# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_dw1177 _database_code_depnum_ccdc_archive 'CCDC 892665' #TrackingRef '- compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H23 N6 V2 1-, C16 H32 Li O4 1+' _chemical_formula_sum 'C39 H55 Li N6 O4 V2' _chemical_formula_weight 780.71 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' V V 0.3005 0.5294 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.30410(10) _cell_length_b 20.2762(3) _cell_length_c 13.8669(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.35(3) _cell_angle_gamma 90.00 _cell_volume 3920(1) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 22164 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 34260 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 29.98 _reflns_number_total 11221 _reflns_number_gt 7794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Several restraints were also employed, simu 0.01 0.01 3.8 c26 c27 c25 c24 o1 simu 0.01 0.01 3.8 c35 o3 c34 c33 c32 DFIX 31.000 N1 H1N N2 H2N N5 H5N N6 H6N. ; _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^)+(0.1190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11221 _refine_ls_number_parameters 483 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.085 _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 V1 V 0.34034(2) 0.587088(16) 0.29182(2) 0.02420(11) Uani 1 1 d . . . V2 V 0.50876(2) 0.585068(16) 0.39354(2) 0.02422(11) Uani 1 1 d . . . N1 N 0.41666(11) 0.49999(9) 0.34395(12) 0.0268(3) Uani 1 1 d D . . H1N H 0.4106(17) 0.4720(11) 0.3878(17) 0.031(3) Uiso 1 1 d D . . N2 N 0.43867(13) 0.57678(9) 0.22373(13) 0.0275(4) Uani 1 1 d D . . H2N H 0.4448(16) 0.6069(11) 0.1820(17) 0.031(3) Uiso 1 1 d D . . N3 N 0.62456(12) 0.53245(9) 0.40844(13) 0.0304(4) Uani 1 1 d . . . H3N H 0.6188 0.4967 0.3703 0.036 Uiso 1 1 calc R . . N4 N 0.61548(12) 0.63179(9) 0.50924(13) 0.0325(4) Uani 1 1 d . . . H4N H 0.6036 0.6654 0.5421 0.039 Uiso 1 1 calc R . . N5 N 0.42434(12) 0.67314(9) 0.33829(12) 0.0277(4) Uani 1 1 d D . . H5N H 0.4290(17) 0.6982(11) 0.2923(17) 0.031(3) Uiso 1 1 d D . . N6 N 0.40474(13) 0.59483(8) 0.45744(13) 0.0270(3) Uani 1 1 d D . . H6N H 0.4000(16) 0.5651(11) 0.4996(17) 0.031(3) Uiso 1 1 d D . . C1 C 0.18890(16) 0.59855(13) 0.28948(19) 0.0422(6) Uani 1 1 d . . . H1 H 0.1742 0.6060 0.3525 0.051 Uiso 1 1 calc R . . C2 C 0.19361(16) 0.53671(12) 0.24489(18) 0.0388(5) Uani 1 1 d . . . H2 H 0.1822 0.4928 0.2705 0.047 Uiso 1 1 calc R . . C3 C 0.20761(16) 0.54824(12) 0.15244(17) 0.0377(5) Uani 1 1 d . . . H3 H 0.2075 0.5139 0.1007 0.045 Uiso 1 1 calc R . . C4 C 0.21116(16) 0.61659(13) 0.13928(18) 0.0409(5) Uani 1 1 d . . . H4 H 0.2144 0.6392 0.0768 0.049 Uiso 1 1 calc R . . C5 C 0.19977(16) 0.64772(13) 0.2239(2) 0.0447(6) Uani 1 1 d . . . H5 H 0.1942 0.6963 0.2323 0.054 Uiso 1 1 calc R . . C6 C 0.43121(13) 0.46655(10) 0.26380(14) 0.0265(4) Uani 1 1 d . . . C7 C 0.43651(15) 0.39970(11) 0.24975(17) 0.0323(4) Uani 1 1 d . . . H7 H 0.4282 0.3694 0.2976 0.039 Uiso 1 1 calc R . . C8 C 0.45440(16) 0.37666(12) 0.16371(18) 0.0374(5) Uani 1 1 d . . . H8 H 0.4583 0.3306 0.1535 0.045 Uiso 1 1 calc R . . C9 C 0.46623(17) 0.42057(11) 0.09463(18) 0.0372(5) Uani 1 1 d . . . H9 H 0.4783 0.4044 0.0369 0.045 Uiso 1 1 calc R . . C10 C 0.46089(16) 0.48854(12) 0.10765(16) 0.0345(5) Uani 1 1 d . . . H10 H 0.4687 0.5185 0.0591 0.041 Uiso 1 1 calc R . . C11 C 0.44397(13) 0.51178(10) 0.19287(14) 0.0263(4) Uani 1 1 d . . . C12 C 0.71286(14) 0.55338(11) 0.47932(15) 0.0307(4) Uani 1 1 d . . . C13 C 0.80237(16) 0.52557(12) 0.49997(18) 0.0393(5) Uani 1 1 d . . . H13 H 0.8059 0.4865 0.4639 0.047 Uiso 1 1 calc R . . C14 C 0.88605(16) 0.55409(14) 0.5722(2) 0.0450(6) Uani 1 1 d . . . H14 H 0.9464 0.5349 0.5846 0.054 Uiso 1 1 calc R . . C15 C 0.88190(17) 0.61061(14) 0.62654(19) 0.0454(6) Uani 1 1 d . . . H15 H 0.9393 0.6305 0.6753 0.054 Uiso 1 1 calc R . . C16 C 0.79309(16) 0.63815(13) 0.60923(18) 0.0417(5) Uani 1 1 d . . . H16 H 0.7906 0.6764 0.6476 0.050 Uiso 1 1 calc R . . C17 C 0.70792(15) 0.61043(11) 0.53658(15) 0.0318(4) Uani 1 1 d . . . C18 C 0.40259(14) 0.70540(10) 0.41486(15) 0.0280(4) Uani 1 1 d . . . C19 C 0.38758(16) 0.77178(11) 0.42464(17) 0.0359(5) Uani 1 1 d . . . H19 H 0.3953 0.8030 0.3776 0.043 Uiso 1 1 calc R . . C20 C 0.36060(17) 0.79249(12) 0.50558(19) 0.0409(5) Uani 1 1 d . . . H20 H 0.3505 0.8380 0.5134 0.049 Uiso 1 1 calc R . . C21 C 0.34880(15) 0.74744(12) 0.57327(17) 0.0382(5) Uani 1 1 d . . . H21 H 0.3296 0.7622 0.6266 0.046 Uiso 1 1 calc R . . C22 C 0.36470(15) 0.68033(12) 0.56467(16) 0.0338(5) Uani 1 1 d . . . H22 H 0.3580 0.6497 0.6129 0.041 Uiso 1 1 calc R . . C23 C 0.39051(14) 0.65875(10) 0.48472(15) 0.0284(4) Uani 1 1 d . . . Li1 Li 0.8650(3) 0.6185(2) 0.2091(3) 0.0478(10) Uani 1 1 d . . . O1 O 0.76684(13) 0.67225(10) 0.22253(13) 0.0478(4) Uani 1 1 d U . . C24 C 0.7634(2) 0.68066(14) 0.3243(2) 0.0478(6) Uani 1 1 d U . . H24A H 0.8165 0.7094 0.3705 0.057 Uiso 1 1 calc R . . H24B H 0.7690 0.6375 0.3597 0.057 Uiso 1 1 calc R . . C25 C 0.6694(2) 0.71155(19) 0.3034(3) 0.0689(8) Uani 1 1 d U . . H25A H 0.6384 0.6893 0.3446 0.083 Uiso 1 1 calc R . . H25B H 0.6776 0.7589 0.3227 0.083 Uiso 1 1 calc R . . C26 C 0.6137(3) 0.7037(3) 0.1933(3) 0.1092(14) Uani 1 1 d U . . H26A H 0.5774 0.7447 0.1639 0.131 Uiso 1 1 calc R . . H26B H 0.5671 0.6674 0.1813 0.131 Uiso 1 1 calc R . . C27 C 0.6749(2) 0.68909(16) 0.1406(2) 0.0573(7) Uani 1 1 d U . . H27A H 0.6806 0.7279 0.1002 0.069 Uiso 1 1 calc R . . H27B H 0.6488 0.6517 0.0910 0.069 Uiso 1 1 calc R . . O2 O 0.82876(14) 0.52765(10) 0.21502(16) 0.0575(5) Uani 1 1 d . . . C28 C 0.7351(2) 0.50872(16) 0.2051(3) 0.0623(8) Uani 1 1 d . . . H28A H 0.6856 0.5230 0.1358 0.075 Uiso 1 1 calc R . . H28B H 0.7210 0.5291 0.2620 0.075 Uiso 1 1 calc R . . C29 C 0.7365(3) 0.4340(2) 0.2141(4) 0.0911(12) Uani 1 1 d . . . H29A H 0.7325 0.4203 0.2807 0.109 Uiso 1 1 calc R . . H29B H 0.6821 0.4143 0.1536 0.109 Uiso 1 1 calc R . . C30 C 0.8293(4) 0.4132(2) 0.2134(5) 0.121(2) Uani 1 1 d . . . H30A H 0.8736 0.3973 0.2843 0.145 Uiso 1 1 calc R . . H30B H 0.8193 0.3774 0.1614 0.145 Uiso 1 1 calc R . . C31 C 0.8687(3) 0.4720(2) 0.1837(3) 0.0881(11) Uani 1 1 d . . . H31A H 0.9396 0.4724 0.2206 0.106 Uiso 1 1 calc R . . H31B H 0.8504 0.4728 0.1064 0.106 Uiso 1 1 calc R . . O3 O 0.87647(13) 0.62772(12) 0.07704(14) 0.0599(5) Uani 1 1 d U . . C32 C 0.8027(3) 0.6383(2) -0.0233(2) 0.0787(9) Uani 1 1 d U . . H32A H 0.7741 0.6825 -0.0263 0.094 Uiso 1 1 calc R . . H32B H 0.7518 0.6048 -0.0379 0.094 Uiso 1 1 calc R . . C33 C 0.8435(2) 0.63372(18) -0.1040(2) 0.0653(7) Uani 1 1 d U . . H33A H 0.8498 0.6780 -0.1307 0.078 Uiso 1 1 calc R . . H33B H 0.8027 0.6059 -0.1645 0.078 Uiso 1 1 calc R . . C34 C 0.9397(2) 0.60282(19) -0.0452(2) 0.0661(7) Uani 1 1 d U . . H34A H 0.9374 0.5549 -0.0597 0.079 Uiso 1 1 calc R . . H34B H 0.9884 0.6233 -0.0655 0.079 Uiso 1 1 calc R . . C35 C 0.9610(3) 0.6147(3) 0.0622(3) 0.0979(10) Uani 1 1 d U . . H35A H 1.0050 0.6529 0.0873 0.117 Uiso 1 1 calc R . . H35B H 0.9940 0.5758 0.1048 0.117 Uiso 1 1 calc R . . O4 O 0.98014(12) 0.65229(9) 0.31932(13) 0.0466(4) Uani 1 1 d . . . C36 C 1.0085(2) 0.71876(15) 0.3091(2) 0.0571(7) Uani 1 1 d . . . H36A H 0.9538 0.7493 0.2933 0.068 Uiso 1 1 calc R . . H36B H 1.0298 0.7215 0.2509 0.068 Uiso 1 1 calc R . . C37 C 1.0888(3) 0.73675(19) 0.4119(3) 0.0768(10) Uani 1 1 d . . . H37A H 1.0877 0.7843 0.4273 0.092 Uiso 1 1 calc R . . H37B H 1.1518 0.7253 0.4123 0.092 Uiso 1 1 calc R . . C38 C 1.0670(3) 0.6947(2) 0.4900(3) 0.0927(13) Uani 1 1 d . . . H38A H 1.1263 0.6845 0.5532 0.111 Uiso 1 1 calc R . . H38B H 1.0214 0.7174 0.5128 0.111 Uiso 1 1 calc R . . C39 C 1.0231(2) 0.63302(16) 0.4288(2) 0.0559(7) Uani 1 1 d . . . H39A H 1.0729 0.5990 0.4407 0.067 Uiso 1 1 calc R . . H39B H 0.9740 0.6150 0.4508 0.067 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 V1 0.02467(18) 0.02621(19) 0.02291(17) 0.00275(12) 0.01100(14) 0.00097(13) V2 0.02464(18) 0.02665(19) 0.02288(17) 0.00164(12) 0.01133(14) 0.00120(12) N1 0.0302(9) 0.0276(9) 0.0261(8) 0.0033(6) 