9) . 11_554 ? N17 Mn3 O3 107.37(9) 26_565 11_554 ? O3 Mn3 O3 95.11(5) 26_565 11_554 ? N17 Mn3 O3 72.63(9) . . ? N17 Mn3 O3 107.37(9) 26_565 . ? O3 Mn3 O3 95.12(5) 26_565 . ? O3 Mn3 O3 145.26(17) 11_554 . ? N17 Mn3 O3 107.37(9) . 20_656 ? N17 Mn3 O3 72.63(9) 26_565 20_656 ? O3 Mn3 O3 145.26(17) 26_565 20_656 ? O3 Mn3 O3 95.11(5) 11_554 20_656 ? O3 Mn3 O3 95.11(5) . 20_656 ? C6 O1 Mn1 114.2(3) . . ? C6 O1 Mn2 118.0(3) . . ? Mn1 O1 Mn2 127.64(17) . . ? C12 O2 Mn1 113.3(3) . 26_565 ? C12 O2 Mn2 119.0(3) . . ? Mn1 O2 Mn2 127.61(17) 26_565 . ? C23 O3 Mn2 113.1(3) . . ? C23 O3 Mn3 118.2(3) . . ? Mn2 O3 Mn3 128.65(15) . . ? O17 O16 O17 161(4) 22_776 . ? O16 O17 O18 176(3) . . ? O16 O17 O17 10(2) . 22_776 ? O18 O17 O17 168(2) . 22_776 ? O19 O18 O17 169(7) . . ? C1 N1 C4 116.6(5) . . ? C1 N1 Mn1 127.9(4) . . ? C4 N1 Mn1 115.4(4) . . ? C4 N2 C3 116.3(6) . . ? C5 N4 N5 117.3(5) . . ? C5 N4 Mn1 123.2(4) . . ? N5 N4 Mn1 119.3(3) . . ? C6 N5 N4 110.2(4) . . ? C7 N6 C11 119.6(4) . . ? C7 N6 Mn2 120.5(3) . . ? C11 N6 Mn2 119.9(3) . . ? C12 N7 N8 108.6(4) . . ? C13 N8 N7 116.8(5) . . ? C13 N8 Mn1 123.7(4) . 26_565 ? N7 N8 Mn1 119.6(3) . 26_565 ? C14 N10 C15 115.5(6) . . ? C14 N11 C17 114.8(5) . . ? C14 N11 Mn1 115.4(4) . 26_565 ? C17 N11 Mn1 129.8(5) . 26_565 ? C18 N12 C21 115.8(5) . . ? C18 N12 Mn2 129.9(4) . . ? C21 N12 Mn2 114.2(3) . . ? C21 N13 C20 117.1(6) . . ? C22 N15 N16 115.7(4) . . ? C22 N15 Mn2 124.9(4) . . ? N16 N15 Mn2 119.4(3) . . ? C23 N16 N15 108.3(4) . . ? C24 N17 C24 120.7(6) . 11_554 ? C24 N17 Mn3 119.7(3) . . ? C24 N17 Mn3 119.7(3) 11_554 . ? O6 N18 O4 121.4(8) . . ? O6 N18 O5 119.3(8) . . ? O4 N18 O5 119.3(7) . . ? O8 N19 O7 121(5) . . ? O8 N19 O9 117(4) . . ? O7 N19 O9 105(4) . . ? N1 C1 C2 122.3(6) . . ? C3 C2 C1 116.4(6) . . ? N2 C3 C2 122.5(6) . . ? N2 C4 N1 125.9(5) . . ? N2 C4 C5 118.4(5) . . ? N1 C4 C5 115.7(5) . . ? N4 C5 N3 127.5(6) . . ? N4 C5 C4 113.8(5) . . ? N3 C5 C4 118.7(5) . . ? O1 C6 N5 123.9(5) . . ? O1 C6 C7 117.5(4) . . ? N5 C6 C7 118.5(5) . . ? N6 C7 C8 122.1(5) . . ? N6 C7 C6 111.9(4) . . ? C8 C7 C6 126.0(5) . . ? C7 C8 C9 117.7(5) . . ? C10 C9 C8 120.7(5) . . ? C9 C10 C11 118.1(5) . . ? N6 C11 C10 121.8(5) . . ? N6 C11 C12 112.7(4) . . ? C10 C11 C12 125.5(5) . . ? N7 C12 O2 126.1(5) . . ? N7 C12 C11 118.0(4) . . ? O2 C12 C11 115.8(4) . . ? N8 C13 N9 127.8(5) . . ? N8 C13 C14 114.5(5) . . ? N9 C13 C14 117.7(5) . . ? N10 C14 N11 127.6(6) . . ? N10 C14 C13 117.6(6) . . ? N11 C14 C13 114.8(5) . . ? N10 C15 C16 121.9(6) . . ? C15 C16 C17 118.8(6) . . ? N11 C17 C16 121.4(7) . . ? N12 C18 C19 121.8(6) . . ? C18 C19 C20 117.4(6) . . ? N13 C20 C19 121.2(6) . . ? N13 C21 N12 126.6(5) . . ? N13 C21 C22 118.0(5) . . ? N12 C21 C22 115.3(5) . . ? N15 C22 N14 126.4(5) . . ? N15 C22 C21 115.0(5) . . ? N14 C22 C21 118.6(5) . . ? N16 C23 O3 126.4(5) . . ? N16 C23 C24 117.2(4) . . ? O3 C23 C24 116.4(4) . . ? N17 C24 C25 121.9(5) . . ? N17 C24 C23 112.9(4) . . ? C25 C24 C23 125.2(5) . . ? C24 C25 C26 117.5(5) . . ? C25 C26 C25 120.6(7) . 