# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Murray, Keith' _publ_contact_author_email k.s.murray@sci.monash.edu.au _publ_section_title ; Synthesis and characterization of homo- and hetero-valent tetra- hexa- hepta- and decanuclear manganese clusters using pyridyl functionalized \^I^2^-diketone, carboxylate and triethanolamine ligands. ; _publ_author_name K.Murray # Attachment '- 1 Mn10final3.CIF' #========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 768051' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C116 H82 Mn10 N6 O35, 4(C H2 Cl2) ; _chemical_formula_sum 'C120 H90 Cl8 Mn10 N6 O35' _chemical_formula_weight 3009.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.000(3) _cell_length_b 15.770(3) _cell_length_c 26.938(5) _cell_angle_alpha 77.53(3) _cell_angle_beta 76.12(3) _cell_angle_gamma 77.04(3) _cell_volume 5939(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 64555 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8935 _exptl_absorpt_correction_T_max 0.9446 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77506 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 64555 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 18730 _reflns_number_gt 15165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data was collected on the Australian synchrotron in which only a wavelength of 0.77 A and a resolution of ~0.9 A was possible. We were also restricted to one 360 degree phi scan. The asymmetric unit consists of the cluster and 4 solvent DCM molecules. Only one of the DCM molecules could be modelled satisfactorily hence the squeeze program was employed which removed the electron density of the other three. Thermal restraints (SIMU, DELU and ISOR) were placed on the phenyl ring which is disordered over two positions. (C1A - C6A and C104 - C109). All non H-atoms were refined anisotropically, with all H-atoms placed in calculated positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+12.8973P] 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 18730 _refine_ls_number_parameters 1566 _refine_ls_number_restraints 163 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.032 _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 0.26230(3) 0.56407(4) 0.15064(2) 0.01850(13) Uani 1 1 d . . . Mn2 Mn 0.05929(3) 0.54397(4) 0.19096(2) 0.01840(13) Uani 1 1 d . . . Mn3 Mn 0.10768(3) 0.70367(4) 0.11347(2) 0.01717(13) Uani 1 1 d . . . Mn4 Mn 0.13531(3) 0.68476(4) 0.22734(2) 0.01753(13) Uani 1 1 d . . . Mn5 Mn 0.19922(4) 0.52266(4) 0.29040(2) 0.02026(14) Uani 1 1 d . . . Mn6 Mn -0.05846(3) 0.74777(4) 0.23539(2) 0.01850(13) Uani 1 1 d . . . Mn7 Mn 0.26350(3) 0.79194(4) 0.16256(2) 0.01822(13) Uani 1 1 d . . . Mn8 Mn 0.29310(4) 0.69975(4) 0.30135(2) 0.02596(15) Uani 1 1 d . . . Mn9 Mn 0.00981(4) 0.68937(4) 0.35782(2) 0.02166(14) Uani 1 1 d . . . Mn10 Mn 0.07807(4) 0.90929(4) 0.24070(2) 0.02192(14) Uani 1 1 d . . . O1 O 0.14543(15) 0.58093(16) 0.13094(9) 0.0175(5) Uani 1 1 d . . . O2 O 0.31604(16) 0.59795(17) 0.07010(10) 0.0231(6) Uani 1 1 d . . . O3 O 0.00016(16) 0.66981(17) 0.08606(10) 0.0229(6) Uani 1 1 d . . . O4 O 0.27852(17) 0.43811(17) 0.15381(11) 0.0256(6) Uani 1 1 d . . . O5 O 0.12970(17) 0.41397(17) 0.18209(10) 0.0242(6) Uani 1 1 d . . . O6 O 0.38370(16) 0.54983(17) 0.16586(10) 0.0238(6) Uani 1 1 d . . . O7 O 0.34594(18) 0.48198(19) 0.24811(11) 0.0326(7) Uani 1 1 d . . . O8 O 0.14441(16) 0.56013(16) 0.23038(9) 0.0195(5) Uani 1 1 d . . . O9 O -0.03125(16) 0.55227(17) 0.14743(10) 0.0235(6) Uani 1 1 d . . . O10 O 0.04151(16) 0.70000(16) 0.18520(9) 0.0192(5) Uani 1 1 d . . . O11 O 0.22630(15) 0.68408(16) 0.16227(9) 0.0187(5) Uani 1 1 d . . . O12 O -0.02674(16) 0.50113(17) 0.25180(10) 0.0221(6) Uani 1 1 d . . . O13 O -0.12679(17) 0.62978(17) 0.25606(10) 0.0243(6) Uani 1 1 d . . . O14 O 0.06310(16) 0.82707(16) 0.09499(9) 0.0208(5) Uani 1 1 d . . . O15 O 0.19178(17) 0.87167(18) 0.10053(10) 0.0257(6) Uani 1 1 d . . . O16 O 0.16071(16) 0.79826(16) 0.21589(10) 0.0200(5) Uani 1 1 d . . . O17 O 0.02904(16) 0.71154(17) 0.27707(9) 0.0213(5) Uani 1 1 d . . . O18 O 0.21144(16) 0.63925(17) 0.27541(9) 0.0210(5) Uani 1 1 d . . . O19 O 0.37527(16) 0.76804(17) 0.10924(10) 0.0230(6) Uani 1 1 d . . . O20 O 0.35699(16) 0.73895(17) 0.21953(10) 0.0238(6) Uani 1 1 d . . . O21 O 0.17606(17) 0.40410(17) 0.29879(10) 0.0242(6) Uani 1 1 d . . . O22 O 0.06993(16) 0.54711(17) 0.34872(9) 0.0220(6) Uani 1 1 d . . . O23 O -0.03103(16) 0.88424(17) 0.20820(10) 0.0223(6) Uani 1 1 d . . . O24 O 0.01811(19) 1.03971(19) 0.21383(12) 0.0335(7) Uani 1 1 d . . . O25 O 0.25991(18) 0.48263(19) 0.35138(10) 0.0293(6) Uani 1 1 d . . . O26 O 0.3303(2) 0.5899(2) 0.35835(12) 0.0376(7) Uani 1 1 d . . . O27 O 0.29493(17) 0.90513(17) 0.16655(10) 0.0240(6) Uani 1 1 d . . . O28 O 0.20526(18) 0.95136(19) 0.23907(11) 0.0302(6) Uani 1 1 d . . . O29 O 0.2311(2) 0.7957(2) 0.34646(11) 0.0361(7) Uani 1 1 d . A . O30 O 0.12990(19) 0.70519(19) 0.38149(11) 0.0333(7) Uani 1 1 d . A . O31 O 0.0220(2) 0.9060(2) 0.31747(11) 0.0369(7) Uani 1 1 d . . . O32 O -0.0535(2) 0.81613(19) 0.38093(11) 0.0336(7) Uani 1 1 d . . . O33 O -0.14367(18) 0.7010(2) 0.35632(11) 0.0328(7) Uani 1 1 d . . . O34 O -0.15930(17) 0.80372(18) 0.28540(10) 0.0253(6) Uani 1 1 d . . . O35 O 0.19702(16) 0.70351(17) 0.04709(10) 0.0214(6) Uani 1 1 d . . . N1 N 0.4366(2) 0.7210(2) 0.29856(13) 0.0296(8) Uani 1 1 d . . . N2 N 0.6207(2) 0.7359(3) 0.06534(14) 0.0374(9) Uani 1 1 d . . . N3 N -0.14332(19) 0.8033(2) 0.18245(11) 0.0202(7) Uani 1 1 d . . . N4 N -0.1742(3) 1.2098(3) 0.19531(18) 0.0501(11) Uani 1 1 d . . . N5 N -0.0464(2) 0.5994(2) 0.43018(12) 0.0234(7) Uani 1 1 d . . . N6 N 0.0626(3) 0.2252(3) 0.36104(16) 0.0464(11) Uani 1 1 d . . . C1 C 0.2752(2) 0.6504(3) 0.03730(14) 0.0221(8) Uani 1 1 d . . . C2 C 0.3209(2) 0.6523(3) -0.01891(14) 0.0225(8) Uani 1 1 d . . . C3 C 0.2893(3) 0.7183(3) -0.05730(15) 0.0291(9) Uani 1 1 d . . . H3 H 0.2371 0.7629 -0.0482 0.035 Uiso 1 1 calc R . . C4 C 0.3338(3) 0.7195(3) -0.10882(17) 0.0382(11) Uani 1 1 d . . . H4 H 0.3119 0.7646 -0.1351 0.046 Uiso 1 1 calc R . . C5 C 0.4103(3) 0.6546(3) -0.12182(17) 0.0406(11) Uani 1 1 d . . . H5 H 0.4418 0.6561 -0.1570 0.049 Uiso 1 1 calc R . . C6 C 0.4410(3) 0.5877(3) -0.08398(17) 0.0377(11) Uani 1 1 d . . . H6 H 0.4923 0.5425 -0.0933 0.045 Uiso 1 1 calc R . . C7 C 0.3972(3) 0.5866(3) -0.03262(16) 0.0306(9) Uani 1 1 d . . . H7 H 0.4190 0.5411 -0.0065 0.037 Uiso 1 1 calc R . . C8 C -0.0332(2) 0.6011(3) 0.10247(14) 0.0236(8) Uani 1 1 d . . . C9 C -0.0795(2) 0.5710(3) 0.06751(15) 0.0239(8) Uani 1 1 d . . . C10 C -0.1305(3) 0.5028(3) 0.08586(17) 0.0336(10) Uani 1 1 d . . . H10 H -0.1384 0.4763 0.1214 0.040 Uiso 1 1 calc R . . C11 C -0.1695(3) 0.4737(3) 0.05256(19) 0.0430(12) Uani 1 1 d . . . H11 H -0.2057 0.4284 0.0656 0.052 Uiso 1 1 calc R . . C12 C -0.1564(3) 0.5099(3) 0.00058(19) 0.0425(12) Uani 1 1 d . . . H12 H -0.1824 0.4889 -0.0223 0.051 Uiso 1 1 calc R . . C13 C -0.1046(3) 0.5776(3) -0.01832(17) 0.0350(10) Uani 1 1 d . . . H13 H -0.0945 0.6022 -0.0542 0.042 Uiso 1 1 calc R . . C14 C -0.0685(3) 0.6084(3) 0.01510(16) 0.0291(9) Uani 1 1 d . . . H14 H -0.0354 0.6560 0.0023 0.035 Uiso 1 1 calc R . . C15 C 0.2145(3) 0.3898(3) 0.16435(14) 0.0232(8) Uani 1 1 d . . . C16 C 0.2467(3) 0.2991(3) 0.15283(16) 0.0277(9) Uani 1 1 d . . . C17 C 0.1822(3) 0.2526(3) 0.14794(16) 0.0299(9) Uani 1 1 d . . . H17 H 0.1180 0.2790 0.1528 0.036 Uiso 1 1 calc R . . C18 C 0.2098(3) 0.1684(3) 0.13615(18) 0.0392(11) Uani 1 1 d . . . H18 H 0.1649 0.1372 0.1328 0.047 Uiso 1 1 calc R . . C19 C 0.3030(3) 0.1300(3) 0.1292(2) 0.0454(12) Uani 1 1 d . . . H19 H 0.3226 0.0726 0.1203 0.054 Uiso 1 1 calc R . . C20 C 0.3686(3) 0.1754(3) 0.1354(2) 0.0449(12) Uani 1 1 d . . . H20 H 0.4327 0.1484 0.1314 0.054 Uiso 1 1 calc R . . C21 C 0.3402(3) 0.2599(3) 0.14726(17) 0.0353(10) Uani 1 1 d . . . H21 H 0.3847 0.2908 0.1516 0.042 Uiso 1 1 calc R . . C22 C 0.1117(2) 0.8870(3) 0.09076(14) 0.0217(8) Uani 1 1 d . . . C23 C 0.0669(3) 0.9794(3) 0.07242(15) 0.0261(9) Uani 1 1 d . . . C24 C 0.1135(3) 1.0491(3) 0.0664(2) 0.0444(12) Uani 1 1 d . . . H24 H 0.1735 1.0381 0.0748 0.053 Uiso 1 1 calc R . . C25 C 0.0726(4) 1.1344(3) 0.0482(3) 0.0596(16) Uani 1 1 d . . . H25 H 0.1060 1.1811 0.0433 0.072 Uiso 1 1 calc R . . C26 C -0.0155(3) 1.1531(3) 0.0370(2) 0.0452(12) Uani 1 1 d . . . H26 H -0.0430 1.2121 0.0250 0.054 Uiso 1 1 calc R . . C27 C -0.0634(3) 1.0839(3) 0.04369(17) 0.0355(10) Uani 1 1 d . . . H27 H -0.1245 1.0956 0.0368 0.043 Uiso 1 1 calc R . . C28 C -0.0214(3) 0.9979(3) 0.06050(15) 0.0290(9) Uani 1 1 d . . . H28 H -0.0536 0.9508 0.0639 0.035 Uiso 1 1 calc R . . C29 C -0.1012(2) 0.5503(3) 0.27232(15) 0.0237(8) Uani 1 1 d . . . C30 C -0.1604(3) 0.5029(3) 0.31903(15) 0.0261(9) Uani 1 1 d . . . C31 C -0.2379(3) 0.5516(3) 0.34657(19) 0.0422(11) Uani 1 1 d . . . H31 H -0.2547 0.6134 0.3357 0.051 Uiso 1 1 calc R . . C32 C -0.2907(4) 0.5080(4) 0.3906(2) 0.0635(17) Uani 1 1 d . . . H32 H -0.3432 0.5408 0.4102 0.076 Uiso 1 1 calc R . . C33 C -0.2682(5) 0.4194(4) 0.4058(2) 0.0689(19) Uani 1 1 d . . . H33 H -0.3055 0.3910 0.4357 0.083 Uiso 1 1 calc R . . C34 C -0.1923(4) 0.3703(4) 0.37860(19) 0.0523(14) Uani 1 1 d . . . H34 H -0.1773 0.3082 0.3892 0.063 Uiso 1 1 calc R . . C35 C -0.1372(3) 0.4129(3) 0.33504(17) 0.0348(10) Uani 1 1 d . . . H35 H -0.0837 0.3798 0.3164 0.042 Uiso 1 1 calc R . . C36 C -0.1844(2) 0.7565(3) 0.16211(15) 0.0262(9) Uani 1 1 d . . . H36 H -0.1742 0.6941 0.1719 0.031 Uiso 1 1 calc R . . C37 C -0.2420(3) 0.7965(3) 0.12689(16) 0.0330(10) Uani 1 1 d . . . H37 H -0.2699 0.7622 0.1120 0.040 Uiso 1 1 calc R . . C38 C -0.2575(3) 0.8874(3) 0.11415(17) 0.0360(10) Uani 1 1 d . . . H38 H -0.2968 0.9166 0.0904 0.043 Uiso 1 1 calc R . . C39 C -0.2161(3) 0.9360(3) 0.13591(16) 0.0326(10) Uani 1 1 d . . . H39 H -0.2277 0.9987 0.1278 0.039 Uiso 1 1 calc R . . C40 C -0.1577(3) 0.8932(3) 0.16942(15) 0.0266(9) Uani 1 1 d . . . C41 C -0.0988(2) 0.9379(3) 0.19056(14) 0.0238(9) Uani 1 1 d . . . C42 C -0.1186(3) 1.0277(3) 0.18916(16) 0.0289(9) Uani 1 1 d . . . H42 H -0.1743 1.0602 0.1785 0.035 Uiso 1 1 calc R . . C43 C -0.0606(3) 1.0738(3) 0.20267(16) 0.0304(9) Uani 1 1 d . . . C44 C -0.0910(3) 1.1707(3) 0.20504(17) 0.0353(10) Uani 1 1 d . . . C45 C -0.0322(3) 1.2130(3) 0.21892(18) 0.0370(10) Uani 1 1 d . . . H45 H 0.0268 1.1819 0.2259 0.044 Uiso 1 1 calc R . . C46 C -0.2021(4) 1.2959(4) 0.2002(2) 0.0606(16) Uani 1 1 d . . . H46 H -0.2621 1.3249 0.1941 0.073 Uiso 1 1 calc R . . C47 C -0.1475(4) 1.3433(3) 0.2136(2) 0.0506(13) Uani 1 1 d . . . H47 H -0.1700 1.4037 0.2166 0.061 Uiso 1 1 calc R . . C48 C -0.0608(3) 1.3030(3) 0.2226(2) 0.0424(11) Uani 1 1 d . . . H48 H -0.0212 1.3348 0.2311 0.051 Uiso 1 1 calc R . . C49 C -0.1059(3) 0.6309(3) 0.47026(15) 0.0267(9) Uani 1 1 d . . . H49 H -0.1156 0.6923 0.4710 0.032 Uiso 1 1 calc R . . C50 C -0.1544(3) 0.5773(3) 0.51107(15) 0.0280(9) Uani 1 1 d . . . H50 H -0.1950 0.6012 0.5397 0.034 Uiso 1 1 calc R . . C51 C -0.1420(3) 0.4892(3) 0.50882(16) 0.0349(10) Uani 1 1 d . . . H51 H -0.1742 0.4510 0.5360 0.042 Uiso 1 1 calc R . . C52 C -0.0816(3) 0.4561(3) 0.46636(15) 0.0288(9) Uani 1 1 d . . . H52 H -0.0732 0.3956 0.4638 0.035 Uiso 1 1 calc R . . C53 C -0.0341(2) 0.5136(3) 0.42799(14) 0.0245(9) Uani 1 1 d . . . C54 C 0.0357(2) 0.4851(3) 0.38140(14) 0.0227(8) Uani 1 1 d . . . C55 C 0.0583(3) 0.3963(3) 0.37593(15) 0.0278(9) Uani 1 1 d . . . H55 H 0.0291 0.3554 0.4027 0.033 Uiso 1 1 calc R . . C56 C 0.1209(3) 0.3629(3) 0.33379(15) 0.0245(8) Uani 1 1 d . . . C57 C 0.1234(3) 0.2711(3) 0.32693(15) 0.0277(9) Uani 1 1 d . . . C58 C 0.1850(3) 0.2364(3) 0.28587(16) 0.0353(10) Uani 1 1 d . . . H58 H 0.2261 0.2710 0.2618 0.042 Uiso 1 1 calc R . . C59 C 0.0650(4) 0.1431(4) 0.3540(2) 0.0562(15) Uani 1 1 d . . . H59 H 0.0219 0.1103 0.3777 0.067 Uiso 1 1 calc R . . C60 C 0.1255(4) 0.1025(3) 0.31504(19) 0.0463(12) Uani 1 1 d . . . H60 H 0.1252 0.0435 0.3124 0.056 Uiso 1 1 calc R . . C61 C 0.1863(3) 0.1511(3) 0.28019(17) 0.0395(11) Uani 1 1 d . . . H61 H 0.2287 0.1263 0.2525 0.047 Uiso 1 1 calc R . . C62 C 0.4707(3) 0.7160(3) 0.34069(18) 0.0394(11) Uani 1 1 d . . . H62 H 0.4329 0.7008 0.3739 0.047 Uiso 1 1 calc R . . C63 C 0.5591(3) 0.7321(4) 0.33801(18) 0.0447(12) Uani 1 1 d . . . H63 H 0.5815 0.7289 0.3686 0.054 Uiso 1 1 calc R . . C64 C 0.6138(3) 0.7531(3) 0.28921(18) 0.0431(12) Uani 1 1 d . . . H64 H 0.6745 0.7649 0.2858 0.052 Uiso 1 1 calc R . . C65 C 0.5791(3) 0.7567(3) 0.24580(17) 0.0344(10) Uani 1 1 d . . . H65 H 0.6162 0.7697 0.2121 0.041 Uiso 1 1 calc R . . C66 C 0.4894(3) 0.7410(3) 0.25174(16) 0.0282(9) Uani 1 1 d . . . C67 C 0.4435(2) 0.7466(3) 0.20690(15) 0.0243(8) Uani 1 1 d . . . C68 C 0.4945(2) 0.7556(3) 0.15710(15) 0.0257(9) Uani 1 1 d . . . H68 H 0.5574 0.7628 0.1522 0.031 Uiso 1 1 calc R . . C69 C 0.4612(2) 0.7550(3) 0.11300(15) 0.0245(8) Uani 1 1 d . . . C70 C 0.5311(3) 0.7357(3) 0.06527(15) 0.0265(9) Uani 1 1 d . . . C71 C 0.5027(3) 0.7151(3) 0.02538(17) 0.0359(10) Uani 1 1 d . . . H71 H 0.4384 0.7168 0.0268 0.043 Uiso 1 1 calc R . . C72 C 0.6838(3) 0.7143(4) 0.02404(18) 0.0441(12) Uani 1 1 d . . . H72 H 0.7474 0.7146 0.0232 0.053 Uiso 1 1 calc R . . C73 C 0.6626(3) 0.6914(4) -0.01764(18) 0.0448(12) Uani 1 1 d . . . H73 H 0.7105 0.6757 -0.0461 0.054 Uiso 1 1 calc R . . C74 C 0.5703(3) 0.6915(4) -0.01736(19) 0.0498(14) Uani 1 1 d . . . H74 H 0.5533 0.6760 -0.0456 0.060 Uiso 1 1 calc R . . C75 C 0.2823(3) 0.9356(3) 0.20883(16) 0.0278(9) Uani 1 1 d . . . C76 C 0.3676(3) 0.9523(3) 0.22249(17) 0.0304(9) Uani 1 1 d . . . C77 C 0.4471(3) 0.9629(3) 0.18481(19) 0.0345(10) Uani 1 1 d . . . H77 H 0.4485 0.9585 0.1500 0.041 Uiso 1 1 calc R . . C78 C 0.5246(3) 0.9800(3) 0.1977(2) 0.0493(13) Uani 1 1 d . . . H78 H 0.5783 0.9893 0.1715 0.059 Uiso 1 1 calc R . . C79 C 0.5237(3) 0.9834(4) 0.2492(2) 0.0587(16) Uani 1 1 d . . . H79 H 0.5768 0.9950 0.2583 0.070 Uiso 1 1 calc R . . C80 C 0.4452(4) 0.9699(4) 0.2869(2) 0.0552(15) Uani 1 1 d . . . H80 H 0.4452 0.9705 0.3221 0.066 Uiso 1 1 calc R . . C81 C 0.3667(3) 0.9556(3) 0.27400(19) 0.0400(11) Uani 1 1 d . . . H81 H 0.3124 0.9480 0.3000 0.048 Uiso 1 1 calc R . . C82 C 0.3176(3) 0.5123(3) 0.36790(15) 0.0286(9) Uani 1 1 d . . . C83 C 0.3756(3) 0.4464(3) 0.40181(16) 0.0332(10) Uani 1 1 d . . . C84 C 0.4173(4) 0.4747(4) 0.4351(2) 0.0579(15) Uani 1 1 d . . . H84 H 0.4075 0.5357 0.4369 0.069 Uiso 1 1 calc R . . C85 C 0.4724(5) 0.4138(5) 0.4653(3) 0.089(3) Uani 1 1 d . . . H85 H 0.4978 0.4326 0.4894 0.107 Uiso 1 1 calc R . . C86 C 0.4908(6) 0.3265(5) 0.4609(4) 0.109(3) Uani 1 1 d . . . H86 H 0.5300 0.2854 0.4815 0.131 Uiso 1 1 calc R . . C87 C 0.4527(6) 0.2969(5) 0.4264(3) 0.091(2) Uani 1 1 d . . . H87 H 0.4677 0.2367 0.4223 0.110 Uiso 1 1 calc R . . C88 C 0.3928(4) 0.3574(4) 0.3984(2) 0.0519(13) Uani 1 1 d . . . H88 H 0.3632 0.3378 0.3766 0.062 Uiso 1 1 calc R . . C89 C -0.0424(3) 0.8916(3) 0.35599(16) 0.0330(10) Uani 1 1 d . . . C90 C -0.1119(3) 0.9705(3) 0.37330(19) 0.0430(12) Uani 1 1 d . . . C91 C -0.1767(4) 0.9605(4) 0.4196(2) 0.0664(18) Uani 1 1 d . . . H91 H -0.1746 0.9050 0.4421 0.080 Uiso 1 1 calc R . . C92 C -0.2438(5) 1.0313(5) 0.4325(3) 0.098(3) Uani 1 1 d . . . H92 H -0.2881 1.0246 0.4642 0.118 Uiso 1 1 calc R . . C93 C -0.2476(6) 1.1118(5) 0.4003(3) 0.107(3) Uani 1 1 d . . . H93 H -0.2943 1.1603 0.4099 0.129 Uiso 1 1 calc R . . C94 C -0.1846(5) 1.1224(4) 0.3545(3) 0.080(2) Uani 1 1 d . . . H94 H -0.1882 1.1779 0.3321 0.096 Uiso 1 1 calc R . . C95 C -0.1159(4) 1.0525(4) 0.3410(2) 0.0539(14) Uani 1 1 d . . . H95 H -0.0711 1.0603 0.3096 0.065 Uiso 1 1 calc R . . C96 C -0.1828(2) 0.7721(3) 0.33374(15) 0.0292(9) Uani 1 1 d . . . C97 C -0.2650(3) 0.8275(3) 0.36327(17) 0.0400(11) Uani 1 1 d . . . C98 C -0.3019(3) 0.7934(4) 0.41459(19) 0.0550(15) Uani 1 1 d . . . H98 H -0.2771 0.7357 0.4303 0.066 Uiso 1 1 calc R . . C99 C -0.3770(4) 0.8470(6) 0.4423(2) 0.085(2) Uani 1 1 d . . . H99 H -0.4014 0.8265 0.4777 0.102 Uiso 1 1 calc R . . C100 C -0.4152(4) 0.9281(6) 0.4186(3) 0.097(3) Uani 1 1 d . . . H1A H -0.4679 0.9623 0.4372 0.116 Uiso 1 1 calc R . . C101 C -0.3784(4) 0.9605(6) 0.3684(3) 0.088(3) Uani 1 1 d . . . H2A H -0.4045 1.0178 0.3527 0.106 Uiso 1 1 calc R . . C102 C -0.3031(4) 0.9106(4) 0.3402(2) 0.0551(15) Uani 1 1 d . . . H3A H -0.2779 0.9332 0.3052 0.066 Uiso 1 1 calc R . . C103 C 0.1656(3) 0.7699(3) 0.38152(16) 0.0353(10) Uani 1 1 d . . . C104 C 0.1185(3) 0.8317(2) 0.42172(13) 0.030(2) Uani 0.50 1 d PGU A 1 C105 C 0.0629(3) 0.7965(3) 0.46729(14) 0.035(2) Uani 0.50 1 d PGU A 1 H105 H 0.0495 0.7391 0.4712 0.043 Uiso 0.50 1 calc PR A 1 C106 C 0.0270(3) 0.8454(3) 0.50718(15) 0.048(3) Uani 0.50 1 d PGU A 1 H106 H -0.0110 0.8213 0.5383 0.058 Uiso 0.50 1 calc PR A 1 C107 C 0.0466(3) 0.9294(3) 0.50152(16) 0.069(3) Uani 0.50 1 d PGU A 1 H107 H 0.0221 0.9628 0.5288 0.083 Uiso 0.50 1 calc PR A 1 C108 C 0.1022(4) 0.9646(3) 0.45595(18) 0.081(4) Uani 0.50 1 d PGU A 1 H108 H 0.1157 1.0220 0.4521 0.098 Uiso 0.50 1 calc PR A 1 C109 C 0.1382(3) 0.9157(2) 0.41605(15) 0.062(3) Uani 0.50 1 d PGU A 1 H109 H 0.1762 0.9398 0.3849 0.075 Uiso 0.50 1 calc PR A 1 C110 C 0.40207(16) 0.5142(2) 0.21108(11) 0.0252(9) Uani 1 1 d G . . C111 C 0.49933(15) 0.51394(17) 0.21713(9) 0.0275(9) Uani 1 1 d G . . C112 C 0.52126(18) 0.4897(2) 0.26562(11) 0.0407(11) Uani 1 1 d G . . H4A H 0.4772 0.4676 0.2945 0.049 Uiso 1 1 calc R . . C113 C 0.6081(3) 0.4976(4) 0.2724(2) 0.0512(13) Uani 1 1 d . . . H5A H 0.6238 0.4796 0.3057 0.061 Uiso 1 1 calc R . . C114 C 0.6719(3) 0.5318(3) 0.2303(2) 0.0483(13) Uani 1 1 d . . . H6A H 0.7298 0.5403 0.2351 0.058 Uiso 1 1 calc R . . C115 C 0.6509(3) 0.5532(3) 0.1820(2) 0.0399(11) Uani 1 1 d . . . H7A H 0.6958 0.5737 0.1530 0.048 Uiso 1 1 calc R . . C116 C 0.5647(3) 0.5452(3) 0.17477(17) 0.0298(9) Uani 1 1 d . . . H8A H 0.5503 0.5610 0.1411 0.036 Uiso 1 1 calc R . . C1A C 0.1497(6) 0.8020(6) 0.4308(3) 0.034(2) Uani 0.50 1 d PU A 2 C2A C 0.0796(7) 0.7815(7) 0.4715(4) 0.043(3) Uani 0.50 1 d PU A 2 H2A1 H 0.0394 0.7450 0.4684 0.051 Uiso 0.50 1 calc PR A 2 C3A C 0.0658(7) 0.8135(8) 0.5180(4) 0.050(3) Uani 0.50 1 d PU A 2 H3A1 H 0.0237 0.7917 0.5480 0.060 Uiso 0.50 1 calc PR A 2 C4A C 0.1141(10) 0.8768(10) 0.5192(5) 0.083(4) Uani 0.50 1 d PU A 2 H4A1 H 0.0992 0.9055 0.5485 0.100 Uiso 0.50 1 calc PR A 2 C5A C 0.1838(12) 0.8988(12) 0.4785(6) 0.100(4) Uani 0.50 1 d PU A 2 H5A1 H 0.2211 0.9382 0.4813 0.120 Uiso 0.50 1 calc PR A 2 C6A C 0.2010(10) 0.8651(10) 0.4335(5) 0.080(4) Uani 0.50 1 d PU A 2 H6A1 H 0.2468 0.8840 0.4046 0.096 Uiso 0.50 1 calc PR A 2 Cl1S Cl 0.37319(9) 0.05447(9) 0.00241(5) 0.0528(3) Uani 1 1 d . . . Cl2S Cl 0.35605(15) -0.09842(11) -0.03680(8) 0.0849(6) Uani 1 1 d . . . C1S C 0.3737(4) -0.0591(3) 0.0162(2) 0.0477(12) Uani 1 1 d . . . H5B H 0.3239 -0.0722 0.0467 0.057 Uiso 1 1 calc R . . H6B H 0.4343 -0.0907 0.0250 0.057 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 0.0120(3) 0.0198(3) 0.0272(3) -0.0118(2) -0.0004(2) -0.0064(2) Mn2 0.0130(3) 0.0214(3) 0.0239(3) -0.0099(2) 0.0008(2) -0.0088(2) Mn3 0.0114(3) 0.0195(3) 0.0231(3) -0.0110(2) 0.0020(2) -0.0069(2) Mn4 0.0117(3) 0.0211(3) 0.0232(3) -0.0114(2) 0.0011(2) -0.0075(2) Mn5 0.0155(3) 0.0236(3) 0.0245(3) -0.0100(2) -0.0007(2) -0.0074(2) Mn6 0.0117(3) 0.0233(3) 0.0230(3) -0.0114(2) 0.0015(2) -0.0065(2) Mn7 0.0116(3) 0.0207(3) 0.0260(3) -0.0119(2) 0.0008(2) -0.0079(2) Mn8 0.0213(3) 0.0321(4) 0.0312(3) -0.0121(3) -0.0044(2) -0.0130(2) Mn9 0.0206(3) 0.0238(4) 0.0228(3) -0.0111(2) 0.0013(2) -0.0079(2) Mn10 0.0151(3) 0.0227(3) 0.0316(3) -0.0152(2) 0.0003(2) -0.0060(2) O1 0.0135(12) 0.0177(14) 0.0247(13) -0.0109(10) 0.0008(10) -0.0081(9) O2 0.0156(12) 0.0276(16) 0.0289(14) -0.0140(11) 0.0001(11) -0.0059(10) O3 0.0173(13) 0.0261(16) 0.0299(14) -0.0098(11) -0.0016(11) -0.0120(11) O4 0.0198(13) 0.0185(16) 0.0422(16) -0.0124(11) -0.0040(11) -0.0064(10) O5 0.0196(14) 0.0237(16) 0.0317(15) -0.0114(11) 0.0002(11) -0.0080(10) O6 0.0156(13) 0.0245(16) 0.0343(16) -0.0125(11) -0.0022(11) -0.0058(10) O7 0.0178(14) 0.0378(19) 0.0376(17) -0.0071(13) 0.0027(12) -0.0040(12) O8 0.0149(12) 0.0189(15) 0.0267(14) -0.0094(10) 0.0010(10) -0.0076(9) O9 0.0178(13) 0.0280(16) 0.0288(15) -0.0108(11) 0.0004(11) -0.0126(10) O10 0.0137(12) 0.0221(15) 0.0246(13) -0.0113(10) 0.0009(10) -0.0075(10) O11 0.0122(12) 0.0206(15) 0.0262(13) -0.0115(10) 0.0020(10) -0.0080(9) O12 0.0164(13) 0.0252(16) 0.0270(14) -0.0070(11) 0.0005(10) -0.0110(10) O13 0.0173(13) 0.0252(17) 0.0327(15) -0.0076(11) -0.0029(11) -0.0081(10) O14 0.0151(12) 0.0216(15) 0.0265(14) -0.0084(10) 0.0022(10) -0.0079(10) O15 0.0208(14) 0.0281(17) 0.0310(15) -0.0078(11) -0.0043(11) -0.0083(11) O16 0.0127(12) 0.0206(15) 0.0306(14) -0.0135(10) 0.0001(10) -0.0067(10) O17 0.0140(12) 0.0255(16) 0.0271(14) -0.0108(11) 0.0013(10) -0.0089(10) O18 0.0197(13) 0.0216(15) 0.0259(14) -0.0087(10) -0.0031(10) -0.0094(10) O19 0.0147(13) 0.0276(16) 0.0305(14) -0.0106(11) -0.0021(10) -0.0087(10) O20 0.0158(13) 0.0291(17) 0.0320(15) -0.0109(11) -0.0040(11) -0.0108(10) O21 0.0202(13) 0.0271(17) 0.0265(14) -0.0105(11) 0.0002(11) -0.0062(11) O22 0.0184(13) 0.0234(16) 0.0248(14) -0.0083(11) 0.0032(10) -0.0092(10) O23 0.0187(13) 0.0196(16) 0.0316(14) -0.0108(11) -0.0015(11) -0.0072(10) O24 0.0254(15) 0.0274(18) 0.0490(18) -0.0135(13) -0.0017(13) -0.0071(12) O25 0.0275(15) 0.0338(18) 