0.0151(7) 0.0015(7) N2 0.0328(9) 0.0275(9) 0.0255(8) 0.0037(6) 0.0154(7) 0.0001(7) N3 0.0292(9) 0.0305(9) 0.0325(8) -0.0004(7) 0.0137(7) 0.0032(7) N4 0.0301(9) 0.0378(10) 0.0297(8) -0.0059(7) 0.0123(7) -0.0004(8) N5 0.0306(9) 0.0272(9) 0.0273(8) 0.0033(6) 0.0140(7) 0.0012(7) N6 0.0303(9) 0.0286(9) 0.0251(8) 0.0032(6) 0.0144(7) 0.0020(7) C1 0.0275(11) 0.0624(17) 0.0396(12) 0.0017(11) 0.0167(10) 0.0067(10) C2 0.0291(11) 0.0435(14) 0.0420(12) 0.0082(10) 0.0130(10) -0.0047(10) C3 0.0311(11) 0.0449(14) 0.0327(10) -0.0031(9) 0.0089(9) -0.0073(10) C4 0.0289(11) 0.0525(15) 0.0347(11) 0.0165(10) 0.0064(9) -0.0010(10) C5 0.0276(11) 0.0413(14) 0.0584(15) 0.0004(11) 0.0108(11) 0.0061(10) C6 0.0231(9) 0.0307(10) 0.0254(9) -0.0005(7) 0.0096(7) 0.0008(8) C7 0.0294(10) 0.0327(11) 0.0352(10) 0.0020(8) 0.0138(9) 0.0006(8) C8 0.0376(12) 0.0326(12) 0.0441(12) -0.0096(9) 0.0190(10) -0.0011(9) C9 0.0398(12) 0.0411(13) 0.0358(11) -0.0103(9) 0.0207(10) -0.0047(10) C10 0.0358(11) 0.0422(13) 0.0298(10) -0.0026(9) 0.0177(9) -0.0035(10) C11 0.0246(9) 0.0303(10) 0.0245(8) -0.0016(7) 0.0107(7) 0.0002(8) C12 0.0286(10) 0.0370(12) 0.0282(9) 0.0080(8) 0.0135(8) 0.0013(8) C13 0.0346(12) 0.0443(13) 0.0411(11) 0.0091(10) 0.0177(10) 0.0074(10) C14 0.0265(11) 0.0587(17) 0.0483(13) 0.0150(12) 0.0138(10) 0.0069(11) C15 0.0270(11) 0.0559(16) 0.0445(13) 0.0038(11) 0.0061(10) -0.0043(11) C16 0.0336(12) 0.0496(15) 0.0367(11) -0.0027(10) 0.0093(9) -0.0037(10) C17 0.0282(10) 0.0391(12) 0.0277(9) 0.0054(8) 0.0109(8) 0.0001(9) C18 0.0248(9) 0.0293(10) 0.0288(9) -0.0029(7) 0.0101(8) 0.0003(8) C19 0.0333(11) 0.0327(12) 0.0385(11) -0.0021(9) 0.0117(9) -0.0011(9) C20 0.0372(12) 0.0350(13) 0.0451(12) -0.0120(10) 0.0116(10) 0.0036(10) C21 0.0314(11) 0.0485(14) 0.0324(10) -0.0118(9) 0.0107(9) 0.0051(10) C22 0.0287(10) 0.0451(13) 0.0279(9) -0.0008(8) 0.0119(8) 0.0037(9) C23 0.0251(9) 0.0324(11) 0.0264(9) -0.0015(8) 0.0093(8) 0.0030(8) Li1 0.043(2) 0.059(3) 0.042(2) -0.0031(19) 0.0175(18) -0.004(2) O1 0.0405(9) 0.0588(12) 0.0428(9) 0.0006(8) 0.0159(8) 0.0075(8) C24 0.0545(15) 0.0493(15) 0.0435(12) 0.0053(10) 0.0240(11) 0.0106(12) C25 0.0495(16) 0.092(2) 0.0707(18) -0.0063(16) 0.0298(15) 0.0119(15) C26 0.058(2) 0.185(4) 0.082(2) 0.018(2) 0.0262(19) 0.040(2) C27 0.0460(15) 0.0635(18) 0.0501(14) -0.0023(12) 0.0074(12) 0.0050(13) O2 0.0512(11) 0.0495(12) 0.0727(12) -0.0074(9) 0.0264(10) -0.0037(9) C28 0.0547(17) 0.0547(19) 0.078(2) -0.0107(15) 0.0285(16) -0.0132(14) C29 0.090(3) 0.055(2) 0.132(4) -0.023(2) 0.050(3) -0.018(2) C30 0.082(3) 0.059(3) 0.210(6) -0.017(3) 0.049(4) -0.005(2) C31 0.081(3) 0.084(3) 0.098(3) -0.006(2) 0.035(2) 0.026(2) O3 0.0415(9) 0.0977(15) 0.0438(9) 0.0048(9) 0.0207(8) 0.0056(10) C32 0.0639(16) 0.117(2) 0.0532(14) 0.0183(15) 0.0224(13) 0.0339(16) C33 0.0692(16) 0.0820(19) 0.0498(13) 0.0120(13) 0.0298(12) 0.0170(14) C34 0.0554(15) 0.0872(19) 0.0610(14) -0.0011(14) 0.0292(13) 0.0083(14) C35 0.0581(16) 0.164(3) 0.0732(17) 0.0084(19) 0.0288(15) 0.0256(19) O4 0.0403(9) 0.0500(11) 0.0443(9) 0.0038(7) 0.0120(8) -0.0008(8) C36 0.0458(15) 0.0530(18) 0.0707(18) 0.0114(14) 0.0223(14) -0.0006(13) C37 0.062(2) 0.067(2) 0.087(2) -0.0206(19) 0.0168(19) -0.0045(17) C38 0.091(3) 0.118(4) 0.0537(18) -0.019(2) 0.0153(19) -0.006(3) C39 0.0503(16) 0.067(2) 0.0503(14) 0.0134(13) 0.0207(13) 0.0115(14) _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 V1 N1 2.0759(18) . ? V1 N2 2.0908(17) . ? V1 N6 2.0985(17) . ? V1 N5 2.1045(18) . ? V1 C3 2.290(2) . ? V1 C4 2.300(2) . ? V1 C2 2.303(2) . ? V1 C5 2.314(2) . ? V1 C1 2.316(2) . ? V1 V2 2.3742(9) . ? V2 N4 1.9945(19) . ? V2 N3 2.0050(17) . ? V2 N6 2.1266(17) . ? V2 N5 2.1514(18) . ? V2 N1 2.1531(18) . ? V2 N2 2.1541(17) . ? N1 C6 1.396(2) . ? N1 H1N 0.863(19) . ? N2 C11 1.398(3) . ? N2 H2N 0.873(18) . ? N3 C12 1.370(3) . ? N3 H3N 0.8800 . ? N4 C17 1.375(3) . ? N4 H4N 0.8800 . ? N5 C18 1.399(2) . ? N5 H5N 0.841(19) . ? N6 C23 1.392(3) . ? N6 H6N 0.864(19) . ? C1 C5 1.404(4) . ? C1 C2 1.413(4) . ? C1 H1 1.0000 . ? C2 C3 1.404(3) . ? C2 H2 1.0000 . ? C3 C4 1.402(4) . ? C3 H3 1.0000 . ? C4 C5 1.406(4) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 C7 1.377(3) . ? C6 C11 1.416(3) . ? C7 C8 1.409(3) . ? C7 H7 0.9500 . ? C8 C9 1.373(3) . ? C8 H8 0.9500 . ? C9 C10 1.397(3) . ? C9 H9 0.9500 . ? C10 C11 1.392(3) . ? C10 H10 0.9500 . ? C12 C13 1.398(3) . ? C12 C17 1.423(3) . ? C13 C14 1.386(3) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C17 1.395(3) . ? C16 H16 0.9500 . ? C18 C19 1.381(3) . ? C18 C23 1.419(3) . ? C19 C20 1.410(3) . ? C19 H19 0.9500 . ? C20 C21 1.374(3) . ? C20 H20 0.9500 . ? C21 C22 1.396(3) . ? C21 H21 0.9500 . ? C22 C23 1.392(3) . ? C22 H22 0.9500 . ? Li1 O3 1.919(4) . ? Li1 O4 1.921(5) . ? Li1 O1 1.926(5) . ? Li1 O2 1.935(5) . ? O1 C27 1.438(3) . ? O1 C24 1.445(3) . ? C24 C25 1.483(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.417(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.437(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O2 C31 1.433(4) . ? O2 C28 1.434(3) . ? C28 C29 1.519(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.486(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.469(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O3 C32 1.401(4) . ? O3 C35 1.416(4) . ? C32 C33 1.491(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.495(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.408(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? O4 C39 1.437(3) . ? O4 C36 1.440(3) . ? C36 C37 1.493(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.520(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.505(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 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 N1 V1 N2 70.48(6) . . ? N1 V1 N6 74.91(7) . . ? N2 V1 N6 113.64(7) . . ? N1 V1 N5 114.44(7) . . ? N2 V1 N5 76.03(7) . . ? N6 V1 N5 69.57(7) . . ? N1 V1 C3 100.21(8) . . ? N2 V1 C3 97.91(7) . . ? N6 V1 C3 143.35(8) . . ? N5 V1 C3 139.54(8) . . ? N1 V1 C4 133.49(8) . . ? N2 V1 C4 96.69(8) . . ? N6 V1 C4 145.55(8) . . ? N5 V1 C4 104.52(8) . . ? C3 V1 C4 35.56(9) . . ? N1 V1 C2 93.68(8) . . ? N2 V1 C2 128.87(8) . . ? N6 V1 C2 107.79(8) . . ? N5 V1 C2 148.82(8) . . ? C3 V1 C2 35.59(8) . . ? C4 V1 C2 59.17(8) . . ? N1 V1 C5 152.72(8) . . ? N2 V1 C5 126.22(8) . . ? N6 V1 C5 110.10(9) . . ? N5 V1 C5 91.84(8) . . ? C3 V1 C5 59.15(9) . . ? C4 V1 C5 35.47(9) . . ? C2 V1 C5 59.08(9) . . ? N1 V1 C1 120.42(8) . . ? N2 V1 C1 154.97(8) . . ? N6 V1 C1 91.35(8) . . ? N5 V1 C1 113.74(8) . . ? C3 V1 C1 59.23(9) . . ? C4 V1 C1 59.03(9) . . ? C2 V1 C1 35.62(9) . . ? C5 V1 C1 35.31(9) . . ? N1 V1 V2 57.40(5) . . ? N2 V1 V2 57.27(5) . . ? N6 V1 V2 56.37(5) . . ? N5 V1 V2 57.04(5) . . ? C3 V1 V2 149.69(6) . . ? C4 V1 V2 149.50(6) . . ? C2 V1 V2 148.58(6) . . ? C5 V1 V2 148.24(7) . . ? C1 V1 V2 147.68(6) . . ? N4 V2 N3 76.94(8) . . ? N4 V2 N6 97.24(7) . . ? N3 V2 N6 142.04(7) . . ? N4 V2 N5 93.70(7) . . ? N3 V2 N5 148.64(7) . . ? N6 V2 N5 68.18(6) . . ? N4 V2 N1 148.05(7) . . ? N3 V2 N1 92.35(7) . . ? N6 V2 N1 72.77(6) . . ? N5 V2 N1 109.47(7) . . ? N4 V2 N2 142.17(7) . . ? N3 V2 N2 95.26(7) . . ? N6 V2 N2 109.99(7) . . ? N5 V2 N2 73.75(7) . . ? N1 V2 N2 67.86(6) . . ? N4 V2 V1 142.94(6) . . ? N3 V2 V1 140.12(5) . . ? N6 V2 V1 55.25(5) . . ? N5 V2 V1 55.16(5) . . ? N1 V2 V1 54.32(5) . . ? N2 V2 V1 54.74(5) . . ? C6 N1 V1 112.80(12) . . ? C6 N1 V2 110.19(12) . . ? V1 N1 V2 68.28(6) . . ? C6 N1 H1N 109.9(16) . . ? V1 N1 H1N 126.5(16) . . ? V2 N1 H1N 123.2(16) . . ? C11 N2 V1 112.07(12) . . ? C11 N2 V2 110.03(12) . . ? V1 N2 V2 67.99(5) . . ? C11 N2 H2N 114.9(16) . . ? V1 N2 H2N 121.6(16) . . ? V2 N2 H2N 121.9(16) . . ? C12 N3 V2 118.52(14) . . ? C12 N3 H3N 120.7 . . ? V2 N3 H3N 120.7 . . ? C17 N4 V2 118.71(15) . . ? C17 N4 H4N 120.6 . . ? V2 N4 H4N 120.6 . . ? C18 N5 V1 108.27(12) . . ? C18 N5 V2 114.44(12) . . ? V1 N5 V2 67.80(6) . . ? C18 N5 H5N 114.5(16) . . ? V1 N5 H5N 120.0(16) . . ? V2 N5 H5N 123.0(16) . . ? C23 N6 V1 108.15(12) . . ? C23 N6 V2 115.33(13) . . ? V1 N6 V2 68.37(5) . . ? C23 N6 H6N 