# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_jose _database_code_depnum_ccdc_archive 'CCDC 888448' #TrackingRef 'web_deposit_cif_file_0_Lise-MarieChamoreau_1340629901.jose-publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H82 Mn6 N12 O24, C2 H6 O, H2 O' _chemical_formula_sum 'C70 H90 Mn6 N12 O26' _chemical_formula_weight 1845.18 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2590(16) _cell_length_b 13.314(4) _cell_length_c 24.578(11) _cell_angle_alpha 105.19(3) _cell_angle_beta 94.24(3) _cell_angle_gamma 103.155(18) _cell_volume 4036(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 3 _cell_measurement_theta_max 17 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 63152 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.1436 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18345 _reflns_number_gt 10207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; This crystal was poorly diffracting and it was not possible to find a unique one (all were multiples). These difficulties must explain the low quality of this structure. C38 atom was refined isotropically because it was impossible to obtain positive definite adp's. Geometrical restraints were introduced for disordered EtOH molecules. Thus, Uij of atoms C32 and C64 were constrained. 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^)+(0.0609P)^2^+135.8948P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18345 _refine_ls_number_parameters 1012 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.2046 _refine_ls_R_factor_gt 0.1326 _refine_ls_wR_factor_ref 0.3580 _refine_ls_wR_factor_gt 0.3297 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.106 _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 0.03214(13) 0.62571(14) 0.50571(8) 0.0191(4) Uani 1 1 d . . . Mn2 Mn 0.25892(13) 0.70184(14) 0.58412(8) 0.0212(4) Uani 1 1 d . . . Mn3 Mn 0.22238(14) 0.51727(14) 0.46330(8) 0.0211(4) Uani 1 1 d . . . O1 O 0.1717(6) 0.6176(6) 0.5166(3) 0.0206(17) Uani 1 1 d . . . O2 O -0.1152(6) 0.6225(6) 0.5039(4) 0.0217(18) Uani 1 1 d . . . O3 O 0.1466(7) 0.7470(7) 0.6176(4) 0.028(2) Uani 1 1 d . . . O4 O 0.3492(7) 0.7844(7) 0.6514(4) 0.028(2) Uani 1 1 d . . . O5 O 0.3438(7) 0.5382(7) 0.5156(4) 0.030(2) Uani 1 1 d . . . O6 O 0.2623(6) 0.4113(7) 0.4070(3) 0.0243(19) Uani 1 1 d . . . O7 O 0.0028(6) 0.4982(6) 0.4422(3) 0.0181(16) Uani 1 1 d . . . O8 O 0.0425(7) 0.7298(8) 0.4521(4) 0.037(2) Uani 1 1 d . . . O9 O 0.2035(7) 0.8030(8) 0.4384(4) 0.035(2) Uani 1 1 d . . . O10 O 0.2928(8) 0.8362(7) 0.5445(4) 0.036(2) Uani 1 1 d D B . H10C H 0.2799 0.8315 0.5096 0.054 Uiso 1 1 d R . . O11 O 0.3028(7) 0.6475(7) 0.4274(4) 0.036(2) Uani 1 1 d D D . H11C H 0.2752 0.7000 0.4374 0.054 Uiso 1 1 d R . . O12 O 0.2184(7) 0.5439(7) 0.6170(4) 0.032(2) Uani 1 1 d . . . H12C H 0.2037 0.4936 0.5860 0.047 Uiso 1 1 d R . . N1 N 0.0634(7) 0.7413(7) 0.5775(4) 0.019(2) Uani 1 1 d . . . N2 N 0.0304(10) 0.8684(11) 0.6502(5) 0.046(3) Uani 1 1 d . . . H2A H -0.0019 0.9198 0.6590 0.069 Uiso 1 1 d R . . H2B H 0.0850 0.8725 0.6740 0.069 Uiso 1 1 d R . . N3 N 0.3739(8) 0.6411(8) 0.5556(4) 