11_554 ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 30.93 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.012 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.110 #===END data_shelxl(8) _database_code_depnum_ccdc_archive 'CCDC 299035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H108.40 Cl10 Cu9 N66 O65.20' _chemical_formula_weight 4228.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 20.9857(14) _cell_length_b 20.9857(14) _cell_length_c 17.3731(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7651.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 24434 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.8 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4270.00 _exptl_absorpt_coefficient_mu 1.517 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7611 _exptl_absorpt_correction_T_max 0.8280 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 75957 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 30.97 _reflns_number_total 10853 _reflns_number_gt 9809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_publication_material 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0910P)^2^+23.3167P] 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 SHELXL _refine_ls_extinction_coef 0.00010(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10853 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.1023 _refine_ls_wR_factor_ref 0.2479 _refine_ls_wR_factor_gt 0.2406 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _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 Cu1 Cu 0.19990(3) 0.51767(3) 0.19717(4) 0.03561(18) Uani 1 1 d . . . Cu2 Cu 0.35875(3) 0.40799(3) 0.22252(3) 0.03125(17) Uani 1 1 d . . . Cu3 Cu 0.2500 0.2500 0.2500 0.0299(3) Uani 1 4 d S . . Cl1 Cl 0.54082(9) 0.22051(8) -0.07869(11) 0.0612(4) Uani 1 1 d . . . Cl2 Cl 0.59979(8) 0.43593(7) 0.04861(9) 0.0503(4) Uani 1 1 d . . . Cl3 Cl 0.7937(2) 0.6074(2) 0.1909(3) 0.0685(9) Uiso 0.50 1 d P . . O1 O 0.27649(17) 0.46029(17) 0.1684(2) 0.0354(8) Uani 1 1 d . . . O2 O 0.44370(19) 0.33930(19) 0.2175(2) 0.0408(8) Uani 1 1 d . . . O3 O 0.30653(16) 0.33602(16) 0.2750(2) 0.0324(7) Uani 1 1 d . . . O4 O 0.5587(3) 0.2612(4) -0.0255(3) 0.085(2) Uani 1 1 d . . . O5 O 0.5295(5) 0.2523(4) -0.1510(4) 0.122(3) Uani 1 1 d . . . O6 O 0.5902(3) 0.1744(3) -0.0865(5) 0.105(3) Uani 1 1 d . . . O7 O 0.4824(3) 0.1906(3) -0.0549(3) 0.0700(14) Uani 1 1 d . . . O8 O 0.6228(3) 0.3791(2) 0.0867(3) 0.0625(13) Uani 1 1 d . . . O9 O 0.5349(2) 0.4259(3) 0.0264(3) 0.0694(14) Uani 1 1 d . . . O10 O 0.6033(3) 0.4888(2) 0.1003(3) 0.0705(15) Uani 1 1 