113.6(16) . . ? V1 N6 H6N 123.8(16) . . ? V2 N6 H6N 120.2(16) . . ? C5 C1 C2 107.8(2) . . ? C5 C1 V1 72.27(13) . . ? C2 C1 V1 71.69(13) . . ? C5 C1 H1 126.0 . . ? C2 C1 H1 126.0 . . ? V1 C1 H1 126.0 . . ? C3 C2 C1 107.8(2) . . ? C3 C2 V1 71.70(13) . . ? C1 C2 V1 72.69(13) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? V1 C2 H2 125.9 . . ? C4 C3 C2 108.2(2) . . ? C4 C3 V1 72.62(13) . . ? C2 C3 V1 72.71(13) . . ? C4 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? V1 C3 H3 125.7 . . ? C3 C4 C5 108.1(2) . . ? C3 C4 V1 71.82(12) . . ? C5 C4 V1 72.80(13) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? V1 C4 H4 125.8 . . ? C1 C5 C4 108.1(2) . . ? C1 C5 V1 72.42(14) . . ? C4 C5 V1 71.73(13) . . ? C1 C5 H5 125.8 . . ? C4 C5 H5 125.8 . . ? V1 C5 H5 125.8 . . ? C7 C6 N1 128.98(18) . . ? C7 C6 C11 120.42(17) . . ? N1 C6 C11 110.58(17) . . ? C6 C7 C8 119.32(19) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.2(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 121.2(2) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 119.0(2) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 N2 129.31(18) . . ? C10 C11 C6 119.83(19) . . ? N2 C11 C6 110.84(16) . . ? N3 C12 C13 128.0(2) . . ? N3 C12 C17 112.87(18) . . ? C13 C12 C17 119.1(2) . . ? C14 C13 C12 121.0(2) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.1(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 119.8(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 121.1(2) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.4 . . ? N4 C17 C16 128.4(2) . . ? N4 C17 C12 112.81(18) . . ? C16 C17 C12 118.8(2) . . ? C19 C18 N5 129.14(19) . . ? C19 C18 C23 120.57(18) . . ? N5 C18 C23 110.18(17) . . ? C18 C19 C20 118.9(2) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 120.7(2) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 120.9(2) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 N6 129.53(19) . . ? C22 C23 C18 119.58(19) . . ? N6 C23 C18 110.85(16) . . ? O3 Li1 O4 108.0(2) . . ? O3 Li1 O1 114.8(2) . . ? O4 Li1 O1 102.5(2) . . ? O3 Li1 O2 105.9(2) . . ? O4 Li1 O2 119.4(2) . . ? O1 Li1 O2 106.6(2) . . ? C27 O1 C24 109.0(2) . . ? C27 O1 Li1 127.3(2) . . ? C24 O1 Li1 120.4(2) . . ? O1 C24 C25 106.4(2) . . ? O1 C24 H24A 110.5 . . ? C25 C24 H24A 110.5 . . ? O1 C24 H24B 110.5 . . ? C25 C24 H24B 110.5 . . ? H24A C24 H24B 108.6 . . ? C26 C25 C24 105.5(3) . . ? C26 C25 H25A 110.6 . . ? C24 C25 H25A 110.6 . . ? C26 C25 H25B 110.6 . . ? C24 C25 H25B 110.6 . . ? H25A C25 H25B 108.8 . . ? C25 C26 C27 110.0(3) . . ? C25 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? C25 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C26 C27 O1 106.1(2) . . ? C26 C27 H27A 110.5 . . ? O1 C27 H27A 110.5 . . ? C26 C27 H27B 110.5 . . ? O1 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C31 O2 C28 107.1(3) . . ? C31 O2 Li1 124.8(3) . . ? C28 O2 Li1 122.9(2) . . ? O2 C28 C29 106.2(3) . . ? O2 C28 H28A 110.5 . . ? C29 C28 H28A 110.5 . . ? O2 C28 H28B 110.5 . . ? C29 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? C30 C29 C28 105.3(3) . . ? C30 C29 H29A 110.7 . . ? C28 C29 H29A 110.7 . . ? C30 C29 H29B 110.7 . . ? C28 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C31 C30 C29 106.0(4) . . ? C31 C30 H30A 110.5 . . ? C29 C30 H30A 110.5 . . ? C31 C30 H30B 110.5 . . ? C29 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? O2 C31 C30 106.2(3) . . ? O2 C31 H31A 110.5 . . ? C30 C31 H31A 110.5 . . ? O2 C31 H31B 110.5 . . ? C30 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C32 O3 C35 107.1(2) . . ? C32 O3 Li1 127.6(2) . . ? C35 O3 Li1 124.7(2) . . ? O3 C32 C33 108.7(3) . . ? O3 C32 H32A 109.9 . . ? C33 C32 H32A 109.9 . . ? O3 C32 H32B 109.9 . . ? C33 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C32 C33 C34 103.9(2) . . ? C32 C33 H33A 111.0 . . ? C34 C33 H33A 111.0 . . ? C32 C33 H33B 111.0 . . ? C34 C33 H33B 111.0 . . ? H33A C33 H33B 109.0 . . ? C35 C34 C33 104.6(3) . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? C34 C35 O3 111.0(3) . . ? C34 C35 H35A 109.4 . . ? O3 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? O3 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C39 O4 C36 109.5(2) . . ? C39 O4 Li1 127.8(2) . . ? C36 O4 Li1 118.0(2) . . ? O4 C36 C37 107.3(2) . . ? O4 C36 H36A 110.3 . . ? C37 C36 H36A 110.3 . . ? O4 C36 H36B 110.3 . . ? C37 C36 H36B 110.3 . . ? H36A C36 H36B 108.5 . . ? C36 C37 C38 101.9(3) . . ? C36 C37 H37A 111.4 . . ? C38 C37 H37A 111.4 . . ? C36 C37 H37B 111.4 . . ? C38 C37 H37B 111.4 . . ? H37A C37 H37B 109.2 . . ? C39 C38 C37 104.0(3) . . ? C39 C38 H38A 111.0 . . ? C37 C38 H38A 111.0 . . ? C39 C38 H38B 111.0 . . ? C37 C38 H38B 111.0 . . ? H38A C38 H38B 109.0 . . ? O4 C39 C38 105.8(3) . . ? O4 C39 H39A 110.6 . . ? C38 C39 H39A 110.6 . . ? O4 C39 H39B 110.6 . . ? C38 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.292 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.067 data_dw1207 _database_code_depnum_ccdc_archive 'CCDC 892666' #TrackingRef 'compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H68 Mn6 N12 O5, 4(C4 H8 O)' _chemical_formula_sum 'C68 H100 Mn6 N12 O9' _chemical_formula_weight 1559.24 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2698(2) _cell_length_b 16.7091(3) _cell_length_c 16.7888(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.7800(10) _cell_angle_gamma 90.00 _cell_volume 3644.12(11) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 17802 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 32704 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6640 _reflns_number_gt 4771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^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_number_reflns 6640 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 1.02985(4) 1.10452(3) 0.07105(3) 0.03043(16) Uani 1 1 d . . . Mn2 Mn 1.16292(4) 0.96297(3) 0.05247(3) 0.03295(16) Uani 1 1 d . . . Mn3 Mn 0.94304(4) 0.94198(3) 0.10496(3) 0.03288(16) Uani 1 1 d . . . O1 O 0.8890(2) 0.87254(18) 0.20744(16) 0.0555(7) Uani 1 1 d . B . O2 O 1.3285(2) 0.91652(18) 0.10325(16) 0.0549(7) Uani 1 1 d . . . O3 O 1.0000 1.0000 0.0000 0.0298(7) Uani 1 2 d S . . O4 O 0.9144(4) 1.1957(2) 0.4219(3) 0.1187(17) Uani 1 1 d . . . O5 O 1.5060(10) 0.9921(10) 0.7015(6) 0.264(5) Uani 1 1 d . . . N1 N 1.1061(2) 0.91596(17) 0.15746(16) 0.0346(6) Uani 1 1 d . . . H1A H 1.1180 0.8619 0.1642 0.042 Uiso 1 1 calc R . . N2 N 1.0054(2) 1.05595(17) 0.17405(15) 0.0333(6) Uani 1 1 d . . . H2A H 0.9540 1.0827 0.1924 0.040 Uiso 1 1 calc R . . N3 N 1.2073(2) 1.00041(17) -0.06182(16) 0.0344(6) Uani 1 1 d . . . H3A H 1.2593 1.0377 -0.0520 0.041 Uiso 1 1 calc R . . N4 N 1.1159(2) 0.85708(17) -0.03594(16) 0.0346(6) Uani 1 1 d . . . H4A H 1.1179 0.8098 -0.0076 0.041 Uiso 1 1 calc R . . N5 N 0.9240(2) 0.83441(17) 0.01766(16) 0.0345(6) Uani 1 1 d . . . H5A H 0.9675 0.7928 0.0371 0.041 Uiso 1 1 calc R . . N6 N 0.8184(2) 0.90930(17) -0.10568(16) 0.0331(6) Uani 1 1 d . . . H6A H 0.7983 0.9102 -0.1615 0.040 Uiso 1 1 calc R . . C1 C 1.1343(3) 0.9576(2) 0.2310(2) 0.0362(8) Uani 1 1 d . . . C2 C 1.2063(3) 0.9297(3) 0.2983(2) 0.0460(9) Uani 1 1 d . . . H2B H 1.2398 0.8808 0.2941 0.055 Uiso 1 1 calc R . . C3 C 1.2296(3) 0.9715(3) 0.3699(2) 0.0560(11) Uani 1 1 d . . . H3B H 1.2777 0.9506 0.4139 0.067 Uiso 1 1 calc R . . C4 C 1.1827(3) 1.0439(3) 0.3778(2) 0.0542(11) Uani 1 1 d . . . H4B H 1.1989 1.0729 0.4268 0.065 Uiso 1 1 calc R . . C5 C 1.1111(3) 1.0734(2) 0.3121(2) 0.0440(9) Uani 1 1 d . . . H5B H 1.0802 1.1233 0.3168 0.053 Uiso 1 1 calc R . . C6 C 1.0842(3) 1.0314(2) 0.2401(2) 0.0363(8) Uani 1 1 d . . . C7 C 1.2386(2) 0.9312(2) -0.09701(19) 0.0345(8) Uani 1 1 d . . . C8 C 1.3193(3) 0.9298(3) -0.1393(2) 0.0429(9) Uani 1 1 d . . . H8A H 1.3513 0.9781 -0.1487 0.051 Uiso 1 1 calc R . . C9 C 1.3530(3) 0.8592(3) -0.1675(2) 0.0510(10) Uani 1 1 d . . . H9A H 1.4081 0.8601 -0.1950 0.061 Uiso 1 1 calc R . . C10 C 1.3076(3) 0.7882(3) -0.1562(2) 0.0526(10) Uani 1 1 d . . . H10A H 1.3308 0.7403 -0.1758 0.063 Uiso 1 1 calc R . . C11 C 1.2264(3) 