0.0318(15) -0.0088(12) -0.0056(12) -0.0135(12) O26 0.0354(17) 0.040(2) 0.0466(19) -0.0101(14) -0.0163(14) -0.0137(13) O27 0.0218(13) 0.0224(16) 0.0316(15) -0.0124(11) -0.0016(11) -0.0086(10) O28 0.0208(14) 0.0310(18) 0.0443(17) -0.0205(13) 0.0015(13) -0.0109(11) O29 0.0334(16) 0.048(2) 0.0303(16) -0.0142(13) 0.0009(13) -0.0149(13) O30 0.0322(16) 0.0339(19) 0.0424(17) -0.0170(13) -0.0112(13) -0.0095(13) O31 0.0335(16) 0.044(2) 0.0375(17) -0.0207(14) 0.0001(14) -0.0109(13) O32 0.0369(17) 0.0307(19) 0.0359(16) -0.0139(13) -0.0020(13) -0.0093(13) O33 0.0235(14) 0.046(2) 0.0311(16) -0.0084(13) -0.0024(12) -0.0127(13) O34 0.0177(13) 0.0325(17) 0.0268(15) -0.0141(11) 0.0027(11) -0.0057(11) O35 0.0162(13) 0.0201(15) 0.0300(14) -0.0135(11) 0.0017(10) -0.0055(10) N1 0.0239(17) 0.039(2) 0.0329(19) -0.0161(15) -0.0040(15) -0.0122(14) N2 0.0182(18) 0.059(3) 0.039(2) -0.0202(18) -0.0007(15) -0.0095(16) N3 0.0118(14) 0.024(2) 0.0247(16) -0.0084(13) 0.0035(12) -0.0060(12) N4 0.053(3) 0.037(3) 0.069(3) -0.023(2) -0.030(2) 0.0080(19) N5 0.0229(17) 0.021(2) 0.0273(17) -0.0123(13) 0.0006(13) -0.0054(13) N6 0.054(3) 0.040(3) 0.050(2) -0.0264(19) 0.0136(19) -0.0259(19) C1 0.0202(19) 0.022(2) 0.029(2) -0.0137(16) 0.0022(16) -0.0122(15) C2 0.0188(18) 0.027(2) 0.026(2) -0.0155(16) 0.0036(15) -0.0122(15) C3 0.027(2) 0.031(3) 0.032(2) -0.0163(17) 0.0044(17) -0.0097(17) C4 0.046(3) 0.041(3) 0.029(2) -0.0081(19) 0.0012(19) -0.016(2) C5 0.037(3) 0.055(3) 0.032(2) -0.023(2) 0.0123(19) -0.018(2) C6 0.025(2) 0.054(3) 0.039(3) -0.031(2) 0.0051(18) -0.0080(19) C7 0.022(2) 0.042(3) 0.032(2) -0.0200(18) 0.0008(17) -0.0082(17) C8 0.0114(17) 0.034(3) 0.028(2) -0.0156(17) 0.0029(15) -0.0066(15) C9 0.0163(18) 0.027(2) 0.035(2) -0.0143(16) -0.0037(16) -0.0092(15) C10 0.027(2) 0.043(3) 0.037(2) -0.0131(19) -0.0010(18) -0.0183(18) C11 0.041(3) 0.048(3) 0.053(3) -0.016(2) -0.007(2) -0.030(2) C12 0.042(3) 0.049(3) 0.050(3) -0.022(2) -0.016(2) -0.017(2) C13 0.030(2) 0.044(3) 0.036(2) -0.0140(19) -0.0096(18) -0.0084(19) C14 0.025(2) 0.030(3) 0.035(2) -0.0105(17) -0.0029(17) -0.0089(16) C15 0.027(2) 0.021(2) 0.026(2) -0.0108(15) -0.0057(16) -0.0060(15) C16 0.025(2) 0.023(2) 0.035(2) -0.0085(16) -0.0021(17) -0.0051(16) C17 0.029(2) 0.026(3) 0.038(2) -0.0140(17) -0.0012(17) -0.0097(17) C18 0.046(3) 0.031(3) 0.047(3) -0.015(2) -0.005(2) -0.015(2) C19 0.052(3) 0.025(3) 0.056(3) -0.017(2) 0.000(2) -0.004(2) C20 0.038(3) 0.031(3) 0.057(3) -0.013(2) 0.000(2) 0.006(2) C21 0.036(2) 0.028(3) 0.043(3) -0.0142(18) -0.0045(19) -0.0039(18) C22 0.020(2) 0.027(2) 0.0211(19) -0.0093(15) 0.0009(15) -0.0089(15) C23 0.023(2) 0.030(3) 0.026(2) -0.0111(16) -0.0010(16) -0.0057(16) C24 0.036(3) 0.026(3) 0.081(4) -0.015(2) -0.025(2) -0.0072(19) C25 0.051(3) 0.025(3) 0.114(5) -0.006(3) -0.036(3) -0.014(2) C26 0.043(3) 0.030(3) 0.066(3) -0.005(2) -0.022(2) -0.004(2) C27 0.031(2) 0.033(3) 0.042(3) -0.0088(19) -0.0090(19) -0.0007(18) C28 0.027(2) 0.033(3) 0.029(2) -0.0087(17) -0.0022(16) -0.0092(17) C29 0.0184(19) 0.031(3) 0.029(2) -0.0104(17) -0.0056(16) -0.0129(16) C30 0.024(2) 0.032(3) 0.026(2) -0.0100(16) -0.0004(16) -0.0149(16) C31 0.031(2) 0.045(3) 0.049(3) -0.016(2) 0.013(2) -0.019(2) C32 0.060(4) 0.070(5) 0.058(3) -0.028(3) 0.034(3) -0.037(3) C33 0.085(4) 0.076(5) 0.045(3) -0.012(3) 0.027(3) -0.054(4) C34 0.068(4) 0.050(4) 0.039(3) 0.004(2) 0.000(2) -0.034(3) C35 0.036(2) 0.037(3) 0.036(2) -0.0064(19) -0.0022(18) -0.0204(19) C36 0.0185(19) 0.035(3) 0.027(2) -0.0104(17) 0.0018(16) -0.0107(16) C37 0.023(2) 0.047(3) 0.034(2) -0.0088(19) -0.0073(17) -0.0140(18) C38 0.028(2) 0.048(3) 0.036(2) -0.006(2) -0.0087(18) -0.0123(19) C39 0.023(2) 0.036(3) 0.036(2) -0.0041(18) -0.0025(17) -0.0053(17) C40 0.0181(19) 0.032(3) 0.028(2) -0.0088(17) 0.0035(16) -0.0074(16) C41 0.0133(18) 0.035(3) 0.024(2) -0.0094(16) 0.0006(15) -0.0048(15) C42 0.028(2) 0.022(3) 0.037(2) -0.0111(17) -0.0064(17) 0.0005(16) C43 0.028(2) 0.025(3) 0.034(2) -0.0080(17) 0.0008(17) -0.0013(17) C44 0.036(2) 0.031(3) 0.039(2) -0.0123(18) -0.0041(19) -0.0023(18) C45 0.026(2) 0.025(3) 0.057(3) -0.0095(19) 0.0013(19) -0.0057(17) C46 0.064(4) 0.034(3) 0.093(4) -0.029(3) -0.042(3) 0.017(2) C47 0.061(3) 0.029(3) 0.066(3) -0.019(2) -0.022(3) 0.003(2) C48 0.041(3) 0.030(3) 0.059(3) -0.017(2) -0.004(2) -0.0084(19) C49 0.024(2) 0.031(3) 0.027(2) -0.0133(16) -0.0011(16) -0.0060(16) C50 0.024(2) 0.032(3) 0.028(2) -0.0138(17) 0.0035(16) -0.0066(16) C51 0.033(2) 0.043(3) 0.028(2) -0.0089(18) 0.0068(18) -0.0169(19) C52 0.032(2) 0.026(2) 0.029(2) -0.0098(16) 0.0000(17) -0.0084(17) C53 0.0176(19) 0.033(3) 0.025(2) -0.0104(16) -0.0028(15) -0.0060(15) C54 0.0208(19) 0.024(2) 0.028(2) -0.0140(16) -0.0028(15) -0.0074(15) C55 0.030(2) 0.027(3) 0.028(2) -0.0110(16) 0.0024(16) -0.0101(16) C56 0.023(2) 0.027(2) 0.027(2) -0.0113(16) -0.0053(16) -0.0055(16) C57 0.029(2) 0.028(3) 0.030(2) -0.0134(17) -0.0041(17) -0.0091(17) C58 0.038(2) 0.032(3) 0.033(2) -0.0112(18) 0.0019(19) -0.0035(18) C59 0.069(4) 0.040(4) 0.064(3) -0.031(3) 0.018(3) -0.030(3) C60 0.063(3) 0.035(3) 0.050(3) -0.023(2) -0.004(2) -0.018(2) C61 0.053(3) 0.029(3) 0.037(2) -0.0195(19) -0.003(2) 0.000(2) C62 0.029(2) 0.061(3) 0.036(2) -0.020(2) -0.0031(19) -0.016(2) C63 0.038(3) 0.071(4) 0.036(3) -0.018(2) -0.010(2) -0.021(2) C64 0.027(2) 0.065(4) 0.048(3) -0.021(2) -0.010(2) -0.018(2) C65 0.020(2) 0.049(3) 0.038(2) -0.016(2) -0.0004(18) -0.0132(18) C66 0.022(2) 0.031(3) 0.036(2) -0.0163(17) -0.0050(17) -0.0069(16) C67 0.0160(19) 0.022(2) 0.039(2) -0.0104(16) -0.0062(16) -0.0064(14) C68 0.0101(17) 0.036(3) 0.035(2) -0.0170(17) -0.0015(16) -0.0062(15) C69 0.018(2) 0.024(2) 0.034(2) -0.0123(16) 0.0011(16) -0.0085(15) C70 0.019(2) 0.028(2) 0.033(2) -0.0087(16) -0.0007(16) -0.0063(15) C71 0.021(2) 0.056(3) 0.037(2) -0.021(2) 0.0033(18) -0.0176(19) C72 0.020(2) 0.073(4) 0.042(3) -0.026(2) 0.0020(19) -0.007(2) C73 0.024(2) 0.075(4) 0.035(3) -0.021(2) 0.0035(19) -0.008(2) C74 0.043(3) 0.080(4) 0.037(3) -0.028(3) 0.004(2) -0.031(3) C75 0.026(2) 0.023(2) 0.040(2) -0.0098(17) -0.0083(18) -0.0090(16) C76 0.024(2) 0.024(2) 0.049(3) -0.0172(18) -0.0071(18) -0.0054(16) C77 0.021(2) 0.034(3) 0.054(3) -0.019(2) -0.0057(19) -0.0052(17) C78 0.031(3) 0.049(3) 0.079(4) -0.030(3) -0.010(2) -0.012(2) C79 0.034(3) 0.071(4) 0.091(4) -0.043(3) -0.023(3) -0.010(2) C80 0.045(3) 0.071(4) 0.066(4) -0.039(3) -0.021(3) -0.009(3) C81 0.034(2) 0.042(3) 0.053(3) -0.026(2) -0.011(2) -0.0063(19) C82 0.027(2) 0.038(3) 0.023(2) -0.0106(17) 0.0006(16) -0.0105(17) C83 0.030(2) 0.044(3) 0.029(2) -0.0004(18) -0.0066(17) -0.0201(19) C84 0.072(4) 0.057(4) 0.059(3) 0.006(3) -0.036(3) -0.031(3) C85 0.108(6) 0.088(6) 0.099(5) 0.018(4) -0.077(5) -0.051(4) C86 0.139(7) 0.073(6) 0.142(8) 0.044(5) -0.110(7) -0.050(5) C87 0.122(6) 0.054(5) 0.114(6) 0.011(4) -0.074(5) -0.019(4) C88 0.062(3) 0.046(4) 0.051(3) 0.006(2) -0.027(3) -0.015(2) C89 0.030(2) 0.043(3) 0.032(2) -0.020(2) -0.0004(19) -0.0116(19) C90 0.047(3) 0.038(3) 0.045(3) -0.022(2) 0.007(2) -0.012(2) C91 0.076(4) 0.044(4) 0.064(4) -0.027(3) 0.034(3) -0.015(3) C92 0.091(5) 0.059(5) 0.113(6) -0.043(4) 0.063(5) -0.012(4) C93 0.109(6) 0.041(5) 0.137(7) -0.038(4) 0.041(5) 0.009(4) C94 0.083(5) 0.037(4) 0.100(5) -0.024(3) 0.019(4) 0.000(3) C95 0.060(3) 0.038(3) 0.060(3) -0.021(2) 0.008(3) -0.011(2) C96 0.0131(18) 0.048(3) 0.030(2) -0.0141(19) -0.0015(16) -0.0099(17) C97 0.023(2) 0.065(4) 0.036(3) -0.022(2) -0.0051(19) -0.004(2) C98 0.026(2) 0.108(5) 0.033(3) -0.025(3) 0.002(2) -0.009(3) C99 0.038(3) 0.173(8) 0.039(3) -0.042(4) 0.007(3) -0.004(4) C100 0.049(4) 0.166(8) 0.060(4) -0.059(5) -0.004(3) 0.042(4) C101 0.058(4) 0.129(7) 0.068(4) -0.058(4) -0.021(3) 0.048(4) C102 0.048(3) 0.077(4) 0.039(3) -0.031(3) -0.009(2) 0.012(3) C103 0.032(2) 0.049(3) 0.033(2) -0.018(2) -0.0033(19) -0.018(2) C104 0.043(5) 0.026(5) 0.023(4) -0.011(3) 0.002(4) -0.012(4) C105 0.040(5) 0.034(5) 0.032(5) -0.009(4) 0.003(4) -0.015(4) C106 0.066(6) 0.049(6) 0.031(5) -0.014(4) 0.005(4) -0.022(5) C107 0.107(7) 0.059(7) 0.041(5) -0.028(4) 0.012(5) -0.024(5) C108 0.124(8) 0.062(7) 0.059(6) -0.030(5) 0.021(6) -0.041(6) C109 0.106(7) 0.038(5) 0.042(5) -0.017(4) 0.016(5) -0.035(5) C110 0.0161(19) 0.026(2) 0.034(2) -0.0139(17) 0.0014(17) -0.0045(15) C111 0.0179(19) 0.033(3) 0.035(2) -0.0188(17) -0.0041(16) -0.0004(16) C112 0.031(2) 0.049(3) 0.042(3) -0.015(2) -0.008(2) 0.001(2) C113 0.038(3) 0.065(4) 0.058(3) -0.023(3) -0.023(2) 0.001(2) C114 0.023(2) 0.054(3) 0.080(4) -0.032(3) -0.017(2) -0.003(2) C115 0.019(2) 0.044(3) 0.063(3) -0.025(2) -0.004(2) -0.0067(18) C116 0.019(2) 0.034(3) 0.040(2) -0.0176(18) -0.0014(17) -0.0053(16) C1A 0.025(4) 0.041(6) 0.043(5) -0.025(4) 0.001(3) -0.013(4) C2A 0.051(5) 0.047(6) 0.036(5) -0.015(4) -0.001(4) -0.023(4) C3A 0.050(6) 0.062(6) 0.043(5) -0.025(4) 0.002(4) -0.018(5) C4A 0.092(7) 0.097(8) 0.078(6) -0.058(6) 0.018(5) -0.051(6) C5A 0.117(8) 0.122(8) 0.092(7) -0.071(6) 0.019(6) -0.077(6) C6A 0.084(7) 0.103(8) 0.075(6) -0.055(6) 0.022(5) -0.061(6) Cl1S 0.0515(7) 0.0434(8) 0.0676(8) -0.0097(6) -0.0142(6) -0.0145(5) Cl2S 0.1217(15) 0.0485(11) 0.1079(14) -0.0192(8) -0.0707(12) -0.0063(9) C1S 0.050(3) 0.038(3) 0.055(3) -0.002(2) -0.011(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.898(2) . ? Mn1 O6 1.916(2) . ? Mn1 O11 1.921(2) . ? Mn1 O4 1.932(3) . ? Mn1 O2 2.120(3) . ? Mn1 O8 2.432(3) . ? Mn1 Mn3 3.0166(13) . ? Mn1 Mn2 3.0415(11) . ? Mn1 Mn4 3.1151(14) . ? Mn2 O1 1.885(2) . ? Mn2 O12 1.925(3) . ? Mn2 O8 1.933(2) . ? Mn2 O9 1.963(3) . ? Mn2 O5 2.120(3) . ? Mn2 O10 2.390(3) . ? Mn2 Mn3 3.0081(13) . ? Mn2 Mn4 3.1308(10) . ? Mn3 O1 1.879(3) . ? Mn3 O14 1.908(3) . ? Mn3 O10 1.944(2) . ? Mn3 O35 1.961(2) . ? Mn3 O3 2.135(2) . ? Mn3 O11 2.385(2) . ? Mn3 Mn4 3.1350(10) . ? Mn4 O17 1.852(2) . ? Mn4 O18 1.854(3) . ? Mn4 O16 1.859(2) . ? Mn4 O8 1.924(2) . ? Mn4 O11 1.947(2) . ? Mn4 O10 1.955(2) . ? Mn4 Mn6 2.8245(10) . ? Mn4 Mn5 2.8542(13) . ? Mn4 Mn7 2.8590(13) . ? Mn5 O18 1.836(3) . ? Mn5 O8 1.909(3) . ? Mn5 O21 1.934(3) . ? Mn5 O25 1.984(3) . ? Mn5 O22 2.201(3) . ? Mn5 O7 2.243(3) . ? Mn6 O17 1.845(3) . ? Mn6 O10 1.899(2) . ? Mn6 O34 1.954(3) . ? Mn6 N3 2.062(3) . ? Mn6 O23 2.216(3) . ? Mn6 O13 2.227(3) . ? Mn7 O16 1.839(2) . ? Mn7 O11 1.907(2) . ? Mn7 O19 1.952(3) . ? Mn7 O27 1.976(3) . ? Mn7 O15 2.209(3) . ? Mn7 O20 2.230(3) . ? Mn8 O18 2.030(2) . ? Mn8 O29 2.062(3) . ? Mn8 O26 2.121(3) . ? Mn8 O20 2.196(3) . ? Mn8 N1 2.233(3) . ? Mn9 O17 2.086(3) . ? Mn9 O30 2.129(3) . ? Mn9 O32 2.165(3) . ? Mn9 N5 2.253(3) . ? Mn9 O22 2.265(3) . ? Mn9 O33 2.278(3) . ? Mn10 O31 2.031(3) . ? Mn10 O16 2.045(3) . ? Mn10 O24 2.098(3) . ? Mn10 O28 2.144(3) . ? Mn10 O23 2.174(3) . ? O2 C1 1.248(5) . ? O3 C8 1.246(5) . ? O4 C15 1.299(5) . ? O5 C15 1.250(5) . ? O6 C110 1.293(4) . ? O7 C110 1.238(4) . ? O9 C8 1.290(5) . ? O12 C29 1.286(5) . ? O13 C29 1.240(5) . ? O14 C22 1.289(4) . ? O15 C22 1.251(4) . ? O19 C69 1.284(4) . ? O20 C67 1.286(4) . ? O21 C56 1.265(5) . ? O22 C54 1.278(5) . ? O23 C41 1.284(5) . ? O24 C43 1.261(5) . ? O25 C82 1.274(5) . ? O26 C82 1.242(5) . ? O27 C75 1.287(5) . ? O28 C75 1.252(5) . ? O29 C103 1.262(5) . ? O30 C103 1.254(5) . ? O31 C89 1.256(5) . ? O32 C89 1.260(5) . ? O33 C96 1.246(5) . ? O34 C96 1.283(5) . ? O35 C1 1.285(5) . ? N1 C62 1.333(5) . ? N1 C66 1.334(5) . ? N2 C72 1.328(6) . ? N2 C70 1.345(5) . ? N3 C36 1.329(5) . ? N3 C40 1.365(5) . ? N4 C44 1.321(6) . ? N4 C46 1.354(7) . ? N5 C49 1.334(5) . ? N5 C53 1.335(5) . ? N6 C59 1.340(6) . ? N6 C57 1.343(6) . ? C1 C2 1.502(5) . ? C2 C3 1.388(6) . ? C2 C7 1.397(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(7) . ? C4 H4 0.9500 . ? C5 C6 1.381(7) . ? C5 H5 0.9500 . ? C6 C7 1.380(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.500(5) . ? C9 C14 1.393(6) . ? C9 C10 1.394(6) . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.378(7) . ? C11 H11 0.9500 . ? C12 C13 1.396(6) . ? C12 H12 0.9500 . ? C13 C14 1.372(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.479(6) . ? C16 C17 1.382(6) . ? C16 C21 1.386(6) . ? C17 C18 1.382(6) . ? C17 H17 0.9500 . ? C18 C19 1.378(7) . ? C18 H18 0.9500 . ? C19 C20 1.398(7) . ? C19 H19 0.9500 . ? C20 C21 1.388(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.493(6) . ? C23 C24 1.390(6) . ? C23 C28 1.391(6) . ? C24 C25 1.385(7) . ? C24 H24 0.9500 . ? C25 C26 1.378(7) . ? C25 H25 0.9500 . ? C26 C27 1.395(7) . ? C26 H26 0.9500 . ? C27 C28 1.389(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.512(5) . ? C30 C35 1.381(6) . ? C30 C31 1.387(6) . ? C31 C32 1.396(7) . ? C31 H31 0.9500 . ? C32 C33 1.356(9) . ? C32 H32 0.9500 . ? C33 C34 1.372(9) . ? C33 H33 0.9500 . ? C34 C35 1.397(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.391(6) . ? C36 H36 0.9500 . ? C37 C38 1.381(7) . ? C37 H37 0.9500 . ? C38 C39 1.378(6) . ? C38 H38 0.9500 . ? C39 C40 1.374(6) . ? C39 H39 0.9500 . ? C40 C41 1.515(5) . ? C41 C42 1.375(6) . ? C42 C43 1.401(6) . ? C42 H42 0.9500 . ? C43 C44 1.504(6) . ? C44 C45 1.376(6) . ? C45 C48 1.406(7) . ? C45 H45 0.9500 . ? C46 C47 1.375(8) . ? C46 H46 0.9500 . ? C47 C48 1.367(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.394(6) . ? C49 H49 0.9500 . ? C50 C51 1.373(6) . ? C50 H50 0.9500 . ? C51 C52 1.396(6) . ? C51 H51 0.9500 . ? C52 C53 1.389(6) . ? C52 H52 0.9500 . ? C53 C54 1.508(5) . ? C54 C55 1.396(6) . ? C55 C56 1.405(5) . ? C55 H55 0.9500 . ? C56 C57 1.489(6) . ? C57 C58 1.386(6) . ? C58 C61 1.381(6) . ? C58 H58 0.9500 . ? C59 C60 1.381(7) . ? C59 H59 0.9500 . ? C60 C61 1.375(7) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.388(6) . ? C62 H62 0.9500 . ? C63 C64 1.388(7) . ? C63 H63 0.9500 . ? C64 C65 1.375(6) . ? C64 H64 0.9500 . ? C65 C66 1.388(6) . ? C65 H65 0.9500 . ? C66 C67 1.506(5) . ? C67 C68 1.371(6) . ? C68 C69 1.397(5) . ? C68 H68 0.9500 . ? C69 C70 1.492(5) . ? C70 C71 1.370(6) . ? C71 C74 1.396(6) . ? C71 H71 0.9500 . ? C72 C73 1.375(7) . ? C72 H72 0.9500 . ? C73 C74 1.382(7) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 C76 1.504(5) . ? C76 C77 1.384(6) . ? C76 C81 1.396(6) . ? C77 C78 1.385(6) . ? C77 H77 0.9500 . ? C78 C79 1.398(8) . ? C78 H78 0.9500 . ? C79 C80 1.382(8) . ? C79 H79 0.9500 . ? C80 C81 1.382(6) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C83 1.495(6) . ? C83 C88 1.388(7) . ? C83 C84 1.401(7) . ? C84 C85 1.377(8) . ? C84 H84 0.9500 . ? C85 C86 1.368(11) . ? C85 H85 0.9500 . ? C86 C87 1.404(10) . ? C86 H86 0.9500 . ? C87 C88 1.384(8) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C90 1.512(6) . ? C90 C91 1.388(7) . ? C90 C95 1.392(7) . ? C91 C92 1.369(8) . ? C91 H91 0.9500 . ? C92 C93 1.372(10) . ? C92 H92 0.9500 . ? C93 C94 1.365(10) . ? C93 H93 0.9500 . ? C94 C95 1.376(8) . ? C94 H94 0.9500 . ? C95 H95 0.9500 . ? C96 C97 1.504(6) . ? C97 C102 1.384(7) . ? C97 C98 1.397(7) . ? C98 C99 1.408(8) . ? C98 H98 0.9500 . ? C99 C100 1.367(11) . ? C99 H99 0.9500 . ? C100 C101 1.366(10) . ? C100 H1A 0.9500 . ? C101 C102 1.386(7) . ? C101 H2A 0.9500 . ? C102 H3A 0.9500 . ? C103 C1A 1.469(9) . ? C103 C104 1.550(5) . ? C104 C105 1.3900 . ? C104 C109 1.3900 . ? C105 C106 1.3900 . ? C105 H105 0.9500 . ? C106 C107 1.3900 . ? C106 H106 0.9500 . ? C107 C108 1.3900 . ? C107 H107 0.9500 . ? C108 C109 1.3900 . ? C108 H108 0.9500 . ? C109 H109 0.9500 . ? C110 C111 1.5053 . ? C111 C112 1.3765 . ? C111 C116 1.394(5) . ? C112 C113 1.394(6) . ? C112 H4A 0.9500 . ? C113 C114 1.394(8) . ? C113 H5A 0.9500 . ? C114 C115 1.365(7) . ? C114 H6A 0.9500 . ? C115 C116 1.390(6) . ? C115 H7A 0.9500 . ? C116 H8A 0.9500 . ? C1A C2A 1.364(13) . ? C1A C6A 1.410(14) . ? C2A C3A 1.402(13) . ? C2A H2A1 0.9500 . ? C3A C4A 1.369(16) . ? C3A H3A1 0.9500 . ? C4A C5A 1.365(19) . ? C4A H4A1 0.9500 . ? C5A C6A 1.373(17) . ? C5A H5A1 0.9500 . ? C6A H6A1 0.9500 . ? Cl1S C1S 1.748(5) . ? Cl2S C1S 1.768(5) . ? C1S H5B 0.9900 . ? C1S H6B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O6 176.23(11) . . ? O1 Mn1 O11 86.14(10) . . ? O6 Mn1 O11 93.80(11) . . ? O1 Mn1 O4 90.60(11) . . ? O6 Mn1 O4 90.28(11) . . ? O11 Mn1 O4 166.83(11) . . ? O1 Mn1 O2 85.12(10) . . ? O6 Mn1 O2 91.13(11) . . ? O11 Mn1 O2 94.72(11) . . ? O4 Mn1 O2 97.71(11) . . ? O1 Mn1 O8 73.45(9) . . ? O6 Mn1 O8 110.18(10) . . ? O11 Mn1 O8 74.73(10) . . ? O4 Mn1 O8 92.11(10) . . ? O2 Mn1 O8 156.52(9) . . ? O1 Mn1 Mn3 36.79(7) . . ? O6 Mn1 Mn3 141.69(8) . . ? O11 Mn1 Mn3 52.22(7) . . ? O4 Mn1 Mn3 126.98(8) . . ? O2 Mn1 Mn3 76.76(8) . . ? O8 Mn1 Mn3 80.29(7) . . ? O1 Mn1 Mn2 36.33(7) . . ? O6 Mn1 Mn2 147.44(8) . . ? O11 Mn1 Mn2 88.20(7) . . ? O4 Mn1 Mn2 81.68(8) . . ? O2 Mn1 Mn2 121.13(7) . . ? O8 Mn1 Mn2 39.42(6) . . ? Mn3 Mn1 Mn2 59.54(3) . . ? O1 Mn1 Mn4 78.67(7) . . ? O6 Mn1 Mn4 103.49(8) . . ? O11 Mn1 Mn4 36.62(7) . . ? O4 Mn1 Mn4 130.21(8) . . ? O2 Mn1 Mn4 128.90(8) . . ? O8 Mn1 Mn4 38.15(6) . . ? Mn3 Mn1 Mn4 61.47(3) . . ? Mn2 Mn1 Mn4 61.12(3) . . ? O1 Mn2 O12 177.57(11) . . ? O1 Mn2 O8 86.84(10) . . ? O12 Mn2 O8 93.66(10) . . ? O1 Mn2 O9 89.27(10) . . ? O12 Mn2 O9 90.67(10) . . ? O8 Mn2 O9 169.04(11) . . ? O1 Mn2 O5 85.66(10) . . ? O12 Mn2 O5 91.93(11) . . ? O8 Mn2 O5 93.38(10) . . ? O9 Mn2 O5 96.54(11) . . ? O1 Mn2 O10 74.61(10) . . ? O12 Mn2 O10 107.82(10) . . ? O8 Mn2 O10 74.28(10) . . ? O9 Mn2 O10 94.81(10) . . ? O5 Mn2 O10 157.07(9) . . ? O1 Mn2 Mn3 36.89(8) . . ? O12 Mn2 Mn3 145.47(8) . . ? O8 Mn2 Mn3 88.79(8) . . ? O9 Mn2 Mn3 81.97(8) . . ? O5 Mn2 Mn3 122.34(8) . . ? O10 Mn2 Mn3 40.20(6) . . ? O1 Mn2 Mn1 36.62(7) . . ? O12 Mn2 Mn1 142.94(8) . . ? O8 Mn2 Mn1 53.02(7) . . ? O9 Mn2 Mn1 125.19(8) . . ? O5 Mn2 Mn1 76.41(7) . . ? O10 Mn2 Mn1 80.76(6) . . ? Mn3 Mn2 Mn1 59.82(3) . . ? O1 Mn2 Mn4 78.41(7) . . ? O12 Mn2 Mn4 103.36(8) . . ? O8 Mn2 Mn4 35.66(8) . . ? O9 Mn2 Mn4 133.42(8) . . ? O5 Mn2 Mn4 126.47(7) . . ? O10 Mn2 Mn4 38.63(6) . . ? Mn3 Mn2 Mn4 61.38(2) . . ? Mn1 Mn2 Mn4 60.60(3) . . ? O1 Mn3 O14 176.79(10) . . ? O1 Mn3 O10 86.55(11) . . ? O14 Mn3 O10 93.23(11) . . ? O1 Mn3 O35 90.07(11) . . ? O14 Mn3 O35 90.76(11) . . ? O10 Mn3 O35 168.40(10) . . ? O1 Mn3 O3 84.61(10) . . ? O14 Mn3 O3 92.23(11) . . ? O10 Mn3 O3 96.10(10) . . ? O35 Mn3 O3 94.63(10) . . ? O1 Mn3 O11 74.32(9) . . ? O14 Mn3 O11 108.72(10) . . ? O10 Mn3 O11 74.95(9) . . ? O35 Mn3 O11 93.45(9) . . ? O3 Mn3 O11 157.42(10) . . ? O1 Mn3 Mn2 37.01(7) . . ? O14 Mn3 Mn2 141.55(7) . . ? O10 Mn3 Mn2 52.51(8) . . ? O35 Mn3 Mn2 126.42(8) . . ? O3 Mn3 Mn2 76.92(8) . . ? O11 Mn3 Mn2 81.32(7) . . ? O1 Mn3 Mn1 37.21(7) . . ? O14 Mn3 Mn1 146.00(8) . . ? O10 Mn3 Mn1 88.77(8) . . ? O35 Mn3 Mn1 81.87(8) . . ? O3 Mn3 Mn1 121.32(8) . . ? O11 Mn3 Mn1 39.52(6) . . ? Mn2 Mn3 Mn1 60.64(3) . . ? O1 Mn3 Mn4 78.36(8) . . ? O14 Mn3 Mn4 103.34(8) . . ? O10 Mn3 Mn4 36.60(7) . . ? O35 Mn3 Mn4 131.80(8) . . ? O3 Mn3 Mn4 129.77(7) . . ? O11 Mn3 Mn4 38.35(6) . . ? Mn2 Mn3 Mn4 61.24(3) . . ? Mn1 Mn3 Mn4 60.81(3) . . ? O17 Mn4 O18 94.04(11) . . ? O17 Mn4 O16 92.31(11) . . ? O18 Mn4 O16 94.49(11) . . ? O17 Mn4 O8 102.49(11) . . ? O18 Mn4 O8 79.50(11) . . ? O16 Mn4 O8 164.33(10) . . ? O17 Mn4 O11 163.04(11) . . ? O18 Mn4 O11 101.40(11) . . ? O16 Mn4 O11 79.64(11) . . ? O8 Mn4 O11 87.33(11) . . ? O17 Mn4 O10 81.23(10) . . ? O18 Mn4 O10 163.00(11) . . ? O16 Mn4 O10 101.98(11) . . ? O8 Mn4 O10 85.56(11) . . ? O11 Mn4 O10 85.85(10) . . ? O17 Mn4 Mn6 40.09(8) . . ? O18 Mn4 Mn6 133.87(8) . . ? O16 Mn4 Mn6 92.46(8) . . ? O8 Mn4 Mn6 102.16(8) . . ? O11 Mn4 Mn6 124.70(8) . . ? O10 Mn4 Mn6 42.10(7) . . ? O17 Mn4 Mn5 92.75(9) . . ? O18 Mn4 Mn5 39.12(8) . . ? O16 Mn4 Mn5 133.58(8) . . ? O8 Mn4 Mn5 41.69(7) . . ? O11 Mn4 Mn5 103.64(8) . . ? O10 Mn4 Mn5 124.40(8) . . ? Mn6 Mn4 Mn5 119.49(4) . . ? O17 Mn4 Mn7 131.31(8) . . ? O18 Mn4 Mn7 93.15(8) . . ? O16 Mn4 Mn7 39.10(7) . . ? O8 Mn4 Mn7 126.17(8) . . ? O11 Mn4 Mn7 41.59(7) . . ? O10 Mn4 Mn7 102.26(8) . . ? Mn6 Mn4 Mn7 119.20(4) . . ? Mn5 Mn4 Mn7 121.10(3) . . ? O17 Mn4 Mn1 151.76(8) . . ? O18 Mn4 Mn1 91.13(8) . . ? O16 Mn4 Mn1 114.95(8) . . ? O8 Mn4 Mn1 51.32(7) . . ? O11 Mn4 Mn1 36.05(7) . . ? O10 Mn4 Mn1 85.77(7) . . ? Mn6 Mn4 Mn1 126.26(3) . . ? Mn5 Mn4 Mn1 74.18(3) . . ? Mn7 Mn4 Mn1 75.93(3) . . ? O17 Mn4 Mn2 94.65(8) . . ? O18 Mn4 Mn2 115.02(8) . . ? O16 Mn4 Mn2 149.02(8) . . ? O8 Mn4 Mn2 35.84(7) . . ? O11 Mn4 Mn2 85.21(7) . . ? O10 Mn4 Mn2 49.72(8) . . ? Mn6 Mn4 Mn2 74.26(3) . . ? Mn5 Mn4 Mn2 76.20(3) . . ? Mn7 Mn4 Mn2 124.90(3) . . ? Mn1 Mn4 Mn2 58.28(2) . . ? O17 Mn4 Mn3 116.84(8) . . ? O18 Mn4 Mn3 147.96(8) . . ? O16 Mn4 Mn3 92.69(8) . . ? O8 Mn4 Mn3 85.28(8) . . ? O11 Mn4 Mn3 49.49(7) . . ? O10 Mn4 Mn3 36.36(7) . . ? Mn6 Mn4 Mn3 76.80(4) . . ? Mn5 Mn4 Mn3 125.06(3) . . ? Mn7 Mn4 Mn3 73.42(3) . . ? Mn1 Mn4 Mn3 57.72(3) . . ? Mn2 Mn4 Mn3 57.38(3) . . ? O18 Mn5 O8 80.33(11) . . ? O18 Mn5 O21 172.02(11) . . ? O8 Mn5 O21 91.77(11) . . ? O18 Mn5 O25 99.73(12) . . ? O8 Mn5 O25 178.25(11) . . ? O21 Mn5 O25 88.19(12) . . ? O18 Mn5 O22 93.09(11) . . ? O8 Mn5 O22 97.35(10) . . ? O21 Mn5 O22 86.77(10) . . ? O25 Mn5 O22 84.39(11) . . ? O18 Mn5 O7 91.31(11) . . ? O8 Mn5 O7 96.53(11) . . ? O21 Mn5 O7 90.70(11) . . ? O25 Mn5 O7 81.72(11) . . ? O22 Mn5 O7 165.95(10) . . ? O18 Mn5 Mn4 39.56(8) . . ? O8 Mn5 Mn4 42.09(8) . . ? O21 Mn5 Mn4 132.49(8) . . ? O25 Mn5 Mn4 138.31(9) . . ? O22 Mn5 Mn4 88.76(8) . . ? O7 Mn5 Mn4 103.03(8) . . ? O17 Mn6 O10 82.96(11) . . ? O17 Mn6 O34 97.31(11) . . ? O10 Mn6 O34 176.64(11) . . ? O17 Mn6 N3 170.75(11) . . ? O10 Mn6 N3 93.73(11) . . ? O34 Mn6 N3 85.49(11) . . ? O17 Mn6 