d . . . O11 O 0.6380(2) 0.4491(2) -0.0175(3) 0.0593(12) Uani 1 1 d . . . O12 O 0.8365(6) 0.6081(6) 0.2558(8) 0.088(4) Uiso 0.50 1 d P . . O13 O 0.7368(16) 0.5776(17) 0.2141(19) 0.224(13) Uiso 0.50 1 d P . . O14 O 0.8272(6) 0.6041(6) 0.1234(7) 0.068(3) Uiso 0.50 1 d P . . O15 O 0.7518(14) 0.6583(13) 0.1874(16) 0.181(9) Uiso 0.50 1 d P . . O16 O 0.3534(11) 0.3141(11) -0.3249(14) 0.150(7) Uiso 0.50 1 d P . . O17 O 0.3749(13) 0.2634(13) -0.2412(16) 0.103(7) Uiso 0.30 1 d P . . O18 O 0.4305(7) 0.3198(7) -0.3633(9) 0.092(4) Uiso 0.50 1 d P . . O19 O 0.7603(5) 0.3510(5) 0.0717(6) 0.090(3) Uiso 0.70 1 d P . . O20 O 0.8232(11) 0.3925(11) 0.0472(14) 0.126(7) Uiso 0.40 1 d P . . O21 O 0.7812(6) 0.4161(6) 0.0933(8) 0.101(4) Uiso 0.60 1 d P . . O22 O 0.7545(13) 0.4490(13) 0.1353(17) 0.108(8) Uiso 0.30 1 d P . . N1 N 0.1055(2) 0.5508(2) 0.1873(3) 0.0399(10) Uani 1 1 d . . . N2 N 0.0175(2) 0.5420(3) 0.1012(3) 0.0457(11) Uani 1 1 d . . . N3 N 0.1003(2) 0.4771(3) 0.0000(3) 0.0481(12) Uani 1 1 d . . . H4 H 0.1260 0.4557 -0.0306 0.058 Uiso 1 1 calc R . . H5 H 0.0609 0.4852 -0.0145 0.058 Uiso 1 1 calc R . . N4 N 0.1769(2) 0.4883(2) 0.0962(3) 0.0352(9) Uani 1 1 d . . . N5 N 0.2205(2) 0.4533(2) 0.0534(3) 0.0361(9) Uani 1 1 d . . . N6 N 0.36469(19) 0.38156(19) 0.1126(2) 0.0303(8) Uani 1 1 d . . . N7 N 0.2529(2) 0.6094(2) 0.1781(3) 0.0446(11) Uani 1 1 d . . . N8 N 0.3060(3) 0.6884(3) 0.2526(4) 0.0540(13) Uani 1 1 d . . . N9 N 0.2675(3) 0.6290(3) 0.3821(3) 0.0513(12) Uani 1 1 d . . . H12 H 0.2583 0.6098 0.4257 0.062 Uiso 1 1 calc R . . H13 H 0.2870 0.6661 0.3824 0.062 Uiso 1 1 calc R . . N10 N 0.2232(2) 0.5482(2) 0.3038(3) 0.0347(9) Uani 1 1 d . . . N11 N 0.2060(2) 0.5109(2) 0.3667(2) 0.0343(9) Uani 1 1 d . . . H21 H 0.2075 0.5224 0.4141 0.041 Uiso 1 1 d . . . N12 N 0.4148(2) 0.4911(2) 0.2142(2) 0.0339(9) Uani 1 1 d . . . N13 N 0.4360(3) 0.5825(2) 0.2925(3) 0.0466(12) Uani 1 1 d . . . N14 N 0.3811(2) 0.5172(2) 0.4154(3) 0.0432(11) Uani 1 1 d . . . H17 H 0.3635 0.4967 0.4542 0.052 Uiso 1 1 calc R . . H18 H 0.3983 0.5550 0.4228 0.052 Uiso 1 1 calc R . . N15 N 0.35776(19) 0.43558(19) 0.3271(2) 0.0319(8) Uani 1 1 d . . . N16 N 0.3296(2) 0.39807(19) 0.3831(2) 0.0315(8) Uani 1 1 d . . . N17 N 0.2500 0.2500 0.1386(3) 0.0282(11) Uani 1 2 d S . . C1 C 0.0690(3) 0.5823(3) 0.2376(4) 0.0523(15) Uani 1 1 d . . . H1 H 0.0868 0.5961 0.2850 0.063 Uiso 1 1 calc R . . C2 C 0.0059(3) 0.5949(4) 0.2217(4) 0.062(2) Uani 1 1 d . . . H2 H -0.0199 0.6177 0.2572 0.074 Uiso 1 1 calc R . . C3 C -0.0185(3) 0.5734(4) 0.1529(4) 0.0569(17) Uani 1 1 d . . . H3 H -0.0622 0.5810 0.1416 0.068 Uiso 1 1 calc R . . C4 C 0.0780(3) 0.5326(3) 0.1211(3) 0.0398(11) Uani 1 1 d . . . C5 C 0.1208(3) 0.4969(3) 0.0679(3) 0.0376(11) Uani 1 1 d . . . C6 C 0.2699(2) 0.4421(2) 0.0979(3) 0.0338(10) Uani 1 1 d . . . C7 