0.7872(2) -0.1151(2) 0.0449(9) Uani 1 1 d . . . H11A H 1.1943 0.7383 -0.1078 0.054 Uiso 1 1 calc R . . C12 C 1.1921(2) 0.8574(2) -0.0845(2) 0.0353(8) Uani 1 1 d . . . C13 C 0.8204(3) 0.8104(2) -0.0043(2) 0.0349(8) Uani 1 1 d . . . C14 C 0.7731(3) 0.7522(2) 0.0341(2) 0.0449(9) Uani 1 1 d . . . H14A H 0.8110 0.7252 0.0796 0.054 Uiso 1 1 calc R . . C15 C 0.6703(3) 0.7334(3) 0.0060(3) 0.0564(11) Uani 1 1 d . . . H15A H 0.6392 0.6932 0.0318 0.068 Uiso 1 1 calc R . . C16 C 0.6140(3) 0.7735(3) -0.0595(3) 0.0564(11) Uani 1 1 d . . . H16A H 0.5442 0.7606 -0.0783 0.068 Uiso 1 1 calc R . . C17 C 0.6590(3) 0.8331(2) -0.0984(2) 0.0449(9) Uani 1 1 d . . . H17A H 0.6196 0.8603 -0.1431 0.054 Uiso 1 1 calc R . . C18 C 0.7628(2) 0.8524(2) -0.0711(2) 0.0334(8) Uani 1 1 d . . . C19 C 0.9530(4) 0.8240(5) 0.2661(4) 0.112(3) Uani 1 1 d . B . H19A H 1.0067 0.8566 0.2998 0.135 Uiso 1 1 calc R . . H19B H 0.9863 0.7826 0.2391 0.135 Uiso 1 1 calc R . . C20 C 0.8879(5) 0.7868(5) 0.3168(4) 0.109(2) Uani 1 1 d . . . H20A H 0.8652 0.7335 0.2963 0.131 Uiso 1 1 calc R A 1 H20B H 0.9252 0.7820 0.3733 0.131 Uiso 1 1 calc R A 1 C21 C 0.8069(10) 0.8370(8) 0.3112(8) 0.129(5) Uani 0.70 1 d P B 1 H21A H 0.8218 0.8788 0.3528 0.155 Uiso 0.70 1 calc PR B 1 H21B H 0.7455 0.8076 0.3184 0.155 Uiso 0.70 1 calc PR B 1 C21' C 0.7779(11) 0.7911(10) 0.2649(9) 0.050(4) Uani 0.30 1 d P B 2 H21C H 0.7252 0.7915 0.2981 0.060 Uiso 0.30 1 calc PR B 2 H21D H 0.7638 0.7481 0.2245 0.060 Uiso 0.30 1 calc PR B 2 C22 C 0.7899(4) 0.8738(4) 0.2257(4) 0.0908(19) Uani 1 1 d . . . H22A H 0.7414 0.8419 0.1864 0.109 Uiso 1 1 calc R B 1 H22B H 0.7638 0.9287 0.2257 0.109 Uiso 1 1 calc R B 1 C23 C 1.3460(4) 0.8342(3) 0.1224(3) 0.0720(14) Uani 1 1 d . . . H23A H 1.2895 0.8017 0.0922 0.086 Uiso 1 1 calc R . . H23B H 1.3509 0.8253 0.1807 0.086 Uiso 1 1 calc R . . C24 C 1.4439(5) 0.8125(4) 0.0989(6) 0.137(3) Uani 1 1 d . . . H24A H 1.4859 0.7791 0.1410 0.164 Uiso 1 1 calc R . . H24B H 1.4305 0.7827 0.0475 0.164 Uiso 1 1 calc R . . C25 C 1.4951(4) 0.8852(4) 0.0901(5) 0.107(2) Uani 1 1 d . . . H25A H 1.5251 0.8831 0.0414 0.128 Uiso 1 1 calc R . . H25B H 1.5507 0.8940 0.1375 0.128 Uiso 1 1 calc R . . C26 C 1.4201(3) 0.9502(3) 0.0829(3) 0.0620(12) Uani 1 1 d . . . H26A H 1.4467 0.9938 0.1203 0.074 Uiso 1 1 calc R . . H26B H 1.4050 0.9713 0.0273 0.074 Uiso 1 1 calc R . . C27 C 0.8420(5) 1.0851(4) 0.3495(4) 0.103(2) Uani 1 1 d . . . H27A H 0.7692 1.0695 0.3383 0.124 Uiso 1 1 calc R . . H27B H 0.8747 1.0616 0.3076 0.124 Uiso 1 1 calc R . . C28 C 0.8933(6) 1.0578(4) 0.4302(4) 0.104(2) Uani 1 1 d . . . H28A H 0.9476 1.0191 0.4262 0.125 Uiso 1 1 calc R . . H28B H 0.8439 1.0324 0.4584 0.125 Uiso 1 1 calc R . . C29 C 0.8517(5) 1.1722(4) 0.3496(4) 0.103(2) Uani 1 1 d . . . H29A H 0.8815 1.1894 0.3036 0.124 Uiso 1 1 calc R . . H29B H 0.7836 1.1969 0.3440 0.124 Uiso 1 1 calc R . . C30 C 0.9373(7) 1.1300(4) 0.4735(4) 0.120(3) Uani 1 1 d . . . H30A H 0.9083 1.1378 0.5222 0.144 Uiso 1 1 calc R . . H30B H 1.0120 1.1241 0.4907 0.144 Uiso 1 1 calc R . . C31 C 1.5124(11) 0.9231(8) 0.6526(9) 0.190(5) Uani 1 1 d . . . H31A H 1.5813 0.9183 0.6405 0.228 Uiso 1 1 calc R . . H31B H 1.4973 0.8744 0.6806 0.228 Uiso 1 1 calc R . . C32 C 1.4036(11) 1.0088(16) 0.5793(10) 0.235(10) Uani 1 1 d . . . H32A H 1.3313 1.0081 0.5845 0.282 Uiso 1 1 calc R . . H32B H 1.4079 1.0328 0.5268 0.282 Uiso 1 1 calc R . . C33 C 1.4649(15) 1.0522(9) 0.6445(12) 0.249(8) Uani 1 1 d . . . H33A H 1.5199 1.0816 0.6261 0.299 Uiso 1 1 calc R . . H33B H 1.4228 1.0902 0.6681 0.299 Uiso 1 1 calc R . . C34 C 1.4430(17) 0.9344(11) 0.5854(9) 0.234(9) Uani 1 1 d . . . H34A H 1.3869 0.8958 0.5837 0.281 Uiso 1 1 calc R . . H34B H 1.4745 0.9240 0.5385 0.281 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 0.0303(3) 0.0285(3) 0.0329(3) 0.0002(2) 0.0073(2) -0.0004(2) Mn2 0.0324(3) 0.0317(3) 0.0349(3) 0.0003(2) 0.0075(2) 0.0006(2) Mn3 0.0337(3) 0.0312(3) 0.0339(3) 0.0009(2) 0.0075(2) -0.0018(2) O1 0.0524(16) 0.0641(19) 0.0527(16) 0.0213(14) 0.0169(12) 0.0043(14) O2 0.0397(15) 0.061(2) 0.0641(17) 0.0106(14) 0.0100(12) 0.0074(13) O3 0.0320(17) 0.0272(17) 0.0301(16) -0.0027(13) 0.0060(13) -0.0034(13) O4 0.151(4) 0.061(3) 0.118(3) -0.003(2) -0.035(3) -0.020(3) O5 0.320(13) 0.283(14) 0.174(8) -0.055(10) 0.019(8) -0.049(11) N1 0.0395(16) 0.0287(16) 0.0359(15) 0.0019(12) 0.0082(12) -0.0003(12) N2 0.0325(15) 0.0349(17) 0.0332(15) 0.0012(12) 0.0084(11) 0.0020(12) N3 0.0320(15) 0.0321(16) 0.0396(15) 0.0004(13) 0.0088(12) -0.0030(12) N4 0.0319(15) 0.0311(16) 0.0417(16) 0.0034(12) 0.0099(12) 0.0013(12) N5 0.0340(15) 0.0298(16) 0.0396(16) 0.0040(12) 0.0073(12) -0.0013(12) N6 0.0320(15) 0.0325(16) 0.0350(15) -0.0002(12) 0.0073(11) -0.0027(12) C1 0.0361(18) 0.040(2) 0.0338(18) 0.0030(15) 0.0093(14) -0.0048(16) C2 0.046(2) 0.047(2) 0.044(2) 0.0107(18) 0.0057(16) 0.0081(18) C3 0.060(3) 0.057(3) 0.043(2) 0.0060(19) -0.0095(19) 0.000(2) C4 0.064(3) 0.060(3) 0.033(2) -0.0030(18) -0.0023(18) -0.001(2) C5 0.051(2) 0.040(2) 0.040(2) -0.0023(17) 0.0082(16) 0.0013(18) C6 0.0361(18) 0.040(2) 0.0334(18) 0.0034(15) 0.0081(14) -0.0041(15) C7 0.0308(17) 0.039(2) 0.0327(17) -0.0017(15) 0.0045(13) 0.0022(15) C8 0.0366(19) 0.051(2) 0.043(2) 0.0002(17) 0.0129(15) 0.0011(17) C9 0.038(2) 0.062(3) 0.057(2) -0.010(2) 0.0194(17) -0.0024(19) C10 0.046(2) 0.050(3) 0.065(3) -0.016(2) 0.0181(19) 0.0015(19) C11 0.041(2) 0.037(2) 0.059(2) -0.0091(18) 0.0147(17) -0.0004(16) C12 0.0287(17) 0.039(2) 0.0374(18) -0.0022(15) 0.0057(14) 0.0017(15) C13 0.0369(19) 0.0278(19) 0.0419(19) -0.0052(15) 0.0126(15) -0.0032(15) C14 0.042(2) 0.039(2) 0.055(2) 0.0086(18) 0.0119(17) -0.0002(17) C15 0.050(2) 0.043(2) 0.081(3) 0.013(2) 0.024(2) -0.0137(19) C16 0.036(2) 0.053(3) 0.081(3) 0.000(2) 0.0134(19) -0.0116(19) C17 0.037(2) 0.042(2) 0.055(2) -0.0005(18) 0.0060(16) -0.0016(17) C18 0.0332(18) 0.0273(19) 0.0407(19) -0.0059(15) 0.0102(14) 0.0001(14) C19 0.069(3) 0.145(6) 0.122(5) 0.098(5) 0.019(3) 0.004(4) C20 0.101(5) 0.134(6) 0.094(4) 0.060(4) 0.021(3) -0.017(4) C21 0.160(11) 0.127(10) 0.135(10) 0.073(8) 0.113(9) 0.064(9) C21' 0.054(8) 0.065(11) 0.037(8) 0.006(7) 0.025(6) -0.013(7) C22 0.076(4) 0.097(4) 0.113(4) 0.048(4) 0.051(3) 0.026(3) C23 0.056(3) 0.067(3) 0.092(3) 0.022(3) 0.012(2) 0.007(2) C24 0.078(4) 0.076(5) 0.272(10) 0.019(5) 0.073(5) 0.020(3) C25 0.066(4) 0.072(4) 0.196(7) -0.020(4) 0.058(4) -0.003(3) C26 0.039(2) 0.072(3) 0.073(3) -0.001(2) 0.003(2) -0.002(2) C27 0.117(5) 0.093(5) 0.090(4) -0.009(3) -0.001(4) -0.029(4) C28 0.135(6) 0.081(4) 0.091(4) 0.008(3) 0.008(4) -0.014(4) C29 0.107(5) 0.081(5) 0.112(5) -0.006(4) -0.001(4) 0.006(4) C30 0.189(8) 0.100(5) 0.059(3) -0.008(3) -0.004(4) -0.011(5) C31 0.250(15) 0.168(12) 0.165(11) -0.032(10) 0.074(11) -0.006(10) C32 0.145(10) 0.40(3) 0.142(11) 0.079(15) -0.008(8) 0.037(15) C33 0.32(2) 0.165(13) 0.242(17) 0.049(13) 0.013(16) 0.081(14) C34 0.35(2) 0.233(18) 0.110(9) -0.052(11) 0.016(11) -0.071(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 N6 1.992(3) 3_775 ? Mn1 N2 1.996(3) . ? Mn1 N5 2.001(3) 3_775 ? Mn1 N4 2.008(3) 3_775 ? Mn1 O3 2.1064(5) . ? Mn1 Mn2 3.0059(7) . ? Mn1 Mn3 3.0488(7) . ? Mn1 Mn3 3.1463(7) 3_775 ? Mn1 Mn2 3.1542(7) 3_775 ? Mn2 N1 2.199(3) . ? Mn2 N3 2.209(3) . ? Mn2 O3 2.2484(5) . ? Mn2 N6 2.308(3) 3_775 ? Mn2 N4 2.312(3) . ? Mn2 O2 2.322(3) . ? Mn2 Mn1 3.1542(7) 3_775 ? Mn2 Mn3 3.1572(7) 3_775 ? Mn2 Mn3 3.2347(7) . ? Mn3 N3 2.200(3) 3_775 ? Mn3 N1 2.207(3) . ? Mn3 O3 2.2716(5) . ? Mn3 N2 2.294(3) . ? Mn3 N5 2.300(3) . ? Mn3 O1 2.308(3) . ? Mn3 Mn1 3.1463(7) 3_775 ? Mn3 Mn2 3.1572(7) 3_775 ? O1 C22 1.410(6) . ? O1 C19 1.418(5) . ? O2 C23 1.421(6) . ? O2 C26 1.442(5) . ? O3 Mn1 2.1064(5) 3_775 ? O3 Mn2 2.2484(5) 3_775 ? O3 Mn3 2.2716(5) 3_775 ? O4 C29 1.383(7) . ? O4 C30 1.394(7) . ? O5 C33 1.417(15) . ? O5 C31 1.427(13) . ? N1 C1 1.400(4) . ? N1 H1A 0.9200 . ? N2 C6 1.420(4) . ? N2 H2A 0.9200 . ? N3 C7 1.400(4) . ? N3 Mn3 2.200(3) 3_775 ? N3 H3A 0.9200 . ? N4 C12 1.423(4) . ? N4 Mn1 2.008(3) 3_775 ? N4 H4A 0.9200 . ? N5 C13 1.407(4) . ? N5 Mn1 2.001(3) 3_775 ? N5 H5A 0.9200 . ? N6 C18 1.400(4) . ? N6 Mn1 1.992(3) 3_775 ? N6 Mn2 2.308(3) 3_775 ? N6 H6A 0.9200 . ? C1 C2 1.401(5) . ? C1 C6 1.424(5) . ? C2 C3 1.370(6) . ? C2 H2B 0.9400 . ? C3 C4 1.379(6) . ? C3 H3B 0.9400 . ? C4 C5 1.391(5) . ? C4 H4B 0.9400 . ? C5 C6 1.380(5) . ? C5 H5B 0.9400 . ? C7 C8 1.401(5) . ? C7 C12 1.413(5) . ? C8 C9 1.380(6) . ? C8 H8A 0.9400 . ? C9 C10 1.362(6) . ? C9 H9A 0.9400 . ? C10 C11 1.393(5) . ? C10 H10A 0.9400 . ? C11 C12 1.395(5) . ? C11 H11A 0.9400 . ? C13 C14 1.386(5) . ? C13 C18 1.409(5) . ? C14 C15 1.385(5) . ? C14 H14A 0.9400 . ? C15 C16 1.372(6) . ? C15 H15A 0.9400 . ? C16 C17 1.389(6) . ? C16 H16A 0.9400 . ? C17 C18 1.398(5) . ? C17 H17A 0.9400 . ? C19 C20 1.469(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.351(11) . ? C20 C21' 1.542(16) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.536(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21' C22 1.553(17) . ? C21' H21C 0.9800 . ? C21' H21D 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.478(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.414(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.462(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.460(8) . ? C27 C29 1.461(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C30 1.467(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C34 1.316(17) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C34 1.34(2) . ? C32 C33 1.42(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Mn1 N2 91.91(11) 3_775 . ? N6 Mn1 N5 80.32(11) 3_775 3_775 ? N2 Mn1 N5 168.67(11) . 3_775 ? N6 Mn1 N4 167.99(12) 3_775 3_775 ? N2 Mn1 N4 93.85(11) . 3_775 ? N5 Mn1 N4 92.36(11) 3_775 3_775 ? N6 Mn1 O3 97.54(8) 3_775 . ? N2 Mn1 O3 96.22(8) . . ? N5 Mn1 O3 92.99(8) 3_775 . ? N4 Mn1 O3 92.31(8) 3_775 . ? N6 Mn1 Mn2 50.12(8) 3_775 . ? N2 Mn1 Mn2 88.44(8) . . ? N5 Mn1 Mn2 92.79(8) 3_775 . ? N4 Mn1 Mn2 140.52(8) 3_775 . ? O3 Mn1 Mn2 48.342(14) . . ? N6 Mn1 Mn3 103.89(8) 3_775 . ? N2 Mn1 Mn3 48.81(8) . . ? N5 Mn1 Mn3 141.05(8) 3_775 . ? N4 Mn1 Mn3 87.79(8) 3_775 . ? O3 Mn1 Mn3 48.134(13) . . ? Mn2 Mn1 Mn3 64.581(17) . . ? N6 Mn1 Mn3 86.73(8) 3_775 3_775 ? N2 Mn1 Mn3 141.56(9) . 3_775 ? N5 Mn1 Mn3 46.85(8) 3_775 3_775 ? N4 Mn1 Mn3 95.23(8) 3_775 3_775 ? O3 Mn1 Mn3 46.190(13) . 3_775 ? Mn2 Mn1 Mn3 61.702(16) . 3_775 ? Mn3 Mn1 Mn3 94.323(18) . 3_775 ? N6 Mn1 Mn2 141.84(8) 3_775 3_775 ? N2 Mn1 Mn2 99.83(8) . 3_775 ? N5 Mn1 Mn2 91.33(8) 3_775 3_775 ? N4 Mn1 Mn2 47.02(8) 3_775 3_775 ? O3 Mn1 Mn2 45.397(13) . 3_775 ? Mn2 Mn1 Mn2 93.739(18) . 3_775 ? Mn3 Mn1 Mn2 61.162(16) . 3_775 ? Mn3 Mn1 Mn2 61.781(16) 3_775 3_775 ? N1 Mn2 N3 173.29(10) . . ? N1 Mn2 O3 87.30(7) . . ? N3 Mn2 O3 89.26(7) . . ? N1 Mn2 N6 92.71(10) . 3_775 ? N3 Mn2 N6 92.74(10) . 3_775 ? O3 Mn2 N6 85.16(7) . 3_775 ? N1 Mn2 N4 98.60(10) . . ? N3 Mn2 N4 75.17(10) . . ? O3 Mn2 N4 81.21(7) . . ? N6 Mn2 N4 161.81(10) 3_775 . ? N1 Mn2 O2 92.28(10) . . ? N3 Mn2 O2 90.79(10) . . ? O3 Mn2 O2 176.30(8) . . ? N6 Mn2 O2 98.53(10) 3_775 . ? N4 Mn2 O2 95.23(10) . . ? N1 Mn2 Mn1 83.87(8) . . ? N3 Mn2 Mn1 97.67(8) . . ? O3 Mn2 Mn1 44.423(13) . . ? N6 Mn2 Mn1 41.48(7) 3_775 . ? N4 Mn2 Mn1 125.56(7) . . ? O2 Mn2 Mn1 139.18(8) . . ? N1 Mn2 Mn1 91.99(7) . 3_775 ? N3 Mn2 Mn1 81.62(7) . 3_775 ? O3 Mn2 Mn1 41.838(12) . 3_775 ? N6 Mn2 Mn1 126.42(7) 3_775 3_775 ? N4 Mn2 Mn1 39.46(7) . 3_775 ? O2 Mn2 Mn1 134.54(8) . 3_775 ? Mn1 Mn2 Mn1 86.261(18) . 3_775 ? N1 Mn2 Mn3 133.15(7) . 3_775 ? N3 Mn2 Mn3 44.15(7) . 3_775 ? O3 Mn2 Mn3 45.996(13) . 3_775 ? N6 Mn2 Mn3 81.55(7) 3_775 3_775 ? N4 Mn2 Mn3 80.32(7) . 3_775 ? O2 Mn2 Mn3 134.57(7) . 3_775 ? Mn1 Mn2 Mn3 61.337(16) . 3_775 ? Mn1 Mn2 Mn3 57.771(15) 3_775 3_775 ? N1 Mn2 Mn3 42.86(7) . . ? N3 Mn2 Mn3 133.02(7) . . ? O3 Mn2 Mn3 44.592(12) . . ? N6 Mn2 Mn3 91.50(7) 3_775 . ? N4 Mn2 Mn3 87.23(7) . . ? O2 Mn2 Mn3 134.61(7) . . ? Mn1 Mn2 Mn3 58.352(16) . . ? Mn1 Mn2 Mn3 58.988(15) 3_775 . ? Mn3 Mn2 Mn3 90.588(17) 3_775 . ? N3 Mn3 N1 165.22(11) 3_775 . ? N3 Mn3 O3 88.90(7) 3_775 . ? N1 Mn3 O3 86.53(7) . . ? N3 Mn3 N2 90.71(10) 3_775 . ? N1 Mn3 N2 74.84(10) . . ? O3 Mn3 N2 83.98(7) . . ? N3 Mn3 N5 99.09(10) 3_775 . ? N1 Mn3 N5 94.10(10) . . ? O3 Mn3 N5 81.36(7) . . ? N2 Mn3 N5 162.16(10) . . ? N3 Mn3 O1 93.81(10) 3_775 . ? N1 Mn3 O1 91.83(10) . . ? O3 Mn3 O1 175.06(8) . . ? N2 Mn3 O1 100.10(11) . . ? N5 Mn3 O1 94.12(10) . . ? N3 Mn3 Mn1 84.29(8) 3_775 . ? N1 Mn3 Mn1 82.70(8) . . ? O3 Mn3 Mn1 43.674(13) . . ? N2 Mn3 Mn1 40.89(7) . . ? N5 Mn3 Mn1 125.00(7) . . ? O1 Mn3 Mn1 140.71(8) . . ? N3 Mn3 Mn1 93.94(7) 3_775 3_775 ? N1 Mn3 Mn1 92.04(7) . 3_775 ? O3 Mn3 Mn1 42.003(12) . 3_775 ? N2 Mn3 Mn1 125.53(7) . 3_775 ? N5 Mn3 Mn1 39.40(7) . 3_775 ? O1 Mn3 Mn1 133.52(8) . 3_775 ? Mn1 Mn3 Mn1 85.677(18) . 3_775 ? N3 Mn3 Mn2 44.39(7) 3_775 3_775 ? N1 Mn3 Mn2 131.78(7) . 3_775 ? O3 Mn3 Mn2 45.394(13) . 3_775 ? N2 Mn3 Mn2 93.37(7) . 3_775 ? N5 Mn3 Mn2 83.54(7) . 3_775 ? O1 Mn3 Mn2 136.38(7) . 3_775 ? Mn1 Mn3 Mn2 61.066(16) . 3_775 ? Mn1 Mn3 Mn2 56.961(15) 3_775 3_775 ? N3 Mn3 Mn2 132.11(8) 3_775 . ? N1 Mn3 Mn2 42.66(7) . . ? O3 Mn3 Mn2 44.018(12) . . ? N2 Mn3 Mn2 78.20(7) . . ? N5 Mn3 Mn2 84.19(7) . . ? O1 Mn3 Mn2 133.84(7) . . ? Mn1 Mn3 Mn2 57.067(16) . . ? Mn1 Mn3 Mn2 59.231(15) 3_775 . ? Mn2 Mn3 Mn2 89.412(17) 3_775 . ? C22 O1 C19 108.2(4) . . ? C22 O1 Mn3 126.8(3) . . ? C19 O1 Mn3 124.9(3) . . ? C23 O2 C26 108.9(3) . . ? C23 O2 Mn2 120.4(3) . . ? C26 O2 Mn2 124.2(2) . . ? Mn1 O3 Mn1 180.000(15) . 3_775 ? Mn1 O3 Mn2 87.235(18) . . ? Mn1 O3 Mn2 92.765(18) 3_775 . ? Mn1 O3 Mn2 92.765(18) . 3_775 ? Mn1 O3 Mn2 87.235(18) 3_775 3_775 ? Mn2 O3 Mn2 180.0 . 3_775 ? Mn1 O3 Mn3 88.192(18) . . ? Mn1 O3 Mn3 91.808(18) 3_775 . ? Mn2 O3 Mn3 91.390(18) . . ? Mn2 O3 Mn3 88.610(18) 3_775 . ? Mn1 O3 Mn3 91.808(18) . 3_775 ? Mn1 O3 Mn3 88.192(18) 3_775 3_775 ? Mn2 O3 Mn3 88.610(18) . 3_775 ? Mn2 O3 Mn3 91.390(18) 3_775 3_775 ? Mn3 O3 Mn3 180.0 . 3_775 ? C29 O4 C30 109.7(5) . . ? C33 O5 C31 104.2(10) . . ? C1 N1 Mn2 117.2(2) . . ? C1 N1 Mn3 108.5(2) . . ? Mn2 N1 Mn3 94.48(10) . . ? C1 N1 H1A 111.8 . . ? Mn2 N1 H1A 111.8 . . ? Mn3 N1 H1A 111.8 . . ? C6 N2 Mn1 124.7(2) . . ? C6 N2 Mn3 106.7(2) . . ? Mn1 N2 Mn3 90.29(10) . . ? C6 N2 H2A 110.9 . . ? Mn1 N2 H2A 110.9 . . ? Mn3 N2 H2A 110.9 . . ? C7 N3 Mn3 123.4(2) . 3_775 ? C7 N3 Mn2 106.7(2) . . ? Mn3 N3 Mn2 91.47(10) 3_775 . ? C7 N3 H3A 111.0 . . ? Mn3 N3 H3A 111.0 3_775 . ? Mn2 N3 H3A 111.0 . . ? C12 N4 Mn1 125.8(2) . 3_775 ? C12 N4 Mn2 103.6(2) . . ? Mn1 N4 Mn2 93.52(11) 3_775 . ? C12 N4 H4A 110.5 . . ? Mn1 N4 H4A 110.5 3_775 . ? Mn2 N4 H4A 110.5 . . ? C13 N5 Mn1 112.4(2) . 3_775 ? C13 N5 Mn3 111.3(2) . . ? Mn1 N5 Mn3 93.75(11) 3_775 . ? C13 N5 H5A 112.7 . . ? Mn1 N5 H5A 112.7 3_775 . ? Mn3 N5 H5A 112.7 . . ? C18 N6 Mn1 112.8(2) . 3_775 ? C18 N6 Mn2 119.4(2) . 3_775 ? Mn1 N6 Mn2 88.40(10) 3_775 3_775 ? C18 N6 H6A 111.4 . . ? Mn1 N6 H6A 111.4 3_775 . ? Mn2 N6 H6A 111.4 3_775 . ? N1 C1 C2 124.1(3) . . ? N1 C1 C6 118.5(3) . . ? C2 C1 C6 117.3(3) . . ? C3 C2 C1 122.2(4) . . ? C3 C2 H2B 118.9 . . ? C1 C2 H2B 118.9 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3B 119.8 . . ? C4 C3 H3B 119.8 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4B 120.6 . . ? C5 C4 H4B 120.6 . . ? C6 C5 C4 121.9(4) . . ? C6 C5 H5B 119.1 . . ? C4 C5 H5B 119.1 . . ? C5 C6 N2 123.7(3) . . ? C5 C6 C1 119.4(3) . . ? N2 C6 C1 116.9(3) . . ? N3 C7 C8 123.5(3) . . ? N3 C7 C12 118.8(3) . . ? C8 C7 C12 117.6(3) . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C10 C11 C12 121.1(4) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C11 C12 C7 119.6(3) . . ? C11 C12 N4 122.1(3) . . ? C7 C12 N4 118.1(3) . . ? C14 C13 N5 126.2(3) . . ? C14 C13 C18 119.7(3) . . ? N5 C13 C18 114.1(3) . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C16 C17 C18 120.0(4) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 N6 126.0(3) . . ? C17 C18 C13 119.0(3) . . ? N6 C18 C13 115.0(3) . . ? O1 C19 C20 107.7(5) . . ? O1 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O1 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C21 C20 C19 104.5(6) . . ? C21 C20 C21' 44.2(8) . . ? C19 C20 C21' 104.7(6) . . ? C21 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? C21' C20 H20A 69.9 . . ? C21 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? C21' C20 H20B 141.6 . . ? H20A C20 H20B 108.9 . . ? C20 C21 C22 106.1(7) . . ? C20 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? C20 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C20 C21' C22 96.6(9) . . ? C20 C21' H21C 112.4 . . ? C22 C21' H21C 112.4 . . ? C20 C21' H21D 112.4 . . ? C22 C21' H21D 112.4 . . ? H21C C21' H21D 110.0 . . ? O1 C22 C21 103.4(6) . . ? O1 C22 C21' 105.0(7) . . ? C21 C22 C21' 41.8(6) . . ? O1 C22 H22A 111.1 . . ? C21 C22 H22A 111.1 . . ? C21' C22 H22A 71.9 . . ? O1 C22 H22B 111.1 . . ? C21 C22 H22B 111.1 . . ? C21' C22 H22B 140.0 . . ? H22A C22 H22B 109.1 . . ? O2 C23 C24 106.8(4) . . ? O2 C23 H23A 110.4 . . ? C24 C23 H23A 110.4 . . ? O2 C23 H23B 110.4 . . ? C24 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? C25 C24 C23 106.5(5) . . ? C25 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? C25 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C24 C25 C26 108.3(5) . . ? C24 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? C24 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O2 C26 C25 106.4(4) . . ? O2 C26 H26A 110.4 . . ? C25 C26 H26A 110.4 . . ? O2 C26 H26B 110.4 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C28 C27 C29 106.6(5) . . ? C28 C27 H27A 110.4 . . ? C29 C27 H27A 110.4 . . ? C28 C27 H27B 110.4 . . ? C29 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 C30 105.4(6) . . ? C27 C28 H28A 110.7 . . ? C30 C28 H28A 110.7 . . ? C27 C28 H28B 110.7 . . ? C30 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? O4 C29 C27 108.8(5) . . ? O4 C29 H29A 109.9 . . ? C27 C29 H29A 109.9 . . ? O4 C29 H29B 109.9 . . ? C27 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O4 C30 C28 109.1(5) . . ? O4 C30 H30A 109.9 . . ? C28 C30 H30A 109.9 . . ? O4 C30 H30B 109.9 . . ? C28 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C34 C31 O5 105.3(13) . . ? C34 C31 H31A 110.7 . . ? O5 C31 H31A 110.7 . . ? C34 C31 H31B 110.7 . . ? O5 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C34 C32 C33 105.1(12) . . ? C34 C32 H32A 110.7 . . ? C33 C32 H32A 110.7 . . ? C34 C32 H32B 110.7 . . ? C33 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? O5 C33 C32 103.8(14) . . ? O5 C33 H33A 111.0 . . ? C32 C33 H33A 111.0 . . ? O5 C33 H33B 111.0 . . ? C32 C33 H33B 111.0 . . ? H33A C33 H33B 109.0 . . ? C31 C34 C32 113.0(15) . . ? C31 C34 H34A 109.0 . . ? C32 C34 H34A 109.0 . . ? C31 C34 H34B 109.0 . . ? C32 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Mn1 Mn2 N1 101.14(12) 3_775 . . . ? N2 Mn1 Mn2 N1 7.35(10) . . . . ? N5 Mn1 Mn2 N1 176.08(10) 3_775 . . . ? N4 Mn1 Mn2 N1 -86.81(15) 3_775 . . . ? O3 Mn1 Mn2 N1 -92.41(7) . . . . ? Mn3 Mn1 Mn2 N1 -36.89(7) . . . . ? Mn3 Mn1 Mn2 N1 -147.42(7) 3_775 . . . ? Mn2 Mn1 Mn2 N1 -92.41(7) 3_775 . . . ? N6 Mn1 Mn2 N3 -85.44(12) 3_775 . . . ? N2 Mn1 Mn2 N3 -179.23(10) . . . . ? N5 Mn1 Mn2 N3 -10.50(10) 3_775 . . . ? N4 Mn1 Mn2 N3 86.62(15) 3_775 . . . ? O3 Mn1 Mn2 N3 81.02(7) . . . . ? Mn3 Mn1 Mn2 N3 136.53(7) . . . . ? Mn3 Mn1 Mn2 N3 26.00(7) 3_775 . . . ? Mn2 Mn1 Mn2 N3 81.02(7) 3_775 . . . ? N6 Mn1 Mn2 O3 -166.45(10) 3_775 . . . ? N2 Mn1 Mn2 O3 99.75(8) . . . . ? N5 Mn1 Mn2 O3 -91.52(8) 3_775 . . . ? N4 Mn1 Mn2 O3 5.60(13) 3_775 . . . ? Mn3 Mn1 Mn2 O3 55.512(14) . . . . ? Mn3 Mn1 Mn2 O3 -55.016(14) 3_775 . . . ? Mn2 Mn1 Mn2 O3 0.0 3_775 . . . ? N2 Mn1 Mn2 N6 -93.79(13) . . . 3_775 ? N5 Mn1 Mn2 N6 74.93(13) 3_775 . . 3_775 ? N4 Mn1 Mn2 N6 172.05(16) 3_775 . . 3_775 ? O3 Mn1 Mn2 N6 166.45(10) . . . 3_775 ? Mn3 Mn1 Mn2 N6 -138.04(10) . . . 3_775 ? Mn3 Mn1 Mn2 N6 111.44(10) 3_775 . . 3_775 ? Mn2 Mn1 Mn2 N6 166.45(10) 3_775 . . 3_775 ? N6 Mn1 Mn2 N4 -162.65(14) 3_775 . . . ? N2 Mn1 Mn2 N4 103.55(12) . . . . ? N5 Mn1 Mn2 N4 -87.72(11) 3_775 . . . ? N4 Mn1 Mn2 N4 9.4(2) 3_775 . . . ? O3 Mn1 Mn2 N4 3.80(9) . . . . ? Mn3 Mn1 Mn2 N4 59.31(9) . . . . ? Mn3 Mn1 Mn2 N4 -51.22(9) 3_775 . . . ? Mn2 Mn1 Mn2 N4 3.80(9) 3_775 . . . ? N6 Mn1 Mn2 O2 14.77(15) 3_775 . . . ? N2 Mn1 Mn2 O2 -79.02(13) . . . . ? N5 Mn1 Mn2 O2 89.70(13) 3_775 . . . ? N4 Mn1 Mn2 O2 -173.18(16) 3_775 . . . ? O3 Mn1 Mn2 O2 -178.78(11) . . . . ? Mn3 Mn1 Mn2 O2 -123.27(11) . . . . ? Mn3 Mn1 Mn2 O2 126.21(11) 3_775 . . . ? Mn2 Mn1 Mn2 O2 -178.78(11) 3_775 . . . ? N6 Mn1 Mn2 Mn1 -166.45(10) 3_775 . . 3_775 ? N2 Mn1 Mn2 Mn1 99.75(8) . . . 3_775 ? N5 Mn1 Mn2 Mn1 -91.52(8) 3_775 . . 3_775 ? N4 Mn1 Mn2 Mn1 5.60(13) 3_775 . . 3_775 ? O3 Mn1 Mn2 Mn1 0.0 . . . 3_775 ? Mn3 Mn1 Mn2 Mn1 55.512(14) . . . 3_775 ? Mn3 Mn1 Mn2 Mn1 -55.016(14) 3_775 . . 3_775 ? Mn2 Mn1 Mn2 Mn1 0.0 3_775 . . 3_775 ? N6 Mn1 Mn2 Mn3 -111.44(10) 3_775 . . 3_775 ? N2 Mn1 Mn2 Mn3 154.77(8) . . . 3_775 ? N5 Mn1 Mn2 Mn3 -36.50(8) 3_775 . . 3_775 ? N4 Mn1 Mn2 Mn3 60.62(13) 3_775 . . 3_775 ? O3 Mn1 Mn2 Mn3 55.016(14) . . . 3_775 ? Mn3 Mn1 Mn2 Mn3 110.528(16) . . . 3_775 ? Mn2 Mn1 Mn2 Mn3 55.016(14) 3_775 . . 3_775 ? N6 Mn1 Mn2 Mn3 138.04(10) 3_775 . . . ? N2 Mn1 Mn2 Mn3 44.24(8) . . . . ? N5 Mn1 Mn2 Mn3 -147.03(8) 3_775 . . . ? N4 Mn1 Mn2 Mn3 -49.91(13) 3_775 . . . ? O3 Mn1 Mn2 Mn3 -55.512(14) . . . . ? Mn3 Mn1 Mn2 Mn3 -110.528(16) 3_775 . . . ? Mn2 Mn1 Mn2 Mn3 -55.512(14) 3_775 . . . ? N6 Mn1 Mn3 N3 177.90(11) 3_775 . . 3_775 ? N2 Mn1 Mn3 N3 97.74(12) . . . 3_775 ? N5 Mn1 Mn3 N3 -90.35(15) 3_775 . . 3_775 ? N4 Mn1 Mn3 N3 0.68(10) 3_775 . . 3_775 ? O3 Mn1 Mn3 N3 -94.40(7) . . . 3_775 ? Mn2 Mn1 Mn3 N3 -150.19(7) . . . 3_775 ? Mn3 Mn1 Mn3 N3 -94.40(7) 3_775 . . 3_775 ? Mn2 Mn1 Mn3 N3 -40.06(7) 3_775 . . 3_775 ? N6 Mn1 Mn3 N1 4.92(11) 3_775 . . . ? N2 Mn1 Mn3 N1 -75.24(13) . . . . ? N5 Mn1 Mn3 N1 96.68(15) 3_775 . . . ? N4 Mn1 Mn3 N1 -172.30(11) 3_775 . . . ? O3 Mn1 Mn3 N1 92.62(7) . . . . ? Mn2 Mn1 Mn3 N1 36.83(7) . . . . ? Mn3 Mn1 Mn3 N1 92.62(7) 3_775 . . . ? Mn2 Mn1 Mn3 N1 146.96(7) 3_775 . . . ? N6 Mn1 Mn3 O3 -87.69(8) 3_775 . . . ? N2 Mn1 Mn3 O3 -167.86(11) . . . . ? N5 Mn1 Mn3 O3 4.06(13) 3_775 . . . ? N4 Mn1 Mn3 O3 95.08(8) 3_775 . . . ? Mn2 Mn1 Mn3 O3 -55.785(14) . . . . ? Mn3 Mn1 Mn3 O3 0.0 3_775 . . . ? Mn2 Mn1 Mn3 O3 54.342(14) 3_775 . . . ? N6 Mn1 Mn3 N2 80.16(13) 3_775 . . . ? N5 Mn1 Mn3 N2 171.91(17) 3_775 . . . ? N4 Mn1 Mn3 N2 -97.06(13) 3_775 . . . ? O3 Mn1 Mn3 N2 167.86(11) . . . . ? Mn2 Mn1 Mn3 N2 112.07(11) . . . . ? Mn3 Mn1 Mn3 N2 167.86(11) 3_775 . . . ? Mn2 Mn1 Mn3 N2 -137.80(11) 3_775 . . . ? N6 Mn1 Mn3 N5 -84.99(12) 3_775 . . . ? N2 Mn1 Mn3 N5 -165.15(14) . . . . ? N5 Mn1 Mn3 N5 6.8(2) 3_775 . . . ? N4 Mn1 Mn3 N5 97.79(12) 3_775 . . . ? O3 Mn1 Mn3 N5 2.71(8) . . . . ? Mn2 Mn1 Mn3 N5 -53.08(9) . . . . ? Mn3 Mn1 Mn3 N5 2.71(8) 3_775 . . . ? Mn2 Mn1 Mn3 N5 57.05(9) 3_775 . . . ? N6 Mn1 Mn3 O1 88.86(13) 3_775 . . . ? N2 Mn1 Mn3 O1 8.70(15) . . . . ? N5 Mn1 Mn3 O1 -179.38(16) 3_775 . . . ? N4 Mn1 Mn3 O1 -88.36(13) 3_775 . . . ? O3 Mn1 Mn3 O1 176.56(11) . . . . ? Mn2 Mn1 Mn3 O1 120.77(11) . . . . ? Mn3 Mn1 Mn3 O1 176.56(11) 3_775 . . . ? Mn2 Mn1 Mn3 O1 -129.10(11) 3_775 . . . ? N6 Mn1 Mn3 Mn1 -87.69(8) 3_775 . . 3_775 ? N2 Mn1 Mn3 Mn1 -167.86(11) . . . 3_775 ? N5 Mn1 Mn3 Mn1 4.06(13) 3_775 . . 3_775 ? N4 Mn1 Mn3 Mn1 95.08(8) 3_775 . . 3_775 ? O3 Mn1 Mn3 Mn1 0.0 . . . 3_775 ? Mn2 Mn1 Mn3 Mn1 -55.785(14) . . . 3_775 ? Mn3 Mn1 Mn3 Mn1 0.0 3_775 . . 3_775 ? Mn2 Mn1 Mn3 Mn1 54.342(14) 3_775 . . 3_775 ? N6 Mn1 Mn3 Mn2 -142.04(8) 3_775 . . 3_775 ? N2 Mn1 Mn3 Mn2 137.80(11) . . . 3_775 ? N5 Mn1 Mn3 Mn2 -50.28(13) 3_775 . . 3_775 ? N4 Mn1 Mn3 Mn2 40.74(8) 3_775 . . 3_775 ? O3 Mn1 Mn3 Mn2 -54.342(14) . . . 3_775 ? Mn2 Mn1 Mn3 Mn2 -110.127(17) . . . 3_775 ? Mn3 Mn1 Mn3 Mn2 -54.342(14) 3_775 . . 3_775 ? N6 Mn1 Mn3 Mn2 -31.91(8) 3_775 . . . ? N2 Mn1 Mn3 Mn2 -112.07(11) . . . . ? N5 Mn1 Mn3 Mn2 59.84(13) 3_775 . . . ? N4 Mn1 Mn3 Mn2 150.87(8) 3_775 . . . ? O3 Mn1 Mn3 Mn2 55.785(15) . . . . ? Mn3 Mn1 Mn3 Mn2 55.785(14) 3_775 . . . ? Mn2 Mn1 Mn3 Mn2 110.127(17) 3_775 . . . ? N1 Mn2 Mn3 N3 160.48(15) . . . 3_775 ? N3 Mn2 Mn3 N3 -27.0(2) . . . 