O23 96.16(11) . . ? O10 Mn6 O23 93.63(10) . . ? O34 Mn6 O23 83.01(11) . . ? N3 Mn6 O23 75.37(11) . . ? O17 Mn6 O13 99.72(11) . . ? O10 Mn6 O13 94.82(10) . . ? O34 Mn6 O13 88.44(11) . . ? N3 Mn6 O13 89.14(11) . . ? O23 Mn6 O13 162.80(9) . . ? O17 Mn6 Mn4 40.29(8) . . ? O10 Mn6 Mn4 43.66(7) . . ? O34 Mn6 Mn4 135.92(8) . . ? N3 Mn6 Mn4 134.32(8) . . ? O23 Mn6 Mn4 89.53(7) . . ? O13 Mn6 Mn4 106.88(7) . . ? O16 Mn7 O11 81.17(11) . . ? O16 Mn7 O19 172.26(11) . . ? O11 Mn7 O19 92.44(11) . . ? O16 Mn7 O27 95.10(11) . . ? O11 Mn7 O27 176.27(10) . . ? O19 Mn7 O27 91.29(11) . . ? O16 Mn7 O15 96.70(11) . . ? O11 Mn7 O15 95.93(11) . . ? O19 Mn7 O15 88.26(10) . . ? O27 Mn7 O15 84.37(11) . . ? O16 Mn7 O20 90.44(10) . . ? O11 Mn7 O20 97.75(10) . . ? O19 Mn7 O20 86.08(10) . . ? O27 Mn7 O20 82.32(10) . . ? O15 Mn7 O20 165.40(10) . . ? O16 Mn7 Mn4 39.61(8) . . ? O11 Mn7 Mn4 42.64(7) . . ? O19 Mn7 Mn4 133.19(8) . . ? O27 Mn7 Mn4 133.71(8) . . ? O15 Mn7 Mn4 105.65(7) . . ? O20 Mn7 Mn4 87.96(7) . . ? O18 Mn8 O29 119.34(11) . . ? O18 Mn8 O26 94.60(11) . . ? O29 Mn8 O26 101.29(12) . . ? O18 Mn8 O20 86.80(10) . . ? O29 Mn8 O20 119.43(11) . . ? O26 Mn8 O20 132.19(11) . . ? O18 Mn8 N1 147.65(11) . . ? O29 Mn8 N1 92.71(12) . . ? O26 Mn8 N1 82.33(13) . . ? O20 Mn8 N1 72.42(11) . . ? O17 Mn9 O30 110.93(11) . . ? O17 Mn9 O32 105.77(11) . . ? O30 Mn9 O32 85.37(11) . . ? O17 Mn9 N5 142.88(11) . . ? O30 Mn9 N5 97.51(12) . . ? O32 Mn9 N5 99.66(11) . . ? O17 Mn9 O22 84.14(10) . . ? O30 Mn9 O22 92.82(10) . . ? O32 Mn9 O22 169.92(10) . . ? N5 Mn9 O22 70.71(10) . . ? O17 Mn9 O33 84.82(10) . . ? O30 Mn9 O33 159.02(11) . . ? O32 Mn9 O33 76.78(11) . . ? N5 Mn9 O33 75.08(11) . . ? O22 Mn9 O33 102.81(10) . . ? O31 Mn10 O16 119.47(12) . . ? O31 Mn10 O24 98.05(13) . . ? O16 Mn10 O24 142.43(11) . . ? O31 Mn10 O28 98.23(12) . . ? O16 Mn10 O28 86.47(10) . . ? O24 Mn10 O28 90.23(11) . . ? O31 Mn10 O23 104.73(11) . . ? O16 Mn10 O23 87.80(10) . . ? O24 Mn10 O23 80.36(11) . . ? O28 Mn10 O23 156.14(11) . . ? Mn3 O1 Mn2 106.11(12) . . ? Mn3 O1 Mn1 106.01(11) . . ? Mn2 O1 Mn1 107.05(12) . . ? C1 O2 Mn1 127.2(2) . . ? C8 O3 Mn3 125.7(2) . . ? C15 O4 Mn1 128.2(2) . . ? C15 O5 Mn2 127.2(2) . . ? C110 O6 Mn1 122.6(2) . . ? C110 O7 Mn5 137.6(2) . . ? Mn5 O8 Mn4 96.23(11) . . ? Mn5 O8 Mn2 148.64(14) . . ? Mn4 O8 Mn2 108.50(12) . . ? Mn5 O8 Mn1 111.75(10) . . ? Mn4 O8 Mn1 90.53(10) . . ? Mn2 O8 Mn1 87.56(9) . . ? C8 O9 Mn2 126.3(2) . . ? Mn6 O10 Mn3 149.78(15) . . ? Mn6 O10 Mn4 94.25(11) . . ? Mn3 O10 Mn4 107.04(11) . . ? Mn6 O10 Mn2 113.84(11) . . ? Mn3 O10 Mn2 87.29(9) . . ? Mn4 O10 Mn2 91.65(10) . . ? Mn7 O11 Mn1 148.12(13) . . ? Mn7 O11 Mn4 95.77(11) . . ? Mn1 O11 Mn4 107.32(12) . . ? Mn7 O11 Mn3 113.02(12) . . ? Mn1 O11 Mn3 88.26(9) . . ? Mn4 O11 Mn3 92.16(9) . . ? C29 O12 Mn2 123.1(3) . . ? C29 O13 Mn6 134.2(2) . . ? C22 O14 Mn3 123.8(2) . . ? C22 O15 Mn7 137.3(2) . . ? Mn7 O16 Mn4 101.28(12) . . ? Mn7 O16 Mn10 127.63(14) . . ? Mn4 O16 Mn10 129.18(12) . . ? Mn6 O17 Mn4 99.63(12) . . ? Mn6 O17 Mn9 129.56(12) . . ? Mn4 O17 Mn9 130.24(13) . . ? Mn5 O18 Mn4 101.33(12) . . ? Mn5 O18 Mn8 129.02(14) . . ? Mn4 O18 Mn8 129.55(14) . . ? C69 O19 Mn7 128.5(2) . . ? C67 O20 Mn8 119.9(2) . . ? C67 O20 Mn7 120.5(2) . . ? Mn8 O20 Mn7 118.36(11) . . ? C56 O21 Mn5 130.2(2) . . ? C54 O22 Mn5 122.8(2) . . ? C54 O22 Mn9 119.4(2) . . ? Mn5 O22 Mn9 117.13(11) . . ? C41 O23 Mn10 130.3(2) . . ? C41 O23 Mn6 113.1(2) . . ? Mn10 O23 Mn6 112.61(12) . . ? C43 O24 Mn10 132.4(3) . . ? C82 O25 Mn5 133.5(3) . . ? C82 O26 Mn8 132.9(3) . . ? C75 O27 Mn7 124.5(3) . . ? C75 O28 Mn10 127.7(2) . . ? C103 O29 Mn8 110.3(3) . . ? C103 O30 Mn9 134.9(3) . . ? C89 O31 Mn10 150.6(3) . . ? C89 O32 Mn9 127.8(3) . . ? C96 O33 Mn9 116.9(2) . . ? C96 O34 Mn6 125.7(3) . . ? C1 O35 Mn3 127.3(2) . . ? C62 N1 C66 119.3(3) . . ? C62 N1 Mn8 123.6(3) . . ? C66 N1 Mn8 117.1(3) . . ? C72 N2 C70 116.9(4) . . ? C36 N3 C40 120.2(3) . . ? C36 N3 Mn6 123.5(3) . . ? C40 N3 Mn6 116.3(2) . . ? C44 N4 C46 117.1(4) . . ? C49 N5 C53 119.2(3) . . ? C49 N5 Mn9 121.8(3) . . ? C53 N5 Mn9 117.6(2) . . ? C59 N6 C57 116.8(4) . . ? O2 C1 O35 126.0(3) . . ? O2 C1 C2 117.5(3) . . ? O35 C1 C2 116.5(3) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 121.3(3) . . ? C7 C2 C1 119.1(4) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.5(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.1(4) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O3 C8 O9 125.6(3) . . ? O3 C8 C9 118.2(3) . . ? O9 C8 C9 116.2(3) . . ? C14 C9 C10 118.6(4) . . ? C14 C9 C8 120.1(3) . . ? C10 C9 C8 121.2(4) . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C9 121.1(4) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? O5 C15 O4 125.8(3) . . ? O5 C15 C16 118.5(3) . . ? O4 C15 C16 115.6(3) . . ? C17 C16 C21 119.7(4) . . ? C17 C16 C15 119.2(4) . . ? C21 C16 C15 121.0(4) . . ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 119.6(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C16 C21 C20 119.7(4) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? O15 C22 O14 124.2(3) . . ? O15 C22 C23 120.1(3) . . ? O14 C22 C23 115.7(3) . . ? C24 C23 C28 118.5(4) . . ? C24 C23 C22 120.4(4) . . ? C28 C23 C22 121.1(3) . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 121.5(4) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 118.8(4) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 119.8(4) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C23 121.2(4) . . ? C27 C28 H28 119.4 . . ? C23 C28 H28 119.4 . . ? O13 C29 O12 125.3(3) . . ? O13 C29 C30 120.2(3) . . ? O12 C29 C30 114.5(4) . . ? C35 C30 C31 120.0(4) . . ? C35 C30 C29 121.0(4) . . ? C31 C30 C29 118.9(4) . . ? C30 C31 C32 118.7(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C33 C32 C31 121.0(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 120.9(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C33 C34 C35 119.1(5) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C30 C35 C34 120.3(5) . . ? C30 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? N3 C36 C37 121.8(4) . . ? N3 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C38 C37 C36 118.1(4) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? C39 C38 C37 120.1(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 119.6(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N3 C40 C39 120.2(4) . . ? N3 C40 C41 115.0(3) . . ? C39 C40 C41 124.6(4) . . ? O23 C41 C42 125.7(4) . . ? O23 C41 C40 113.4(3) . . ? C42 C41 C40 120.9(3) . . ? C41 C42 C43 123.3(4) . . ? C41 C42 H42 118.4 . . ? C43 C42 H42 118.4 . . ? O24 C43 C42 124.6(4) . . ? O24 C43 C44 115.1(4) . . ? C42 C43 C44 120.3(4) . . ? N4 C44 C45 123.7(4) . . ? N4 C44 C43 118.1(4) . . ? C45 C44 C43 118.3(4) . . ? C44 C45 C48 118.9(4) . . ? C44 C45 H45 120.6 . . ? C48 C45 H45 120.6 . . ? N4 C46 C47 123.1(5) . . ? N4 C46 H46 118.4 . . ? C47 C46 H46 118.4 . . ? C48 C47 C46 119.6(5) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C45 117.7(4) . . ? C47 C48 H48 121.1 . . ? C45 C48 H48 121.1 . . ? N5 C49 C50 122.6(4) . . ? N5 C49 H49 118.7 . . ? C50 C49 H49 118.7 . . ? C51 C50 C49 118.2(4) . . ? C51 C50 H50 120.9 . . ? C49 C50 H50 120.9 . . ? C50 C51 C52 119.5(4) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C53 C52 C51 118.6(4) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? N5 C53 C52 121.8(3) . . ? N5 C53 C54 114.7(3) . . ? C52 C53 C54 123.5(4) . . ? O22 C54 C55 124.4(3) . . ? O22 C54 C53 115.3(3) . . ? C55 C54 C53 120.3(3) . . ? C54 C55 C56 124.9(4) . . ? C54 C55 H55 117.5 . . ? C56 C55 H55 117.5 . . ? O21 C56 C55 126.4(4) . . ? O21 C56 C57 114.3(3) . . ? C55 C56 C57 119.3(4) . . ? N6 C57 C58 122.2(4) . . ? N6 C57 C56 117.5(3) . . ? C58 C57 C56 120.3(4) . . ? C61 C58 C57 119.5(4) . . ? C61 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? N6 C59 C60 124.9(5) . . ? N6 C59 H59 117.5 . . ? C60 C59 H59 117.5 . . ? C61 C60 C59 117.3(5) . . ? C61 C60 H60 121.4 . . ? C59 C60 H60 121.4 . . ? C60 C61 C58 119.3(4) . . ? C60 C61 H61 120.3 . . ? C58 C61 H61 120.3 . . ? N1 C62 C63 122.6(4) . . ? N1 C62 H62 118.7 . . ? C63 C62 H62 118.7 . . ? C64 C63 C62 117.9(4) . . ? C64 C63 H63 121.0 . . ? C62 C63 H63 121.0 . . ? C65 C64 C63 119.4(4) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? C64 C65 C66 119.2(4) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? N1 C66 C65 121.6(4) . . ? N1 C66 C67 114.9(3) . . ? C65 C66 C67 123.5(4) . . ? O20 C67 C68 124.7(3) . . ? O20 C67 C66 115.2(3) . . ? C68 C67 C66 120.1(3) . . ? C67 C68 C69 125.1(3) . . ? C67 C68 H68 117.5 . . ? C69 C68 H68 117.5 . . ? O19 C69 C68 126.6(3) . . ? O19 C69 C70 115.6(3) . . ? C68 C69 C70 117.9(3) . . ? N2 C70 C71 123.7(4) . . ? N2 C70 C69 116.7(3) . . ? C71 C70 C69 119.5(3) . . ? C70 C71 C74 118.4(4) . . ? C70 C71 H71 120.8 . . ? C74 C71 H71 120.8 . . ? N2 C72 C73 123.9(4) . . ? N2 C72 H72 118.1 . . ? C73 C72 H72 118.1 . . ? C72 C73 C74 118.8(4) . . ? C72 C73 H73 120.6 . . ? C74 C73 H73 120.6 . . ? C73 C74 C71 118.3(4) . . ? C73 C74 H74 120.8 . . ? C71 C74 H74 120.8 . . ? O28 C75 O27 125.0(3) . . ? O28 C75 C76 118.4(4) . . ? O27 C75 C76 116.6(3) . . ? C77 C76 C81 119.9(4) . . ? C77 C76 C75 120.8(4) . . ? C81 C76 C75 119.3(4) . . ? C76 C77 C78 120.2(4) . . ? C76 C77 H77 119.9 . . ? C78 C77 H77 119.9 . . ? C77 C78 C79 119.9(5) . . ? C77 C78 H78 120.1 . . ? C79 C78 H78 120.1 . . ? C80 C79 C78 119.5(4) . . ? C80 C79 H79 120.2 . . ? C78 C79 H79 120.2 . . ? C79 C80 C81 120.7(5) . . ? C79 C80 H80 119.6 . . ? C81 C80 H80 119.6 . . ? C80 C81 C76 119.6(5) . . ? C80 C81 H81 120.2 . . ? C76 C81 H81 120.2 . . ? O26 C82 O25 126.3(4) . . ? O26 C82 C83 117.6(4) . . ? O25 C82 C83 116.1(4) . . ? C88 C83 C84 119.5(5) . . ? C88 C83 C82 120.3(4) . . ? C84 C83 C82 120.2(5) . . ? C85 C84 C83 119.8(6) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C86 C85 C84 120.3(6) . . ? C86 C85 H85 119.8 . . ? C84 C85 H85 119.8 . . ? C85 C86 C87 120.9(6) . . ? C85 C86 H86 119.6 . . ? C87 C86 H86 119.6 . . ? C88 C87 C86 118.6(7) . . ? C88 C87 H87 120.7 . . ? C86 C87 H87 120.7 . . ? C87 C88 C83 120.8(6) . . ? C87 C88 H88 119.6 . . ? C83 C88 H88 119.6 . . ? O31 C89 O32 124.6(4) . . ? O31 C89 C90 117.6(4) . . ? O32 C89 C90 117.8(4) . . ? C91 C90 C95 119.3(5) . . ? C91 C90 C89 120.5(5) . . ? C95 C90 C89 120.1(4) . . ? C92 C91 C90 119.5(6) . . ? C92 C91 H91 120.2 . . ? C90 C91 H91 120.2 . . ? C91 C92 C93 120.8(6) . . ? C91 C92 H92 119.6 . . ? C93 C92 H92 119.6 . . ? C94 C93 C92 120.3(6) . . ? C94 C93 H93 119.8 . . ? C92 C93 H93 119.8 . . ? C93 C94 C95 119.9(6) . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C94 C95 C90 120.1(5) . . ? C94 C95 H95 119.9 . . ? C90 C95 H95 119.9 . . ? O33 C96 O34 125.1(4) . . ? O33 C96 C97 120.1(4) . . ? O34 C96 C97 114.8(4) . . ? C102 C97 C98 120.7(5) . . ? C102 C97 C96 120.7(4) . . ? C98 C97 C96 118.6(5) . . ? C97 C98 C99 118.0(6) . . ? C97 C98 H98 121.0 . . ? C99 C98 H98 121.0 . . ? C100 C99 C98 120.6(6) . . ? C100 C99 H99 119.7 . . ? C98 C99 H99 119.7 . . ? C101 C100 C99 120.6(5) . . ? C101 C100 H1A 119.7 . . ? C99 C100 H1A 119.7 . . ? C100 C101 C102 120.5(7) . . ? C100 C101 H2A 119.8 . . ? C102 C101 H2A 119.8 . . ? C97 C102 C101 119.5(6) . . ? C97 C102 H3A 120.2 . . ? C101 C102 H3A 120.2 . . ? O30 C103 O29 124.0(4) . . ? O30 C103 C1A 117.8(5) . . ? O29 C103 C1A 116.0(5) . . ? O30 C103 C104 119.3(4) . . ? O29 C103 C104 116.0(4) . . ? C105 C104 C109 120.0 . . ? C105 C104 C103 117.3(2) . . ? C109 C104 C103 122.4(2) . . ? C104 C105 C106 120.0 . . ? C104 C105 H105 120.0 . . ? C106 C105 H105 120.0 . . ? C107 C106 C105 120.0 . . ? C107 C106 H106 120.0 . . ? C105 C106 H106 120.0 . . ? C106 C107 C108 120.0 . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? C109 C108 C107 120.0 . . ? C109 C108 H108 120.0 . . ? C107 C108 H108 120.0 . . ? C108 C109 C104 120.0 . . ? C108 C109 H109 120.0 . . ? C104 C109 H109 120.0 . . ? O7 C110 O6 124.6(2) . . ? O7 C110 C111 120.0(2) . . ? O6 C110 C111 115.4(2) . . ? C112 C111 C116 119.8(2) . . ? C112 C111 C110 119.6 . . ? C116 C111 C110 120.3(2) . . ? C111 C112 C113 120.0(3) . . ? C111 C112 H4A 120.0 . . ? C113 C112 H4A 120.0 . . ? C114 C113 C112 119.9(4) . . ? C114 C113 H5A 120.0 . . ? C112 C113 H5A 120.0 . . ? C115 C114 C113 119.7(4) . . ? C115 C114 H6A 120.1 . . ? C113 C114 H6A 120.1 . . ? C114 C115 C116 120.7(4) . . ? C114 C115 H7A 119.6 . . ? C116 C115 H7A 119.6 . . ? C115 C116 C111 119.7(4) . . ? C115 C116 H8A 120.1 . . ? C111 C116 H8A 120.1 . . ? C2A C1A C6A 118.8(9) . . ? C2A C1A C103 122.3(7) . . ? C6A C1A C103 118.4(8) . . ? C1A C2A C3A 121.1(9) . . ? C1A C2A H2A1 119.5 . . ? C3A C2A H2A1 119.5 . . ? C4A C3A C2A 118.6(10) . . ? C4A C3A H3A1 120.7 . . ? C2A C3A H3A1 120.7 . . ? C5A C4A C3A 120.3(11) . . ? C5A C4A H4A1 119.8 . . ? C3A C4A H4A1 119.8 . . ? C4A C5A C6A 121.3(12) . . ? C4A C5A H5A1 119.4 . . ? C6A C5A H5A1 119.4 . . ? C5A C6A C1A 119.1(11) . . ? C5A C6A H6A1 120.5 . . ? C1A C6A H6A1 120.5 . . ? Cl1S C1S Cl2S 112.1(3) . . ? Cl1S C1S H5B 109.2 . . ? Cl2S C1S H5B 109.2 . . ? Cl1S C1S H6B 109.2 . . ? Cl2S C1S H6B 109.2 . . ? H5B C1S H6B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.759 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.092 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.039 0.701 0.899 13 1 ' ' 2 0.432 0.114 0.358 290 59 ' ' 3 0.568 0.886 0.642 292 59 ' ' 4 0.456 0.898 0.534 9 0 ' ' 5 0.544 0.102 0.466 8 0 ' ' 6 0.961 0.299 0.101 13 1 ' ' _platon_squeeze_details ; ; # Attachment '- 2 Mn6(dppd)final3.CIF' #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 768052' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C104 H72 Mn6 N16 O16, 4(B2 F8) ; _chemical_formula_sum 'C104 H72 B4 F16 Mn6 N16 O16' _chemical_formula_weight 2478.66 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' B B 0.0013 0.0007 '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' 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 tetragonal _symmetry_space_group_name_H-M I41 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x, -y, z' 'y, -x+1/2, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1, z+3/4' _cell_length_a 29.3102(4) _cell_length_b 29.3102(4) _cell_length_c 15.2712(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13119.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.54 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5000 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.774 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47271 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 26.36 _reflns_number_total 13420 _reflns_number_gt 9593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains half the cluster as well as two tetrafluoro- borate counterions, one of which is disordered over two sites, some of the thermal parameters are fixed to 10.2. One of the pyridyl rings of the cluster had to be restrained to an idealised ring position with the thermal parameters fixed to 10.15. All non H-atoms were refined anisotropically, except for the pyridyl ring (C9-C13 and N2) and BF4 molecule (B5 and F5s-F8s) which the thermal parameters are fixed. The ISOR restraint was placed on atoms F7S, C1, C2, C8 and C7, while Bond restraints (DFIX) were placed on both tetrafluoroborate counter ions. All H-atoms were placed in calculated positions. The two BF4 anions displayed high thermal parameters and thus is a likely cause of the close (~2.3 A) distance between the fluoride atoms. No solvent molecules other than the BF4 counter ions were found in the lattice hence large solvent accesible voids are present thus the squeeze program was utilized. ; _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^)+(0.1797P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(3) _refine_ls_number_reflns 13420 _refine_ls_number_parameters 652 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2451 _refine_ls_wR_factor_gt 0.2254 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.970 _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 1.08153(3) 0.52679(3) 0.00759(6) 0.0295(3) Uani 1 1 d . . . Mn2 Mn 0.97122(3) 0.58004(3) 0.05070(6) 0.0255(2) Uani 1 1 d . . . Mn3 Mn 0.85370(3) 0.57256(3) 0.02602(7) 0.0260(2) Uani 1 1 d . . . F1S F 0.7095(3) 0.8698(3) 0.0168(8) 0.136(4) Uani 1 1 d D A 3 F2S F 0.7392(4) 0.9387(3) 0.0453(10) 0.166(5) Uani 1 1 d D A 3 F3S F 0.7685(4) 0.8948(4) -0.0502(7) 0.142(4) Uani 1 1 d D A 3 F4S F 0.7735(4) 0.8781(4) 0.0826(9) 0.168(5) Uani 1 1 d D A 3 F5S F 0.5576(5) 0.8068(5) 0.0388(12) 0.200 Uiso 1 1 d D B 2 F6S F 0.5956(5) 0.8676(5) 0.0361(12) 0.200 Uiso 1 1 d D . . F7S F 0.6172(6) 0.8031(6) 0.0969(12) 0.200 Uiso 1 1 d D . . F8S F 0.6257(5) 0.8090(5) -0.0386(11) 0.200 Uiso 1 1 d D . . O1 O 1.15155(15) 0.50312(15) 0.0163(4) 0.0336(10) Uani 1 1 d . . . O2 O 1.1111(2) 0.58513(18) 0.0670(5) 0.0601(18) Uani 1 1 d . . . O3 O 1.02698(17) 0.54312(18) 0.1104(3) 0.0368(11) Uani 1 1 d . . . O4 O 1.01797(16) 0.55140(16) -0.0528(3) 0.0340(11) Uani 1 1 d . . . O5 O 0.92745(14) 0.54551(15) -0.0514(3) 0.0277(9) Uani 1 1 d . . . O6 O 1.08093(16) 0.47081(15) 0.1070(3) 0.0306(10) Uani 1 1 d . . . O7 O 0.91040(15) 0.62187(14) 0.0384(3) 0.0289(9) Uani 1 1 d . . . O8 O 0.81827(15) 0.63724(15) 0.0109(3) 0.0352(11) Uani 1 1 d . . . N1 N 1.22441(19) 0.4516(2) 0.0402(4) 0.0358(14) Uani 1 1 d . . . N3 N 0.98063(19) 0.60528(19) 0.1928(4) 0.0329(13) Uani 1 1 d . . . N4 N 1.14731(18) 0.42225(19) 0.1800(4) 0.0319(14) Uani 1 1 d . . . N5 N 1.0957(2) 0.5479(2) -0.1354(5) 0.0457(16) Uani 1 1 d . . . N6 N 0.8508(2) 0.57373(19) -0.1286(4) 0.0323(13) Uani 1 1 d . . . N7 N 0.99354(18) 0.65001(18) 0.0081(4) 0.0340(14) Uani 1 1 d . . . N8 N 0.8080(2) 0.7539(2) -0.0413(5) 0.0479(17) Uani 1 1 d . . . C1 C 1.2608(2) 0.4229(3) 0.0440(5) 0.0424(17) Uani 1 1 d U . . H1 H 1.2560 0.3917 0.0510 0.051 Uiso 1 1 calc R . . C2 C 1.3056(3) 0.4396(3) 0.0376(6) 0.051(2) Uani 1 1 d U . . H2 H 1.3304 0.4197 0.0368 0.061 Uiso 1 1 calc R . . C3 C 1.3121(3) 0.4863(4) 0.0325(7) 0.066(3) Uani 1 1 d . . . H3 H 1.3414 0.4984 0.0283 0.079 Uiso 1 1 calc R . . C4 C 1.2736(3) 0.5155(4) 0.0337(8) 0.065(3) Uani 1 1 d . . . H4 H 1.2770 0.5470 0.0310 0.079 Uiso 1 1 calc R . . C5 C 1.2314(3) 0.4960(3) 0.0390(6) 0.051(2) Uani 1 1 d . . . C6 C 1.1889(2) 0.5243(3) 0.0420(7) 0.049(2) Uani 1 1 d . . . C7 C 1.1883(4) 0.5690(3) 0.0725(9) 0.080(3) Uani 1 1 d U . . H7 H 1.2165 0.5828 0.0822 0.096 Uiso 1 1 calc R . . C8 C 1.1518(4) 0.5938(4) 0.0890(10) 0.088(4) Uani 1 1 d U . . C9 C 1.1599(5) 0.6388(4) 0.1303(9) 0.150 Uiso 1 1 d G . . C10 C 1.1250(4) 0.6622(5) 0.1726(9) 0.150 Uiso 1 1 d G . . H10 H 1.0971 0.6480 0.1826 0.180 Uiso 1 1 calc R . . C14 C 0.9567(3) 0.6367(3) 0.2332(5) 0.0385(17) Uani 1 1 d . . . H14 H 0.9355 0.6532 0.2007 0.046 Uiso 1 1 calc R . . C15 C 0.9612(4) 0.6469(4) 0.3236(7) 0.071(3) Uani 1 1 d . . . H15 H 0.9450 0.6706 0.3496 0.085 Uiso 1 1 calc R . . C16 C 0.9920(6) 0.6191(5) 0.3726(8) 0.118(6) Uani 1 1 d . . . H16 H 0.9939 0.6223 0.4331 0.141 Uiso 1 1 calc R . . C17 C 1.0177(5) 0.5891(4) 0.3325(7) 0.081(4) Uani 1 1 d . . . H17 H 1.0396 0.5729 0.3637 0.098 Uiso 1 1 calc R . . C18 C 1.0119(3) 0.5812(3) 0.2397(5) 0.049(2) Uani 1 1 d . . . C19 C 1.0357(3) 0.5446(3) 0.1918(5) 0.0384(16) Uani 1 1 d . . . C20 C 1.0667(3) 0.5154(3) 0.2320(4) 0.0375(17) Uani 1 1 d . . . H20 H 1.0733 0.5197 0.2910 0.045 Uiso 1 1 calc R . . C21 C 1.0884(3) 0.4798(2) 0.1873(5) 0.0361(16) Uani 1 1 d . . . C22 C 1.1197(2) 0.4480(2) 0.2345(4) 0.0297(14) Uani 1 1 d . . . C23 C 1.1227(3) 0.4449(3) 0.3224(6) 0.048(2) Uani 1 1 d . . . H23 H 1.1056 0.4645 0.3575 0.058 Uiso 1 1 calc R . . C24 C 1.1515(3) 0.4121(3) 0.3617(4) 0.0420(18) Uani 1 1 d . . . H24 H 1.1526 0.4085 0.4222 0.050 Uiso 1 1 calc R . . C25 C 1.1774(3) 0.3862(3) 0.3079(5) 0.0441(19) Uani 1 1 d . . . H25 H 1.1970 0.3643 0.3311 0.053 Uiso 1 1 calc R . . C26 C 1.1747(2) 0.3925(2) 0.2168(5) 0.0323(15) Uani 1 1 d . . . H26 H 1.1932 0.3748 0.1810 0.039 Uiso 1 1 calc R . . C27 C 1.1365(3) 0.5474(4) -0.1759(8) 0.071(3) Uani 1 1 d . . . H27 H 1.1621 0.5399 -0.1429 0.085 Uiso 1 1 calc R . . C28 C 1.1422(4) 0.5566(5) -0.2583(8) 0.091(4) Uani 1 1 d . . . H28 H 1.1714 0.5582 -0.2822 0.109 Uiso 1 1 calc R . . C29 C 1.1045(5) 0.5640(6) -0.3094(10) 0.106(5) Uani 1 1 d . . . H29 H 1.1077 0.5680 -0.3694 0.128 Uiso 1 1 calc R . . C30 C 1.0619(4) 0.5656(5) -0.2722(7) 0.080(4) Uani 1 1 d . . . H30 H 1.0363 0.5724 -0.3060 0.096 Uiso 1 1 calc R . . C31 C 1.0576(3) 0.5569(3) -0.1835(5) 0.0438(18) Uani 1 1 d . . . C32 C 1.0146(2) 0.5559(2) -0.1353(4) 0.0276(13) Uani 1 1 d . . . C33 C 0.9724(2) 0.5612(3) -0.1779(4) 0.0331(15) Uani 1 1 d . . . H33 H 0.9720 0.5672 -0.2377 0.040 Uiso 1 1 calc R . . C34 C 0.9308(2) 0.5577(2) -0.1331(4) 0.0271(13) Uani 1 1 d . . . C35 C 0.8855(2) 0.5659(3) -0.1811(5) 0.0396(17) Uani 1 1 d . . . C36 C 0.8848(3) 0.5653(4) -0.2700(5) 0.060(3) Uani 1 1 d . . . H36 H 0.9107 0.5605 -0.3040 0.072 Uiso 1 1 calc R . . C37 C 0.8408(5) 0.5726(5) -0.3057(9) 0.088(4) Uani 1 1 d . . . H37 H 0.8368 0.5727 -0.3661 0.106 Uiso 1 1 calc R . . C38 C 0.8040(4) 0.5795(4) -0.2518(8) 0.075(3) Uani 1 1 d . . . H38 H 0.7749 0.5822 -0.2752 0.090 Uiso 1 1 calc R . . C39 C 0.8102(3) 0.5821(4) -0.1685(5) 0.055(2) Uani 1 1 d . . . H39 H 0.7854 0.5901 -0.1336 0.066 Uiso 1 1 calc R . . C40 C 1.0378(3) 0.6642(3) 0.0001(7) 0.057(3) Uani 1 1 d . . . H40 H 1.0606 0.6424 -0.0074 0.068 Uiso 1 1 calc R . . C41 C 1.0500(3) 0.7106(3) 0.0028(8) 0.062(3) Uani 1 1 d . . . H41 H 1.0804 0.7192 -0.0021 0.075 Uiso 1 1 calc R . . C42 C 1.0168(3) 0.7429(3) 0.0125(9) 0.073(3) Uani 1 1 d . . . H42 H 1.0243 0.7736 0.0164 0.088 Uiso 1 1 calc R . . C43 C 0.9711(2) 0.7288(2) 0.0163(6) 0.0430(18) Uani 1 1 d . . . H43 H 0.9477 0.7502 0.0208 0.052 Uiso 1 1 calc R . . C44 C 0.9612(3) 0.6827(3) 0.0133(5) 0.0388(16) Uani 1 1 d . . . C45 C 0.9138(2) 0.6632(2) 0.0165(4) 0.0309(14) Uani 1 1 d . . . C46 C 0.8769(2) 0.6917(2) -0.0087(5) 0.0316(14) Uani 1 1 d . . . H46 H 0.8829 0.7214 -0.0267 0.038 Uiso 1 1 calc R . . C47 C 0.8315(2) 0.6762(2) -0.0072(4) 0.0297(14) Uani 1 1 d . . . C48 C 0.7953(3) 0.7104(3) -0.0383(5) 0.0413(18) Uani 1 1 d . . . C49 C 0.7510(3) 0.6950(3) -0.0566(7) 0.061(3) Uani 1 1 d . . . H49 H 0.7438 0.6642 -0.0539 0.073 Uiso 1 1 calc R . . C50 C 0.7182(4) 0.7271(5) -0.0788(10) 0.094(5) Uani 1 1 d . . . H50 H 0.6889 0.7180 -0.0946 0.113 Uiso 1 1 calc R . . C51 C 0.7298(4) 0.7727(4) -0.0769(9) 0.080(4) Uani 1 1 d . . . H51 H 0.7079 0.7953 -0.0845 0.095 Uiso 1 1 calc R . . C52 C 0.7748(3) 0.7837(3) -0.0635(8) 0.063(3) Uani 1 1 d . . . H52 H 0.7832 0.8141 -0.0703 0.075 Uiso 1 1 calc R . . B1S B 0.7470(3) 0.8958(3) 0.0238(7) 0.070(3) Uani 1 1 d D A 3 B5 B 0.5998(6) 0.8229(6) 0.0270(13) 0.200 Uiso 1 1 d D B 2 C11 C 1.1319(4) 0.7069(5) 0.2001(9) 0.150 Uiso 1 1 d G . . H11 H 1.1086 0.7226 0.2284 0.180 Uiso 1 1 calc R . . C12 C 1.1736(5) 0.7282(4) 0.1852(9) 0.150 Uiso 1 1 d G . . H12 H 1.1782 0.7581 0.2036 0.180 Uiso 1 1 calc R . . C13 C 1.2084(4) 0.7047(5) 0.1429(9) 0.150 Uiso 1 1 d G . . H13 H 1.2363 0.7189 0.1330 0.180 Uiso 1 1 calc R . . N2 N 1.2016(4) 0.6600(5) 0.1154(9) 0.150 Uiso 1 1 d G . . 