C 0.3218(2) 0.4042(2) 0.0630(3) 0.0323(10) Uani 1 1 d . . . C8 C 0.3271(3) 0.3927(3) -0.0159(3) 0.0383(11) Uani 1 1 d . . . H6 H 0.2961 0.4088 -0.0507 0.046 Uiso 1 1 calc R . . C9 C 0.3784(3) 0.3575(3) -0.0427(3) 0.0409(12) Uani 1 1 d . . . H7 H 0.3831 0.3494 -0.0963 0.049 Uiso 1 1 calc R . . C10 C 0.4223(3) 0.3343(3) 0.0086(3) 0.0396(11) Uani 1 1 d . . . H8 H 0.4576 0.3100 -0.0090 0.048 Uiso 1 1 calc R . . C11 C 0.4146(2) 0.3470(2) 0.0870(3) 0.0312(9) Uani 1 1 d . . . C12 C 0.4575(2) 0.3262(2) 0.1499(3) 0.0333(10) Uani 1 1 d . . . C13 C 0.2719(3) 0.6383(3) 0.1135(4) 0.0575(17) Uani 1 1 d . . . H9 H 0.2594 0.6213 0.0651 0.069 Uiso 1 1 calc R . . C14 C 0.3090(4) 0.6923(4) 0.1158(5) 0.072(2) Uani 1 1 d . . . H10 H 0.3240 0.7118 0.0699 0.087 Uiso 1 1 calc R . . C15 C 0.3233(4) 0.7166(4) 0.1861(5) 0.074(2) Uani 1 1 d . . . H11 H 0.3467 0.7553 0.1886 0.089 Uiso 1 1 calc R . . C16 C 0.2713(3) 0.6364(3) 0.2444(4) 0.0416(12) Uani 1 1 d . . . C17 C 0.2518(3) 0.6020(2) 0.3158(3) 0.0369(11) Uani 1 1 d . . . C18 C 0.4434(3) 0.5192(3) 0.1546(3) 0.0427(12) Uani 1 1 d . . . H14 H 0.4466 0.4972 0.1070 0.051 Uiso 1 1 calc R . . C19 C 0.4683(3) 0.5800(3) 0.1610(4) 0.0535(15) Uani 1 1 d . . . H15 H 0.4887 0.5999 0.1185 0.064 Uiso 1 1 calc R . . C20 C 0.4626(4) 0.6108(3) 0.2309(4) 0.0565(17) Uani 1 1 d . . . H16 H 0.4780 0.6532 0.2356 0.068 Uiso 1 1 calc R . . C21 C 0.4127(3) 0.5244(2) 0.2806(3) 0.0369(11) Uani 1 1 d . . . C22 C 0.3816(2) 0.4912(2) 0.3458(3) 0.0344(10) Uani 1 1 d . . . C23 C 0.3066(2) 0.3478(2) 0.3489(3) 0.0304(9) Uani 1 1 d . . . C24 C 0.2500 0.2500 -0.0197(4) 0.0403(16) Uani 1 2 d S . . H19 H 0.2500 0.2500 -0.0744 0.048 Uiso 1 2 calc SR . . C25 C 0.2001(2) 0.2788(2) 0.0209(3) 0.0346(10) Uani 1 1 d . . . H20 H 0.1659 0.2988 -0.0057 0.042 Uiso 1 1 calc R . . C26 C 0.2016(2) 0.2776(2) 0.0997(3) 0.0308(9) 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 Cu1 0.0360(3) 0.0365(3) 0.0343(3) 0.0003(2) -0.0019(3) 0.0026(2) Cu2 0.0337(3) 0.0312(3) 0.0289(3) -0.0026(2) 0.0001(2) -0.0031(2) Cu3 0.0287(3) 0.0287(3) 0.0323(6) 0.000 0.000 0.000 Cl1 0.0710(11) 0.0485(8) 0.0641(11) 0.0019(8) 0.0134(9) 0.0014(7) Cl2 0.0577(9) 0.0495(8) 0.0435(7) -0.0026(6) 0.0065(6) -0.0119(6) O1 0.0377(18) 0.0369(18) 0.0317(18) -0.0028(14) -0.0017(15) 0.0013(14) O2 0.043(2) 0.047(2) 0.0330(19) -0.0026(16) -0.0008(16) 0.0056(17) O3 0.0324(17) 0.0330(17) 0.0318(17) -0.0047(14) 0.0005(14) -0.0037(13) O4 0.058(3) 0.158(6) 0.038(3) -0.001(3) 0.013(2) 0.035(3) O5 0.196(9) 0.101(5) 0.069(4) 0.043(4) -0.031(5) -0.053(5) O6 0.080(4) 0.065(4) 0.171(8) -0.033(4) 0.041(5) 0.002(3) O7 0.063(3) 0.081(4) 0.066(3) 0.004(3) 0.007(3) -0.002(3) O8 0.075(3) 0.052(3) 0.060(3) 0.004(2) 0.005(3) -0.008(2) O9 0.057(3) 0.085(4) 0.067(3) -0.001(3) 0.008(3) -0.016(3) O10 0.108(4) 0.053(3) 