3_775 ? O3 Mn2 Mn3 N3 -13.45(10) . . . 3_775 ? N6 Mn2 Mn3 N3 68.11(12) 3_775 . . 3_775 ? N4 Mn2 Mn3 N3 -93.72(12) . . . 3_775 ? O2 Mn2 Mn3 N3 171.66(14) . . . 3_775 ? Mn1 Mn2 Mn3 N3 41.82(10) . . . 3_775 ? Mn1 Mn2 Mn3 N3 -64.51(10) 3_775 . . 3_775 ? Mn3 Mn2 Mn3 N3 -13.45(10) 3_775 . . 3_775 ? N3 Mn2 Mn3 N1 172.48(15) . . . . ? O3 Mn2 Mn3 N1 -173.93(11) . . . . ? N6 Mn2 Mn3 N1 -92.37(13) 3_775 . . . ? N4 Mn2 Mn3 N1 105.80(13) . . . . ? O2 Mn2 Mn3 N1 11.19(15) . . . . ? Mn1 Mn2 Mn3 N1 -118.66(11) . . . . ? Mn1 Mn2 Mn3 N1 135.01(11) 3_775 . . . ? Mn3 Mn2 Mn3 N1 -173.93(11) 3_775 . . . ? N1 Mn2 Mn3 O3 173.93(11) . . . . ? N3 Mn2 Mn3 O3 -13.59(11) . . . . ? N6 Mn2 Mn3 O3 81.56(7) 3_775 . . . ? N4 Mn2 Mn3 O3 -80.28(7) . . . . ? O2 Mn2 Mn3 O3 -174.89(11) . . . . ? Mn1 Mn2 Mn3 O3 55.263(15) . . . . ? Mn1 Mn2 Mn3 O3 -51.065(14) 3_775 . . . ? Mn3 Mn2 Mn3 O3 0.0 3_775 . . . ? N1 Mn2 Mn3 N2 80.36(13) . . . . ? N3 Mn2 Mn3 N2 -107.16(13) . . . . ? O3 Mn2 Mn3 N2 -93.56(7) . . . . ? N6 Mn2 Mn3 N2 -12.00(9) 3_775 . . . ? N4 Mn2 Mn3 N2 -173.84(10) . . . . ? O2 Mn2 Mn3 N2 91.55(13) . . . . ? Mn1 Mn2 Mn3 N2 -38.30(7) . . . . ? Mn1 Mn2 Mn3 N2 -144.63(7) 3_775 . . . ? Mn3 Mn2 Mn3 N2 -93.56(7) 3_775 . . . ? N1 Mn2 Mn3 N5 -102.51(13) . . . . ? N3 Mn2 Mn3 N5 69.98(13) . . . . ? O3 Mn2 Mn3 N5 83.57(7) . . . . ? N6 Mn2 Mn3 N5 165.13(9) 3_775 . . . ? N4 Mn2 Mn3 N5 3.29(9) . . . . ? O2 Mn2 Mn3 N5 -91.32(13) . . . . ? Mn1 Mn2 Mn3 N5 138.83(7) . . . . ? Mn1 Mn2 Mn3 N5 32.50(7) 3_775 . . . ? Mn3 Mn2 Mn3 N5 83.57(7) 3_775 . . . ? N1 Mn2 Mn3 O1 -12.37(15) . . . . ? N3 Mn2 Mn3 O1 160.11(15) . . . . ? O3 Mn2 Mn3 O1 173.70(11) . . . . ? N6 Mn2 Mn3 O1 -104.74(13) 3_775 . . . ? N4 Mn2 Mn3 O1 93.43(13) . . . . ? O2 Mn2 Mn3 O1 -1.18(16) . . . . ? Mn1 Mn2 Mn3 O1 -131.03(11) . . . . ? Mn1 Mn2 Mn3 O1 122.64(11) 3_775 . . . ? Mn3 Mn2 Mn3 O1 173.70(11) 3_775 . . . ? N1 Mn2 Mn3 Mn1 118.66(11) . . . . ? N3 Mn2 Mn3 Mn1 -68.86(11) . . . . ? O3 Mn2 Mn3 Mn1 -55.263(15) . . . . ? N6 Mn2 Mn3 Mn1 26.30(7) 3_775 . . . ? N4 Mn2 Mn3 Mn1 -135.54(7) . . . . ? O2 Mn2 Mn3 Mn1 129.85(11) . . . . ? Mn1 Mn2 Mn3 Mn1 -106.328(17) 3_775 . . . ? Mn3 Mn2 Mn3 Mn1 -55.263(15) 3_775 . . . ? N1 Mn2 Mn3 Mn1 -135.01(11) . . . 3_775 ? N3 Mn2 Mn3 Mn1 37.47(11) . . . 3_775 ? O3 Mn2 Mn3 Mn1 51.065(14) . . . 3_775 ? N6 Mn2 Mn3 Mn1 132.62(7) 3_775 . . 3_775 ? N4 Mn2 Mn3 Mn1 -29.21(7) . . . 3_775 ? O2 Mn2 Mn3 Mn1 -123.82(11) . . . 3_775 ? Mn1 Mn2 Mn3 Mn1 106.328(17) . . . 3_775 ? Mn3 Mn2 Mn3 Mn1 51.064(14) 3_775 . . 3_775 ? N1 Mn2 Mn3 Mn2 173.93(11) . . . 3_775 ? N3 Mn2 Mn3 Mn2 -13.59(11) . . . 3_775 ? O3 Mn2 Mn3 Mn2 0.0 . . . 3_775 ? N6 Mn2 Mn3 Mn2 81.56(7) 3_775 . . 3_775 ? N4 Mn2 Mn3 Mn2 -80.28(7) . . . 3_775 ? O2 Mn2 Mn3 Mn2 -174.89(11) . . . 3_775 ? Mn1 Mn2 Mn3 Mn2 55.263(15) . . . 3_775 ? Mn1 Mn2 Mn3 Mn2 -51.064(14) 3_775 . . 3_775 ? Mn3 Mn2 Mn3 Mn2 0.0 3_775 . . 3_775 ? N3 Mn3 O1 C22 0.7(4) 3_775 . . . ? N1 Mn3 O1 C22 167.0(4) . . . . ? O3 Mn3 O1 C22 -122.5(8) . . . . ? N2 Mn3 O1 C22 92.1(4) . . . . ? N5 Mn3 O1 C22 -98.8(4) . . . . ? Mn1 Mn3 O1 C22 86.3(4) . . . . ? Mn1 Mn3 O1 C22 -98.4(4) 3_775 . . . ? Mn2 Mn3 O1 C22 -13.8(5) 3_775 . . . ? Mn2 Mn3 O1 C22 175.3(4) . . . . ? N3 Mn3 O1 C19 -175.7(5) 3_775 . . . ? N1 Mn3 O1 C19 -9.4(5) . . . . ? O3 Mn3 O1 C19 61.1(10) . . . . ? N2 Mn3 O1 C19 -84.3(5) . . . . ? N5 Mn3 O1 C19 84.8(5) . . . . ? Mn1 Mn3 O1 C19 -90.1(5) . . . . ? Mn1 Mn3 O1 C19 85.1(5) 3_775 . . . ? Mn2 Mn3 O1 C19 169.8(5) 3_775 . . . ? Mn2 Mn3 O1 C19 -1.1(5) . . . . ? N1 Mn2 O2 C23 56.2(3) . . . . ? N3 Mn2 O2 C23 -117.9(3) . . . . ? O3 Mn2 O2 C23 -27.2(13) . . . . ? N6 Mn2 O2 C23 149.2(3) 3_775 . . . ? N4 Mn2 O2 C23 -42.7(3) . . . . ? Mn1 Mn2 O2 C23 139.4(3) . . . . ? Mn1 Mn2 O2 C23 -38.9(3) 3_775 . . . ? Mn3 Mn2 O2 C23 -124.3(3) 3_775 . . . ? Mn3 Mn2 O2 C23 48.6(3) . . . . ? N1 Mn2 O2 C26 -155.3(3) . . . . ? N3 Mn2 O2 C26 30.7(3) . . . . ? O3 Mn2 O2 C26 121.3(11) . . . . ? N6 Mn2 O2 C26 -62.2(3) 3_775 . . . ? N4 Mn2 O2 C26 105.9(3) . . . . ? Mn1 Mn2 O2 C26 -72.0(3) . . . . ? Mn1 Mn2 O2 C26 109.7(3) 3_775 . . . ? Mn3 Mn2 O2 C26 24.3(4) 3_775 . . . ? Mn3 Mn2 O2 C26 -162.9(3) . . . . ? N6 Mn1 O3 Mn1 -74(100) 3_775 . . 3_775 ? N2 Mn1 O3 Mn1 -166(100) . . . 3_775 ? N5 Mn1 O3 Mn1 7(100) 3_775 . . 3_775 ? N4 Mn1 O3 Mn1 99(100) 3_775 . . 3_775 ? Mn2 Mn1 O3 Mn1 -84(100) . . . 3_775 ? Mn3 Mn1 O3 Mn1 -176(100) . . . 3_775 ? Mn3 Mn1 O3 Mn1 4(100) 3_775 . . 3_775 ? Mn2 Mn1 O3 Mn1 96(100) 3_775 . . 3_775 ? N6 Mn1 O3 Mn2 10.45(8) 3_775 . . . ? N2 Mn1 O3 Mn2 -82.32(8) . . . . ? N5 Mn1 O3 Mn2 91.07(8) 3_775 . . . ? N4 Mn1 O3 Mn2 -176.44(8) 3_775 . . . ? Mn3 Mn1 O3 Mn2 -91.480(18) . . . . ? Mn3 Mn1 O3 Mn2 88.520(18) 3_775 . . . ? Mn2 Mn1 O3 Mn2 180.0 3_775 . . . ? N6 Mn1 O3 Mn2 -169.55(8) 3_775 . . 3_775 ? N2 Mn1 O3 Mn2 97.68(8) . . . 3_775 ? N5 Mn1 O3 Mn2 -88.93(8) 3_775 . . 3_775 ? N4 Mn1 O3 Mn2 3.56(8) 3_775 . . 3_775 ? Mn2 Mn1 O3 Mn2 180.0 . . . 3_775 ? Mn3 Mn1 O3 Mn2 88.521(18) . . . 3_775 ? Mn3 Mn1 O3 Mn2 -91.479(18) 3_775 . . 3_775 ? N6 Mn1 O3 Mn3 101.93(8) 3_775 . . . ? N2 Mn1 O3 Mn3 9.16(8) . . . . ? N5 Mn1 O3 Mn3 -177.45(8) 3_775 . . . ? N4 Mn1 O3 Mn3 -84.96(8) 3_775 . . . ? Mn2 Mn1 O3 Mn3 91.480(18) . . . . ? Mn3 Mn1 O3 Mn3 180.0 3_775 . . . ? Mn2 Mn1 O3 Mn3 -88.521(18) 3_775 . . . ? N6 Mn1 O3 Mn3 -78.07(8) 3_775 . . 3_775 ? N2 Mn1 O3 Mn3 -170.84(8) . . . 3_775 ? N5 Mn1 O3 Mn3 2.55(8) 3_775 . . 3_775 ? N4 Mn1 O3 Mn3 95.04(8) 3_775 . . 3_775 ? Mn2 Mn1 O3 Mn3 -88.520(18) . . . 3_775 ? Mn3 Mn1 O3 Mn3 180.0 . . . 3_775 ? Mn2 Mn1 O3 Mn3 91.479(18) 3_775 . . 3_775 ? N1 Mn2 O3 Mn1 83.99(8) . . . . ? N3 Mn2 O3 Mn1 -101.77(8) . . . . ? N6 Mn2 O3 Mn1 -8.96(7) 3_775 . . . ? N4 Mn2 O3 Mn1 -176.87(7) . . . . ? O2 Mn2 O3 Mn1 167.5(11) . . . . ? Mn1 Mn2 O3 Mn1 180.0 3_775 . . . ? Mn3 Mn2 O3 Mn1 -91.877(18) 3_775 . . . ? Mn3 Mn2 O3 Mn1 88.123(18) . . . . ? N1 Mn2 O3 Mn1 -96.01(8) . . . 3_775 ? N3 Mn2 O3 Mn1 78.23(8) . . . 3_775 ? N6 Mn2 O3 Mn1 171.04(7) 3_775 . . 3_775 ? N4 Mn2 O3 Mn1 3.13(7) . . . 3_775 ? O2 Mn2 O3 Mn1 -12.5(11) . . . 3_775 ? Mn1 Mn2 O3 Mn1 180.0 . . . 3_775 ? Mn3 Mn2 O3 Mn1 88.123(18) 3_775 . . 3_775 ? Mn3 Mn2 O3 Mn1 -91.877(18) . . . 3_775 ? N1 Mn2 O3 Mn2 -159(60) . . . 3_775 ? N3 Mn2 O3 Mn2 15(60) . . . 3_775 ? N6 Mn2 O3 Mn2 108(60) 3_775 . . 3_775 ? N4 Mn2 O3 Mn2 -60(60) . . . 3_775 ? O2 Mn2 O3 Mn2 -75(60) . . . 3_775 ? Mn1 Mn2 O3 Mn2 117(60) . . . 3_775 ? Mn1 Mn2 O3 Mn2 -63(60) 3_775 . . 3_775 ? Mn3 Mn2 O3 Mn2 25(60) 3_775 . . 3_775 ? Mn3 Mn2 O3 Mn2 -155(60) . . . 3_775 ? N1 Mn2 O3 Mn3 -4.13(8) . . . . ? N3 Mn2 O3 Mn3 170.11(8) . . . . ? N6 Mn2 O3 Mn3 -97.08(7) 3_775 . . . ? N4 Mn2 O3 Mn3 95.00(7) . . . . ? O2 Mn2 O3 Mn3 79.4(11) . . . . ? Mn1 Mn2 O3 Mn3 -88.123(18) . . . . ? Mn1 Mn2 O3 Mn3 91.877(18) 3_775 . . . ? Mn3 Mn2 O3 Mn3 180.0 3_775 . . . ? N1 Mn2 O3 Mn3 175.87(8) . . . 3_775 ? N3 Mn2 O3 Mn3 -9.89(8) . . . 3_775 ? N6 Mn2 O3 Mn3 82.92(7) 3_775 . . 3_775 ? N4 Mn2 O3 Mn3 -85.00(7) . . . 3_775 ? O2 Mn2 O3 Mn3 -100.6(11) . . . 3_775 ? Mn1 Mn2 O3 Mn3 91.877(18) . . . 3_775 ? Mn1 Mn2 O3 Mn3 -88.123(18) 3_775 . . 3_775 ? Mn3 Mn2 O3 Mn3 180.0 . . . 3_775 ? N3 Mn3 O3 Mn1 82.87(8) 3_775 . . . ? N1 Mn3 O3 Mn1 -83.07(8) . . . . ? N2 Mn3 O3 Mn1 -7.96(7) . . . . ? N5 Mn3 O3 Mn1 -177.76(7) . . . . ? O1 Mn3 O3 Mn1 -153.8(8) . . . . ? Mn1 Mn3 O3 Mn1 180.0 3_775 . . . ? Mn2 Mn3 O3 Mn1 92.811(18) 3_775 . . . ? Mn2 Mn3 O3 Mn1 -87.189(18) . . . . ? N3 Mn3 O3 Mn1 -97.13(8) 3_775 . . 3_775 ? N1 Mn3 O3 Mn1 96.93(8) . . . 3_775 ? N2 Mn3 O3 Mn1 172.04(7) . . . 3_775 ? N5 Mn3 O3 Mn1 2.24(7) . . . 3_775 ? O1 Mn3 O3 Mn1 26.2(8) . . . 3_775 ? Mn1 Mn3 O3 Mn1 180.0 . . . 3_775 ? Mn2 Mn3 O3 Mn1 -87.189(18) 3_775 . . 3_775 ? Mn2 Mn3 O3 Mn1 92.811(18) . . . 3_775 ? N3 Mn3 O3 Mn2 170.06(8) 3_775 . . . ? N1 Mn3 O3 Mn2 4.12(8) . . . . ? N2 Mn3 O3 Mn2 79.23(7) . . . . ? N5 Mn3 O3 Mn2 -90.57(7) . . . . ? O1 Mn3 O3 Mn2 -66.6(8) . . . . ? Mn1 Mn3 O3 Mn2 87.189(18) . . . . ? Mn1 Mn3 O3 Mn2 -92.811(18) 3_775 . . . ? Mn2 Mn3 O3 Mn2 180.0 3_775 . . . ? N3 Mn3 O3 Mn2 -9.94(8) 3_775 . . 3_775 ? N1 Mn3 O3 Mn2 -175.88(8) . . . 3_775 ? N2 Mn3 O3 Mn2 -100.77(7) . . . 