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 0.0259(5) 0.0261(5) 0.0367(6) -0.0005(4) -0.0056(4) 0.0077(4) Mn2 0.0226(5) 0.0237(5) 0.0301(5) 0.0010(4) -0.0015(4) 0.0074(4) Mn3 0.0190(4) 0.0212(5) 0.0378(5) 0.0008(4) 0.0017(4) 0.0050(4) F1S 0.112(6) 0.125(7) 0.170(10) 0.063(7) -0.022(7) -0.015(5) F2S 0.139(8) 0.119(8) 0.241(14) -0.071(9) 0.048(9) -0.010(6) F3S 0.136(8) 0.144(9) 0.147(9) -0.018(7) 0.062(7) -0.022(6) F4S 0.133(8) 0.173(10) 0.198(12) 0.096(9) -0.030(8) -0.049(7) O1 0.029(2) 0.025(2) 0.047(3) 0.004(2) 0.004(2) 0.0007(18) O2 0.062(4) 0.025(3) 0.093(5) -0.020(3) -0.027(3) 0.015(3) O3 0.042(3) 0.043(3) 0.025(2) -0.011(2) -0.006(2) 0.015(2) O4 0.031(2) 0.027(2) 0.043(3) -0.007(2) 0.007(2) 0.0005(19) O5 0.022(2) 0.030(2) 0.031(2) -0.0068(19) -0.0030(18) 0.0061(18) O6 0.034(2) 0.031(2) 0.027(2) -0.0131(19) -0.0084(19) 0.0094(19) O7 0.030(2) 0.026(2) 0.030(2) 0.0016(19) -0.0001(18) -0.0004(18) O8 0.029(2) 0.026(2) 0.051(3) -0.002(2) -0.001(2) 0.0010(19) N1 0.026(3) 0.042(3) 0.039(3) 0.005(3) 0.000(2) 0.004(2) N3 0.031(3) 0.025(3) 0.043(3) -0.002(2) 0.009(3) 0.008(2) N4 0.019(3) 0.025(3) 0.052(4) 0.002(2) -0.012(2) 0.002(2) N5 0.027(3) 0.046(4) 0.065(4) 0.014(3) 0.013(3) 0.003(3) N6 0.032(3) 0.024(3) 0.040(3) -0.002(2) -0.014(2) -0.001(2) N7 0.020(3) 0.026(3) 0.055(4) -0.005(3) -0.013(3) 0.002(2) N8 0.035(3) 0.032(3) 0.076(5) 0.026(3) -0.005(3) -0.004(3) C1 0.026(3) 0.060(4) 0.041(4) 0.010(3) -0.002(3) -0.001(3) C2 0.033(4) 0.066(5) 0.055(4) 0.003(4) -0.007(3) -0.001(3) C3 0.032(4) 0.088(7) 0.078(7) 0.020(6) -0.004(4) -0.026(4) C4 0.024(4) 0.079(6) 0.094(7) 0.019(6) -0.016(4) -0.013(4) C5 0.039(4) 0.055(5) 0.059(5) -0.004(4) -0.011(4) -0.015(4) C6 0.029(4) 0.033(4) 0.085(6) 0.002(4) -0.022(4) -0.007(3) C7 0.066(6) 0.042(5) 0.131(8) -0.020(5) -0.019(6) -0.005(4) C8 0.089(7) 0.051(5) 0.124(8) -0.041(5) -0.035(6) -0.011(5) C14 0.038(4) 0.035(4) 0.042(4) 0.000(3) -0.003(3) 0.012(3) C15 0.085(8) 0.070(7) 0.057(6) -0.010(5) -0.011(5) 0.038(6) C16 0.175(15) 0.134(12) 0.045(6) -0.039(7) -0.015(7) 0.089(12) C17 0.134(11) 0.059(6) 0.051(5) -0.022(5) -0.042(6) 0.043(7) C18 0.052(5) 0.062(5) 0.035(4) -0.002(4) 0.002(3) 0.031(4) C19 0.042(4) 0.038(4) 0.035(4) -0.004(3) -0.004(3) 0.015(3) C20 0.050(4) 0.047(4) 0.015(3) -0.003(3) -0.003(3) 0.019(4) C21 0.036(4) 0.020(3) 0.052(4) -0.001(3) -0.007(3) 0.013(3) C22 0.030(3) 0.030(3) 0.029(3) -0.008(3) -0.005(3) 0.005(3) C23 0.033(4) 0.056(5) 0.056(5) -0.010(4) -0.009(3) 0.017(4) C24 0.054(5) 0.059(5) 0.013(3) 0.010(3) -0.002(3) 0.003(4) C25 0.039(4) 0.048(4) 0.046(4) 0.024(4) -0.014(3) 0.008(3) C26 0.020(3) 0.028(3) 0.049(4) -0.004(3) 0.002(3) 0.006(3) C27 0.039(5) 0.094(8) 0.080(7) 0.023(6) 0.017(5) 0.005(5) C28 0.046(6) 0.160(13) 0.067(7) 0.035(8) 0.033(5) -0.004(7) C29 0.081(9) 0.163(15) 0.075(8) 0.031(9) 0.012(7) 0.022(9) C30 0.050(6) 0.123(10) 0.066(6) 0.050(7) 0.014(5) 0.016(6) C31 0.038(4) 0.051(5) 0.042(4) 0.002(4) 0.001(3) -0.001(3) C32 0.030(3) 0.029(3) 0.024(3) -0.003(3) -0.004(3) 0.003(3) C33 0.039(4) 0.041(4) 0.019(3) 0.004(3) -0.003(3) 0.000(3) C34 0.029(3) 0.019(3) 0.033(3) -0.008(3) -0.014(3) -0.003(2) C35 0.021(3) 0.044(4) 0.053(5) 0.010(3) -0.011(3) 0.001(3) C36 0.044(5) 0.105(8) 0.032(4) 0.015(4) -0.005(4) -0.010(5) C37 0.082(8) 0.113(11) 0.069(7) 0.013(7) -0.008(6) -0.005(7) C38 0.048(5) 0.100(8) 0.078(7) -0.022(6) -0.021(5) 0.023(5) C39 0.035(4) 0.090(7) 0.040(4) -0.007(4) -0.005(3) 0.012(4) C40 0.027(4) 0.029(4) 0.115(8) 0.019(4) 0.000(4) 0.001(3) C41 0.020(4) 0.057(5) 0.109(9) 0.006(5) -0.001(4) -0.006(4) C42 0.037(5) 0.051(5) 0.132(11) 0.022(6) -0.009(6) -0.005(4) C43 0.028(3) 0.027(3) 0.074(6) 0.006(4) 0.005(4) 0.000(3) C44 0.038(4) 0.039(4) 0.040(4) 0.002(3) 0.003(3) -0.003(3) C45 0.031(3) 0.035(4) 0.027(3) -0.003(3) 0.001(3) 0.002(3) C46 0.031(3) 0.024(3) 0.039(4) 0.001(3) -0.007(3) 0.012(3) C47 0.015(3) 0.037(4) 0.037(3) 0.002(3) 0.003(2) 0.002(3) C48 0.033(4) 0.048(4) 0.042(4) 0.014(3) -0.014(3) -0.006(3) C49 0.032(4) 0.046(5) 0.104(8) 0.030(5) -0.030(5) -0.001(4) C50 0.038(5) 0.102(9) 0.143(12) 0.070(9) -0.032(6) -0.004(6) C51 0.051(6) 0.069(7) 0.118(9) 0.042(7) -0.024(6) 0.017(5) C52 0.043(5) 0.043(5) 0.102(8) 0.029(5) -0.004(5) 0.013(4) B1S 0.059(7) 0.071(8) 0.080(8) -0.018(7) 0.009(7) -0.006(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 O2 2.121(6) . ? Mn1 O1 2.170(4) . ? Mn1 O4 2.200(5) . ? Mn1 O6 2.236(5) . ? Mn1 O3 2.291(5) . ? Mn1 N5 2.307(7) . ? Mn1 O5 2.317(5) 3_765 ? Mn2 O3 2.162(5) . ? Mn2 O7 2.172(4) . ? Mn2 N7 2.249(6) . ? Mn2 O4 2.254(5) . ? Mn2 O5 2.258(4) . ? Mn2 O6 2.302(4) 3_765 ? Mn2 N3 2.309(6) . ? Mn3 O8 2.174(4) . ? Mn3 O7 2.211(4) . ? Mn3 O1 2.229(4) 3_765 ? Mn3 N4 2.356(6) 3_765 ? Mn3 N6 2.364(6) . ? Mn3 N1 2.406(6) 3_765 ? F1S B1S 1.342(8) . ? F2S B1S 1.321(8) . ? F3S B1S 1.295(8) . ? F4S B1S 1.295(9) . ? F5S B5 1.335(10) . ? F6S B5 1.322(10) . ? F7S B5 1.319(10) . ? F8S B5 1.322(10) . ? O1 C6 1.317(8) . ? O1 Mn3 2.229(4) 3_765 ? O2 C8 1.265(13) . ? O3 C19 1.270(9) . ? O4 C32 1.270(8) . ? O5 C34 1.302(8) . ? O5 Mn1 2.317(5) 3_765 ? O6 C21 1.273(9) . ? O6 Mn2 2.302(4) 3_765 ? O7 C45 1.260(8) . ? O8 C47 1.237(8) . ? N1 C5 1.316(10) . ? N1 C1 1.362(9) . ? N1 Mn3 2.406(6) 3_765 ? N3 C14 1.311(9) . ? N3 C18 1.360(10) . ? N4 C26 1.312(9) . ? N4 C22 1.386(9) . ? N4 Mn3 2.356(6) 3_765 ? N5 C27 1.348(11) . ? N5 C31 1.363(11) . ? N6 C35 1.315(10) . ? N6 C39 1.360(10) . ? N7 C44 1.352(9) . ? N7 C40 1.369(9) . ? N8 C48 1.329(10) . ? N8 C52 1.349(10) . ? C1 C2 1.404(11) . ? C1 H1 0.9300 . ? C2 C3 1.386(13) . ? C2 H2 0.9300 . ? C3 C4 1.415(14) . ? C3 H3 0.9300 . ? C4 C5 1.367(11) . ? C4 H4 0.9300 . ? C5 C6 1.498(12) . ? C6 C7 1.392(13) . ? C7 C8 1.318(17) . ? C7 H7 0.9300 . ? C8 C9 1.481(13) . ? C9 C10 1.3900 . ? C9 N2 1.3900 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C14 C15 1.420(13) . ? C14 H14 0.9300 . ? C15 C16 1.429(16) . ? C15 H15 0.9300 . ? C16 C17 1.308(15) . ? C16 H16 0.9300 . ? C17 C18 1.447(12) . ? C17 H17 0.9300 . ? C18 C19 1.474(10) . ? C19 C20 1.391(10) . ? C20 C21 1.399(10) . ? C20 H20 0.9300 . ? C21 C22 1.493(9) . ? C22 C23 1.348(11) . ? C23 C24 1.414(11) . ? C23 H23 0.9300 . ? C24 C25 1.353(12) . ? C24 H24 0.9300 . ? C25 C26 1.405(11) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.297(16) . ? C27 H27 0.9300 . ? C28 C29 1.372(18) . ? C28 H28 0.9300 . ? C29 C30 1.373(17) . ? C29 H29 0.9300 . ? C30 C31 1.384(13) . ? C30 H30 0.9300 . ? C31 C32 1.460(10) . ? C32 C33 1.406(9) . ? C33 C34 1.400(10) . ? C33 H33 0.9300 . ? C34 C35 1.536(9) . ? C35 C36 1.357(11) . ? C36 C37 1.417(16) . ? C36 H36 0.9300 . ? C37 C38 1.371(17) . ? C37 H37 0.9300 . ? C38 C39 1.287(14) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.406(12) . ? C40 H40 0.9300 . ? C41 C42 1.366(13) . ? C41 H41 0.9300 . ? C42 C43 1.404(11) . ? C42 H42 0.9300 . ? C43 C44 1.381(10) . ? C43 H43 0.9300 . ? C44 C45 1.504(10) . ? C45 C46 1.419(9) . ? C46 C47 1.405(9) . ? C46 H46 0.9300 . ? C47 C48 1.535(10) . ? C48 C49 1.402(11) . ? C49 C50 1.387(13) . ? C49 H49 0.9300 . ? C50 C51 1.379(17) . ? C50 H50 0.9300 . ? C51 C52 1.374(14) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 N2 1.3900 . ? C13 H13 0.9300 . ? 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 O2 Mn1 O1 81.1(2) . . ? O2 Mn1 O4 105.1(2) . . ? O1 Mn1 O4 158.6(2) . . ? O2 Mn1 O6 107.7(2) . . ? O1 Mn1 O6 74.42(17) . . ? O4 Mn1 O6 121.25(18) . . ? O2 Mn1 O3 79.8(2) . . ? O1 Mn1 O3 133.22(19) . . ? O4 Mn1 O3 68.16(17) . . ? O6 Mn1 O3 71.49(17) . . ? O2 Mn1 N5 96.6(3) . . ? O1 Mn1 N5 88.5(2) . . ? O4 Mn1 N5 70.6(2) . . ? O6 Mn1 N5 147.3(2) . . ? O3 Mn1 N5 135.9(2) . . ? O2 Mn1 O5 161.79(19) . 3_765 ? O1 Mn1 O5 80.73(16) . 3_765 ? O4 Mn1 O5 92.34(16) . 3_765 ? O6 Mn1 O5 65.92(15) . 3_765 ? O3 Mn1 O5 112.21(18) . 3_765 ? N5 Mn1 O5 84.2(2) . 3_765 ? O3 Mn2 O7 160.00(18) . . ? O3 Mn2 N7 111.0(2) . . ? O7 Mn2 N7 72.48(18) . . ? O3 Mn2 O4 69.48(17) . . ? O7 Mn2 O4 130.44(18) . . ? N7 Mn2 O4 87.7(2) . . ? O3 Mn2 O5 119.75(17) . . ? O7 Mn2 O5 74.17(16) . . ? N7 Mn2 O5 112.0(2) . . ? O4 Mn2 O5 72.21(17) . . ? O3 Mn2 O6 91.17(19) . 3_765 ? O7 Mn2 O6 81.53(16) . 3_765 ? N7 Mn2 O6 153.10(18) . 3_765 ? O4 Mn2 O6 115.13(17) . 3_765 ? O5 Mn2 O6 65.82(17) . 3_765 ? O3 Mn2 N3 70.96(18) . . ? O7 Mn2 N3 89.91(19) . . ? N7 Mn2 N3 86.8(2) . . ? O4 Mn2 N3 134.88(19) . . ? O5 Mn2 N3 149.32(19) . . ? O6 Mn2 N3 86.30(19) 3_765 . ? O8 Mn3 O7 78.34(16) . . ? O8 Mn3 O1 145.90(17) . 3_765 ? O7 Mn3 O1 135.10(16) . 3_765 ? O8 Mn3 N4 92.5(2) . 3_765 ? O7 Mn3 N4 83.21(18) . 3_765 ? O1 Mn3 N4 97.5(2) 3_765 3_765 ? O8 Mn3 N6 82.2(2) . . ? O7 Mn3 N6 95.91(19) . . ? O1 Mn3 N6 86.85(19) 3_765 . ? N4 Mn3 N6 174.69(18) 3_765 . ? O8 Mn3 N1 79.16(19) . 3_765 ? O7 Mn3 N1 154.17(18) . 3_765 ? O1 Mn3 N1 69.35(18) 3_765 3_765 ? N4 Mn3 N1 85.3(2) 3_765 3_765 ? N6 Mn3 N1 93.4(2) . 3_765 ? C6 O1 Mn1 130.8(5) . . ? C6 O1 Mn3 120.4(4) . 3_765 ? Mn1 O1 Mn3 104.89(18) . 3_765 ? C8 O2 Mn1 131.3(6) . . ? C19 O3 Mn2 123.2(4) . . ? C19 O3 Mn1 122.5(5) . . ? Mn2 O3 Mn1 110.1(2) . . ? C32 O4 Mn1 121.1(4) . . ? C32 O4 Mn2 127.5(4) . . ? Mn1 O4 Mn2 110.0(2) . . ? C34 O5 Mn2 119.7(4) . . ? C34 O5 Mn1 129.2(4) . 3_765 ? Mn2 O5 Mn1 101.90(18) . 3_765 ? C21 O6 Mn1 120.0(4) . . ? C21 O6 Mn2 127.4(5) . 3_765 ? Mn1 O6 Mn2 103.09(18) . 3_765 ? C45 O7 Mn2 120.1(4) . . ? C45 O7 Mn3 131.6(4) . . ? Mn2 O7 Mn3 104.80(18) . . ? C47 O8 Mn3 132.7(4) . . ? C5 N1 C1 119.4(7) . . ? C5 N1 Mn3 115.9(5) . 3_765 ? C1 N1 Mn3 124.6(5) . 3_765 ? C14 N3 C18 118.5(7) . . ? C14 N3 Mn2 127.1(5) . . ? C18 N3 Mn2 114.2(5) . . ? C26 N4 C22 117.5(6) . . ? C26 N4 Mn3 118.6(5) . 3_765 ? C22 N4 Mn3 123.8(4) . 3_765 ? C27 N5 C31 118.8(8) . . ? C27 N5 Mn1 126.3(7) . . ? C31 N5 Mn1 114.6(5) . . ? C35 N6 C39 115.8(7) . . ? C35 N6 Mn3 125.4(5) . . ? C39 N6 Mn3 118.8(5) . . ? C44 N7 C40 117.1(6) . . ? C44 N7 Mn2 115.2(5) . . ? C40 N7 Mn2 125.3(5) . . ? C48 N8 C52 115.3(7) . . ? N1 C1 C2 120.9(8) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 118.5(8) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.2(8) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.0(9) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 123.7(9) . . ? N1 C5 C6 114.7(6) . . ? C4 C5 C6 121.6(8) . . ? O1 C6 C7 122.3(8) . . ? O1 C6 C5 114.9(7) . . ? C7 C6 C5 122.8(7) . . ? C8 C7 C6 126.3(10) . . ? C8 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? O2 C8 C7 127.2(9) . . ? O2 C8 C9 116.2(11) . . ? C7 C8 C9 116.3(11) . . ? C10 C9 N2 120.0 . . ? C10 C9 C8 121.4(12) . . ? N2 C9 C8 118.0(12) . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? N3 C14 C15 123.8(8) . . ? N3 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C14 C15 C16 116.6(9) . . ? C14 C15 H15 121.7 . . ? C16 C15 H15 121.7 . . ? C17 C16 C15 120.1(10) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.9(10) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? N3 C18 C17 120.8(8) . . ? N3 C18 C19 115.8(7) . . ? C17 C18 C19 123.1(8) . . ? O3 C19 C20 122.9(6) . . ? O3 C19 C18 114.5(6) . . ? C20 C19 C18 122.5(7) . . ? C19 C20 C21 122.7(6) . . ? C19 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? O6 C21 C20 123.1(6) . . ? O6 C21 C22 116.1(6) . . ? C20 C21 C22 120.6(6) . . ? C23 C22 N4 121.5(7) . . ? C23 C22 C21 124.3(7) . . ? N4 C22 C21 114.2(6) . . ? C22 C23 C24 120.5(8) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 117.4(7) . . ? C25 C24 H24 121.3 . . ? C23 C24 H24 121.3 . . ? C24 C25 C26 119.7(7) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N4 C26 C25 123.2(7) . . ? N4 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C28 C27 N5 123.9(11) . . ? C28 C27 H27 118.0 . . ? N5 C27 H27 118.0 . . ? C27 C28 C29 118.7(11) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C28 C29 C30 120.3(12) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 118.7(11) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? N5 C31 C30 119.3(8) . . ? N5 C31 C32 115.5(7) . . ? C30 C31 C32 125.2(8) . . ? O4 C32 C33 122.7(6) . . ? O4 C32 C31 115.8(6) . . ? C33 C32 C31 121.5(6) . . ? C34 C33 C32 122.0(6) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? O5 C34 C33 123.7(6) . . ? O5 C34 C35 115.8(6) . . ? C33 C34 C35 120.5(6) . . ? N6 C35 C36 126.9(7) . . ? N6 C35 C34 113.9(7) . . ? C36 C35 C34 119.2(8) . . ? C35 C36 C37 113.4(10) . . ? C35 C36 H36 123.3 . . ? C37 C36 H36 123.3 . . ? C38 C37 C36 120.4(11) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 119.5(10) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 N6 123.7(9) . . ? C38 C39 H39 118.2 . . ? N6 C39 H39 118.2 . . ? N7 C40 C41 122.0(7) . . ? N7 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C42 C41 C40 119.6(7) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 118.7(8) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 119.2(7) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? N7 C44 C43 123.2(7) . . ? N7 C44 C45 112.3(6) . . ? C43 C44 C45 124.4(7) . . ? O7 C45 C46 125.3(6) . . ? O7 C45 C44 116.6(6) . . ? C46 C45 C44 118.0(6) . . ? C47 C46 C45 121.7(6) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? O8 C47 C46 126.8(6) . . ? O8 C47 C48 117.0(6) . . ? C46 C47 C48 116.0(6) . . ? N8 C48 C49 124.1(7) . . ? N8 C48 C47 116.3(6) . . ? C49 C48 C47 119.5(7) . . ? C48 C49 C50 118.2(9) . . ? C48 C49 H49 120.9 . . ? C50 C49 H49 120.9 . . ? C51 C50 C49 118.7(9) . . ? C51 C50 H50 120.6 . . ? C49 C50 H50 120.6 . . ? C50 C51 C52 117.8(9) . . ? C50 C51 H51 121.1 . . ? C52 C51 H51 121.1 . . ? N8 C52 C51 125.3(9) . . ? N8 C52 H52 117.3 . . ? C51 C52 H52 117.3 . . ? F4S B1S F3S 107.8(11) . . ? F4S B1S F2S 108.2(12) . . ? F3S B1S F2S 108.7(11) . . ? F4S B1S F1S 108.6(9) . . ? F3S B1S F1S 108.5(10) . . ? F2S B1S F1S 114.8(10) . . ? F7S B5 F8S 104.7(16) . . ? F7S B5 F6S 112.8(19) . . ? F8S B5 F6S 116.1(16) . . ? F7S B5 F5S 95.4(15) . . ? F8S B5 F5S 121.7(19) . . ? F6S B5 F5S 104.5(15) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N2 C13 C12 120.0 . . ? N2 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 N2 C9 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.931 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.144 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.003 0.274 3895 265 ' ' _platon_squeeze_details ; ; # Attachment '- 3 MN7(BF4)final3.CIF' #========================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 768053' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C90 H75 Mn7 N7 O18, 2(C H4 O), 2(B F4), 2(C H2 Cl2) ; _chemical_formula_sum 'C94 H87 B2 F8 Mn7 N7 O20 Cl4' _chemical_formula_weight 2334.74 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' B B 0.0013 0.0007 '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' _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 13.7852(10) _cell_length_b 14.7338(10) _cell_length_c 15.1269(11) _cell_angle_alpha 64.941(3) _cell_angle_beta 88.285(4) _cell_angle_gamma 89.973(3) _cell_volume 2781.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 30.38 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 59886 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.67 _reflns_number_total 16754 _reflns_number_gt 13180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains half the cluster as well as one tetrafluoro- borate one MeOH solvent molecule, which was disordered over three positions and a disordered DCM molecule. The DCM molecule could not be satisfactorily modelled thus the squeeze program was employed to remove the electron denisty. Bond length (DFIX) and thermal restraints (ISOR) were placed on the disordered MeOH molecule (O1s, C2s, O2S, C3S, O4S and C4S). The central manganese ion, tea and three hydroxides are disordered over two sites each at 50% occupancy. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _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^)+(0.0870P)^2^+2.8261P] 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 16754 _refine_ls_number_parameters 714 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _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 0.54931(5) 0.01120(5) 0.49211(5) 0.01695(13) Uani 0.50 1 d P . . Mn2 Mn 0.51098(3) 0.05592(3) 0.69072(3) 0.02354(9) Uani 1 1 d . . . Mn3 Mn 0.45585(3) 0.23212(3) 0.47211(3) 0.02253(9) Uani 1 1 d . . . Mn4 Mn 0.48222(3) 0.18214(3) 0.27764(3) 0.02366(9) Uani 1 1 d . . . F1S F 0.84852(13) -0.35864(14) 1.25392(14) 0.0444(4) Uani 1 1 d . . . F2S F 0.89476(19) -0.44118(16) 1.16319(18) 0.0641(6) Uani 1 1 d . . . F3S F 0.88701(14) -0.27211(14) 1.09314(14) 0.0467(5) Uani 1 1 d . . . F4S F 0.74948(15) -0.3658(2) 1.14031(17) 0.0740(8) Uani 1 1 d . . . O1 O 0.6148(3) -0.1353(3) 0.5860(3) 0.0208(7) Uani 0.50 1 d P . 1 O1S O 0.9613(4) -0.1044(5) 0.9371(6) 0.068(2) Uani 0.40 1 d PD A 5 H1S H 0.9519 -0.1638 0.9784 0.082 Uiso 0.40 1 calc PR A 5 O2 O 0.5813(3) 0.0584(3) 0.3334(3) 0.0206(6) Uani 0.50 1 d P . 1 O2S O 0.9793(6) -0.0838(8) 0.8088(8) 0.102(3) Uani 0.40 1 d PDU B 4 H2S H 1.0017 -0.0785 0.7554 0.122 Uiso 0.40 1 d P C 4 O3 O 0.5787(3) 0.1304(3) 0.5427(2) 0.0205(6) Uani 0.50 1 d P . 1 O4 O 0.5665(3) -0.1207(2) 0.5774(2) 0.0156(6) Uani 0.50 1 d P . 2 O4S O 0.9725(8) -0.1947(10) 0.7046(10) 0.055(3) Uani 0.20 1 d PD D 6 H4S H 0.9806 -0.1841 0.6463 0.066 Uiso 0.20 1 d P E 6 O5 O 0.5390(2) 0.0373(2) 0.3695(2) 0.0144(6) Uani 0.50 1 d P . 2 O6 O 0.5355(2) 0.0984(2) 0.5413(2) 0.0141(6) Uani 0.50 1 d P . 2 O7 O 0.58243(12) -0.08114(13) 0.77665(13) 0.0250(3) Uani 1 1 d . . . O8 O 0.62716(14) 0.11297(14) 0.74001(16) 0.0359(4) Uani 1 1 d . . . O9 O 0.41600(12) 0.18370(13) 0.62257(13) 0.0246(3) Uani 1 1 d . . . O10 O 0.32187(14) 0.30727(14) 0.45699(14) 0.0328(4) Uani 1 1 d . . . O11 O 0.52135(13) 0.29263(14) 0.32713(14) 0.0300(4) Uani 1 1 d . . . O12 O 0.59024(15) 0.26043(19) 0.16966(16) 0.0430(5) Uani 1 1 d . . . N1 N 0.7208(3) 0.0398(3) 0.4710(3) 0.0206(7) Uani 0.50 1 d P . 1 N2 N 0.40012(16) 0.05247(17) 0.80393(16) 0.0306(5) Uani 1 1 d . . . N3 N 0.55692(16) 0.35756(18) 0.45850(17) 0.0312(5) Uani 1 1 d . . . N4 N 0.64592(16) -0.25830(16) 0.80778(17) 0.0307(5) Uani 1 1 d . . . C1 C 0.7670(3) -0.0586(3) 0.5037(3) 0.0196(8) Uani 0.50 1 d P . 1 H1A H 0.8364 -0.0523 0.5156 0.024 Uiso 0.50 1 calc PR . 1 H1B H 0.7632 -0.0829 0.4521 0.024 Uiso 0.50 1 calc PR . 1 C2 C 0.7173(3) -0.1332(3) 0.5961(3) 0.0207(8) Uani 0.50 1 d P . 1 H2A H 0.7437 -0.2007 0.6123 0.025 Uiso 0.50 1 calc PR . 1 H2B H 0.7312 -0.1151 0.6506 0.025 Uiso 0.50 1 calc PR . 1 C2S C 1.0603(5) -0.0799(6) 0.9320(6) 0.0453(19) Uani 0.40 1 d PD A 5 H2S1 H 1.0662 -0.0143 0.9326 0.068 Uiso 0.40 1 d P F 5 H2S2 H 1.0896 -0.0784 0.8745 0.068 Uiso 0.40 1 d P G 5 H2S3 H 1.0914 -0.1279 0.9888 0.068 Uiso 0.40 1 d P H 5 C3 C 0.7421(3) 0.1028(4) 0.3658(3) 0.0228(9) Uani 0.50 1 d P . 1 H3A H 0.8122 0.1001 0.3511 0.027 Uiso 0.50 1 calc PR . 1 H3B H 0.7258 0.1734 0.3500 0.027 Uiso 0.50 1 calc PR . 1 C3S C 1.0665(11) -0.0885(13) 0.8614(15) 0.113(5) Uani 0.40 1 d PDU B 4 H3S1 H 1.0820 -0.0208 0.8611 0.169 Uiso 0.40 1 d P I 4 H3S2 H 1.1175 -0.1225 0.8626 0.169 Uiso 0.40 1 d P J 4 H3S3 H 1.0398 -0.1224 0.9404 0.169 Uiso 0.40 1 d P K 4 C4 C 0.6835(3) 0.0662(4) 0.3036(3) 0.0220(9) Uani 0.50 1 d P . 1 H4A H 0.6918 0.1136 0.2340 0.026 Uiso 0.50 1 calc PR . 1 H4B H 0.7072 -0.0001 0.3112 0.026 Uiso 0.50 1 calc PR . 1 C4S C 0.9642(16) -0.0995(13) 0.7118(16) 0.067(5) Uani 0.20 1 d PDU D 6 H4S1 H 1.0157 -0.0568 0.6571 0.100 Uiso 0.20 1 d P L 6 H4S2 H 0.9850 -0.1086 0.7682 0.100 Uiso 0.20 1 d P M 6 H4S3 H 0.9056 -0.0754 0.6890 0.100 Uiso 0.20 1 d P N 6 C5 C 0.7485(3) 0.0920(3) 0.5308(3) 0.0208(8) Uani 0.50 1 d P . 1 H5A H 0.8137 0.1232 0.5090 0.025 Uiso 0.50 1 calc PR . 1 H5B H 0.7518 0.0431 0.6000 0.025 Uiso 0.50 1 calc PR . 1 C6 C 0.6761(3) 0.1715(3) 0.5222(4) 0.0209(8) Uani 0.50 1 d P . 