0.050(3) -0.007(2) 0.003(3) -0.010(3) O11 0.052(3) 0.077(3) 0.049(3) 0.004(2) 0.012(2) -0.010(2) N1 0.041(2) 0.046(2) 0.033(2) 0.0006(19) -0.0045(18) 0.0067(19) N2 0.039(2) 0.058(3) 0.040(2) -0.003(2) -0.004(2) 0.010(2) N3 0.036(2) 0.068(3) 0.040(3) -0.007(2) -0.006(2) 0.008(2) N4 0.032(2) 0.040(2) 0.033(2) -0.0002(18) -0.0011(17) 0.0038(17) N5 0.029(2) 0.044(2) 0.035(2) 0.0009(18) -0.0005(17) 0.0011(17) N6 0.0325(19) 0.0309(19) 0.0275(19) -0.0018(15) 0.0016(16) -0.0059(15) N7 0.051(3) 0.040(2) 0.042(3) -0.001(2) 0.002(2) -0.006(2) N8 0.059(3) 0.042(3) 0.061(3) 0.002(2) 0.001(3) -0.011(2) N9 0.068(3) 0.044(3) 0.042(3) -0.001(2) -0.004(2) -0.006(2) N10 0.036(2) 0.035(2) 0.033(2) 0.0002(17) 0.0012(17) -0.0013(17) N11 0.039(2) 0.036(2) 0.028(2) -0.0013(16) -0.0025(17) 0.0010(17) N12 0.037(2) 0.032(2) 0.033(2) -0.0014(16) -0.0006(17) -0.0062(16) N13 0.062(3) 0.034(2) 0.044(3) 0.000(2) 0.002(2) -0.014(2) N14 0.057(3) 0.039(2) 0.034(2) -0.0050(19) 0.002(2) -0.010(2) N15 0.034(2) 0.0309(19) 0.031(2) -0.0034(16) 0.0008(16) -0.0034(16) N16 0.039(2) 0.0303(19) 0.0253(19) -0.0003(15) 0.0000(16) -0.0031(16) N17 0.026(2) 0.029(3) 0.030(3) 0.000 0.000 -0.001(2) C1 0.057(4) 0.066(4) 0.035(3) -0.006(3) -0.005(3) 0.019(3) C2 0.052(4) 0.087(5) 0.047(4) -0.019(3) -0.006(3) 0.027(4) C3 0.047(3) 0.075(4) 0.048(4) -0.005(3) -0.007(3) 0.017(3) C4 0.036(3) 0.044(3) 0.039(3) 0.003(2) -0.003(2) 0.001(2) C5 0.038(3) 0.045(3) 0.030(2) 0.005(2) -0.001(2) 0.006(2) C6 0.037(2) 0.033(2) 0.031(2) -0.0001(19) -0.0013(19) -0.0029(19) C7 0.032(2) 0.031(2) 0.034(2) 0.0000(19) -0.0019(19) -0.0051(18) C8 0.039(3) 0.044(3) 0.032(3) -0.004(2) -0.001(2) -0.005(2) C9 0.039(3) 0.052(3) 0.031(2) -0.006(2) 0.001(2) -0.001(2) C10 0.036(3) 0.046(3) 0.037(3) -0.010(2) 0.001(2) -0.001(2) C11 0.033(2) 0.033(2) 0.028(2) -0.0011(18) 0.0002(18) -0.0049(18) C12 0.033(2) 0.035(2) 0.032(2) -0.0042(19) 0.0025(19) -0.0054(18) C13 0.066(4) 0.061(4) 0.046(4) 0.001(3) 0.012(3) -0.009(3) C14 0.094(6) 0.073(5) 0.050(4) 0.010(4) 0.016(4) -0.023(4) C15 0.082(6) 0.060(4) 0.081(6) 0.005(4) 0.010(5) -0.033(4) C16 0.044(3) 0.036(3) 0.045(3) -0.001(2) 0.001(2) -0.001(2) C17 0.043(3) 0.033(2) 0.034(3) -0.001(2) -0.003(2) 0.001(2) C18 0.048(3) 0.045(3) 0.036(3) 0.000(2) 0.000(2) -0.007(2) C19 0.056(4) 0.058(4) 0.046(3) 0.009(3) 0.004(3) -0.017(3) C20 0.070(4) 0.046(3) 0.053(4) 0.003(3) -0.002(3) -0.021(3) C21 0.043(3) 0.033(2) 0.035(3) 0.000(2) -0.001(2) -0.002(2) C22 0.038(2) 0.031(2) 0.034(2) -0.0004(19) -0.002(2) -0.0021(19) C23 0.029(2) 0.031(2) 0.031(2) -0.0002(18) -0.0004(18) 0.0013(17) C24 0.043(4) 0.047(4) 0.031(4) 0.000 0.000 0.000(3) C25 0.035(2) 0.036(2) 0.032(2) 0.000(2) -0.005(2) 0.0010(19) C26 0.027(2) 0.031(2) 0.034(2) 0.0033(19) -0.0028(18) -0.0034(17) _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 