3_775 ? N5 Mn3 O3 Mn2 89.43(7) . . . 3_775 ? O1 Mn3 O3 Mn2 113.4(8) . . . 3_775 ? Mn1 Mn3 O3 Mn2 -92.811(18) . . . 3_775 ? Mn1 Mn3 O3 Mn2 87.189(18) 3_775 . . 3_775 ? Mn2 Mn3 O3 Mn2 180.0 . . . 3_775 ? N3 Mn3 O3 Mn3 -115(100) 3_775 . . 3_775 ? N1 Mn3 O3 Mn3 79(100) . . . 3_775 ? N2 Mn3 O3 Mn3 154(100) . . . 3_775 ? N5 Mn3 O3 Mn3 -15(100) . . . 3_775 ? O1 Mn3 O3 Mn3 9(100) . . . 3_775 ? Mn1 Mn3 O3 Mn3 162(100) . . . 3_775 ? Mn1 Mn3 O3 Mn3 -18(100) 3_775 . . 3_775 ? Mn2 Mn3 O3 Mn3 -105(100) 3_775 . . 3_775 ? Mn2 Mn3 O3 Mn3 75(100) . . . 3_775 ? N3 Mn2 N1 C1 -168.4(8) . . . . ? O3 Mn2 N1 C1 -109.2(2) . . . . ? N6 Mn2 N1 C1 -24.2(2) 3_775 . . . ? N4 Mn2 N1 C1 170.1(2) . . . . ? O2 Mn2 N1 C1 74.5(2) . . . . ? Mn1 Mn2 N1 C1 -64.8(2) . . . . ? Mn1 Mn2 N1 C1 -150.8(2) 3_775 . . . ? Mn3 Mn2 N1 C1 -105.1(2) 3_775 . . . ? Mn3 Mn2 N1 C1 -113.5(3) . . . . ? N3 Mn2 N1 Mn3 -54.9(9) . . . . ? O3 Mn2 N1 Mn3 4.27(8) . . . . ? N6 Mn2 N1 Mn3 89.29(10) 3_775 . . . ? N4 Mn2 N1 Mn3 -76.42(11) . . . . ? O2 Mn2 N1 Mn3 -172.06(11) . . . . ? Mn1 Mn2 N1 Mn3 48.70(8) . . . . ? Mn1 Mn2 N1 Mn3 -37.32(8) 3_775 . . . ? Mn3 Mn2 N1 Mn3 8.34(15) 3_775 . . . ? N3 Mn3 N1 C1 44.2(5) 3_775 . . . ? O3 Mn3 N1 C1 116.4(2) . . . . ? N2 Mn3 N1 C1 31.7(2) . . . . ? N5 Mn3 N1 C1 -162.5(2) . . . . ? O1 Mn3 N1 C1 -68.3(2) . . . . ? Mn1 Mn3 N1 C1 72.7(2) . . . . ? Mn1 Mn3 N1 C1 158.0(2) 3_775 . . . ? Mn2 Mn3 N1 C1 112.45(19) 3_775 . . . ? Mn2 Mn3 N1 C1 120.6(2) . . . . ? N3 Mn3 N1 Mn2 -76.4(4) 3_775 . . . ? O3 Mn3 N1 Mn2 -4.22(8) . . . . ? N2 Mn3 N1 Mn2 -88.93(11) . . . . ? N5 Mn3 N1 Mn2 76.84(11) . . . . ? O1 Mn3 N1 Mn2 171.11(11) . . . . ? Mn1 Mn3 N1 Mn2 -47.94(8) . . . . ? Mn1 Mn3 N1 Mn2 37.43(8) 3_775 . . . ? Mn2 Mn3 N1 Mn2 -8.16(15) 3_775 . . . ? N6 Mn1 N2 C6 3.8(3) 3_775 . . . ? N5 Mn1 N2 C6 -42.6(7) 3_775 . . . ? N4 Mn1 N2 C6 -165.7(3) 3_775 . . . ? O3 Mn1 N2 C6 101.6(3) . . . . ? Mn2 Mn1 N2 C6 53.8(3) . . . . ? Mn3 Mn1 N2 C6 110.7(3) . . . . ? Mn3 Mn1 N2 C6 90.9(3) 3_775 . . . ? Mn2 Mn1 N2 C6 147.3(3) 3_775 . . . ? N6 Mn1 N2 Mn3 -106.86(11) 3_775 . . . ? N5 Mn1 N2 Mn3 -153.3(6) 3_775 . . . ? N4 Mn1 N2 Mn3 83.68(11) 3_775 . . . ? O3 Mn1 N2 Mn3 -9.07(8) . . . . ? Mn2 Mn1 N2 Mn3 -56.86(7) . . . . ? Mn3 Mn1 N2 Mn3 -19.72(17) 3_775 . . . ? Mn2 Mn1 N2 Mn3 36.67(8) 3_775 . . . ? N3 Mn3 N2 C6 153.0(2) 3_775 . . . ? N1 Mn3 N2 C6 -30.2(2) . . . . ? O3 Mn3 N2 C6 -118.2(2) . . . . ? N5 Mn3 N2 C6 -83.3(4) . . . . ? O1 Mn3 N2 C6 59.0(2) . . . . ? Mn1 Mn3 N2 C6 -126.6(2) . . . . ? Mn1 Mn3 N2 C6 -111.67(19) 3_775 . . . ? Mn2 Mn3 N2 C6 -162.7(2) 3_775 . . . ? Mn2 Mn3 N2 C6 -74.0(2) . . . . ? N3 Mn3 N2 Mn1 -80.42(11) 3_775 . . . ? N1 Mn3 N2 Mn1 96.42(11) . . . . ? O3 Mn3 N2 Mn1 8.40(7) . . . . ? N5 Mn3 N2 Mn1 43.3(4) . . . . ? O1 Mn3 N2 Mn1 -174.42(10) . . . . ? Mn1 Mn3 N2 Mn1 14.94(13) 3_775 . . . ? Mn2 Mn3 N2 Mn1 -36.08(8) 3_775 . . . ? Mn2 Mn3 N2 Mn1 52.62(7) . . . . ? N1 Mn2 N3 C7 -56.3(10) . . . . ? O3 Mn2 N3 C7 -115.38(19) . . . . ? N6 Mn2 N3 C7 159.5(2) 3_775 . . . ? N4 Mn2 N3 C7 -34.3(2) . . . . ? O2 Mn2 N3 C7 60.9(2) . . . . ? Mn1 Mn2 N3 C7 -159.12(19) . . . . ? Mn1 Mn2 N3 C7 -74.07(19) 3_775 . . . ? Mn3 Mn2 N3 C7 -125.6(2) 3_775 . . . ? Mn3 Mn2 N3 C7 -105.88(19) . . . . ? N1 Mn2 N3 Mn3 69.3(9) . . . 3_775 ? O3 Mn2 N3 Mn3 10.22(8) . . . 3_775 ? N6 Mn2 N3 Mn3 -74.90(10) 3_775 . . 3_775 ? N4 Mn2 N3 Mn3 91.32(10) . . . 3_775 ? O2 Mn2 N3 Mn3 -173.48(11) . . . 3_775 ? Mn1 Mn2 N3 Mn3 -33.52(9) . . . 3_775 ? Mn1 Mn2 N3 Mn3 51.52(7) 3_775 . . 3_775 ? Mn3 Mn2 N3 Mn3 19.72(15) . . . 3_775 ? N1 Mn2 N4 C12 -149.3(2) . . . . ? N3 Mn2 N4 C12 33.28(19) . . . . ? O3 Mn2 N4 C12 124.85(19) . . . . ? N6 Mn2 N4 C12 82.9(4) 3_775 . . . ? O2 Mn2 N4 C12 -56.1(2) . . . . ? Mn1 Mn2 N4 C12 122.16(18) . . . . ? Mn1 Mn2 N4 C12 128.1(2) 3_775 . . . ? Mn3 Mn2 N4 C12 78.22(19) 3_775 . . . ? Mn3 Mn2 N4 C12 169.29(19) . . . . ? N1 Mn2 N4 Mn1 82.61(11) . . . 3_775 ? N3 Mn2 N4 Mn1 -94.85(11) . . . 3_775 ? O3 Mn2 N4 Mn1 -3.28(7) . . . 3_775 ? N6 Mn2 N4 Mn1 -45.2(4) 3_775 . . 3_775 ? O2 Mn2 N4 Mn1 175.72(10) . . . 3_775 ? Mn1 Mn2 N4 Mn1 -5.97(14) . . . 3_775 ? Mn3 Mn2 N4 Mn1 -49.91(8) 3_775 . . 3_775 ? Mn3 Mn2 N4 Mn1 41.16(8) . . . 3_775 ? N3 Mn3 N5 C13 -30.8(2) 3_775 . . . ? N1 Mn3 N5 C13 155.9(2) . . . . ? O3 Mn3 N5 C13 -118.2(2) . . . . ? N2 Mn3 N5 C13 -153.3(3) . . . . ? O1 Mn3 N5 C13 63.8(2) . . . . ? Mn1 Mn3 N5 C13 -120.1(2) . . . . ? Mn1 Mn3 N5 C13 -115.9(2) 3_775 . . . ? Mn2 Mn3 N5 C13 -72.5(2) 3_775 . . . ? Mn2 Mn3 N5 C13 -162.5(2) . . . . ? N3 Mn3 N5 Mn1 85.11(11) 3_775 . . 3_775 ? N1 Mn3 N5 Mn1 -88.22(11) . . . 3_775 ? O3 Mn3 N5 Mn1 -2.37(7) . . . 3_775 ? N2 Mn3 N5 Mn1 -37.5(4) . . . 3_775 ? O1 Mn3 N5 Mn1 179.64(10) . . . 3_775 ? Mn1 Mn3 N5 Mn1 -4.26(13) . . . 3_775 ? Mn2 Mn3 N5 Mn1 43.40(8) 3_775 . . 3_775 ? Mn2 Mn3 N5 Mn1 -46.67(8) . . . 3_775 ? Mn2 N1 C1 C2 -107.3(3) . . . . ? Mn3 N1 C1 C2 147.4(3) . . . . ? Mn2 N1 C1 C6 75.3(3) . . . . ? Mn3 N1 C1 C6 -30.0(4) . . . . ? N1 C1 C2 C3 -178.2(4) . . . . ? C6 C1 C2 C3 -0.8(6) . . . . ? C1 C2 C3 C4 -0.7(7) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? C4 C5 C6 N2 174.5(4) . . . . ? C4 C5 C6 C1 -3.0(6) . . . . ? Mn1 N2 C6 C5 105.0(4) . . . . ? Mn3 N2 C6 C5 -152.6(3) . . . . ? Mn1 N2 C6 C1 -77.4(4) . . . . ? Mn3 N2 C6 C1 24.9(3) . . . . ? N1 C1 C6 C5 -179.8(3) . . . . ? C2 C1 C6 C5 2.6(5) . . . . ? N1 C1 C6 N2 2.5(5) . . . . ? C2 C1 C6 N2 -175.0(3) . . . . ? Mn3 N3 C7 C8 113.0(3) 3_775 . . . ? Mn2 N3 C7 C8 -143.7(3) . . . . ? Mn3 N3 C7 C12 -71.8(4) 3_775 . . . ? Mn2 N3 C7 C12 31.5(3) . . . . ? N3 C7 C8 C9 174.8(3) . . . . ? C12 C7 C8 C9 -0.4(5) . . . . ? C7 C8 C9 C10 1.0(6) . . . . ? C8 C9 C10 C11 -0.3(6) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C10 C11 C12 C7 1.5(5) . . . . ? C10 C11 C12 N4 -174.1(3) . . . . ? N3 C7 C12 C11 -176.3(3) . . . . ? C8 C7 C12 C11 -0.8(5) . . . . ? N3 C7 C12 N4 -0.6(4) . . . . ? C8 C7 C12 N4 174.9(3) . . . . ? Mn1 N4 C12 C11 -108.5(3) 3_775 . . . ? Mn2 N4 C12 C11 146.9(3) . . . . ? Mn1 N4 C12 C7 75.9(4) 3_775 . . . ? Mn2 N4 C12 C7 -28.7(3) . . . . ? Mn1 N5 C13 C14 163.4(3) 3_775 . . . ? Mn3 N5 C13 C14 -92.9(4) . . . . ? Mn1 N5 C13 C18 -17.8(4) 3_775 . . . ? Mn3 N5 C13 C18 85.9(3) . . . . ? N5 C13 C14 C15 -179.4(4) . . . . ? C18 C13 C14 C15 1.8(6) . . . . ? C13 C14 C15 C16 -1.2(6) . . . . ? C14 C15 C16 C17 0.1(7) . . . . ? C15 C16 C17 C18 0.2(6) . . . . ? C16 C17 C18 N6 178.2(4) . . . . ? C16 C17 C18 C13 0.4(5) . . . . ? Mn1 N6 C18 C17 -162.4(3) 3_775 . . . ? Mn2 N6 C18 C17 95.9(4) 3_775 . . . ? Mn1 N6 C18 C13 15.4(3) 3_775 . . . ? Mn2 N6 C18 C13 -86.2(3) 3_775 . . . ? C14 C13 C18 C17 -1.4(5) . . . . ? N5 C13 C18 C17 179.6(3) . . . . ? C14 C13 C18 N6 -179.4(3) . . . . ? N5 C13 C18 N6 1.6(4) . . . . ? C22 O1 C19 C20 6.5(8) . . . . ? Mn3 O1 C19 C20 -176.5(4) . . . . ? O1 C19 C20 C21 -25.0(11) . . . . ? O1 C19 C20 C21' 20.8(11) . . . . ? C19 C20 C21 C22 31.9(13) . . . . ? C21' C20 C21 C22 -64.4(11) . . . . ? C21 C20 C21' C22 59.6(10) . . . . ? C19 C20 C21' C22 -36.3(11) . . . . ? C19 O1 C22 C21 12.1(8) . . . . ? Mn3 O1 C22 C21 -164.8(6) . . . . ? C19 O1 C22 C21' -31.1(8) . . . . ? Mn3 O1 C22 C21' 152.0(6) . . . . ? C20 C21 C22 O1 -28.3(12) . . . . ? C20 C21 C22 C21' 69.3(11) . . . . ? C20 C21' C22 O1 40.9(10) . . . . ? C20 C21' C22 C21 -52.5(8) . . . . ? C26 O2 C23 C24 -10.4(6) . . . . ? Mn2 O2 C23 C24 142.5(5) . . . . ? O2 C23 C24 C25 17.0(9) . . . . ? C23 C24 C25 C26 -17.1(9) . . . . ? C23 O2 C26 C25 0.1(6) . . . . ? Mn2 O2 C26 C25 -151.5(4) . . . . ? C24 C25 C26 O2 10.8(8) . . . . ? C29 C27 C28 C30 -3.4(9) . . . . ? C30 O4 C29 C27 -6.7(9) . . . . ? C28 C27 C29 O4 6.2(9) . . . . ? C29 O4 C30 C28 4.5(9) . . . . ? C27 C28 C30 O4 -0.5(10) . . . . ? C33 O5 C31 C34 -24.7(18) . . . . ? C31 O5 C33 C32 29.3(18) . . . . ? C34 C32 C33 O5 -24(2) . . . . ? O5 C31 C34 C32 10(2) . . . . ? C33 C32 C34 C31 8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O4 0.92 2.48 3.377(5) 166.1 2_745 N5 H5A O4 0.92 2.26 3.179(5) 174.3 2_745 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.386 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.064