1 H6A H 0.6915 0.2003 0.5687 0.025 Uiso 0.50 1 calc PR . 1 H6B H 0.6805 0.2261 0.4554 0.025 Uiso 0.50 1 calc PR . 1 C7 C 0.6685(2) -0.3543(2) 0.8316(2) 0.0405(7) Uani 1 1 d . . . H7 H 0.6302 -0.3921 0.8077 0.049 Uiso 1 1 calc R . . C8 C 0.7460(3) -0.4004(2) 0.8901(3) 0.0479(8) Uani 1 1 d . . . H8 H 0.7606 -0.4684 0.9057 0.057 Uiso 1 1 calc R . . C9 C 0.8007(3) -0.3463(3) 0.9247(3) 0.0526(9) Uani 1 1 d . . . H9 H 0.8529 -0.3768 0.9662 0.063 Uiso 1 1 calc R . . C10 C 0.7795(2) -0.2452(2) 0.8987(3) 0.0474(8) Uani 1 1 d . . . H10 H 0.8176 -0.2059 0.9211 0.057 Uiso 1 1 calc R . . C11 C 0.70142(19) -0.2040(2) 0.8394(2) 0.0326(6) Uani 1 1 d . . . C12 C 0.67031(18) -0.09722(19) 0.80639(19) 0.0277(5) Uani 1 1 d . . . C13 C 0.73278(19) -0.0246(2) 0.8065(2) 0.0343(6) Uani 1 1 d . . . H13 H 0.7952 -0.0446 0.8324 0.041 Uiso 1 1 calc R . . C14 C 0.70932(19) 0.0790(2) 0.7700(2) 0.0309(5) Uani 1 1 d . . . C15 C 0.78527(19) 0.1543(2) 0.7645(2) 0.0309(5) Uani 1 1 d . . . C16 C 0.8758(2) 0.1266(2) 0.8039(3) 0.0441(7) Uani 1 1 d . . . H16 H 0.8912 0.0578 0.8382 0.053 Uiso 1 1 calc R . . C17 C 0.9443(2) 0.2013(3) 0.7925(3) 0.0503(9) Uani 1 1 d . . . H17 H 1.0064 0.1827 0.8196 0.060 Uiso 1 1 calc R . . C18 C 0.9230(2) 0.3014(2) 0.7425(2) 0.0397(7) Uani 1 1 d . . . H18 H 0.9705 0.3514 0.7340 0.048 Uiso 1 1 calc R . . C19 C 0.8320(3) 0.3281(2) 0.7049(3) 0.0458(8) Uani 1 1 d . . . H19 H 0.8164 0.3969 0.6711 0.055 Uiso 1 1 calc R . . C20 C 0.7636(2) 0.2554(2) 0.7162(3) 0.0407(7) Uani 1 1 d . . . H20 H 0.7009 0.2746 0.6907 0.049 Uiso 1 1 calc R . . C21 C 0.4023(2) -0.0088(3) 0.8990(2) 0.0464(8) Uani 1 1 d . . . H21 H 0.4510 -0.0585 0.9206 0.056 Uiso 1 1 calc R . . C22 C 0.3366(3) -0.0029(3) 0.9670(3) 0.0647(12) Uani 1 1 d . . . H22 H 0.3404 -0.0470 1.0342 0.078 Uiso 1 1 calc R . . C23 C 0.2655(3) 0.0685(4) 0.9351(3) 0.0686(14) Uani 1 1 d . . . H23 H 0.2193 0.0740 0.9804 0.082 Uiso 1 1 calc R . . C24 C 0.2616(3) 0.1322(3) 0.8367(2) 0.0518(9) Uani 1 1 d . . . H24 H 0.2132 0.1821 0.8136 0.062 Uiso 1 1 calc R . . C25 C 0.3300(2) 0.1213(2) 0.7729(2) 0.0330(6) Uani 1 1 d . . . C26 C 0.33354(18) 0.18470(18) 0.66470(19) 0.0259(5) Uani 1 1 d . . . C27 C 0.25297(19) 0.2355(2) 0.6175(2) 0.0335(6) Uani 1 1 d . . . H27 H 0.1960 0.2319 0.6558 0.040 Uiso 1 1 calc R . . C28 C 0.24988(19) 0.29326(19) 0.5141(2) 0.0302(5) Uani 1 1 d . . . C29 C 0.1570(2) 0.3400(2) 0.4702(2) 0.0341(6) Uani 1 1 d . . . C30 C 0.0786(3) 0.3468(4) 0.5241(3) 0.0681(13) Uani 1 1 d . . . H30 H 0.0821 0.3217 0.5930 0.082 Uiso 1 1 calc R . . C31 C -0.0067(3) 0.3903(5) 0.4787(3) 0.0897(19) Uani 1 1 d . . . H31 H -0.0604 0.3960 0.5168 0.108 Uiso 1 1 calc R . . C32 C -0.0138(3) 0.4253(3) 0.3789(3) 0.0582(10) Uani 1 1 d . . . H32 H -0.0733 0.4507 0.3485 0.070 Uiso 1 1 calc R . . C33 C 0.0647(3) 0.4228(3) 0.3257(3) 0.0499(8) Uani 1 1 d . . . H33 H 0.0616 0.4498 0.2567 0.060 Uiso 1 1 calc R . . C34 C 0.1502(2) 0.3812(3) 0.3703(2) 0.0455(8) Uani 1 1 d . . . H34 H 0.2053 0.3810 0.3311 0.055 Uiso 1 1 calc R . . C35 C 0.5690(2) 0.3908(2) 0.5273(2) 0.0329(6) Uani 1 1 d . . . H35 H 0.5298 0.3627 0.5856 0.039 Uiso 1 1 calc R . . C36 C 0.6365(2) 0.4647(2) 0.5169(2) 0.0385(6) Uani 1 1 d . . . H36 H 0.6440 0.4865 0.5672 0.046 Uiso 1 1 calc R . . C37 C 0.6924(3) 0.5056(3) 0.4320(3) 0.0468(8) Uani 1 1 d . . . H37 H 0.7390 0.5567 0.4225 0.056 Uiso 1 1 calc R . . C38 C 0.6801(3) 0.4720(3) 0.3610(3) 0.0483(8) Uani 1 1 d . . . H38 H 0.7181 0.4997 0.3019 0.058 Uiso 1 1 calc R . . C39 C 0.6121(2) 0.3976(2) 0.3765(2) 0.0370(6) Uani 1 1 d . . . C40 C 0.5964(2) 0.3519(2) 0.3062(2) 0.0358(6) Uani 1 1 d . . . C41 C 0.6612(2) 0.3694(3) 0.2290(2) 0.0432(8) Uani 1 1 d . . . H41 H 0.7110 0.4182 0.2166 0.052 Uiso 1 1 calc R . . C42 C 0.6579(2) 0.3189(3) 0.1670(2) 0.0384(7) Uani 1 1 d . . . C43 C 0.7385(2) 0.3343(2) 0.0944(2) 0.0367(6) Uani 1 1 d . . . C44 C 0.8277(2) 0.3768(2) 0.0976(3) 0.0430(7) Uani 1 1 d . . . H44 H 0.8387 0.4003 0.1461 0.052 Uiso 1 1 calc R . . C45 C 0.9004(2) 0.3846(3) 0.0294(3) 0.0501(9) Uani 1 1 d . . . H45 H 0.9616 0.4127 0.0323 0.060 Uiso 1 1 calc R . . C46 C 0.8855(3) 0.3521(3) -0.0432(3) 0.0536(9) Uani 1 1 d . . . H46 H 0.9359 0.3583 -0.0897 0.064 Uiso 1 1 calc R . . C47 C 0.7970(3) 0.3109(3) -0.0467(3) 0.0542(9) Uani 1 1 d . . . H47 H 0.7856 0.2898 -0.0968 0.065 Uiso 1 1 calc R . . C48 C 0.7246(2) 0.3002(3) 0.0224(2) 0.0444(7) Uani 1 1 d . . . H48 H 0.6646 0.2693 0.0209 0.053 Uiso 1 1 calc R . . B1S B 0.8442(2) -0.3595(3) 1.1624(3) 0.0398(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0162(3) 0.0163(3) 0.0171(3) -0.0060(2) -0.0005(2) -0.0009(2) Mn2 0.02477(18) 0.02588(18) 0.02110(18) -0.01081(14) -0.00451(13) 0.00601(13) Mn3 0.02635(18) 0.01874(16) 0.02116(18) -0.00724(13) 0.00046(13) 0.00071(13) Mn4 0.02671(19) 0.02233(17) 0.02069(18) -0.00761(14) -0.00513(14) 0.00186(13) F1S 0.0345(9) 0.0491(10) 0.0412(10) -0.0111(8) -0.0009(7) -0.0014(8) F2S 0.0902(17) 0.0431(11) 0.0603(14) -0.0218(10) -0.0237(12) 0.0125(11) F3S 0.0418(10) 0.0438(10) 0.0430(10) -0.0074(8) 0.0017(8) -0.0112(8) F4S 0.0332(10) 0.1041(19) 0.0497(12) 0.0018(12) -0.0106(9) -0.0222(11) O1 0.0248(19) 0.0165(15) 0.0185(16) -0.0051(12) 0.0014(15) -0.0044(14) O1S 0.042(3) 0.035(3) 0.087(5) 0.014(3) -0.014(3) -0.009(3) O2 0.0191(17) 0.0201(16) 0.0228(18) -0.0090(14) -0.0071(14) 0.0026(13) O2S 0.061(5) 0.095(6) 0.127(7) -0.025(5) -0.003(5) 0.007(4) O3 0.0209(17) 0.0200(16) 0.0176(16) -0.0052(13) 0.0007(13) 0.0040(13) O4 0.0139(15) 0.0165(14) 0.0153(15) -0.0056(11) -0.0019(13) 0.0007(12) O4S 0.032(6) 0.081(9) 0.050(7) -0.028(7) -0.003(5) 0.007(6) O5 0.0111(14) 0.0169(14) 0.0129(14) -0.0042(11) 0.0020(11) -0.0046(11) O6 0.0131(14) 0.0134(13) 0.0159(14) -0.0064(11) 0.0001(11) -0.0033(11) O7 0.0216(8) 0.0246(8) 0.0261(9) -0.0076(7) -0.0055(6) 0.0004(6) O8 0.0252(9) 0.0282(9) 0.0508(12) -0.0132(9) -0.0058(8) -0.0010(7) O9 0.0227(8) 0.0257(8) 0.0232(8) -0.0082(7) -0.0006(6) 0.0038(6) O10 0.0281(9) 0.0319(9) 0.0290(10) -0.0038(8) -0.0005(7) 0.0042(7) O11 0.0279(9) 0.0362(10) 0.0275(9) -0.0156(8) 0.0041(7) -0.0102(7) O12 0.0302(10) 0.0718(16) 0.0366(11) -0.0329(11) 0.0069(9) -0.0130(10) N1 0.0184(17) 0.0174(16) 0.0234(19) -0.0062(14) -0.0014(14) -0.0009(13) N2 0.0275(10) 0.0311(11) 0.0251(11) -0.0043(9) 0.0010(8) 0.0047(8) N3 0.0283(11) 0.0365(12) 0.0319(12) -0.0176(10) 0.0019(9) -0.0058(9) N4 0.0288(11) 0.0231(10) 0.0330(12) -0.0046(9) -0.0055(9) 0.0010(8) C1 0.0190(19) 0.0184(18) 0.021(2) -0.0076(16) -0.0021(16) 0.0029(15) C2 0.020(2) 0.0190(19) 0.021(2) -0.0062(16) -0.0015(16) -0.0028(15) C2S 0.043(4) 0.041(4) 0.039(4) -0.004(3) 0.000(3) 0.003(3) C3 0.021(2) 0.024(2) 0.020(2) -0.0055(17) -0.0013(16) 0.0022(16) C3S 0.082(7) 0.087(8) 0.142(10) -0.021(7) -0.031(7) 0.011(6) C4 0.019(2) 0.026(2) 0.019(2) -0.0075(17) -0.0003(16) 0.0008(16) C4S 0.056(8) 0.098(10) 0.052(8) -0.036(7) -0.014(7) 0.020(7) C5 0.0179(19) 0.025(2) 0.021(2) -0.0105(17) -0.0011(16) -0.0002(16) C6 0.021(2) 0.0183(18) 0.025(2) -0.0104(17) -0.0006(17) -0.0034(15) C7 0.0429(16) 0.0266(13) 0.0458(17) -0.0087(12) -0.0116(13) 0.0038(11) C8 0.0521(19) 0.0290(14) 0.055(2) -0.0100(14) -0.0168(16) 0.0145(13) C9 0.0453(18) 0.0386(16) 0.065(2) -0.0119(16) -0.0252(17) 0.0148(14) C10 0.0395(16) 0.0355(15) 0.063(2) -0.0147(15) -0.0261(15) 0.0076(12) C11 0.0273(12) 0.0258(12) 0.0383(15) -0.0069(11) -0.0089(11) 0.0022(9) C12 0.0246(11) 0.0265(11) 0.0265(12) -0.0057(9) -0.0048(9) 0.0019(9) C13 0.0241(12) 0.0297(13) 0.0440(16) -0.0101(11) -0.0098(11) 0.0014(10) C14 0.0256(12) 0.0318(13) 0.0336(14) -0.0123(11) -0.0021(10) -0.0032(10) C15 0.0258(12) 0.0349(13) 0.0314(13) -0.0136(11) 0.0012(10) -0.0080(10) C16 0.0314(14) 0.0388(15) 0.062(2) -0.0207(15) -0.0104(14) -0.0011(12) C17 0.0272(14) 0.0511(19) 0.076(3) -0.0298(18) -0.0089(15) -0.0054(13) C18 0.0340(14) 0.0453(16) 0.0436(17) -0.0229(14) 0.0071(12) -0.0151(12) C19 0.0464(18) 0.0351(15) 0.0523(19) -0.0148(14) -0.0040(15) -0.0092(13) C20 0.0327(14) 0.0340(14) 0.0522(18) -0.0147(13) -0.0071(13) -0.0049(11) C21 0.0417(16) 0.0509(18) 0.0292(15) -0.0004(13) 0.0033(12) 0.0153(14) C22 0.064(2) 0.076(3) 0.0282(16) 0.0020(16) 0.0107(15) 0.030(2) C23 0.061(2) 0.087(3) 0.0320(17) -0.0013(18) 0.0163(16) 0.036(2) C24 0.0440(17) 0.061(2) 0.0326(16) -0.0029(15) 0.0107(13) 0.0214(15) C25 0.0273(12) 0.0353(13) 0.0281(13) -0.0056(11) 0.0025(10) 0.0056(10) C26 0.0230(11) 0.0264(11) 0.0258(12) -0.0088(9) 0.0010(9) 0.0013(9) C27 0.0235(12) 0.0354(13) 0.0320(14) -0.0052(11) 0.0020(10) 0.0063(10) C28 0.0264(12) 0.0251(11) 0.0343(14) -0.0077(10) -0.0033(10) 0.0022(9) C29 0.0276(13) 0.0336(13) 0.0368(15) -0.0105(11) -0.0058(11) 0.0068(10) C30 0.0411(19) 0.115(4) 0.0386(19) -0.023(2) -0.0095(15) 0.038(2) C31 0.047(2) 0.152(5) 0.047(2) -0.020(3) -0.0060(18) 0.055(3) C32 0.0354(17) 0.076(3) 0.051(2) -0.0134(19) -0.0127(15) 0.0218(17) C33 0.0456(18) 0.0480(18) 0.0395(17) -0.0015(14) -0.0147(14) 0.0119(14) C34 0.0350(15) 0.0478(18) 0.0356(16) 0.0002(13) -0.0043(12) 0.0083(13) C35 0.0336(13) 0.0341(13) 0.0355(14) -0.0191(11) 0.0000(11) -0.0004(11) C36 0.0424(16) 0.0374(15) 0.0429(16) -0.0236(13) -0.0032(13) -0.0029(12) C37 0.0502(19) 0.0456(17) 0.0491(19) -0.0250(15) 0.0045(15) -0.0220(15) C38 0.0496(19) 0.056(2) 0.0421(18) -0.0246(15) 0.0089(14) -0.0276(16) C39 0.0333(14) 0.0457(16) 0.0339(15) -0.0192(13) 0.0060(11) -0.0125(12) C40 0.0278(13) 0.0499(17) 0.0314(14) -0.0193(13) 0.0057(11) -0.0125(12) C41 0.0321(14) 0.067(2) 0.0362(16) -0.0285(15) 0.0086(12) -0.0219(14) C42 0.0248(13) 0.0594(19) 0.0321(14) -0.0205(14) 0.0022(11) -0.0087(12) C43 0.0289(13) 0.0448(16) 0.0311(14) -0.0112(12) 0.0015(11) 0.0011(11) C44 0.0297(14) 0.0446(17) 0.0475(18) -0.0129(14) 0.0064(13) -0.0015(12) C45 0.0262(14) 0.0431(17) 0.066(2) -0.0094(16) 0.0141(14) -0.0016(12) C46 0.0453(18) 0.0501(19) 0.055(2) -0.0137(17) 0.0252(16) 0.0053(15) C47 0.052(2) 0.066(2) 0.0419(19) -0.0211(17) 0.0126(16) 0.0066(17) C48 0.0338(15) 0.062(2) 0.0367(16) -0.0204(15) 0.0026(12) 0.0020(14) B1S 0.0286(15) 0.0406(17) 0.0400(18) -0.0068(14) -0.0058(13) -0.0068(13) _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 Mn1 1.3886(13) 2_656 ? Mn1 O5 1.738(3) . ? Mn1 O6 1.744(3) . ? Mn1 O4 1.841(3) . ? Mn1 O4 2.217(4) 2_656 ? Mn1 O5 2.226(4) 2_656 ? Mn1 O6 2.227(3) 2_656 ? Mn1 O2 2.228(4) . ? Mn1 O1 2.230(4) . ? Mn1 O3 2.233(4) . ? Mn1 N1 2.390(4) . ? Mn2 O5 2.071(3) 2_656 ? Mn2 O6 2.090(3) . ? Mn2 O8 2.105(2) . ? Mn2 O7 2.1422(17) . ? Mn2 O9 2.1808(17) . ? Mn2 O3 2.210(3) . ? Mn2 N2 2.245(2) . ? Mn2 O2 2.266(3) 2_656 ? Mn3 O4 2.099(3) 2_656 ? Mn3 O10 2.1209(19) . ? Mn3 O6 2.122(3) . ? Mn3 O9 2.1309(18) . ? Mn3 O11 2.1554(19) . ? Mn3 O1 2.206(4) 2_656 ? Mn3 O3 2.237(3) . ? Mn3 N3 2.250(2) . ? Mn4 O4 2.076(3) 2_656 ? Mn4 O12 2.116(2) . ? Mn4 O11 2.1351(19) . ? Mn4 O5 2.156(3) . ? Mn4 O2 2.160(3) . ? Mn4 O7 2.1827(18) 2_656 ? Mn4 N4 2.226(2) 2_656 ? Mn4 O1 2.269(4) 2_656 ? F1S B1S 1.392(4) . ? F2S B1S 1.387(5) . ? F3S B1S 1.387(4) . ? F4S B1S 1.370(4) . ? O1 C2 1.429(6) . ? O1 Mn3 2.206(4) 2_656 ? O1 Mn4 2.269(4) 2_656 ? O1S C2S 1.402(7) . ? O1S H1S 0.8400 . ? O1S H3S3 1.1109 . ? O2 C4 1.457(6) . ? O2 Mn2 2.266(3) 2_656 ? O2S C3S 1.446(9) . ? O2S H2S 0.8277 . ? O2S H4S2 0.8392 . ? O3 C6 1.444(6) . ? O4 Mn4 2.076(3) 2_656 ? O4 Mn3 2.099(3) 2_656 ? O4 Mn1 2.217(4) 2_656 ? O4S C4S 1.456(10) . ? O4S H4S 0.8331 . ? O5 Mn2 2.071(3) 2_656 ? O5 Mn1 2.226(4) 2_656 ? O6 Mn1 2.227(3) 2_656 ? O7 C12 1.292(3) . ? O7 Mn4 2.1827(18) 2_656 ? O8 C14 1.256(3) . ? O9 C26 1.290(3) . ? O10 C28 1.253(3) . ? O11 C40 1.296(3) . ? O12 C42 1.258(4) . ? N1 C1 1.472(6) . ? N1 C5 1.472(6) . ? N1 C3 1.484(6) . ? N2 C21 1.336(4) . ? N2 C25 1.344(3) . ? N3 C39 1.338(4) . ? N3 C35 1.340(4) . ? N4 C11 1.341(4) . ? N4 C7 1.343(4) . ? N4 Mn4 2.226(2) 2_656 ? C1 C2 1.507(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2S H2S1 0.9738 . ? C2S H2S2 0.9411 . ? C2S H2S3 0.9642 . ? C2S H3S1 1.0901 . ? C2S H3S3 0.6474 . ? C3 C4 1.517(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3S H2S2 0.4379 . ? C3S H3S1 1.0193 . ? C3S H3S2 0.8590 . ? C3S H3S3 1.1321 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4S H2S 0.9965 . ? C4S H4S1 1.0527 . ? C4S H4S2 0.8642 . ? C4S H4S3 0.9002 . ? C5 C6 1.504(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.390(4) . ? C7 H7 0.9500 . ? C8 C9 1.362(5) . ? C8 H8 0.9500 . ? C9 C10 1.403(5) . ? C9 H9 0.9500 . ? C10 C11 1.388(4) . ? C10 H10 0.9500 . ? C11 C12 1.502(4) . ? C12 C13 1.374(4) . ? C13 C14 1.427(4) . ? C13 H13 0.9500 . ? C14 C15 1.501(4) . ? C15 C16 1.384(4) . ? C15 C20 1.390(4) . ? C16 C17 1.402(4) . ? C16 H16 0.9500 . ? C17 C18 1.378(5) . ? C17 H17 0.9500 . ? C18 C19 1.380(5) . ? C18 H18 0.9500 . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.381(5) . ? C21 H21 0.9500 . ? C22 C23 1.377(5) . ? C22 H22 0.9500 . ? C23 C24 1.386(5) . ? C23 H23 0.9500 . ? C24 C25 1.387(4) . ? C24 H24 0.9500 . ? C25 C26 1.501(4) . ? C26 C27 1.377(3) . ? C27 C28 1.432(4) . ? C27 H27 0.9500 . ? C28 C29 1.488(4) . ? C29 C30 1.364(5) . ? C29 C34 1.376(4) . ? C30 C31 1.392(5) . ? C30 H30 0.9500 . ? C31 C32 1.380(6) . ? C31 H31 0.9500 . ? C32 C33 1.338(5) . ? C32 H32 0.9500 . ? C33 C34 1.385(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.386(4) . ? C35 H35 0.9500 . ? C36 C37 1.376(5) . ? C36 H36 0.9500 . ? C37 C38 1.374(5) . ? C37 H37 0.9500 . ? C38 C39 1.381(4) . ? C38 H38 0.9500 . ? C39 C40 1.501(4) . ? C40 C41 1.381(4) . ? C41 C42 1.425(5) . ? C41 H41 0.9500 . ? C42 C43 1.486(4) . ? C43 C44 1.392(4) . ? C43 C48 1.396(5) . ? C44 C45 1.385(5) . ? C44 H44 0.9500 . ? C45 C46 1.391(6) . ? C45 H45 0.9500 . ? C46 C47 1.376(6) . ? C46 H46 0.9500 . ? C47 C48 1.383(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? 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 Mn1 Mn1 O5 90.11(13) 2_656 . ? Mn1 Mn1 O6 89.87(13) 2_656 . ? O5 Mn1 O6 125.05(15) . . ? Mn1 Mn1 O4 85.48(13) 2_656 . ? O5 Mn1 O4 117.05(15) . . ? O6 Mn1 O4 117.71(15) . . ? Mn1 Mn1 O4 55.88(10) 2_656 2_656 ? O5 Mn1 O4 67.88(14) . 2_656 ? O6 Mn1 O4 67.20(14) . 2_656 ? O4 Mn1 O4 141.36(8) . 2_656 ? Mn1 Mn1 O5 51.31(9) 2_656 2_656 ? O5 Mn1 O5 141.41(8) . 2_656 ? O6 Mn1 O5 63.28(13) . 2_656 ? O4 Mn1 O5 66.16(14) . 2_656 ? O4 Mn1 O5 86.80(12) 2_656 2_656 ? Mn1 Mn1 O6 51.55(9) 2_656 2_656 ? O5 Mn1 O6 63.35(13) . 2_656 ? O6 Mn1 O6 141.43(8) . 2_656 ? O4 Mn1 O6 65.58(13) . 2_656 ? O4 Mn1 O6 87.36(12) 2_656 2_656 ? O5 Mn1 O6 87.84(12) 2_656 2_656 ? Mn1 Mn1 O2 106.81(11) 2_656 . ? O5 Mn1 O2 16.80(12) . . ? O6 Mn1 O2 121.69(14) . . ? O4 Mn1 O2 118.98(14) . . ? O4 Mn1 O2 77.22(12) 2_656 . ? O5 Mn1 O2 158.06(12) 2_656 . ? O6 Mn1 O2 76.63(12) 2_656 . ? Mn1 Mn1 O1 101.97(12) 2_656 . ? O5 Mn1 O1 116.36(14) . . ? O6 Mn1 O1 117.31(14) . . ? O4 Mn1 O1 16.49(12) . . ? O4 Mn1 O1 157.85(13) 2_656 . ? O5 Mn1 O1 77.45(13) 2_656 . ? O6 Mn1 O1 76.70(12) 2_656 . ? O2 Mn1 O1 113.05(13) . . ? Mn1 Mn1 O3 106.99(11) 2_656 . ? O5 Mn1 O3 122.44(14) . . ? O6 Mn1 O3 17.13(12) . . ? O4 Mn1 O3 118.75(14) . . ? O4 Mn1 O3 77.50(12) 2_656 . ? O5 Mn1 O3 76.32(12) 2_656 . ? O6 Mn1 O3 158.53(12) 2_656 . ? O2 Mn1 O3 113.92(13) . . ? O1 Mn1 O3 112.99(13) . . ? Mn1 Mn1 N1 176.68(11) 2_656 . ? O5 Mn1 N1 91.30(15) . . ? O6 Mn1 N1 91.78(15) . . ? O4 Mn1 N1 91.20(15) . . ? O4 Mn1 N1 127.43(13) 2_656 . ? O5 Mn1 N1 127.23(13) 2_656 . ? O6 Mn1 N1 126.74(13) 2_656 . ? O2 Mn1 N1 74.71(14) . . ? O1 Mn1 N1 74.72(13) . . ? O3 Mn1 N1 74.73(13) . . ? O5 Mn2 O6 61.35(13) 2_656 . ? O5 Mn2 O8 149.49(11) 2_656 . ? O6 Mn2 O8 107.52(12) . . ? O5 Mn2 O7 78.56(10) 2_656 . ? O6 Mn2 O7 111.55(10) . . ? O8 Mn2 O7 80.33(7) . . ? O5 Mn2 O9 100.38(10) 2_656 . ? O6 Mn2 O9 76.45(9) . . ? O8 Mn2 O9 104.30(7) . . ? O7 Mn2 O9 169.43(7) . . ? O5 Mn2 O3 80.06(14) 2_656 . ? O6 Mn2 O3 20.24(11) . . ? O8 Mn2 O3 87.41(13) . . ? O7 Mn2 O3 111.27(10) . . ? O9 Mn2 O3 78.68(9) . . ? O5 Mn2 N2 107.60(12) 2_656 . ? O6 Mn2 N2 143.98(11) . . ? O8 Mn2 N2 96.96(9) . . ? O7 Mn2 N2 98.09(8) . . ? O9 Mn2 N2 72.08(7) . . ? O3 Mn2 N2 150.62(10) . . ? O5 Mn2 O2 19.41(11) 2_656 2_656 ? O6 Mn2 O2 78.60(14) . 2_656 ? O8 Mn2 O2 158.33(10) . 2_656 ? O7 Mn2 O2 78.12(9) . 2_656 ? O9 Mn2 O2 97.34(9) . 2_656 ? O3 Mn2 O2 98.21(15) . 2_656 ? N2 Mn2 O2 88.38(13) . 2_656 ? O4 Mn3 O10 105.98(12) 2_656 . ? O4 Mn3 O6 63.68(13) 2_656 . ? O10 Mn3 O6 148.33(10) . . ? O4 Mn3 O9 112.73(10) 2_656 . ? O10 Mn3 O9 80.85(7) . . ? O6 Mn3 O9 76.87(10) . . ? O4 Mn3 O11 75.38(10) 2_656 . ? O10 Mn3 O11 104.94(8) . . ? O6 Mn3 O11 101.09(10) . . ? O9 Mn3 O11 168.72(7) . . ? O4 Mn3 O1 18.47(10) 2_656 2_656 ? O10 Mn3 O1 87.52(13) . 2_656 ? O6 Mn3 O1 79.39(14) . 2_656 ? O9 Mn3 O1 110.01(10) . 2_656 ? O11 Mn3 O1 80.21(10) . 2_656 ? O4 Mn3 O3 79.87(15) 2_656 . ? O10 Mn3 O3 159.84(10) . . ? O6 Mn3 O3 19.99(10) . . ? O9 Mn3 O3 79.13(10) . . ? O11 Mn3 O3 95.18(10) . . ? O1 Mn3 O3 97.11(15) 2_656 . ? O4 Mn3 N3 143.21(11) 2_656 . ? O10 Mn3 N3 99.10(8) . . ? O6 Mn3 N3 105.78(11) . . ? O9 Mn3 N3 97.33(8) . . ? O11 Mn3 N3 72.39(8) . . ? O1 Mn3 N3 152.59(11) 2_656 . ? O3 Mn3 N3 85.80(12) . . ? O4 Mn4 O12 149.87(11) 2_656 . ? O4 Mn4 O11 76.30(10) 2_656 . ? O12 Mn4 O11 81.01(8) . . ? O4 Mn4 O5 63.99(14) 2_656 . ? O12 Mn4 O5 107.71(12) . . ? O11 Mn4 O5 111.54(10) . . ? O4 Mn4 O2 81.79(15) 2_656 . ? O12 Mn4 O2 87.55(13) . . ? O11 Mn4 O2 109.69(10) . . ? O5 Mn4 O2 20.17(11) . . ? O4 Mn4 O7 102.27(10) 2_656 2_656 ? O12 Mn4 O7 103.38(8) . 2_656 ? O11 Mn4 O7 170.08(7) . 2_656 ? O5 Mn4 O7 75.89(9) . 2_656 ? O2 Mn4 O7 79.59(10) . 2_656 ? O4 Mn4 N4 105.25(12) 2_656 2_656 ? O12 Mn4 N4 97.37(9) . 2_656 ? O11 Mn4 N4 98.35(8) . 2_656 ? O5 Mn4 N4 143.25(10) . 2_656 ? O2 Mn4 N4 151.96(11) . 2_656 ? O7 Mn4 N4 72.41(8) 2_656 2_656 ? O4 Mn4 O1 17.80(10) 2_656 2_656 ? O12 Mn4 O1 160.12(11) . 2_656 ? O11 Mn4 O1 79.21(10) . 2_656 ? O5 Mn4 O1 78.04(14) . 2_656 ? O2 Mn4 O1 97.23(15) . 2_656 ? O7 Mn4 O1 96.47(10) 2_656 2_656 ? N4 Mn4 O1 87.47(13) 2_656 2_656 ? C2 O1 Mn3 122.7(3) . 2_656 ? C2 O1 Mn1 115.4(3) . . ? Mn3 O1 Mn1 99.76(16) 2_656 . ? C2 O1 Mn4 118.2(3) . 2_656 ? Mn3 O1 Mn4 96.21(14) 2_656 2_656 ? Mn1 O1 Mn4 100.36(17) . 2_656 ? H1S O1S H3S3 86.7 . . ? C4 O2 Mn4 123.6(3) . . ? C4 O2 Mn1 116.1(3) . . ? Mn4 O2 Mn1 98.06(15) . . ? C4 O2 Mn2 117.4(3) . 2_656 ? Mn4 O2 Mn2 97.76(13) . 2_656 ? Mn1 O2 Mn2 99.54(16) . 2_656 ? C3S O2S H2S 102.0 . . ? C3S O2S H4S2 114.0 . . ? H2S O2S H4S2 32.1 . . ? C6 O3 Mn2 124.2(3) . . ? C6 O3 Mn1 115.1(3) . . ? Mn2 O3 Mn1 98.44(15) . . ? C6 O3 Mn3 118.3(3) . . ? Mn2 O3 Mn3 97.21(13) . . ? Mn1 O3 Mn3 98.86(16) . . ? Mn1 O4 Mn4 123.70(18) . 2_656 ? Mn1 O4 Mn3 118.65(17) . 2_656 ? Mn4 O4 Mn3 105.86(14) 2_656 2_656 ? Mn4 O4 Mn1 100.99(15) 2_656 2_656 ? Mn3 O4 Mn1 103.72(15) 2_656 2_656 ? C4S O4S H4S 109.4 . . ? Mn1 O5 Mn2 128.33(18) . 2_656 ? Mn1 O5 Mn4 116.21(17) . . ? Mn2 O5 Mn4 104.14(13) 2_656 . ? Mn2 O5 Mn1 103.00(14) 2_656 2_656 ? Mn4 O5 Mn1 104.07(14) . 2_656 ? Mn1 O6 Mn2 122.40(16) . . ? Mn1 O6 Mn3 122.58(17) . . ? Mn2 O6 Mn3 104.73(13) . . ? Mn2 O6 Mn1 105.21(14) . 2_656 ? Mn3 O6 Mn1 102.48(14) . 2_656 ? C12 O7 Mn2 130.60(16) . . ? C12 O7 Mn4 118.38(16) . 2_656 ? Mn2 O7 Mn4 100.90(7) . 2_656 ? C14 O8 Mn2 132.37(19) . . ? C26 O9 Mn3 130.88(16) . . ? C26 O9 Mn2 119.15(15) . . ? Mn3 O9 Mn2 101.37(7) . . ? C28 O10 Mn3 132.34(17) . . ? C40 O11 Mn4 131.12(19) . . ? C40 O11 Mn3 120.11(18) . . ? Mn4 O11 Mn3 101.88(8) . . ? C42 O12 Mn4 132.2(2) . . ? C1 N1 C5 111.6(4) . . ? C1 N1 C3 111.5(4) . . ? C5 N1 C3 111.1(4) . . ? C1 N1 Mn1 107.3(3) . . ? C5 N1 Mn1 107.5(3) . . ? C3 N1 Mn1 107.5(3) . . ? C21 N2 C25 118.7(2) . . ? C21 N2 Mn2 124.82(19) . . ? C25 N2 Mn2 116.34(17) . . ? C39 N3 C35 118.5(2) . . ? C39 N3 Mn3 116.18(19) . . ? C35 N3 Mn3 125.22(19) . . ? C11 N4 C7 119.0(2) . . ? C11 N4 Mn4 116.61(17) . 2_656 ? C7 N4 Mn4 124.4(2) . 