Cu1 N4 1.920(4) . ? Cu1 N10 2.020(4) . ? Cu1 O1 2.070(4) . ? Cu1 N1 2.106(5) . ? Cu1 N7 2.248(5) . ? Cu1 O2 2.298(4) 8_656 ? Cu2 N15 1.908(4) . ? Cu2 N6 1.993(4) . ? Cu2 O3 2.077(3) . ? Cu2 N12 2.109(4) . ? Cu2 O1 2.251(4) . ? Cu2 O2 2.294(4) . ? Cu3 N17 1.936(6) 6_566 ? Cu3 N17 1.936(6) . ? Cu3 O3 2.203(3) . ? Cu3 O3 2.203(3) 3 ? Cu3 O3 2.203(3) 8_656 ? Cu3 O3 2.203(3) 6_566 ? Cl1 O4 1.313(7) . ? Cl1 O6 1.425(6) . ? Cl1 O7 1.438(6) . ? Cl1 O5 1.441(6) . ? Cl2 O11 1.427(5) . ? Cl2 O10 1.430(5) . ? Cl2 O9 1.432(5) . ? Cl2 O8 1.446(5) . ? Cl3 O16 0.97(2) 4_565 ? Cl3 O18 1.350(15) 4_565 ? Cl3 O14 1.369(13) . ? Cl3 O15 1.38(3) . ? Cl3 O17 1.39(3) 4_565 ? Cl3 O13 1.41(3) . ? Cl3 O12 1.442(14) . ? O1 C6 1.290(6) . ? O2 C12 1.241(6) . ? O2 Cu1 2.298(4) 6_566 ? O3 C23 1.307(6) . ? O12 O17 1.58(3) 4_565 ? O12 O16 1.68(3) 4_565 ? O13 O17 1.38(4) 4_565 ? O13 O15 1.78(4) . ? O14 O18 0.778(16) 4_565 ? O14 O16 1.30(2) 4_565 ? O15 O16 1.35(3) 4_565 ? O15 O17 1.44(3) 4_565 ? O16 Cl3 0.97(2) 2_644 ? O16 O14 1.30(2) 2_644 ? O16 O15 1.35(3) 2_644 ? O16 O12 1.68(3) 2_644 ? O16 O18 1.75(3) . ? O17 O13 1.38(4) 2_644 ? O17 Cl3 1.39(3) 2_644 ? O17 O15 1.44(3) 2_644 ? O17 O12 1.58(3) 2_644 ? O18 O14 0.778(16) 2_644 ? O18 Cl3 1.349(15) 2_644 ? O19 O21 1.484(15) . ? O19 O20 1.64(2) . ? O20 O21 1.29(2) . ? O21 O22 1.15(3) . ? N1 C1 1.336(7) . ? N1 C4 1.342(7) . ? N2 C4 1.331(7) . ? N2 C3 1.347(8) . ? N3 C5 1.322(7) . ? N4 C5 1.290(7) . ? N4 N5 1.388(6) . ? N5 C6 1.314(6) . ? N6 C7 1.334(6) . ? N6 C11 1.350(6) . ? N7 C13 1.337(8) . ? N7 C16 1.340(8) . ? N8 C16 1.320(7) . ? N8 C15 1.346(10) . ? N9 C17 1.324(7) . ? N10 C17 1.297(7) . ? N10 N11 1.391(6) . ? N11 C12 1.340(6) 8_656 ? N12 C18 1.334(7) . ? N12 C21 1.349(7) . ? N13 C21 1.330(7) . ? N13 C20 1.344(8) . ? N14 C22 1.328(7) . ? N15 C22 1.310(6) . ? N15 N16 1.383(6) . ? N16 C23 1.304(6) . ? N17 C26 1.350(5) . ? N17 C26 1.351(5) 3 ? C1 C2 1.379(9) . ? C2 C3 1.377(9) . ? C4 C5 1.491(8) . ? C6 C7 1.478(7) . ? C7 C8 1.397(7) . ? C8 C9 1.387(8) . ? C9 C10 1.371(8) . ? C10 C11 1.396(7) . ? C11 C12 1.482(7) . ? C12 N11 1.340(6) 6_566 ? C13 C14 1.375(10) . ? C14 C15 1.358(11) . ? C16 C17 1.492(8) . ? C18 C19 1.382(8) . ? C19 C20 1.382(10) . ? C21 C22 1.480(7) . ? C23 C26 1.497(7) 6_566 ? C24 C25 1.400(6) . ? C24 C25 1.400(6) 3 ? C25 C26 1.371(7) . ? C26 C23 1.497(7) 8_656 ? 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 N4 Cu1 N10 179.40(19) . . ? N4 Cu1 O1 77.74(16) . . ? N10 Cu1 O1 102.55(16) . . ? N4 Cu1 N1 78.23(18) . . ? N10 Cu1 N1 101.40(18) . . ? O1 Cu1 N1 154.55(17) . . ? N4 Cu1 N7 105.35(19) . . ? N10 Cu1 N7 75.16(18) . . ? O1 Cu1 N7 94.51(17) . . ? N1 Cu1 N7 99.83(19) . . ? N4 Cu1 O2 106.39(17) . 8_656 ? N10 Cu1 O2 73.09(16) . 8_656 ? O1 Cu1 O2 92.32(15) . 8_656 ? N1 Cu1 O2 86.49(17) . 