2_656 ? N1 C1 C2 110.5(4) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 111.4(4) . . ? O1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? O1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O1S C2S H2S1 108.4 . . ? O1S C2S H2S2 110.2 . . ? H2S1 C2S H2S2 109.9 . . ? O1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 108.0 . . ? H2S2 C2S H2S3 110.7 . . ? O1S C2S H3S1 111.9 . . ? H2S1 C2S H3S1 66.8 . . ? H2S2 C2S H3S1 45.2 . . ? H2S3 C2S H3S1 137.6 . . ? O1S C2S H3S3 50.6 . . ? H2S1 C2S H3S3 156.5 . . ? H2S2 C2S H3S3 89.8 . . ? H2S3 C2S H3S3 75.2 . . ? H3S1 C2S H3S3 127.0 . . ? N1 C3 C4 110.4(4) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O2S C3S H2S2 158.5 . . ? O2S C3S H3S1 110.9 . . ? H2S2 C3S H3S1 47.6 . . ? O2S C3S H3S2 126.7 . . ? H2S2 C3S H3S2 71.9 . . ? H3S1 C3S H3S2 112.9 . . ? O2S C3S H3S3 103.2 . . ? H2S2 C3S H3S3 79.9 . . ? H3S1 C3S H3S3 93.4 . . ? H3S2 C3S H3S3 103.0 . . ? O2 C4 C3 109.8(4) . . ? O2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O4S C4S H2S 126.0 . . ? O4S C4S H4S1 99.5 . . ? H2S C4S H4S1 85.4 . . ? O4S C4S H4S2 107.1 . . ? H4S1 C4S H4S2 109.3 . . ? O4S C4S H4S3 106.0 . . ? H2S C4S H4S3 124.2 . . ? H4S1 C4S H4S3 106.5 . . ? H4S2 C4S H4S3 125.4 . . ? N1 C5 C6 110.6(4) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O3 C6 C5 110.8(4) . . ? O3 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O3 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N4 C7 C8 122.3(3) . . ? N4 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C9 C8 C7 118.8(3) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 118.3(3) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? N4 C11 C10 121.9(3) . . ? N4 C11 C12 114.1(2) . . ? C10 C11 C12 123.9(3) . . ? O7 C12 C13 124.5(2) . . ? O7 C12 C11 114.0(2) . . ? C13 C12 C11 121.4(2) . . ? C12 C13 C14 123.8(2) . . ? C12 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? O8 C14 C13 123.7(2) . . ? O8 C14 C15 116.3(2) . . ? C13 C14 C15 120.0(2) . . ? C16 C15 C20 119.4(3) . . ? C16 C15 C14 122.4(3) . . ? C20 C15 C14 118.1(2) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 121.0(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.3(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C15 120.8(3) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? N2 C21 C22 122.7(3) . . ? N2 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C23 C22 C21 118.4(3) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 118.3(3) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? N2 C25 C24 122.0(3) . . ? N2 C25 C26 114.2(2) . . ? C24 C25 C26 123.8(2) . . ? O9 C26 C27 125.0(2) . . ? O9 C26 C25 114.0(2) . . ? C27 C26 C25 121.0(2) . . ? C26 C27 C28 123.9(2) . . ? C26 C27 H27 118.0 . . ? C28 C27 H27 118.0 . . ? O10 C28 C27 123.5(2) . . ? O10 C28 C29 117.2(2) . . ? C27 C28 C29 119.3(2) . . ? C30 C29 C34 117.9(3) . . ? C30 C29 C28 123.2(3) . . ? C34 C29 C28 118.8(3) . . ? C29 C30 C31 120.5(4) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 120.5(4) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 118.9(3) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 120.7(3) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C29 C34 C33 121.3(3) . . ? C29 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? N3 C35 C36 122.6(3) . . ? N3 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C37 C36 C35 118.3(3) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C38 C37 C36 119.4(3) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 119.3(3) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? N3 C39 C38 121.9(3) . . ? N3 C39 C40 114.4(2) . . ? C38 C39 C40 123.7(3) . . ? O11 C40 C41 124.3(3) . . ? O11 C40 C39 114.6(2) . . ? C41 C40 C39 121.0(3) . . ? C40 C41 C42 124.1(3) . . ? C40 C41 H41 117.9 . . ? C42 C41 H41 117.9 . . ? O12 C42 C41 123.9(3) . . ? O12 C42 C43 116.7(3) . . ? C41 C42 C43 119.4(3) . . ? C44 C43 C48 119.0(3) . . ? C44 C43 C42 123.1(3) . . ? C48 C43 C42 117.8(3) . . ? C45 C44 C43 119.4(4) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 121.3(3) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C47 C46 C45 119.1(3) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 120.2(4) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 120.9(3) . . ? C47 C48 H48 119.6 . . ? C43 C48 H48 119.6 . . ? F4S B1S F2S 109.6(3) . . ? F4S B1S F3S 109.9(3) . . ? F2S B1S F3S 109.2(3) . . ? F4S B1S F1S 110.0(3) . . ? F2S B1S F1S 109.2(3) . . ? F3S B1S F1S 109.0(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 30.67 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.110 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.115 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 83 13 ' ' 2 0.150 0.705 0.664 11 1 ' ' 3 0.500 0.500 0.000 300 69 ' ' 4 0.850 0.295 0.336 11 1 ' ' _platon_squeeze_details ; ; # Attachment '- StuartLangleyamendedcif 4.txt' #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 768054' #TrackingRef '- StuartLangleyamendedcif 4.txt' #========================================================================== _publ_section_exptl_refinement ; The asymmetric unit contains two unique Manganese ions, one paa ligand as well one methoxide, one nitrate and one disordered methanol molecule. All non H-atoms were refined anisotropically, SIMU, DELU and ISOR restraints were place on the disorderd MeOH molecule. The bond lengths of the disordered MeOH were restrained to 1.45. All H-atoms were placed in calculated positions. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C60 H72 Mn7 N12 O18, 3(C2 H8 O2), 2(N O3) ; _chemical_formula_sum 'C66 H96 Mn7 N14 O30' _chemical_formula_weight 1950.15 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 cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-y+1/2, -z, x+1/2' 'z+1/2, -x+1/2, -y' '-y, z+1/2, -x+1/2' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' 'y-1/2, z, -x-1/2' '-z-1/2, x-1/2, y' 'y, -z-1/2, x-1/2' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y-1/2, z-1/2, x' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.4997(2) _cell_length_b 20.4997(2) _cell_length_c 20.4997(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8614.75(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4361 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 23.85 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4020 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.529 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16454 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.70 _reflns_number_total 2397 _reflns_number_gt 1712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two unique Manganese ions, one paa ligand as well one methoxide, one nitrate and one disordered methanol molecule. All non H-atoms were refined anisotropically, SIMU, DELU and ISOR restraints were place on the disorderd MeOH molecule. The bond lengths of the disordered MeOH were restrained to 1.45. All H-atoms were placed in calculated positions. ; _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^)+(0.1033P)^2^+25.5029P] 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 2397 _refine_ls_number_parameters 187 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.2034 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.050 _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 0.58121(4) 0.44817(4) 0.12915(4) 0.0441(4) Uani 1 1 d . . . Mn2 Mn 0.5000 0.5000 0.0000 0.0391(5) Uani 1 6 d S . . O1 O 0.54181(17) 0.53825(18) 0.09206(17) 0.0421(9) Uani 1 1 d . . . C1S C 0.8147(13) 0.6422(14) 0.2666(12) 0.140(6) Uani 0.50 1 d PDU A 2 H1S1 H 0.7812 0.6774 0.2929 0.211 Uiso 0.50 1 d P B 2 H1S2 H 0.8514 0.6616 0.2625 0.211 Uiso 0.50 1 d P C 2 H1S3 H 0.8127 0.6066 0.3023 0.211 Uiso 0.50 1 d P D 2 O2 O 0.4900(2) 0.41392(18) 0.17197(19) 0.0494(10) Uani 1 1 d . . . O2S O 0.8435(11) 0.6003(12) 0.2481(11) 0.180(5) Uani 0.50 1 d PDU E 1 H2S H 0.8196 0.6017 0.2809 0.216 Uiso 0.50 1 d P F 1 O3 O 0.3666(2) 0.3536(2) 0.1400(2) 0.0598(11) Uani 1 1 d . . . O3S O 0.4155(2) 0.4766(2) 0.3937(2) 0.0686(14) Uani 1 1 d . . . N1 N 0.5961(3) 0.4822(3) 0.2320(2) 0.0567(13) Uani 1 1 d . . . N1S N 0.4281(3) 0.4281(3) 0.4281(3) 0.054(2) Uani 1 3 d S . . N2 N 0.4914(3) 0.4577(3) 0.2746(2) 0.0637(15) Uani 1 1 d . . . H2 H 0.4666 0.4657 0.3087 0.076 Uiso 1 1 calc R . . C1 C 0.5030(3) 0.5799(3) 0.1371(3) 0.0534(16) Uani 1 1 d . . . H1A H 0.4617 0.5582 0.1472 0.080 Uiso 1 1 calc R . . H1C H 0.4943 0.6220 0.1162 0.080 Uiso 1 1 calc R . . H1B H 0.5276 0.5870 0.1775 0.080 Uiso 1 1 calc R . . O1S O 0.7766(11) 0.6199(11) 0.2084(11) 0.180(5) Uani 0.50 1 d PDU A 2 H1S H 0.7357 0.6175 0.2159 0.216 Uiso 0.50 1 d P G 2 C1S' C 0.8125(13) 0.5865(13) 0.1864(11) 0.140(6) Uani 0.50 1 d PDU E 1 H1S4 H 0.7677 0.6032 0.1870 0.211 Uiso 0.50 1 calc PR E 1 H1S5 H 0.8118 0.5393 0.1791 0.211 Uiso 0.50 1 calc PR E 1 H1S6 H 0.8369 0.6078 0.1512 0.211 Uiso 0.50 1 calc PR E 1 C2 C 0.2819(3) 0.3674(4) 0.2157(4) 0.083(2) Uani 1 1 d . . . H2A H 0.2692 0.3221 0.2071 0.125 Uiso 1 1 calc R . . H2B H 0.2538 0.3969 0.1905 0.125 Uiso 1 1 calc R . . H2C H 0.2770 0.3768 0.2623 0.125 Uiso 1 1 calc R . . C3 C 0.3515(3) 0.3774(3) 0.1959(3) 0.0575(16) Uani 1 1 d . . . C4 C 0.3931(3) 0.4097(3) 0.2366(3) 0.0584(17) Uani 1 1 d . . . H4 H 0.3757 0.4226 0.2775 0.070 Uiso 1 1 calc R . . C5 C 0.4587(3) 0.4262(3) 0.2250(3) 0.0523(15) Uani 1 1 d . . . C6 C 0.5550(4) 0.4797(3) 0.2821(3) 0.0560(16) Uani 1 1 d . . . C7 C 0.5739(4) 0.5008(4) 0.3445(3) 0.079(2) Uani 1 1 d . . . H7 H 0.5437 0.4999 0.3796 0.095 Uiso 1 1 calc R . . C8 C 0.6362(5) 0.5226(4) 0.3544(4) 0.089(3) Uani 1 1 d . . . H8 H 0.6501 0.5349 0.3968 0.107 Uiso 1 1 calc R . . C9 C 0.6770(5) 0.5266(4) 0.3043(4) 0.095(3) Uani 1 1 d . . . H9 H 0.7196 0.5440 0.3097 0.114 Uiso 1 1 calc R . . C10 C 0.6556(4) 0.5044(4) 0.2436(4) 0.080(2) Uani 1 1 d . . . H10 H 0.6856 0.5054 0.2083 0.096 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 0.0467(6) 0.0476(6) 0.0380(5) -0.0034(4) 0.0015(4) 0.0063(4) Mn2 0.0391(5) 0.0391(5) 0.0391(5) 0.0017(5) -0.0017(5) -0.0017(5) O1 0.042(2) 0.043(2) 0.042(2) -0.0020(17) 0.0022(16) 0.0036(16) C1S 0.132(8) 0.141(8) 0.148(8) -0.005(6) 0.007(6) 0.011(6) O2 0.057(2) 0.046(2) 0.045(2) -0.0035(17) 0.0099(19) 0.0068(18) O2S 0.188(8) 0.181(8) 0.171(7) 0.010(6) -0.006(6) -0.010(6) O3 0.057(3) 0.061(3) 0.061(3) 0.006(2) 0.011(2) 0.003(2) O3S 0.090(4) 0.069(3) 0.047(2) 0.016(2) 0.015(2) 0.029(3) N1 0.075(4) 0.050(3) 0.046(3) -0.006(2) -0.005(3) -0.006(3) N1S 0.054(2) 0.054(2) 0.054(2) 0.008(3) 0.008(3) 0.008(3) N2 0.073(4) 0.077(4) 0.041(3) -0.006(3) 0.015(3) -0.005(3) C1 0.051(4) 0.062(4) 0.048(3) -0.017(3) 0.016(3) -0.012(3) O1S 0.188(8) 0.181(8) 0.171(7) 0.010(6) -0.006(6) -0.010(6) C1S' 0.132(8) 0.141(8) 0.148(8) -0.005(6) 0.007(6) 0.011(6) C2 0.056(4) 0.107(6) 0.087(6) 0.018(5) 0.010(4) 0.002(4) C3 0.058(4) 0.058(4) 0.057(4) 0.012(3) 0.011(3) 0.007(3) C4 0.058(4) 0.070(4) 0.047(4) 0.005(3) 0.018(3) 0.008(3) C5 0.068(4) 0.044(3) 0.045(4) 0.005(3) 0.005(3) 0.009(3) C6 0.082(5) 0.044(3) 0.041(4) 0.001(3) 0.009(3) -0.002(3) C7 0.116(7) 0.073(5) 0.049(4) -0.008(4) 0.013(4) -0.031(5) C8 0.127(7) 0.085(6) 0.056(5) -0.011(4) 0.012(5) -0.056(5) C9 0.118(7) 0.107(7) 0.061(5) -0.011(5) -0.007(5) -0.047(6) C10 0.088(6) 0.090(6) 0.061(5) -0.014(4) 0.005(4) -0.023(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 Mn1 O3 2.091(4) 19_656 ? Mn1 O1 2.154(4) . ? Mn1 O1 2.159(4) 18_565 ? Mn1 O2 2.181(4) . ? Mn1 O2 2.231(4) 19_656 ? Mn1 N1 2.242(5) . ? Mn2 O1 2.216(4) . ? Mn2 O1 2.216(4) 6_655 ? Mn2 O1 2.216(4) 13_665 ? Mn2 O1 2.216(4) 7_564 ? Mn2 O1 2.216(4) 19_656 ? Mn2 O1 2.216(4) 18_565 ? O1 C1 1.488(7) . ? O1 Mn1 2.159(4) 19_656 ? C1S O1S 1.497(10) . ? C1S H1S1 1.1315 . ? C1S H1S2 0.8549 . ? C1S H1S3 1.0338 . ? C1S H2S 0.8855 . ? O2 C5 1.288(7) . ? O2 Mn1 2.231(4) 18_565 ? O2S C1S' 1.443(10) . ? O2S H1S2 1.2998 . ? O2S H1S3 1.2823 . ? O2S H2S 0.8314 . ? O3 C3 1.285(8) . ? O3 Mn1 2.091(4) 18_565 ? O3S N1S 1.246(4) . ? N1 C10 1.322(9) . ? N1 C6 1.330(8) . ? N1S O3S 1.246(4) 2 ? N1S O3S 1.246(4) 3 ? N2 C5 1.378(8) . ? N2 C6 1.388(9) . ? N2 H2 0.8800 . ? C1 H1A 0.9800 . ? C1 H1C 0.9800 . ? C1 H1B 0.9800 . ? O1S H1S 0.8520 . ? C1S' H1S4 0.9800 . ? C1S' H1S5 0.9800 . ? C1S' H1S6 0.9800 . ? C2 C3 1.499(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.363(9) . ? C4 C5 1.407(9) . ? C4 H4 0.9500 . ? C6 C7 1.405(9) . ? C7 C8 1.367(11) . ? C7 H7 0.9500 . ? C8 C9 1.326(11) . ? C8 H8 0.9500 . ? C9 C10 1.396(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn1 O1 163.99(17) 19_656 . ? O3 Mn1 O1 94.02(15) 19_656 18_565 ? O1 Mn1 O1 83.21(19) . 18_565 ? O3 Mn1 O2 99.68(17) 19_656 . ? O1 Mn1 O2 95.55(15) . . ? O1 Mn1 O2 82.02(15) 18_565 . ? O3 Mn1 O2 83.92(16) 19_656 19_656 ? O1 Mn1 O2 80.98(14) . 19_656 ? O1 Mn1 O2 99.14(14) 18_565 19_656 ? O2 Mn1 O2 176.16(12) . 19_656 ? O3 Mn1 N1 90.62(19) 19_656 . ? O1 Mn1 N1 96.69(17) . . ? O1 Mn1 N1 162.65(18) 18_565 . ? O2 Mn1 N1 80.72(18) . . ? O2 Mn1 N1 97.98(18) 19_656 . ? O1 Mn2 O1 99.49(12) . 6_655 ? O1 Mn2 O1 180.00(17) . 13_665 ? O1 Mn2 O1 80.51(12) 6_655 13_665 ? O1 Mn2 O1 99.49(12) . 7_564 ? O1 Mn2 O1 99.49(12) 6_655 7_564 ? O1 Mn2 O1 80.51(12) 13_665 7_564 ? O1 Mn2 O1 80.51(12) . 19_656 ? O1 Mn2 O1 80.51(12) 6_655 19_656 ? O1 Mn2 O1 99.49(12) 13_665 19_656 ? O1 Mn2 O1 180.0(2) 7_564 19_656 ? O1 Mn2 O1 80.51(12) . 18_565 ? O1 Mn2 O1 180.00(17) 6_655 18_565 ? O1 Mn2 O1 99.49(12) 13_665 18_565 ? O1 Mn2 O1 80.51(12) 7_564 18_565 ? O1 Mn2 O1 99.49(12) 19_656 18_565 ? C1 O1 Mn1 118.3(3) . . ? C1 O1 Mn1 116.5(3) . 19_656 ? Mn1 O1 Mn1 100.00(15) . 19_656 ? C1 O1 Mn2 121.6(3) . . ? Mn1 O1 Mn2 98.18(14) . . ? Mn1 O1 Mn2 98.04(14) 19_656 . ? O1S C1S H1S1 104.9 . . ? O1S C1S H1S2 121.5 . . ? H1S1 C1S H1S2 106.5 . . ? O1S C1S H1S3 109.2 . . ? H1S1 C1S H1S3 95.2 . . ? H1S2 C1S H1S3 115.5 . . ? O1S C1S H2S 92.3 . . ? H1S1 C1S H2S 120.6 . . ? H1S2 C1S H2S 111.5 . . ? C5 O2 Mn1 134.8(4) . . ? C5 O2 Mn1 126.2(4) . 18_565 ? Mn1 O2 Mn1 96.97(15) . 18_565 ? C1S' O2S H1S2 116.3 . . ? C1S' O2S H1S3 124.2 . . ? H1S2 O2S H1S3 76.6 . . ? C1S' O2S H2S 117.2 . . ? H1S2 O2S H2S 81.7 . . ? C3 O3 Mn1 130.0(4) . 18_565 ? C10 N1 C6 117.3(6) . . ? C10 N1 Mn1 113.7(5) . . ? C6 N1 Mn1 128.9(5) . . ? O3S N1S O3S 119.98(3) 2 . ? O3S N1S O3S 119.98(3) 2 3 ? O3S N1S O3S 119.98(3) . 3 ? C5 N2 C6 133.7(5) . . ? C5 N2 H2 113.1 . . ? C6 N2 H2 113.1 . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? C1S O1S H1S 112.7 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O3 C3 C4 125.5(6) . . ? O3 C3 C2 114.7(7) . . ? C4 C3 C2 119.8(6) . . ? C3 C4 C5 127.7(6) . . ? C3 C4 H4 116.1 . . ? C5 C4 H4 116.1 . . ? O2 C5 N2 118.2(6) . . ? O2 C5 C4 124.8(6) . . ? N2 C5 C4 117.0(6) . . ? N1 C6 N2 121.5(6) . . ? N1 C6 C7 121.0(7) . . ? N2 C6 C7 117.5(6) . . ? C8 C7 C6 119.5(7) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 119.7(8) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.1(8) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N1 C10 C9 124.2(8) . . ? N1 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.965 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.093 # Attachment '- StuartLangleyamendedcif 5.txt' #========================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 768055' #TrackingRef '- StuartLangleyamendedcif 5.txt' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _publ_section_exptl_refinement ; The asymmetric unit contains half the cluster as well as a nitrate, DCM and MeOH molecule. All the non-hydrogen atoms are refined anisotropically. All hydrogen atoms are placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C48 H62 Mn4 N10 O14, 2(C H4 O), 2(C H2 Cl2), 2(N O3) ; _chemical_formula_sum 'C52 H74 Cl4 Mn4 N12 O22' _chemical_formula_weight 1580.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3709(3) _cell_length_b 12.1927(4) _cell_length_c 15.2722(4) _cell_angle_alpha 94.8080(10) _cell_angle_beta 100.4300(10) _cell_angle_gamma 101.7780(10) _cell_volume 1666.72(9) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8803 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.60 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25884 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 30.63 _reflns_number_total 9947 _reflns_number_gt 8724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains half the cluster as well as a nitrate, DCM and MeOH molecule. All the non-hydrogen atoms are refined anisotropically. All hydrogen atoms are placed in calculated positions. ; _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^)+(0.0480P)^2^+1.2472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9947 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.001 _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 0.41968(4) 0.85655(3) 0.44670(2) 0.00886(8) Uani 1 1 d . . . Mn2 Mn 0.63036(3) 1.04617(3) 0.35432(2) 0.00852(8) Uani 1 1 d . . . Cl1S Cl -0.14036(13) 0.47555(11) 0.18566(7) 0.0593(3) Uani 1 1 d . . . Cl2S Cl -0.16420(10) 0.39059(8) -0.00173(6) 0.0416(2) Uani 1 1 d . . . O1 O 0.46480(16) 0.92153(13) 0.32814(10) 0.0104(3) Uani 1 1 d . . . O2 O 0.27003(19) 0.67958(15) 0.42538(12) 0.0151(3) Uani 1 1 d . . . O3 O 0.35141(16) 0.99493(13) 0.52487(10) 0.0093(3) Uani 1 1 d . . . O4 O 0.48681(17) 0.83342(13) 0.58723(10) 0.0111(3) Uani 1 1 d . . . O5 O 0.42561(18) 0.90024(14) 0.75808(11) 0.0133(3) Uani 1 1 d . . . O6 O 0.75816(18) 0.95296(13) 0.28560(11) 0.0123(3) Uani 1 1 d . . . O7 O 0.80983(18) 1.16233(14) 0.38655(11) 0.0142(3) Uani 1 1 d . . . O1S O 0.2904(3) 0.61308(18) 0.21729(14) 0.0327(5) Uani 1 1 d . . . O2S O 0.3192(2) 0.50549(15) 0.32196(12) 0.0189(4) Uani 1 1 d . . . O3S O 0.3209(4) 0.4464(2) 0.18477(15) 0.0571(9) Uani 1 1 d . . . O4S O 0.9404(2) 1.10978(17) 0.03893(12) 0.0238(4) Uani 1 1 d . . . H4S H 1.0120 1.1247 0.0147 0.029 Uiso 1 1 calc R . . N1 N 0.1805(2) 0.86855(16) 0.36295(12) 0.0119(4) Uani 1 1 d . . . N2 N 0.5785(2) 0.73310(16) 0.43893(13) 0.0121(4) Uani 1 1 d . . . N3 N 0.5799(2) 0.67340(16) 0.58345(13) 0.0133(4) Uani 1 1 d . . . H3N H 0.6018 0.6223 0.6156 0.016 Uiso 1 1 calc R . . N4 N 0.8350(2) 0.80752(19) 0.05125(15) 0.0209(4) Uani 1 1 d . . . N5 N 0.8418(2) 0.95635(17) 0.15508(13) 0.0147(4) Uani 1 1 d . . . H5N H 0.8979 0.9963 0.1253 0.018 Uiso 1 1 calc R . . N1S N 0.3098(3) 0.52167(19) 0.23996(14) 0.0208(4) Uani 1 1 d . . . C1 C 0.3423(2) 0.90194(19) 0.25445(14) 0.0123(4) Uani 1 1 d . . . H1A H 0.3180 0.8233 0.2288 0.015 Uiso 1 1 calc R . . H1B H 0.3677 0.9480 0.2084 0.015 Uiso 1 1 calc R . . C2 C 0.2098(2) 0.9315(2) 0.28685(15) 0.0131(4) Uani 1 1 d . . . H2A H 0.2299 1.0120 0.3058 0.016 Uiso 1 1 calc R . . H2B H 0.1230 0.9120 0.2383 0.016 Uiso 1 1 calc R . . C3 C 0.1132(3) 0.6747(2) 0.39878(17) 0.0171(5) Uani 1 1 d . . . H3A H 0.0741 0.6961 0.4507 0.020 Uiso 1 1 calc R . . H3B H 0.0611 0.5982 0.3739 0.020 Uiso 1 1 calc R . . C4 C 0.0882(2) 0.7537(2) 0.32961(16) 0.0156(4) Uani 1 1 d . . . H4A H 0.1138 0.7259 0.2745 0.019 Uiso 1 1 calc R . . H4B H -0.0161 0.7566 0.3166 0.019 Uiso 1 1 calc R . . C5 C 0.1091(2) 0.92891(19) 0.42425(15) 0.0124(4) Uani 1 1 d . . . H5A H 0.0664 0.8772 0.4625 0.015 Uiso 1 1 calc R . . H5B H 0.0291 0.9561 0.3895 0.015 Uiso 1 1 calc R . . C6 C 0.2207(2) 1.02785(19) 0.48199(15) 0.0114(4) Uani 1 1 d . . . H6A H 0.2485 1.0862 0.4449 0.014 Uiso 1 1 calc R . . H6B H 0.1748 1.0592 0.5273 0.014 Uiso 1 1 calc R . . C7 C 0.6151(3) 0.7166(2) 0.35791(16) 0.0149(4) Uani 1 1 d . . . H7 H 0.5968 0.7672 0.3172 0.018 Uiso 1 1 calc R . . C8 C 0.6774(3) 0.6296(2) 0.33189(16) 0.0165(5) Uani 1 1 d . . . H8 H 0.6999 0.6216 0.2752 0.020 Uiso 1 1 calc R . . C9 C 0.7060(3) 0.5541(2) 0.39244(16) 0.0161(4) Uani 1 1 d . . . H9 H 0.7472 0.4939 0.3768 0.019 Uiso 1 1 calc R . . C10 C 0.6722(2) 0.57000(19) 0.47604(16) 0.0145(4) Uani 1 1 d . . . H10 H 0.6909 0.5209 0.5179 0.017 Uiso 1 1 calc R . . C11 C 0.6093(2) 0.66097(18) 0.49727(15) 0.0112(4) Uani 1 1 d . . . C12 C 0.5224(2) 0.75218(18) 0.62584(15) 0.0112(4) Uani 1 1 d . . . C13 C 0.5096(3) 0.7353(2) 0.71563(16) 0.0181(5) Uani 1 1 d . . . H13 H 0.5331 0.6703 0.7364 0.022 Uiso 1 1 calc R . . C14 C 0.4654(3) 0.8076(2) 0.77398(15) 0.0150(4) Uani 1 1 d . . . C15 C 0.4646(4) 0.7815(2) 0.86827(17) 0.0280(6) Uani 1 1 d . . . H15A H 0.3691 0.7834 0.8821 0.042 Uiso 1 1 calc R . . H15B H 0.5404 0.8367 0.9092 0.042 Uiso 1 1 calc R . . H15C H 0.4839 0.7078 0.8738 0.042 Uiso 1 1 calc R . . C16 C 0.7754(3) 0.7026(2) 0.00987(19) 0.0263(6) Uani 1 1 d . . . H16 H 0.8197 0.6746 -0.0343 0.032 Uiso 1 1 calc R . . C17 C 0.6517(3) 0.6340(2) 0.02929(19) 0.0257(6) Uani 1 1 d . . . H17 H 0.6161 0.5605 0.0008 0.031 Uiso 1 1 calc R . . C18 C 0.5820(3) 0.6772(2) 0.09201(17) 0.0216(5) Uani 1 1 d . . . H18 H 0.4965 0.6338 0.1051 0.026 Uiso 1 1 calc R . . C19 C 0.6406(3) 0.7857(2) 0.13529(16) 0.0184(5) Uani 1 1 d . . . H19 H 0.5947 0.8170 0.1772 0.022 Uiso 1 1 calc R . . C20 C 0.7702(3) 0.8470(2) 0.11446(15) 0.0144(4) Uani 1 1 d . . . C21 C 0.8328(2) 1.00686(19) 0.23633(15) 0.0123(4) Uani 1 1 d . . . C22 C 0.9172(3) 1.1213(2) 0.26139(16) 0.0148(4) Uani 1 1 d . . . H22 H 0.9837 1.1508 0.2264 0.018 Uiso 1 1 calc R . . C23 C 0.9040(2) 1.1885(2) 0.33411(16) 0.0141(4) Uani 1 1 d . . . C24 C 1.0028(3) 1.3043(2) 0.36057(18) 0.0242(6) Uani 1 1 d . . . H24A H 0.9429 1.3596 0.3577 0.036 Uiso 1 1 calc R . . H24B H 1.0703 1.3178 0.3203 0.036 Uiso 1 1 calc R . . H24C H 1.0584 1.3096 0.4207 0.036 Uiso 1 1 calc R . . C1S C 0.8074(4) 1.0837(3) -0.0271(2) 0.0354(7) Uani 1 1 d . . . H1S1 H 0.7234 1.0715 0.0016 0.053 Uiso 1 1 calc R . . H1S2 H 0.8047 1.0166 -0.0656 0.053 Uiso 1 1 calc R . . H1S3 H 0.8038 1.1453 -0.0620 0.053 Uiso 1 1 calc R . . C2S C -0.0649(4) 0.4012(3) 0.1091(2) 0.0417(8) Uani 1 1 d . . . H2S1 H -0.0658 0.3260 0.1255 0.050 Uiso 1 1 calc R . . H2S2 H 0.0379 0.4393 0.1125 0.050 Uiso 1 1 calc R . . H2H H 0.289(4) 0.640(3) 0.392(2) 0.028(9) 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 0.01046(14) 0.00807(15) 0.00924(15) 0.00178(11) 0.00337(11) 0.00328(11) Mn2 0.00980(14) 0.00809(15) 0.00845(14) 0.00170(11) 0.00361(11) 0.00199(11) Cl1S 0.0715(7) 0.0761(8) 0.0380(5) -0.0042(5) 0.0098(5) 0.0396(6) Cl2S 0.0442(4) 0.0429(5) 0.0352(4) -0.0026(3) 0.0008(3) 0.0137(4) O1 0.0097(6) 0.0112(7) 0.0101(7) 0.0017(5) 0.0017(5) 0.0021(5) O2 0.0166(8) 0.0114(8) 0.0173(8) -0.0005(6) 0.0032(6) 0.0042(6) O3 0.0081(6) 0.0111(7) 0.0097(7) 0.0033(5) 0.0022(5) 0.0032(5) O4 0.0152(7) 0.0079(7) 0.0113(7) 0.0026(5) 0.0034(6) 0.0039(6) O5 0.0188(8) 0.0122(7) 0.0105(7) 0.0027(6) 0.0043(6) 0.0055(6) O6 0.0151(7) 0.0112(7) 0.0135(7) 0.0035(6) 0.0079(6) 0.0043(6) O7 0.0156(7) 0.0123(8) 0.0134(7) 0.0003(6) 0.0057(6) -0.0016(6) O1S 0.0597(15) 0.0234(10) 0.0243(10) 0.0115(8) 0.0126(10) 0.0238(10) O2S 0.0277(9) 0.0145(8) 0.0167(8) 0.0046(6) 0.0060(7) 0.0075(7) O3S 0.113(3) 0.0447(15) 0.0215(11) -0.0078(10) -0.0030(13) 0.0544(17) O4S 0.0232(9) 0.0309(11) 0.0187(9) 0.0070(8) 0.0103(7) 0.0025(8) N1 0.0110(8) 0.0128(9) 0.0122(8) 0.0006(7) 0.0043(6) 0.0019(7) N2 0.0137(8) 0.0099(8) 0.0140(9) 0.0025(7) 0.0048(7) 