8_656 ? N7 Cu1 O2 148.25(16) . 8_656 ? N15 Cu2 N6 176.69(17) . . ? N15 Cu2 O3 78.28(15) . . ? N6 Cu2 O3 104.55(15) . . ? N15 Cu2 N12 79.63(17) . . ? N6 Cu2 N12 97.46(16) . . ? O3 Cu2 N12 157.80(15) . . ? N15 Cu2 O1 103.97(16) . . ? N6 Cu2 O1 77.50(15) . . ? O3 Cu2 O1 97.65(14) . . ? N12 Cu2 O1 89.79(15) . . ? N15 Cu2 O2 103.60(16) . . ? N6 Cu2 O2 74.95(15) . . ? O3 Cu2 O2 88.26(14) . . ? N12 Cu2 O2 94.79(16) . . ? O1 Cu2 O2 152.43(13) . . ? N17 Cu3 N17 180.0 6_566 . ? N17 Cu3 O3 78.64(9) 6_566 . ? N17 Cu3 O3 101.36(9) . . ? N17 Cu3 O3 78.64(9) 6_566 3 ? N17 Cu3 O3 101.36(9) . 3 ? O3 Cu3 O3 157.29(18) . 3 ? N17 Cu3 O3 101.36(9) 6_566 8_656 ? N17 Cu3 O3 78.64(9) . 8_656 ? O3 Cu3 O3 92.22(3) . 8_656 ? O3 Cu3 O3 92.23(4) 3 8_656 ? N17 Cu3 O3 101.36(9) 6_566 6_566 ? N17 Cu3 O3 78.64(9) . 6_566 ? O3 Cu3 O3 92.22(4) . 6_566 ? O3 Cu3 O3 92.22(3) 3 6_566 ? O3 Cu3 O3 157.28(18) 8_656 6_566 ? O4 Cl1 O6 107.5(4) . . ? O4 Cl1 O7 109.0(4) . . ? O6 Cl1 O7 110.6(4) . . ? O4 Cl1 O5 111.0(4) . . ? O6 Cl1 O5 110.5(6) . . ? O7 Cl1 O5 108.2(4) . . ? O11 Cl2 O10 109.1(3) . . ? O11 Cl2 O9 110.3(3) . . ? O10 Cl2 O9 109.4(4) . . ? O11 Cl2 O8 109.9(3) . . ? O10 Cl2 O8 109.6(3) . . ? O9 Cl2 O8 108.6(3) . . ? O16 Cl3 O18 97.2(16) 4_565 4_565 ? O16 Cl3 O14 64.7(14) 4_565 . ? O18 Cl3 O14 33.2(7) 4_565 . ? O16 Cl3 O15 67.2(15) 4_565 . ? O18 Cl3 O15 133.1(14) 4_565 . ? O14 Cl3 O15 109.2(13) . . ? O16 Cl3 O17 102.5(19) 4_565 4_565 ? O18 Cl3 O17 159.2(14) 4_565 4_565 ? O14 Cl3 O17 167.2(13) . 4_565 ? O15 Cl3 O17 62.7(14) . 4_565 ? O16 Cl3 O13 147(2) 4_565 . ? O18 Cl3 O13 106.4(16) 4_565 . ? O14 Cl3 O13 131.2(15) . . ? O15 Cl3 O13 79.4(16) . . ? O17 Cl3 O13 59.1(15) 4_565 . ? O16 Cl3 O12 86.4(15) 4_565 . ? O18 Cl3 O12 107.4(9) 4_565 . ? O14 Cl3 O12 110.5(8) . . ? O15 Cl3 O12 114.9(13) . . ? O17 Cl3 O12 67.6(12) 4_565 . ? O13 Cl3 O12 108.0(15) . . ? C6 O1 Cu1 108.6(3) . . ? C6 O1 Cu2 109.5(3) . . ? Cu1 O1 Cu2 141.13(18) . . ? C12 O2 Cu2 110.9(3) . . ? C12 O2 Cu1 111.9(3) . 6_566 ? Cu2 O2 Cu1 136.50(18) . 6_566 ? C23 O3 Cu2 107.0(3) . . ? C23 O3 Cu3 110.4(3) . . ? Cu2 O3 Cu3 142.53(17) . . ? Cl3 O12 O17 54.7(11) . 4_565 ? Cl3 O12 O16 34.9(8) . 4_565 ? O17 O12 O16 69.4(14) 4_565 4_565 ? O17 O13 Cl3 59.8(19) 4_565 . ? O17 O13 O15 52.4(17) 4_565 . ? Cl3 O13 O15 49.7(14) . . ? O18 O14 O16 113(2) 4_565 4_565 ? O18 O14 Cl3 72.0(16) 4_565 . ? O16 O14 Cl3 42.4(11) 4_565 . ? O16 O15 Cl3 41.4(13) 4_565 . ? O16 O15 O17 83(2) 4_565 4_565 ? Cl3 O15 O17 58.9(15) . 4_565 ? O16 O15 O13 92(2) 4_565 . ? Cl3 O15 O13 50.9(13) . . ? O17 O15 O13 49.3(15) 4_565 . ? Cl3 O16 O14 72.8(16) 2_644 2_644 ? Cl3 O16 O15 71.4(19) 2_644 2_644 ? O14 O16 O15 116(2) 2_644 2_644 ? Cl3 O16 O12 58.7(13) 2_644 2_644 ? O14 O16 O12 100.8(16) 2_644 2_644 ? O15 O16 O12 103(2) 2_644 2_644 ? Cl3 O16 O18 49.7(12) 2_644 . ? O14 O16 O18 24.0(8) 2_644 . ? O15 O16 O18 107(2) 2_644 . ? O12 O16 O18 81.7(12) 2_644 . ? O13 O17 Cl3 61.0(18) 2_644 2_644 ? O13 O17 O15 78(2) 2_644 2_644 ? Cl3 O17 O15 58.5(16) 2_644 2_644 ? O13 O17 O12 102(2) 2_644 2_644 ? Cl3 O17 O12 57.8(12) 2_644 2_644 ? O15 O17 O12 104(2) 2_644 2_644 ? O14 O18 Cl3 74.7(16) 2_644 2_644 ? O14 O18 O16 42.7(15) 2_644 . ? Cl3 O18 O16 33.1(8) 2_644 . ? O21 O19 O20 48.5(9) . . ? O21 O20 O19 59.5(12) . . ? O22 O21 O20 163(2) . . ? O22 O21 O19 124.6(18) . . ? O20 O21 O19 72.1(13) . . ? C1 N1 C4 117.0(5) . . ? C1 N1 Cu1 130.5(4) . . ? C4 N1 Cu1 112.4(4) . . ? C4 N2 C3 115.7(5) . . ? C5 N4 N5 118.2(4) . . ? C5 N4 Cu1 122.2(4) . . ? N5 N4 Cu1 119.6(3) . . ? C6 N5 N4 107.4(4) . . ? C7 N6 C11 120.2(4) . . ? C7 N6 Cu2 118.5(3) . . ? C11 N6 Cu2 120.9(3) . . ? C13 N7 C16 116.3(5) . . ? C13 N7 Cu1 131.3(4) . . ? C16 N7 Cu1 112.2(4) . . ? C16 N8 C15 114.8(6) . . ? C17 N10 N11 118.9(4) . . ? C17 N10 Cu1 122.4(4) . . ? N11 N10 Cu1 118.6(3) . . ? C12 N11 N10 115.6(4) 8_656 . ? C18 N12 C21 116.7(5) . . ? C18 N12 Cu2 132.0(4) . . ? C21 N12 Cu2 110.6(3) . . ? C21 N13 C20 115.8(5) . . ? C22 N15 N16 119.8(4) . . ? C22 N15 Cu2 120.1(4) . . ? N16 N15 Cu2 120.1(3) . . ? C23 N16 N15 107.4(4) . . ? C26 N17 C26 120.1(6) . 3 ? C26 N17 Cu3 120.0(3) . . ? C26 N17 Cu3 120.0(3) 3 . ? N1 C1 C2 121.0(6) . . ? C3 C2 C1 118.0(6) . . ? N2 C3 C2 122.1(6) . . ? N2 C4 N1 126.3(5) . . ? N2 C4 C5 119.1(5) . . ? N1 C4 C5 114.6(5) . . ? N4 C5 N3 126.4(5) . . ? N4 C5 C4 112.6(5) . . ? N3 C5 C4 121.0(5) . . ? O1 C6 N5 126.1(5) . . ? O1 C6 C7 118.1(4) . . ? N5 C6 C7 115.8(4) . . ? N6 C7 C8 121.2(5) . . ? N6 C7 C6 115.1(4) . . ? C8 C7 C6 123.7(5) . . ? C9 C8 C7 119.0(5) . . ? C10 C9 C8 119.5(5) . . ? C9 C10 C11 119.3(5) . . ? N6 C11 C10 120.9(5) . . ? N6 C11 C12 112.7(4) . . ? C10 C11 C12 126.4(5) . . ? O2 C12 N11 120.7(5) . 6_566 ? O2 C12 C11 119.5(5) . . ? N11 C12 C11 119.8(4) 6_566 . ? N7 C13 C14 121.2(7) . . ? C15 C14 C13 117.4(7) . . ? N8 C15 C14 123.2(7) . . ? N8 C16 N7 126.9(6) . . ? N8 C16 C17 117.5(5) . . ? N7 C16 C17 115.6(5) . . ? N10 C17 N9 128.8(5) . . ? N10 C17 C16 114.5(5) . . ? N9 C17 C16 116.7(5) . . ? N12 C18 C19 121.0(6) . . ? C20 C19 C18 118.0(6) . . ? N13 C20 C19 121.9(6) . . ? N13 C21 N12 126.5(5) . . ? N13 C21 C22 118.5(5) . . ? N12 C21 C22 115.1(4) . . ? N15 C22 N14 126.0(5) . . ? N15 C22 C21 113.5(5) . . ? N14 C22 C21 120.4(5) . . ? N16 C23 O3 126.9(4) . . ? N16 C23 C26 116.0(4) . 6_566 ? O3 C23 C26 117.0(4) . 6_566 ? C25 C24 C25 119.5(7) . 3 ? C26 C25 C24 118.6(5) . . ? N17 C26 C25 121.6(5) . . ? N17 C26 C23 113.4(4) . 8_656 ? C25 C26 C23 125.0(4) . 8_656 ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 30.97 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 1.157 _refine_diff_density_min -1.405 _refine_diff_density_rms 0.119