0.0035(7) N3 0.0208(9) 0.0094(8) 0.0130(9) 0.0048(7) 0.0051(7) 0.0079(7) N4 0.0229(10) 0.0194(10) 0.0222(10) -0.0014(8) 0.0119(8) 0.0036(8) N5 0.0174(9) 0.0125(9) 0.0154(9) 0.0016(7) 0.0089(7) 0.0011(7) N1S 0.0277(11) 0.0187(10) 0.0162(10) -0.0003(8) 0.0012(8) 0.0098(9) C1 0.0126(9) 0.0149(10) 0.0093(9) 0.0019(7) 0.0011(7) 0.0033(8) C2 0.0119(9) 0.0168(11) 0.0116(9) 0.0042(8) 0.0028(7) 0.0043(8) C3 0.0164(10) 0.0131(10) 0.0213(11) 0.0000(9) 0.0063(9) 0.0009(8) C4 0.0113(9) 0.0159(11) 0.0175(11) -0.0010(8) 0.0021(8) 0.0003(8) C5 0.0094(9) 0.0154(10) 0.0131(10) 0.0014(8) 0.0031(7) 0.0039(8) C6 0.0094(9) 0.0134(10) 0.0142(10) 0.0026(8) 0.0049(7) 0.0062(7) C7 0.0195(10) 0.0126(10) 0.0151(10) 0.0040(8) 0.0068(8) 0.0057(8) C8 0.0197(11) 0.0171(11) 0.0158(10) 0.0025(8) 0.0089(9) 0.0061(9) C9 0.0172(10) 0.0130(10) 0.0206(11) 0.0008(8) 0.0067(9) 0.0072(8) C10 0.0151(10) 0.0106(10) 0.0188(11) 0.0027(8) 0.0028(8) 0.0055(8) C11 0.0115(9) 0.0079(9) 0.0147(10) 0.0017(7) 0.0035(7) 0.0021(7) C12 0.0122(9) 0.0090(9) 0.0129(9) 0.0023(7) 0.0033(7) 0.0028(7) C13 0.0300(12) 0.0141(11) 0.0152(11) 0.0080(8) 0.0078(9) 0.0113(9) C14 0.0189(10) 0.0133(10) 0.0142(10) 0.0056(8) 0.0045(8) 0.0044(8) C15 0.0512(18) 0.0261(14) 0.0147(11) 0.0095(10) 0.0121(12) 0.0191(13) C16 0.0289(13) 0.0223(13) 0.0291(14) -0.0056(11) 0.0141(11) 0.0050(11) C17 0.0289(13) 0.0159(12) 0.0289(14) -0.0028(10) 0.0045(11) 0.0008(10) C18 0.0232(12) 0.0213(12) 0.0177(11) 0.0033(9) 0.0045(9) -0.0012(10) C19 0.0191(11) 0.0209(12) 0.0147(10) 0.0017(9) 0.0065(9) 0.0007(9) C20 0.0165(10) 0.0148(10) 0.0129(10) 0.0025(8) 0.0057(8) 0.0033(8) C21 0.0119(9) 0.0136(10) 0.0134(10) 0.0021(8) 0.0047(8) 0.0052(8) C22 0.0144(10) 0.0147(10) 0.0158(10) 0.0031(8) 0.0072(8) 0.0004(8) C23 0.0116(9) 0.0136(10) 0.0161(10) 0.0040(8) 0.0033(8) -0.0007(8) C24 0.0238(12) 0.0189(12) 0.0261(13) -0.0017(10) 0.0110(10) -0.0074(10) C1S 0.0340(15) 0.0393(18) 0.0299(15) 0.0077(13) -0.0008(12) 0.0066(13) C2S 0.0426(19) 0.050(2) 0.0360(18) 0.0036(15) 0.0054(15) 0.0217(16) _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 O1 2.1133(16) . ? Mn1 O4 2.1832(16) . ? Mn1 O3 2.2496(16) . ? Mn1 O2 2.2825(17) . ? Mn1 N2 2.333(2) . ? Mn1 N1 2.4097(19) . ? Mn1 O3 2.4524(15) 2_676 ? Mn2 O1 1.8941(15) . ? Mn2 O5 1.9106(17) 2_676 ? Mn2 O7 1.9203(15) . ? Mn2 O3 1.9392(16) 2_676 ? Mn2 O6 2.1536(16) . ? Mn2 O4 2.2251(16) 2_676 ? Cl1S C2S 1.753(4) . ? Cl2S C2S 1.758(3) . ? O1 C1 1.420(2) . ? O2 C3 1.439(3) . ? O2 H2H 0.74(4) . ? O3 C6 1.430(3) . ? O3 Mn2 1.9392(16) 2_676 ? O3 Mn1 2.4524(15) 2_676 ? O4 C12 1.266(3) . ? O4 Mn2 2.2251(16) 2_676 ? O5 C14 1.288(3) . ? O5 Mn2 1.9106(17) 2_676 ? O6 C21 1.254(3) . ? O7 C23 1.306(3) . ? O1S N1S 1.233(3) . ? O2S N1S 1.274(3) . ? O3S N1S 1.226(3) . ? O4S C1S 1.414(3) . ? O4S H4S 0.8200 . ? N1 C5 1.476(3) . ? N1 C2 1.481(3) . ? N1 C4 1.481(3) . ? N2 C11 1.339(3) . ? N2 C7 1.352(3) . ? N3 C12 1.366(3) . ? N3 C11 1.395(3) . ? N3 H3N 0.8600 . ? N4 C20 1.336(3) . ? N4 C16 1.338(3) . ? N5 C21 1.363(3) . ? N5 C20 1.399(3) . ? N5 H5N 0.8600 . ? C1 C2 1.513(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.508(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.516(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.375(3) . ? C7 H7 0.9300 . ? C8 C9 1.389(4) . ? C8 H8 0.9300 . ? C9 C10 1.378(3) . ? C9 H9 0.9300 . ? C10 C11 1.399(3) . ? C10 H10 0.9300 . ? C12 C13 1.426(3) . ? C13 C14 1.377(3) . ? C13 H13 0.9300 . ? C14 C15 1.501(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.379(4) . ? C16 H16 0.9300 . ? C17 C18 1.379(4) . ? C17 H17 0.9300 . ? C18 C19 1.384(3) . ? C18 H18 0.9300 . ? C19 C20 1.394(3) . ? C19 H19 0.9300 . ? C21 C22 1.439(3) . ? C22 C23 1.363(3) . ? C22 H22 0.9300 . ? C23 C24 1.499(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O4 151.75(6) . . ? O1 Mn1 O3 105.39(6) . . ? O4 Mn1 O3 75.04(6) . . ? O1 Mn1 O2 115.02(6) . . ? O4 Mn1 O2 87.86(6) . . ? O3 Mn1 O2 117.91(6) . . ? O1 Mn1 N2 92.12(7) . . ? O4 Mn1 N2 77.67(6) . . ? O3 Mn1 N2 149.25(6) . . ? O2 Mn1 N2 74.55(6) . . ? O1 Mn1 N1 75.16(6) . . ? O4 Mn1 N1 130.03(6) . . ? O3 Mn1 N1 74.52(6) . . ? O2 Mn1 N1 72.94(6) . . ? N2 Mn1 N1 135.36(6) . . ? O1 Mn1 O3 67.68(5) . 2_676 ? O4 Mn1 O3 85.04(5) . 2_676 ? O3 Mn1 O3 79.10(6) . 2_676 ? O2 Mn1 O3 159.09(6) . 2_676 ? N2 Mn1 O3 84.72(6) . 2_676 ? N1 Mn1 O3 125.98(6) . 2_676 ? O1 Mn2 O5 92.62(7) . 2_676 ? O1 Mn2 O7 174.12(8) . . ? O5 Mn2 O7 92.00(7) 2_676 . ? O1 Mn2 O3 83.72(6) . 2_676 ? O5 Mn2 O3 166.69(7) 2_676 2_676 ? O7 Mn2 O3 92.57(7) . 2_676 ? O1 Mn2 O6 91.11(6) . . ? O5 Mn2 O6 85.60(7) 2_676 . ? O7 Mn2 O6 85.61(7) . . ? O3 Mn2 O6 107.22(7) 2_676 . ? O1 Mn2 O4 95.80(6) . 2_676 ? O5 Mn2 O4 87.14(7) 2_676 2_676 ? O7 Mn2 O4 88.06(7) . 2_676 ? O3 Mn2 O4 80.53(6) 2_676 2_676 ? O6 Mn2 O4 170.19(6) . 2_676 ? C1 O1 Mn2 126.82(14) . . ? C1 O1 Mn1 116.04(13) . . ? Mn2 O1 Mn1 111.02(7) . . ? C3 O2 Mn1 115.07(14) . . ? C3 O2 H2H 107(3) . . ? Mn1 O2 H2H 114(3) . . ? C6 O3 Mn2 120.76(13) . 2_676 ? C6 O3 Mn1 115.70(12) . . ? Mn2 O3 Mn1 104.46(7) 2_676 . ? C6 O3 Mn1 114.83(12) . 2_676 ? Mn2 O3 Mn1 96.95(6) 2_676 2_676 ? Mn1 O3 Mn1 100.90(6) . 2_676 ? C12 O4 Mn1 133.35(14) . . ? C12 O4 Mn2 123.42(14) . 2_676 ? Mn1 O4 Mn2 97.59(6) . 2_676 ? C14 O5 Mn2 129.28(15) . 2_676 ? C21 O6 Mn2 115.54(15) . . ? C23 O7 Mn2 124.60(14) . . ? C1S O4S H4S 109.5 . . ? C5 N1 C2 112.02(19) . . ? C5 N1 C4 110.41(17) . . ? C2 N1 C4 110.43(17) . . ? C5 N1 Mn1 107.32(12) . . ? C2 N1 Mn1 106.52(13) . . ? C4 N1 Mn1 109.99(14) . . ? C11 N2 C7 116.9(2) . . ? C11 N2 Mn1 126.83(15) . . ? C7 N2 Mn1 114.51(15) . . ? C12 N3 C11 131.5(2) . . ? C12 N3 H3N 114.2 . . ? C11 N3 H3N 114.2 . . ? C20 N4 C16 117.8(2) . . ? C21 N5 C20 127.5(2) . . ? C21 N5 H5N 116.2 . . ? C20 N5 H5N 116.2 . . ? O3S N1S O1S 120.9(2) . . ? O3S N1S O2S 119.6(2) . . ? O1S N1S O2S 119.5(2) . . ? O1 C1 C2 109.02(17) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N1 C2 C1 109.50(19) . . ? N1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 109.72(19) . . ? O2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N1 C4 C3 110.30(18) . . ? N1 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N1 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N1 C5 C6 110.99(17) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O3 C6 C5 111.71(18) . . ? O3 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? O3 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 124.1(2) . . ? N2 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? C7 C8 C9 118.3(2) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 118.8(2) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 119.3(2) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 N3 121.0(2) . . ? N2 C11 C10 122.6(2) . . ? N3 C11 C10 116.4(2) . . ? O4 C12 N3 121.3(2) . . ? O4 C12 C13 124.3(2) . . ? N3 C12 C13 114.4(2) . . ? C14 C13 C12 125.1(2) . . ? C14 C13 H13 117.4 . . ? C12 C13 H13 117.4 . . ? O5 C14 C13 127.2(2) . . ? O5 C14 C15 113.6(2) . . ? C13 C14 C15 119.1(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 123.4(3) . . ? N4 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C16 C17 C18 118.4(2) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C19 119.4(2) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 118.3(2) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? N4 C20 C19 122.7(2) . . ? N4 C20 N5 113.7(2) . . ? C19 C20 N5 123.6(2) . . ? O6 C21 N5 120.3(2) . . ? O6 C21 C22 123.8(2) . . ? N5 C21 C22 115.9(2) . . ? C23 C22 C21 123.0(2) . . ? C23 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? O7 C23 C22 126.0(2) . . ? O7 C23 C24 113.5(2) . . ? C22 C23 C24 120.4(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4S C1S H1S1 109.5 . . ? O4S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O4S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? Cl1S C2S Cl2S 112.2(2) . . ? Cl1S C2S H2S1 109.2 . . ? Cl2S C2S H2S1 109.2 . . ? Cl1S C2S H2S2 109.2 . . ? Cl2S C2S H2S2 109.2 . . ? H2S1 C2S H2S2 107.9 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 30.63 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.595 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.136 # Attachment '- StuartLangleyamendedcif 6.txt' #========================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 768056' #TrackingRef '- StuartLangleyamendedcif 6.txt' #========================================================================== _publ_section_exptl_refinement ; The data was collected on the Australian synchrotron in which only a wavelength of 0.77 A and a resolution of ~0.9 A was possible. We were also restricted to only one 360 degree phi scan. The asymmetric unit consists of the cluster as well as acetate and nitrate counter ions with solvent DCM, MeOH and H2O molecules. Bond and thermal restarints are placed on the nitrate groups, with the water molecules thermal parameters restrained using the ISOR command. All non H-atoms were refined anisotropically. H-atoms were placed in calculated positions, except for the H-atoms on the protonated teaH2 ligands in which the majority could not be found. Four of these H-atoms however could be found and were refined freely. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C32 H68 Mn6 N4 O22, C2 H3 O2, C H4 O, C H2 Cl2, 2(N O3), 2(O H2) ; _chemical_formula_sum 'C36 H81 Cl2 Mn6 N6 O33' _chemical_formula_weight 1526.9 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 24.080(5) _cell_length_b 27.460(6) _cell_length_c 19.590(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12954(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10195 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 26.22 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6232 _exptl_absorpt_coefficient_mu 1.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8806 _exptl_absorpt_correction_T_max 0.9376 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77056 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 138066 _diffrn_reflns_av_R_equivalents 0.0921 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.22 _reflns_number_total 10195 _reflns_number_gt 9555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data was collected on the Australian synchrotron in which only a wavelength of 0.77 A and a resolution of ~0.9 A was possible. We were also restricted to only one 360 degree phi scan. The asymmetric unit consists of the cluster as well as acetate and nitrate counter ions with solvent DCM, MeOH and H2O molecules. Bond and thermal restarints are placed on the nitrate groups, with the water molecules thermal parameters restrained using the ISOR command. All non H-atoms were refined anisotropically. H-atoms were placed in calculated positions, except for the H-atoms on the protonated teaH2 ligands in which the majority could not be found. Four of these H-atoms however could be found and were refined freely. ; _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^)+(0.0847P)^2^+163.4371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10195 _refine_ls_number_parameters 790 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2297 _refine_ls_wR_factor_gt 0.2271 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.001 _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 0.15538(4) 0.13952(4) 0.98174(6) 0.0218(3) Uani 1 1 d . . . Mn2 Mn 0.29330(4) 0.19252(4) 0.98839(6) 0.0219(3) Uani 1 1 d . . . Mn3 Mn 0.19025(4) 0.23337(4) 1.06950(5) 0.0177(3) Uani 1 1 d . . . Mn4 Mn 0.18469(4) 0.24584(4) 0.92716(5) 0.0193(3) Uani 1 1 d . . . Mn5 Mn 0.08034(4) 0.28474(4) 1.01535(6) 0.0222(3) Uani 1 1 d . . . Mn6 Mn 0.21739(4) 0.34035(4) 1.01125(6) 0.0271(3) Uani 1 1 d . . . Cl1S Cl 0.52575(19) 0.48162(14) 1.0812(2) 0.1021(14) Uani 1 1 d . . . Cl2S Cl 0.45307(17) 0.42490(18) 1.1652(3) 0.1050(13) Uani 1 1 d . . . O1 O 0.0771(2) 0.1272(2) 1.0378(3) 0.0311(13) Uani 1 1 d D . . O1X O -0.0158(6) 0.0569(5) 1.2412(8) 0.054(4) Uani 0.50 1 d PU A -2 O2 O 0.1725(3) 0.0730(2) 0.9194(3) 0.0443(15) Uani 1 1 d . . . O2S O 0.3936(2) 0.3191(2) 1.0141(4) 0.0443(16) Uani 1 1 d . . . O2X O 0.3744(7) 0.0851(7) 1.1360(9) 0.159(6) Uani 1 1 d U . . H2X H 0.3569 0.0591 1.1422 0.190 Uiso 1 1 calc R . . O3 O 0.2231(2) 0.16138(19) 1.0488(3) 0.0284(12) Uani 1 1 d . . . O3S O 0.4795(3) 0.3394(3) 0.9902(6) 0.082(3) Uani 1 1 d . . . O3X O 0.4092(9) 0.4280(7) 0.7975(9) 0.087(5) Uani 0.50 1 d PU . . O4 O 0.1039(2) 0.15447(19) 0.8936(3) 0.0265(12) Uani 1 1 d . . . O4S O 0.1478(8) 0.0639(6) 0.7857(8) 0.160(6) Uani 1 1 d D . . O4X O 0.1983(11) 0.4591(9) 0.8547(11) 0.111(7) Uani 0.50 1 d PU . . O5 O 0.13036(19) 0.2285(2) 0.8561(3) 0.0272(12) Uani 1 1 d . . . O5S O 0.1734(11) 0.0172(8) 0.7008(8) 0.283(16) Uani 1 1 d D . . O5X O -0.0326(18) 0.4781(18) 1.260(3) 0.24(2) Uani 0.50 1 d PU B -1 O6 O 0.3469(3) 0.1291(3) 1.0190(4) 0.0424(16) Uani 1 1 d . . . O6S O 0.2217(6) 0.0294(6) 0.7942(8) 0.150 Uiso 1 1 d D . . O7 O 0.3550(2) 0.2433(2) 0.9450(3) 0.0347(14) Uani 1 1 d . . . O7S O 0.0000 0.3007(5) 1.2500 0.100(5) Uani 1 2 d S . . O8 O 0.22167(19) 0.1827(2) 0.9145(3) 0.0261(11) Uani 1 1 d . . . O8S O -0.0128(5) 0.3723(3) 1.3037(4) 0.084(3) Uani 1 1 d . . . O9 O 0.3231(2) 0.2201(2) 1.0853(3) 0.0308(13) Uani 1 1 d . . . O9S O 0.4456(10) 0.0041(9) 1.0815(11) 0.122(8) Uani 0.50 1 d PDU C -1 O10 O 0.2464(2) 0.2460(2) 1.1397(3) 0.0271(12) Uani 1 1 d . . . O10' O 0.5305(8) -0.0003(7) 1.0263(12) 0.080(4) Uani 0.50 1 d PD C -1 O10S O 0.4470(15) -0.001(2) 0.9693(12) 0.190(18) Uani 0.50 1 d PDU C -1 O11 O 0.14077(18) 0.22111(17) 0.9961(2) 0.0190(10) Uani 1 1 d . . . O12 O 0.23385(18) 0.25833(18) 0.9973(3) 0.0215(11) Uani 1 1 d . . . O13 O 0.13978(19) 0.20806(19) 1.1390(3) 0.0260(11) Uani 1 1 d . . . O14 O 0.05865(19) 0.23962(18) 1.1029(3) 0.0261(12) Uani 1 1 d . . . O15 O 0.2328(2) 0.2750(2) 0.8572(3) 0.0290(12) Uani 1 1 d . . . O16 O 0.2630(2) 0.3414(2) 0.9140(3) 0.0324(13) Uani 1 1 d . . . O17 O 0.2980(2) 0.3450(2) 1.0614(3) 0.0393(15) Uani 1 1 d . . . O18 O 0.1995(3) 0.4164(3) 0.9768(4) 0.060(2) Uani 1 1 d . . . O19 O 0.1554(2) 0.30491(19) 1.0781(3) 0.0284(12) Uani 1 1 d . . . O20 O 0.14769(19) 0.3089(2) 0.9408(3) 0.0301(13) Uani 1 1 d . . . O21 O 0.0157(2) 0.2431(2) 0.9618(3) 0.0368(14) Uani 1 1 d . . . O22 O 0.0285(2) 0.3399(2) 1.0726(3) 0.0365(14) Uani 1 1 d . . . N1 N 0.1685(3) 0.0716(2) 1.0580(4) 0.0337(16) Uani 1 1 d . . . N2 N 0.3316(2) 0.1564(3) 0.8853(4) 0.0355(17) Uani 1 1 d . . . N2S N 0.1733(7) 0.0265(7) 0.7649(8) 0.150 Uiso 1 1 d D . . N3 N 0.0365(2) 0.3387(3) 0.9332(4) 0.0327(16) Uani 1 1 d . . . N3S N 0.0000 0.3493(5) 1.2500 0.057(3) Uani 1 2 d S . . N4 N 0.2074(3) 0.3922(3) 1.1120(4) 0.0400(18) Uani 1 1 d . . . N4S N 0.4756(8) 0.0024(7) 1.0259(13) 0.080(4) Uani 0.50 1 d PDU C -1 C1 C 0.0690(3) 0.0852(3) 1.0793(5) 0.037(2) Uani 1 1 d . . . H1A H 0.0564 0.0574 1.0512 0.045 Uiso 1 1 calc R . . H1B H 0.0407 0.0917 1.1148 0.045 Uiso 1 1 calc R . . C1S C 0.5195(6) 0.4316(6) 1.1325(9) 0.096(5) Uani 1 1 d . . . H2S H 0.5461 0.4343 1.1707 0.116 Uiso 1 1 calc R . . H1S H 0.5292 0.4022 1.1059 0.116 Uiso 1 1 calc R . . C1X C 0.3772(16) 0.1123(14) 1.200(2) 0.232(15) Uani 1 1 d U . . H1X1 H 0.4143 0.1029 1.2178 0.348 Uiso 1 1 d . . . H1X2 H 0.3484 0.1015 1.2281 0.348 Uiso 1 1 d . . . H1X3 H 0.3763 0.1449 1.1857 0.348 Uiso 1 1 d . . . C2 C 0.1247(3) 0.0741(4) 1.1117(5) 0.042(2) Uani 1 1 d . . . H2A H 0.1341 0.0999 1.1451 0.050 Uiso 1 1 calc R . . H2B H 0.1227 0.0427 1.1363 0.050 Uiso 1 1 calc R . . C2S C 0.4294(3) 0.3490(3) 0.9933(6) 0.042(2) Uani 1 1 d . . . C3 C 0.1648(4) 0.0257(3) 1.0201(6) 0.048(3) Uani 1 1 d . . . H3A H 0.1253 0.0170 1.0134 0.058 Uiso 1 1 calc R . . H3B H 0.1826 -0.0006 1.0468 0.058 Uiso 1 1 calc R . . C3S C 0.4106(5) 0.3991(4) 0.9728(9) 0.085(5) Uani 1 1 d . . . H3S1 H 0.4326 0.4104 0.9338 0.128 Uiso 1 1 calc R . . H3S2 H 0.4156 0.4216 1.0112 0.128 Uiso 1 1 calc R . . H3S3 H 0.3713 0.3981 0.9600 0.128 Uiso 1 1 calc R . . C4 C 0.1924(4) 0.0298(3) 0.9526(6) 0.050(3) Uani 1 1 d . . . H4A H 0.2332 0.0317 0.9587 0.060 Uiso 1 1 calc R . . H4B H 0.1838 0.0008 0.9245 0.060 Uiso 1 1 calc R . . C5 C 0.2246(3) 0.0788(3) 1.0884(5) 0.035(2) Uani 1 1 d . . . H5A H 0.2533 0.0688 1.0551 0.043 Uiso 1 1 calc R . . H5B H 0.2285 0.0582 1.1295 0.043 Uiso 1 1 calc R . . C6 C 0.2334(3) 0.1309(3) 1.1074(4) 0.0321(19) Uani 1 1 d . . . H6A H 0.2079 0.1400 1.1449 0.039 Uiso 1 1 calc R . . H6B H 0.2720 0.1356 1.1235 0.039 Uiso 1 1 calc R . . C7 C 0.3586(3) 0.0931(3) 0.9688(6) 0.049(3) Uani 1 1 d . . . H7A H 0.3256 0.0723 0.9612 0.058 Uiso 1 1 calc R . . H7B H 0.3897 0.0722 0.9841 0.058 Uiso 1 1 calc R . . C8 C 0.3742(3) 0.1195(4) 0.9033(6) 0.047(2) Uani 1 1 d . . . H8A H 0.4106 0.1357 0.9093 0.056 Uiso 1 1 calc R . . H8B H 0.3777 0.0957 0.8657 0.056 Uiso 1 1 calc R . . C9 C 0.2845(3) 0.1331(4) 0.8496(5) 0.039(2) Uani 1 1 d . . . H9A H 0.2747 0.1024 0.8733 0.047 Uiso 1 1 calc R . . H9B H 0.2957 0.1248 0.8024 0.047 Uiso 1 1 calc R . . C10 C 0.2343(3) 0.1660(3) 0.8476(4) 0.0332(19) Uani 1 1 d . . . H10A H 0.2418 0.1941 0.8174 0.040 Uiso 1 1 calc R . . H10B H 0.2021 0.1480 0.8288 0.040 Uiso 1 1 calc R . . C11 C 0.3564(3) 0.1960(4) 0.8459(4) 0.040(2) Uani 1 1 d . . . H11A H 0.3265 0.2148 0.8231 0.047 Uiso 1 1 calc R . . H11B H 0.3806 0.1821 0.8099 0.047 Uiso 1 1 calc R . . C12 C 0.3901(3) 0.2298(4) 0.8903(4) 0.038(2) Uani 1 1 d . . . H12A H 0.4237 0.2130 0.9075 0.046 Uiso 1 1 calc R . . H12B H 0.4018 0.2589 0.8641 0.046 Uiso 1 1 calc R . . C13 C 0.1005(3) 0.1902(3) 0.8544(4) 0.0263(17) Uani 1 1 d . . . C14 C 0.0575(3) 0.1879(4) 0.7979(4) 0.039(2) Uani 1 1 d . . . H14A H 0.0707 0.1663 0.7615 0.058 Uiso 1 1 calc R . . H14B H 0.0515 0.2207 0.7793 0.058 Uiso 1 1 calc R . . H14C H 0.0224 0.1754 0.8162 0.058 Uiso 1 1 calc R . . C15 C 0.2987(3) 0.2387(3) 1.1349(4) 0.0288(18) Uani 1 1 d . . . C16 C 0.3327(3) 0.2542(4) 1.1958(5) 0.049(3) Uani 1 1 d . . . H16A H 0.3187 0.2380 1.2369 0.073 Uiso 1 1 calc R . . H16B H 0.3299 0.2896 1.2015 0.073 Uiso 1 1 calc R . . H16C H 0.3716 0.2452 1.1886 0.073 Uiso 1 1 calc R . . C17 C 0.0867(3) 0.2133(3) 1.1408(4) 0.0249(16) Uani 1 1 d . . . C18 C 0.0578(3) 0.1853(4) 1.1973(5) 0.042(2) Uani 1 1 d . . . H18A H 0.0535 0.2063 1.2374 0.063 Uiso 1 1 calc R . . H18B H 0.0801 0.1567 1.2095 0.063 Uiso 1 1 calc R . . H18C H 0.0211 0.1747 1.1814 0.063 Uiso 1 1 calc R . . C19 C 0.2624(3) 0.3142(3) 0.8644(4) 0.0313(19) Uani 1 1 d . . . C20 C 0.2980(4) 0.3267(4) 0.8029(5) 0.056(3) Uani 1 1 d . . . H20A H 0.2834 0.3561 0.7809 0.084 Uiso 1 1 calc R . . H20B H 0.2972 0.2996 0.7704 0.084 Uiso 1 1 calc R . . H20C H 0.3363 0.3325 0.8177 0.084 Uiso 1 1 calc R . . C21 C 0.3087(3) 0.3787(4) 1.1142(5) 0.045(2) Uani 1 1 d . . . H21A H 0.3183 0.4110 1.0949 0.054 Uiso 1 1 calc R . . H21B H 0.3400 0.3674 1.1429 0.054 Uiso 1 1 calc R . . C22 C 0.2554(3) 0.3819(4) 1.1562(5) 0.044(2) Uani 1 1 d . . . H22A H 0.2494 0.3508 1.1806 0.052 Uiso 1 1 calc R . . H22B H 0.2591 0.4081 1.1907 0.052 Uiso 1 1 calc R . . C23 C 0.1483(3) 0.3230(3) 1.1458(4) 0.0316(18) Uani 1 1 d . . . H23A H 0.1763 0.3083 1.1765 0.038 Uiso 1 1 calc R . . H23B H 0.1109 0.3143 1.1630 0.038 Uiso 1 1 calc R . . C24 C 0.1550(3) 0.3780(3) 1.1449(5) 0.038(2) Uani 1 1 d . . . H24A H 0.1235 0.3928 1.1199 0.045 Uiso 1 1 calc R . . H24B H 0.1544 0.3905 1.1923 0.045 Uiso 1 1 calc R . . C25 C 0.2063(4) 0.4442(3) 1.0910(6) 0.055(3) Uani 1 1 d . . . H25A H 0.2448 0.4565 1.0868 0.065 Uiso 1 1 calc R . . H25B H 0.1871 0.4637 1.1264 0.065 Uiso 1 1 calc R . . C26 C 0.1769(4) 0.4498(4) 1.0244(7) 0.060(3) Uani 1 1 d . . . H26A H 0.1368 0.4434 1.0305 0.072 Uiso 1 1 calc R . . H26B H 0.1815 0.4835 1.0073 0.072 Uiso 1 1 calc R . . C27 C 0.0813(3) 0.3678(3) 0.9002(5) 0.037(2) Uani 1 1 d . . . H27A H 0.0933 0.3940 0.9315 0.045 Uiso 1 1 calc R . . H27B H 0.0666 0.3832 0.8582 0.045 Uiso 1 1 calc R . . C28 C 0.1308(3) 0.3364(3) 0.8822(5) 0.037(2) Uani 1 1 d . . . H28A H 0.1209 0.3140 0.8445 0.044 Uiso 1 1 calc R . . H28B H 0.1619 0.3572 0.8666 0.044 Uiso 1 1 calc R . . C29 C 0.0074(3) 0.3080(3) 0.8830(5) 0.040(2) Uani 1 1 d . . . H29A H 0.0348 0.2942 0.8505 0.049 Uiso 1 1 calc R . . H29B H -0.0191 0.3282 0.8568 0.049 Uiso 1 1 calc R . . C30 C -0.0233(3) 0.2673(3) 0.9174(5) 0.0352(19) Uani 1 1 d . . . H30A H -0.0548 0.2803 0.9441 0.042 Uiso 1 1 calc R . . H30B H -0.0379 0.2442 0.8830 0.042 Uiso 1 1 calc R . . C31 C -0.0033(3) 0.3716(3) 0.9678(5) 0.040(2) Uani 1 1 d . . . H31A H -0.0398 0.3553 0.9721 0.047 Uiso 1 1 calc R . . H31B H -0.0083 0.4015 0.9402 0.047 Uiso 1 1 calc R . . C32 C 0.0183(3) 0.3848(3) 1.0374(5) 0.035(2) Uani 1 1 d . . . H32A H 0.0530 0.4039 1.0335 0.042 Uiso 1 1 calc R . . H32B H -0.0095 0.4045 1.0625 0.042 Uiso 1 1 calc R . . H18 H 0.324(4) 0.336(3) 1.047(5) 0.03(3) Uiso 1 1 d . . . H26 H 0.048(3) 0.135(4) 1.018(5) 0.06(3) Uiso 1 1 d D . . H38 H 0.367(4) 0.263(4) 0.965(5) 0.04(3) Uiso 1 1 d . . . H65 H 0.332(8) 0.114(7) 1.049(10) 0.15(8) 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 0.0102(5) 0.0260(6) 0.0294(6) 0.0046(5) -0.0035(4) 0.0003(4) Mn2 0.0066(5) 0.0331(6) 0.0260(6) 0.0053(5) -0.0005(4) 0.0015(4) Mn3 0.0068(5) 0.0262(6) 0.0202(5) 0.0069(4) 0.0010(4) -0.0018(4) Mn4 0.0061(5) 0.0304(6) 0.0213(6) 0.0094(5) 0.0001(4) 0.0007(4) Mn5 0.0075(5) 0.0240(6) 0.0352(7) 0.0088(5) 0.0032(4) 0.0006(4) Mn6 0.0123(5) 0.0291(6) 0.0398(7) 0.0099(5) 0.0051(5) -0.0050(4) Cl1S 0.115(3) 0.075(2) 0.116(3) 0.033(2) 0.038(3) 0.035(2) Cl2S 0.072(2) 0.119(3) 0.124(3) 0.007(3) 0.012(2) -0.014(2) O1 0.013(3) 0.031(3) 0.049(4) 0.014(3) -0.003(2) 0.002(2) O1X 0.070(8) 0.052(5) 0.038(6) -0.011(5) 0.023(6) 0.003(5) O2 0.040(3) 0.037(3) 0.056(4) -0.003(3) -0.001(3) 0.005(3) O2S 0.014(3) 0.040(3) 0.079(5) 0.003(3) 0.007(3) -0.005(3) O2X 0.136(9) 0.182(10) 0.158(9) 0.043(8) -0.002(7) 0.048(8) O3 0.015(2) 0.035(3) 0.035(3) 0.016(2) -0.007(2) -0.003(2) O3S 0.015(3) 0.045(4) 0.187(10) 0.041(5) 0.028(4) 0.004(3) O3X 0.118(10) 0.078(8) 0.064(8) -0.020(7) -0.004(8) -0.003(8) O4 0.015(2) 0.033(3) 0.031(3) 0.005(2) -0.004(2) -0.003(2) O4S 0.236(18) 0.130(11) 0.115(11) -0.038(9) 0.014(12) -0.003(12) O4X 0.139(11) 0.114(10) 0.080(9) 0.020(8) -0.018(8) -0.016(9) O5 0.011(2) 0.043(3) 0.028(3) 0.012(2) -0.002(2) 0.000(2) O5S 0.45(3) 0.26(2) 0.136(13) -0.125(15) 0.122(18) -0.25(2) O5X 0.25(2) 0.24(2) 0.24(2) -0.008(10) 0.004(10) 0.000(10) O6 0.028(3) 0.049(4) 0.051(4) 0.008(3) 0.000(3) 0.011(3) O7 0.019(3) 0.045(4) 0.039(3) -0.002(3) 0.011(3) -0.009(3) O7S 0.123(12) 0.061(8) 0.116(12) 0.000 0.006(10) 0.000 O8 0.012(2) 0.043(3) 0.023(3) -0.001(2) 0.002(2) 0.001(2) O8S 0.145(9) 0.052(4) 0.054(5) -0.006(4) 0.046(5) -0.006(5) O9 0.012(2) 0.048(3) 0.032(3) 0.005(3) -0.002(2) -0.002(2) O9S 0.124(11) 0.095(10) 0.147(12) 0.001(9) -0.007(9) 0.008(9) O10 0.012(2) 0.045(3) 0.025(3) 0.002(2) -0.001(2) -0.004(2) O10' 0.088(7) 0.032(4) 0.119(10) 0.015(7) 0.020(8) 0.001(6) O10S 0.18(2) 0.18(2) 0.21(2) 0.008(10) 0.002(10) -0.002(10) O11 0.007(2) 0.023(2) 0.027(3) 0.007(2) 0.0004(19) -0.0011(19) O12 0.004(2) 0.028(3) 0.032(3) 0.005(2) 0.0023(19) 0.0002(19) O13 0.011(2) 0.034(3) 0.033(3) 0.008(2) 0.004(2) -0.002(2) O14 0.012(2) 0.026(3) 0.041(3) 0.009(2) 0.005(2) 0.001(2) O15 0.014(2) 0.047(3) 0.026(3) 0.013(2) 0.005(2) 0.000(2) O16 0.017(3) 0.042(3) 0.039(3) 0.009(3) 0.002(2) -0.007(2) O17 0.012(3) 0.053(4) 0.052(4) -0.006(3) 0.005(3) -0.006(3) O18 0.055(4) 0.041(4) 0.084(6) 0.023(4) 0.020(4) 0.003(3) O19 0.019(3) 0.032(3) 0.034(3) 0.000(2) 0.007(2) -0.006(2) O20 0.010(2) 0.044(3) 0.036(3) 0.023(3) 0.003(2) 0.001(2) O21 0.013(3) 0.035(3) 0.063(4) 0.013(3) -0.013(3) -0.002(2) O22 0.024(3) 0.030(3) 0.055(4) 0.009(3) 0.012(3) 0.006(2) N1 0.017(3) 0.032(4) 0.052(4) 0.016(3) -0.003(3) 0.002(3) N2 0.009(3) 0.049(4) 0.049(4) -0.003(3) 0.004(3) 0.007(3) N3 0.011(3) 0.039(4) 0.048(4) 0.015(3) 0.004(3) 0.003(3) N3S 0.057(8) 0.055(8) 0.060(8) 0.000 0.017(7) 0.000 N4 0.022(3) 0.034(4) 0.064(5) -0.006(4) 0.012(3) -0.013(3) N4S 0.088(7) 0.032(4) 0.119(10) 0.015(7) 0.020(8) 0.001(6) C1 0.017(4) 0.040(5) 0.056(6) 0.021(4) 0.001(4) -0.003(3) C1S 0.085(10) 0.090(10) 0.115(12) 0.033(9) 0.031(9) 0.040(8) C1X 0.226(17) 0.238(18) 0.233(18) -0.006(10) -0.014(10) 0.005(10) C2 0.019(4) 0.054(5) 0.052(6) 0.030(5) 0.002(4) 0.001(4) C2S 0.016(4) 0.030(4) 0.082(7) 0.010(4) 0.009(4) 0.000(3) C3 0.030(5) 0.032(5) 0.082(7) 0.015(5) -0.013(5) 0.001(4) C3S 0.042(6) 0.050(7) 0.165(14) 0.049(8) 0.035(8) 0.016(5) C4 0.030(5) 0.034(5) 0.086(8) -0.008(5) -0.006(5) 0.009(4) C5 0.017(4) 0.042(5) 0.047(5) 0.022(4) -0.005(4) 0.004(3) C6 0.018(4) 0.046(5) 0.033(4) 0.021(4) -0.006(3) -0.002(3) C7 0.016(4) 0.040(5) 0.091(8) 0.005(5) -0.005(5) 0.005(4) C8 0.015(4) 0.056(6) 0.069(7) -0.012(5) 0.000(4) 0.011(4) C9 0.020(4) 0.058(6) 0.039(5) -0.017(4) 0.000(4) 0.005(4) C10 0.011(3) 0.057(5) 0.032(4) -0.007(4) 0.000(3) -0.001(3) C11 0.018(4) 0.068(6) 0.032(5) 0.004(4) 0.007(3) 0.000(4) C12 0.014(4) 0.062(6) 0.038(5) 0.003(4) 0.008(3) -0.002(4) C13 0.008(3) 0.049(5) 0.022(4) 0.000(4) 0.001(3) 0.000(3) C14 0.025(4) 0.058(6) 0.034(5) 0.011(4) -0.012(4) -0.009(4) C15 0.015(4) 0.045(5) 0.027(4) 0.009(4) -0.001(3) -0.007(3) C16 0.017(4) 0.094(8) 0.035(5) -0.014(5) -0.006(4) -0.004(4) C17 0.015(4) 0.029(4) 0.031(4) 0.002(3) 0.011(3) -0.003(3) C18 0.023(4) 0.060(6) 0.043(5) 0.020(5) 0.017(4) -0.002(4) C19 0.010(3) 0.056(5) 0.029(4) 0.019(4) 0.001(3) 0.001(3) C20 0.041(5) 0.081(8) 0.046(6) 0.026(5) 0.015(5) -0.021(5) C21 0.022(4) 0.048(5) 0.066(7) -0.009(5) 0.005(4) -0.015(4) C22 0.026(4) 0.055(6) 0.049(5) -0.011(5) 0.008(4) -0.011(4) C23 0.021(4) 0.038(4) 0.036(5) -0.006(4) 0.008(3) -0.010(3) C24 0.022(4) 0.036(5) 0.056(6) -0.007(4) 0.010(4) -0.007(3) C25 0.035(5) 0.033(5) 0.096(9) -0.006(5) 0.016(6) -0.014(4) C26 0.035(5) 0.031(5) 0.115(10) 0.018(6) 0.013(6) -0.006(4) C27 0.017(4) 0.040(5) 0.055(6) 0.025(4) 0.003(4) 0.004(3) C28 0.013(4) 0.050(5) 0.048(5) 0.026(4) 0.001(3) 0.003(3) C29 0.019(4) 0.051(5) 0.051(6) 0.019(4) -0.006(4) 0.001(4) C30 0.014(4) 0.046(5) 0.046(5) 0.005(4) -0.008(3) 0.004(3) C31 0.018(4) 0.033(4) 0.068(6) 0.018(4) 0.004(4) 0.009(3) C32 0.018(4) 0.024(4) 0.065(6) 0.012(4) 0.010(4) 0.003(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 O4 2.165(5) . ? Mn1 O3 2.178(5) . ? Mn1 O1 2.208(5) . ? Mn1 O2 2.235(6) . ? Mn1 O11 2.285(5) . ? Mn1 O8 2.385(5) . ? Mn1 N1 2.411(7) . ? Mn1 Mn4 3.1884(16) . ? Mn1 Mn3 3.2099(16) . ? Mn2 O9 2.167(6) . ? Mn2 O7 2.207(6) . ? Mn2 O3 2.234(5) . ? Mn2 O6 2.248(6) . ? Mn2 O8 2.268(5) . ? Mn2 O12 2.312(5) . ? Mn2 N2 2.432(7) . ? Mn2 Mn3 3.1530(15) . ? Mn2 Mn4 3.2284(15) . ? Mn3 O12 1.890(5) . ? Mn3 O11 1.897(5) . ? Mn3 O13 1.953(5) . ? Mn3 O10 1.959(5) . ? Mn3 O19 2.143(5) . ? Mn3 O3 2.167(6) . ? Mn3 Mn4 2.8127(16) . ? Mn3 Mn5 3.1813(15) . ? Mn3 Mn6 3.2186(16) . ? Mn4 O11 1.845(5) . ? Mn4 O12 1.846(5) . ? Mn4 O20 1.965(6) . ? Mn4 O15 1.965(5) . ? Mn4 O8 1.966(5) . ? Mn4 O5 1.969(5) . ? Mn4 Mn6 3.1732(17) . ? Mn4 Mn5 3.2312(15) . ? Mn5 O14 2.179(5) . ? Mn5 O21 2.199(6) . ? Mn5 O19 2.255(5) . ? Mn5 O22 2.259(6) . ? Mn5 O20 2.281(5) . ? Mn5 O11 2.305(5) . ? Mn5 N3 2.428(7) . ? Mn6 O17 2.179(6) . ? Mn6 O16 2.199(6) . ? Mn6 O19 2.211(5) . ? Mn6 O18 2.236(7) . ? Mn6 O12 2.303(5) . ? Mn6 O20 2.339(6) . ? Mn6 N4 2.446(8) . ? Cl1S C1S 1.708(14) . ? Cl2S C1S 1.732(14) . ? O1 C1 1.423(10) . ? O1 H26 0.819(10) . ? O2 C4 1.436(11) . ? O2S C2S 1.258(10) . ? O2X C1X 1.46(4) . ? O2X H2X 0.8400 . ? O3 C6 1.442(9) . ? O3S C2S 1.236(10) . ? O4 C13 1.248(9) . ? O4S N2S 1.264(9) . ? O5 C13 1.276(10) . ? O5S N2S 1.282(9) . ? O6 C7 1.423(13) . ? O6 H65 0.82(19) . ? O6S N2S 1.301(9) . ? O7 C12 1.416(10) . ? O7 H38 0.74(10) . ? O7S N3S 1.335(18) . ? O8 C10 1.422(9) . ? O8S N3S 1.265(10) . ? O9 C15 1.245(10) . ? O9S N4S 1.310(10) . ? O10 C15 1.279(9) . ? O10' N4S 1.323(10) . ? O10S N4S 1.308(10) . ? O13 C17 1.286(9) . ? O14 C17 1.237(9) . ? O15 C19 1.300(10) . ? O16 C19 1.225(11) . ? O17 C21 1.411(11) . ? O17 H18 0.73(10) . ? O18 C26 1.416(14) . ? O19 C23 1.428(10) . ? O20 C28 1.434(9) . ? O21 C30 1.442(9) . ? O22 C32 1.435(10) . ? N1 C3 1.465(13) . ? N1 C5 1.489(10) . ? N1 C2 1.491(11) . ? N2 C11 1.461(11) . ? N2 C9 1.479(11) . ? N2 C8 1.483(11) . ? N3 C29 1.472(12) . ? N3 C31 1.481(11) . ? N3 C27 1.491(10) . ? N3S O8S 1.265(10) 4_557 ? N4 C24 1.468(10) . ? N4 C22 1.472(12) . ? N4 C25 1.487(12) . ? C1 C2 1.515(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1S H2S 0.9900 . ? C1S H1S 0.9900 . ? C1X H1X1 0.9915 . ? C1X H1X2 0.9333 . ? C1X H1X3 0.9383 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2S C3S 1.504(13) . ? C3 C4 1.483(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.492(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.510(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.510(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.518(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.508(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.517(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.518(11) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.528(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.519(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.492(17) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.513(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.499(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.504(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? 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 O3 149.04(19) . . ? O4 Mn1 O1 86.4(2) . . ? O3 Mn1 O1 112.4(2) . . ? O4 Mn1 O2 79.9(2) . . ? O3 Mn1 O2 114.6(2) . . ? O1 Mn1 O2 107.7(2) . . ? O4 Mn1 O11 79.87(19) . . ? O3 Mn1 O11 76.74(18) . . ? O1 Mn1 O11 87.58(19) . . ? O2 Mn1 O11 153.7(2) . . ? O4 Mn1 O8 81.30(18) . . ? O3 Mn1 O8 72.26(18) . . ? O1 Mn1 O8 157.31(19) . . ? O2 Mn1 O8 88.9(2) . . ? O11 Mn1 O8 71.57(17) . . ? O4 Mn1 N1 135.7(2) . . ? O3 Mn1 N1 75.0(2) . . ? O1 Mn1 N1 71.6(2) . . ? O2 Mn1 N1 71.5(3) . . ? O11 Mn1 N1 134.6(2) . . ? O8 Mn1 N1 129.7(2) . . ? O4 Mn1 Mn4 71.69(14) . . ? O3 Mn1 Mn4 77.54(14) . . ? O1 Mn1 Mn4 119.77(15) . . ? O2 Mn1 Mn4 121.58(18) . . ? O11 Mn1 Mn4 34.68(12) . . ? O8 Mn1 Mn4 37.96(13) . . ? N1 Mn1 Mn4 152.55(17) . . ? O4 Mn1 Mn3 115.13(15) . . ? O3 Mn1 Mn3 42.25(14) . . ? O1 Mn1 Mn3 94.59(16) . . ? O2 Mn1 Mn3 154.18(17) . . ? O11 Mn1 Mn3 35.62(12) . . ? O8 Mn1 Mn3 73.85(13) . . ? N1 Mn1 Mn3 104.77(19) . . ? Mn4 Mn1 Mn3 52.16(3) . . ? O9 Mn2 O7 83.9(2) . . ? O9 Mn2 O3 85.4(2) . . ? O7 Mn2 O3 162.7(2) . . ? O9 Mn2 O6 81.2(2) . . ? O7 Mn2 O6 101.9(2) . . ? O3 Mn2 O6 89.8(2) . . ? O9 Mn2 O8 148.55(19) . . ? O7 Mn2 O8 110.0(2) . . ? O3 Mn2 O8 73.54(18) . . ? O6 Mn2 O8 120.9(2) . . ? O9 Mn2 O12 82.3(2) . . ? O7 Mn2 O12 87.3(2) . . ? O3 Mn2 O12 77.90(18) . . ? O6 Mn2 O12 160.1(2) . . ? O8 Mn2 O12 70.76(18) . . ? O9 Mn2 N2 138.1(2) . . ? O7 Mn2 N2 71.5(2) . . ? O3 Mn2 N2 124.8(2) . . ? O6 Mn2 N2 71.8(3) . . ? O8 Mn2 N2 73.1(2) . . ? O12 Mn2 N2 128.1(2) . . ? O9 Mn2 Mn3 72.23(14) . . ? O7 Mn2 Mn3 119.92(18) . . ? O3 Mn2 Mn3 43.41(14) . . ? O6 Mn2 Mn3 126.36(19) . . ? O8 Mn2 Mn3 76.44(13) . . ? O12 Mn2 Mn3 36.53(12) . . ? N2 Mn2 Mn3 149.59(16) . . ? O9 Mn2 Mn4 115.83(15) . . ? O7 Mn2 Mn4 96.64(17) . . ? O3 Mn2 Mn4 75.95(13) . . ? O6 Mn2 Mn4 156.20(19) . . ? O8 Mn2 Mn4 36.95(14) . . ? O12 Mn2 Mn4 34.11(13) . . ? N2 Mn2 Mn4 100.60(16) . . ? Mn3 Mn2 Mn4 52.29(3) . . ? O12 Mn3 O11 81.1(2) . . ? O12 Mn3 O13 175.2(2) . . ? O11 Mn3 O13 94.3(2) . . ? O12 Mn3 O10 94.4(2) . . ? O11 Mn3 O10 175.2(2) . . ? O13 Mn3 O10 90.2(2) . . ? O12 Mn3 O19 86.8(2) . . ? O11 Mn3 O19 88.6(2) . . ? O13 Mn3 O19 91.6(2) . . ? O10 Mn3 O19 93.1(2) . . ? O12 Mn3 O3 89.3(2) . . ? O11 Mn3 O3 85.7(2) . . ? O13 Mn3 O3 91.9(2) . . ? O10 Mn3 O3 92.3(2) . . ? O19 Mn3 O3 173.6(2) . . ? O12 Mn3 Mn4 40.57(15) . . ? O11 Mn3 Mn4 40.58(14) . . ? O13 Mn3 Mn4 134.82(16) . . ? O10 Mn3 Mn4 134.98(15) . . ? O19 Mn3 Mn4 86.98(15) . . ? O3 Mn3 Mn4 86.72(15) . . ? O12 Mn3 Mn2 46.75(15) . . ? O11 Mn3 Mn2 92.82(15) . . ? O13 Mn3 Mn2 135.60(16) . . ? O10 Mn3 Mn2 82.70(15) . . ? O19 Mn3 Mn2 132.36(14) . . ? O3 Mn3 Mn2 45.10(14) . . ? Mn4 Mn3 Mn2 65.23(4) . . ? O12 Mn3 Mn5 92.97(14) . . ? O11 Mn3 Mn5 45.86(15) . . ? O13 Mn3 Mn5 82.68(15) . . ? O10 Mn3 Mn5 136.90(17) . . ? O19 Mn3 Mn5 45.08(14) . . ? O3 Mn3 Mn5 130.19(14) . . ? Mn4 Mn3 Mn5 64.90(4) . . ? Mn2 Mn3 Mn5 130.13(5) . . ? O12 Mn3 Mn1 92.04(16) . . ? O11 Mn3 Mn1 44.55(15) . . ? O13 Mn3 Mn1 85.69(16) . . ? O10 Mn3 Mn1 134.26(17) . . ? O19 Mn3 Mn1 132.51(15) . . ? O3 Mn3 Mn1 42.50(14) . . ? Mn4 Mn3 Mn1 63.53(4) . . ? Mn2 Mn3 Mn1 69.53(4) . . ? Mn5 Mn3 Mn1 87.69(4) . . ? O12 Mn3 Mn6 44.84(15) . . ? O11 Mn3 Mn6 91.19(15) . . ? O13 Mn3 Mn6 134.30(16) . . ? O10 Mn3 Mn6 87.00(16) . . ? O19 Mn3 Mn6 43.14(14) . . ? O3 Mn3 Mn6 133.80(14) . . ? Mn4 Mn3 Mn6 63.07(4) . . ? Mn2 Mn3 Mn6 89.22(4) . . ? Mn5 Mn3 Mn6 69.27(4) . . ? Mn1 Mn3 Mn6 126.59(5) . . ? O11 Mn4 O12 83.7(2) . . ? O11 Mn4 O20 88.0(2) . . ? O12 Mn4 O20 91.5(2) . . ? O11 Mn4 O15 176.9(2) . . ? O12 Mn4 O15 93.8(2) . . ? O20 Mn4 O15 90.2(2) . . ? O11 Mn4 O8 91.6(2) . . ? O12 Mn4 O8 88.1(2) . . ? O20 Mn4 O8 179.4(2) . . ? O15 Mn4 O8 90.2(2) . . ? O11 Mn4 O5 92.7(2) . . ? O12 Mn4 O5 175.9(2) . . ? O20 Mn4 O5 90.4(2) . . ? O15 Mn4 O5 89.8(2) . . ? O8 Mn4 O5 89.9(2) . . ? O11 Mn4 Mn3 41.99(15) . . ? O12 Mn4 Mn3 41.75(15) . . ? O20 Mn4 Mn3 89.66(16) . . ? O15 Mn4 Mn3 135.48(16) . . ? O8 Mn4 Mn3 89.78(15) . . ? O5 Mn4 Mn3 134.70(15) . . ? O11 Mn4 Mn6 93.62(16) . . ? O12 Mn4 Mn6 45.77(15) . . ? O20 Mn4 Mn6 47.28(16) . . ? O15 Mn4 Mn6 83.27(18) . . ? O8 Mn4 Mn6 132.45(15) . . ? O5 Mn4 Mn6 136.83(16) . . ? Mn3 Mn4 Mn6 64.73(4) . . ? O11 Mn4 Mn1 44.81(15) . . ? O12 Mn4 Mn1 93.58(16) . . ? O20 Mn4 Mn1 131.34(15) . . ? O15 Mn4 Mn1 137.50(17) . . ? O8 Mn4 Mn1 48.28(15) . . ? O5 Mn4 Mn1 82.48(16) . . ? Mn3 Mn4 Mn1 64.32(4) . . ? Mn6 Mn4 Mn1 129.03(5) . . ? O11 Mn4 Mn2 91.46(15) . . ? O12 Mn4 Mn2 44.62(15) . . ? O20 Mn4 Mn2 135.76(17) . . ? O15 Mn4 Mn2 88.06(15) . . ? O8 Mn4 Mn2 43.92(15) . . ? O5 Mn4 Mn2 133.77(17) . . ? Mn3 Mn4 Mn2 62.48(3) . . ? Mn6 Mn4 Mn2 88.69(4) . . ? Mn1 Mn4 Mn2 68.86(3) . . ? O11 Mn4 Mn5 44.31(15) . . ? O12 Mn4 Mn5 92.24(15) . . ? O20 Mn4 Mn5 44.23(14) . . ? O15 Mn4 Mn5 134.18(17) . . ? O8 Mn4 Mn5 135.36(15) . . ? O5 Mn4 Mn5 86.62(15) . . ? Mn3 Mn4 Mn5 63.07(4) . . ? Mn6 Mn4 Mn5 69.20(4) . . ? Mn1 Mn4 Mn5 87.20(4) . . ? Mn2 Mn4 Mn5 125.54(4) . . ? O14 Mn5 O21 84.8(2) . . ? O14 Mn5 O19 84.44(19) . . ? O21 Mn5 O19 162.8(2) . . ? O14 Mn5 O22 81.8(2) . . ? O21 Mn5 O22 101.2(2) . . ? O19 Mn5 O22 90.5(2) . . ? O14 Mn5 O20 147.08(18) . . ? O21 Mn5 O20 110.5(2) . . ? O19 Mn5 O20 72.99(19) . . ? O22 Mn5 O20 121.1(2) . . ? O14 Mn5 O11 81.32(17) . . ? O21 Mn5 O11 88.54(19) . . ? O19 Mn5 O11 76.65(18) . . ? O22 Mn5 O11 159.7(2) . . ? O20 Mn5 O11 70.51(18) . . ? O14 Mn5 N3 139.8(2) . . ? O21 Mn5 N3 72.2(2) . . ? O19 Mn5 N3 124.0(2) . . ? O22 Mn5 N3 71.3(2) . . ? O20 Mn5 N3 73.01(19) . . ? O11 Mn5 N3 128.9(2) . . ? O14 Mn5 Mn3 71.63(13) . . ? O21 Mn5 Mn3 121.15(15) . . ? O19 Mn5 Mn3 42.28(14) . . ? O22 Mn5 Mn3 126.24(17) . . ? O20 Mn5 Mn3 75.56(13) . . ? O11 Mn5 Mn3 36.21(12) . . ? N3 Mn5 Mn3 148.55(15) . . ? O14 Mn5 Mn4 114.79(13) . . ? O21 Mn5 Mn4 97.11(17) . . ? O19 Mn5 Mn4 75.46(14) . . ? O22 Mn5 Mn4 156.39(15) . . ? O20 Mn5 Mn4 36.93(14) . . ? O11 Mn5 Mn4 34.00(11) . . ? N3 Mn5 Mn4 100.69(16) . . ? Mn3 Mn5 Mn4 52.03(3) . . ? O17 Mn6 O16 86.8(2) . . ? O17 Mn6 O19 111.1(2) . . ? O16 Mn6 O19 148.8(2) . . ? O17 Mn6 O18 104.6(3) . . ? O16 Mn6 O18 79.8(3) . . ? O19 Mn6 O18 117.4(2) . . ? O17 Mn6 O12 87.6(2) . . ? O16 Mn6 O12 79.9(2) . . ? O19 Mn6 O12 75.87(18) . . ? O18 Mn6 O12 155.6(3) . . ? O17 Mn6 O20 158.0(2) . . ? O16 Mn6 O20 81.49(19) . . ? O19 Mn6 O20 72.68(19) . . ? O18 Mn6 O20 91.7(3) . . ? O12 Mn6 O20 72.06(18) . . ? O17 Mn6 N4 71.9(3) . . ? O16 Mn6 N4 137.8(2) . . ? O19 Mn6 N4 73.2(2) . . ? O18 Mn6 N4 71.4(3) . . ? O12 Mn6 N4 133.0(2) . . ? O20 Mn6 N4 128.4(2) . . ? O17 Mn6 Mn4 120.21(19) . . ? O16 Mn6 Mn4 71.62(15) . . ? O19 Mn6 Mn4 77.28(14) . . ? O18 Mn6 Mn4 124.0(2) . . ? O12 Mn6 Mn4 35.05(12) . . ? O20 Mn6 Mn4 38.11(14) . . ? N4 Mn6 Mn4 150.52(16) . . ? O17 Mn6 Mn3 94.29(18) . . ? O16 Mn6 Mn3 114.85(16) . . ? O19 Mn6 Mn3 41.51(14) . . ? O18 Mn6 Mn3 156.95(19) . . ? O12 Mn6 Mn3 35.35(12) . . ? O20 Mn6 Mn3 74.10(13) . . ? N4 Mn6 Mn3 102.99(18) . . ? Mn4 Mn6 Mn3 52.21(3) . . ? C1 O1 Mn1 121.7(5) . . ? C1 O1 H26 112(8) . . ? Mn1 O1 H26 116(8) . . ? C4 O2 Mn1 119.2(6) . . ? C1X O2X H2X 109.5 . . ? C6 O3 Mn3 116.3(5) . . ? C6 O3 Mn1 116.7(4) . . ? Mn3 O3 Mn1 95.25(19) . . ? C6 O3 Mn2 120.9(4) . . ? Mn3 O3 Mn2 91.49(19) . . ? Mn1 O3 Mn2 110.6(2) . . ? C13 O4 Mn1 132.6(5) . . ? C13 O5 Mn4 126.3(5) . . ? C7 O6 Mn2 118.0(6) . . ? C7 O6 H65 103(10) . . ? Mn2 O6 H65 111(10) . . ? C12 O7 Mn2 121.9(6) . . ? C12 O7 H38 110(8) . . ? Mn2 O7 H38 123(8) . . ? C10 O8 Mn4 119.9(5) . . ? C10 O8 Mn2 117.7(4) . . ? Mn4 O8 Mn2 99.1(2) . . ? C10 O8 Mn1 119.5(5) . . ? Mn4 O8 Mn1 93.76(19) . . ? Mn2 O8 Mn1 102.5(2) . . ? C15 O9 Mn2 132.1(5) . . ? C15 O10 Mn3 127.0(5) . . ? Mn4 O11 Mn3 97.4(2) . . ? Mn4 O11 Mn1 100.5(2) . . ? Mn3 O11 Mn1 99.8(2) . . ? Mn4 O11 Mn5 101.7(2) . . ? Mn3 O11 Mn5 97.9(2) . . ? Mn1 O11 Mn5 149.4(2) . . ? Mn4 O12 Mn3 97.7(2) . . ? Mn4 O12 Mn6 99.2(2) . . ? Mn3 O12 Mn6 99.8(2) . . ? Mn4 O12 Mn2 101.3(2) . . ? Mn3 O12 Mn2 96.7(2) . . ? Mn6 O12 Mn2 151.6(2) . . ? C17 O13 Mn3 126.7(5) . . ? C17 O14 Mn5 132.3(4) . . ? C19 O15 Mn4 125.8(5) . . ? C19 O16 Mn6 132.3(5) . . ? C21 O17 Mn6 122.2(6) . . ? C21 O17 H18 111(7) . . ? Mn6 O17 H18 124(7) . . ? C26 O18 Mn6 118.7(6) . . ? C23 O19 Mn3 116.1(5) . . ? C23 O19 Mn6 118.6(4) . . ? Mn3 O19 Mn6 95.3(2) . . ? C23 O19 Mn5 119.7(4) . . ? Mn3 O19 Mn5 92.6(2) . . ? Mn6 O19 Mn5 109.1(2) . . ? C28 O20 Mn4 118.9(5) . . ? C28 O20 Mn5 117.7(4) . . ? Mn4 O20 Mn5 98.8(2) . . ? C28 O20 Mn6 118.8(5) . . ? Mn4 O20 Mn6 94.62(19) . . ? Mn5 O20 Mn6 103.9(2) . . ? C30 O21 Mn5 120.5(5) . . ? C32 O22 Mn5 115.7(5) . . ? C3 N1 C5 111.9(7) . . ? C3 N1 C2 110.8(7) . . ? C5 N1 C2 110.7(7) . . ? C3 N1 Mn1 110.0(6) . . ? C5 N1 Mn1 105.2(5) . . ? C2 N1 Mn1 108.0(5) . . ? C11 N2 C9 112.7(7) . . ? C11 N2 C8 110.7(6) . . ? C9 N2 C8 110.3(7) . . ? C11 N2 Mn2 106.9(5) . . ? C9 N2 Mn2 106.1(5) . . ? C8 N2 Mn2 110.0(6) . . ? O4S N2S O5S 118.5(19) . . ? O4S N2S O6S 104.1(17) . . ? O5S N2S O6S 116(2) . . ? C29 N3 C31 110.3(6) . . ? C29 N3 C27 111.1(7) . . ? C31 N3 C27 109.8(7) . . ? C29 N3 Mn5 107.5(5) . . ? C31 N3 Mn5 110.5(5) . . ? C27 N3 Mn5 107.5(4) . . ? O8S N3S O8S 120.0(13) . 4_557 ? O8S N3S O7S 120.0(6) . . ? O8S N3S O7S 120.0(6) 4_557 . ? C24 N4 C22 111.5(7) . . ? C24 N4 C25 111.1(7) . . ? C22 N4 C25 111.1(7) . . ? C24 N4 Mn6 106.5(5) . . ? C22 N4 Mn6 106.6(5) . . ? C25 N4 Mn6 109.7(6) . . ? O10S N4S O9S 114.6(12) . . ? O10S N4S O10' 122(3) . . ? O9S N4S O10' 123(3) . . ? O1 C1 C2 106.3(6) . . ? O1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? Cl1S C1S Cl2S 112.6(8) . . ? Cl1S C1S H2S 109.1 . . ? Cl2S C1S H2S 109.1 . . ? Cl1S C1S H1S 109.1 . . ? Cl2S C1S H1S 109.1 . . ? H2S C1S H1S 107.8 . . ? O2X C1X H1X1 102.1 . . ? O2X C1X H1X2 108.0 . . ? H1X1 C1X H1X2 112.4 . . ? O2X C1X H1X3 103.0 . . ? H1X1 C1X H1X3 112.0 . . ? H1X2 C1X H1X3 117.5 . . ? N1 C2 C1 109.9(7) . . ? N1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O3S C2S O2S 123.0(8) . . ? O3S C2S C3S 118.4(8) . . ? O2S C2S C3S 118.5(8) . . ? N1 C3 C4 111.1(8) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? O2 C4 C3 108.5(7) . . ? O2 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O2 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N1 C5 C6 110.9(6) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? O3 C6 C5 109.4(7) . . ? O3 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O3 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? O6 C7 C8 107.4(8) . . ? O6 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O6 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N2 C8 C7 110.9(7) . . ? N2 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C10 111.6(7) . . ? N2 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N2 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O8 C10 C9 109.9(7) . . ? O8 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O8 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 111.9(7) . . ? N2 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N2 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? O7 C12 C11 106.0(6) . . ? O7 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? O7 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? O4 C13 O5 126.6(7) . . ? O4 C13 C14 117.5(7) . . ? O5 C13 C14 115.9(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O9 C15 O10 125.8(7) . . ? O9 C15 C16 118.5(7) . . ? O10 C15 C16 115.7(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O14 C17 O13 126.3(7) . . ? O14 C17 C18 118.9(6) . . ? O13 C17 C18 114.7(7) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O16 C19 O15 126.7(7) . . ? O16 C19 C20 119.0(8) . . ? O15 C19 C20 114.2(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O17 C21 C22 106.2(7) . . ? O17 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O17 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? N4 C22 C21 110.7(8) . . ? N4 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? O19 C23 C24 108.8(7) . . ? O19 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O19 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N4 C24 C23 111.1(7) . . ? N4 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? N4 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N4 C25 C26 110.5(8) . . ? N4 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N4 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O18 C26 C25 109.1(8) . . ? O18 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O18 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? N3 C27 C28 111.5(7) . . ? N3 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? N3 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? O20 C28 C27 109.7(7) . . ? O20 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? O20 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? N3 C29 C30 111.2(7) . . ? N3 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? N3 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O21 C30 C29 107.1(6) . . ? O21 C30 H30A 110.3 . . ? C29 C30 H30A 110.3 . . ? O21 C30 H30B 110.3 . . ? C29 C30 H30B 110.3 . . ? H30A C30 H30B 108.5 . . ? N3 C31 C32 109.8(7) . . ? N3 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? N3 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O22 C32 C31 106.7(7) . . ? O22 C32 H32A 110.4 . . ? C31 C32 H32A 110.4 . . ? O22 C32 H32B 110.4 . . ? C31 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.307 _refine_diff_density_min -1.650 _refine_diff_density_rms 0.158