0.025(2) Uani 1 1 d . . . N4 N 0.5321(10) 0.6072(13) 0.5554(6) 0.067(5) Uani 1 1 d . . . H4A H 0.5900 0.5989 0.5698 0.101 Uiso 1 1 d R . . H4B H 0.5207 0.5896 0.5170 0.101 Uiso 1 1 d R . . N5 N 0.0917(8) 0.4905(7) 0.4139(4) 0.020(2) Uani 1 1 d . . . N6 N -0.0241(8) 0.4354(10) 0.3315(4) 0.032(3) Uani 1 1 d . . . H6A H -0.0752 0.4593 0.3465 0.048 Uiso 1 1 d R . . H6B H -0.0410 0.3902 0.2972 0.048 Uiso 1 1 d R . . C1 C -0.1407(9) 0.7182(9) 0.5169(5) 0.019(2) Uani 1 1 d . . . C2 C -0.2288(11) 0.7249(11) 0.4863(6) 0.036(3) Uani 1 1 d . . . H2 H -0.2685 0.6636 0.4588 0.043 Uiso 1 1 calc R . . C3 C -0.2619(11) 0.8226(11) 0.4951(6) 0.034(3) Uani 1 1 d . . . H3 H -0.3220 0.8259 0.4744 0.041 Uiso 1 1 calc R . . C4 C -0.2009(11) 0.9095(10) 0.5353(7) 0.038(3) Uani 1 1 d . . . H4 H -0.2175 0.9753 0.5406 0.045 Uiso 1 1 calc R . . C5 C -0.1147(10) 0.9044(10) 0.5688(6) 0.033(3) Uani 1 1 d . . . H5 H -0.0763 0.9653 0.5972 0.039 Uiso 1 1 calc R . . C6 C -0.0852(9) 0.8069(10) 0.5599(6) 0.030(3) Uani 1 1 d . . . C7 C 0.0058(9) 0.8063(10) 0.5984(5) 0.025(3) Uani 1 1 d . . . C8 C 0.4525(9) 0.8273(9) 0.6540(5) 0.025(3) Uani 1 1 d . . . C9 C 0.5009(11) 0.9243(11) 0.6948(7) 0.042(4) Uani 1 1 d . . . H9 H 0.4619 0.9581 0.7202 0.050 Uiso 1 1 calc R . . C10 C 0.6042(12) 0.9700(12) 0.6979(8) 0.049(4) Uani 1 1 d . . . H10 H 0.6347 1.0362 0.7246 0.058 Uiso 1 1 calc R . . C11 C 0.6626(12) 0.9217(15) 0.6635(8) 0.056(5) Uani 1 1 d . . . H11 H 0.7335 0.9546 0.6668 0.068 Uiso 1 1 calc R . . C12 C 0.6212(11) 0.8247(12) 0.6234(6) 0.040(3) Uani 1 1 d . . . H12 H 0.6637 0.7922 0.5999 0.048 Uiso 1 1 calc R . . C13 C 0.5150(9) 0.7750(11) 0.6178(6) 0.028(3) Uani 1 1 d . . . C14 C 0.4725(10) 0.6731(11) 0.5758(6) 0.031(3) Uani 1 1 d . . . C15 C 0.2472(10) 0.4135(10) 0.3512(6) 0.028(3) Uani 1 1 d . . . C16 C 0.3222(11) 0.3894(12) 0.3167(6) 0.037(3) Uani 1 1 d . . . H16 H 0.3800 0.3717 0.3318 0.045 Uiso 1 1 calc R . . C17 C 0.3128(12) 0.3913(14) 0.2617(6) 0.047(4) Uani 1 1 d . . . H17 H 0.3662 0.3793 0.2403 0.056 Uiso 1 1 calc R . . C18 C 0.2262(12) 0.4105(14) 0.2375(7) 0.051(4) Uani 1 1 d . . . H18 H 0.2197 0.4105 0.1995 0.061 Uiso 1 1 calc R . . C19 C 0.1492(12) 0.4298(12) 0.2693(6) 0.037(3) Uani 1 1 d . . . H19 H 0.0895 0.4417 0.2524 0.044 Uiso 1 1 calc R . . C20 C 0.1575(9) 0.4323(9) 0.3266(5) 0.024(3) Uani 1 1 d . . . C21 C 0.0716(9) 0.4536(9) 0.3585(5) 0.019(2) Uani 1 1 d . . . C22 C 0.1057(11) 0.7758(11) 0.4257(6) 0.031(3) Uani 1 1 d . . . C23 C 0.0596(10) 0.8058(9) 0.3768(5) 0.026(3) Uani 1 1 d . . . C24 C -0.0456(12) 0.8060(11) 0.3717(6) 0.037(3) Uani 1 1 d . . . H24 H -0.0876 0.7884 0.3982 0.045 Uiso 1 1 calc R . . C25 C -0.0859(13) 0.8340(13) 0.3248(7) 0.047(4) Uani 1 1 d . . . H25 H -0.1561 0.8343 0.3198 0.057 Uiso 1 1 calc R . . C26 C -0.0230(13) 0.8608(12) 0.2864(7) 0.048(4) Uani 1 1 d . . . H26 H -0.0517 0.8792 0.2558 0.058 Uiso 1 1 calc R . . C27 C 0.0803(12) 0.8615(11) 0.2914(6) 0.038(3) Uani 1 1 d . . . H27 H 0.1222 0.8793 0.2648 0.046 Uiso 1 1 calc R . . C28 C 0.1205(11) 0.8342(11) 0.3382(6) 0.033(3) Uani 1 1 d . . . H28 H 0.1911 0.8355 0.3432 0.040 Uiso 1 1 calc R . . C29 C 0.3165(17) 0.9472(13) 0.5721(9) 0.073(6) Uiso 1 1 d D . . H29A H 0.3477 0.9829 0.5455 0.110 Uiso 0.50 1 calc PR A 1 H29B H 0.3715 0.9609 0.6035 0.110 Uiso 0.50 1 calc PR A 1 H29C H 0.3201 0.9572 0.6128 0.110 Uiso 0.50 1 d PR A 2 H29D H 0.2591 0.9747 0.5606 0.110 Uiso 0.50 1 d PR A 2 C30A C 0.239(4) 1.007(4) 0.596(2) 0.106(17) Uiso 0.50 1 d PD B 1 H30A H 0.2135 1.0387 0.5688 0.159 Uiso 0.50 1 calc PR B 1 H30B H 0.2718 1.0624 0.6305 0.159 Uiso 0.50 1 calc PR B 1 H30C H 0.1810 0.9577 0.6045 0.159 Uiso 0.50 1 calc PR B 1 C30B C 0.416(3) 1.013(4) 0.560(2) 0.112(19) Uiso 0.50 1 d PD B 2 H30D H 0.4750 1.0034 0.5806 0.169 Uiso 0.50 1 calc PR B 2 H30E H 0.4158 1.0877 0.5705 0.169 Uiso 0.50 1 calc PR B 2 H30F H 0.4198 0.9897 0.5195 0.169 Uiso 0.50 1 calc PR B 2 C31 C 0.4004(17) 0.686(2) 0.4220(15) 0.119(12) Uani 1 1 d D . . H31A H 0.4089 0.6395 0.3860 0.142 Uiso 0.50 1 calc PR C 3 H31B H 0.4396 0.6667 0.4509 0.142 Uiso 0.50 1 calc PR C 3 H31C H 0.4327 0.7211 0.4612 0.142 Uiso 0.50 1 d PR C 4 H31D H 0.3984 0.7431 0.4046 0.142 Uiso 0.50 1 d PR C 4 C32A C 0.465(4) 0.793(3) 0.423(3) 0.126(15) Uiso 0.50 1 d PD D 3 H32A H 0.4459 0.8083 0.3881 0.190 Uiso 0.50 1 calc PR D 3 H32B H 0.5373 0.7934 0.4270 0.190 Uiso 0.50 1 calc PR D 3 H32C H 0.4524 0.8468 0.4545 0.190 Uiso 0.50 1 calc PR D 3 C32B C 0.484(4) 0.639(5) 0.397(3) 0.126(15) Uiso 0.50 1 d PD D 4 H32D H 0.5076 0.5991 0.4203 0.190 Uiso 0.50 1 calc PR D 4 H32E H 0.5414 0.6956 0.3945 0.190 Uiso 0.50 1 calc PR D 4 H32F H 0.4564 0.5915 0.3593 0.190 Uiso 0.50 1 calc PR D 4 C33 C 0.300(2) 0.5188(19) 0.6478(9) 0.092(8) Uani 1 1 d D . . H33A H 0.3463 0.5855 0.6720 0.110 Uiso 1 1 calc R . . H33B H 0.3404 0.4844 0.6209 0.110 Uiso 1 1 calc R . . C34 C 0.264(4) 0.447(3) 0.6841(17) 0.21(2) Uani 1 1 d D . . H34A H 0.2260 0.4814 0.7119 0.316 Uiso 1 1 calc R . . H34B H 0.3237 0.4343 0.7031 0.316 Uiso 1 1 calc R . . H34C H 0.2195 0.3800 0.6606 0.316 Uiso 1 1 calc R . . Mn4 Mn 0.02888(13) 0.61997(14) -0.00379(8) 0.0192(4) Uani 1 1 d . . . Mn5 Mn 0.21648(14) 0.61605(15) -0.08187(8) 0.0214(4) Uani 1 1 d . F . Mn6 Mn 0.24006(14) 0.55390(15) 0.03681(8) 0.0199(4) Uani 1 1 d . . . O13 O 0.1623(6) 0.5982(7) -0.0157(3) 0.0211(17) Uani 1 1 d . . . O14 O -0.1181(6) 0.6185(6) -0.0038(3) 0.0207(17) Uani 1 1 d . . . O15 O 0.0880(7) 0.6287(7) -0.1136(4) 0.029(2) Uani 1 1 d . . . O16 O 0.2737(7) 0.6321(7) -0.1480(4) 0.028(2) Uani 1 1 d . . . O17 O 0.3337(7) 0.5199(7) -0.0158(4) 0.028(2) Uani 1 1 d . . . O18 O 0.3094(6) 0.5107(7) 0.0944(3) 0.0225(18) Uani 1 1 d . . . O19 O 0.0312(6) 0.5574(6) 0.0588(3) 0.0181(16) Uani 1 1 d . . . O20 O 0.0652(8) 0.7771(8) 0.0552(4) 0.040(2) Uani 1 1 d . . . O21 O 0.2313(7) 0.8675(8) 0.0658(4) 0.037(2) Uani 1 1 d . . . O22 O 0.2697(7) 0.7916(7) -0.0400(4) 0.032(2) Uani 1 1 d . F . H22C H 0.2797 0.8280 -0.0046 0.048 Uiso 1 1 d R . . O23 O 0.3352(7) 0.7206(7) 0.0735(4) 0.033(2) Uani 1 1 d . H . H23C H 0.3106 0.7713 0.0687 0.049 Uiso 1 1 d R . . N7 N 0.0257(7) 0.6634(8) -0.0730(4) 0.022(2) Uani 1 1 d . . . N8 N -0.0231(10) 0.7473(11) -0.1355(5) 0.046(3) Uani 1 1 d . . . H8A H 0.0275 0.7344 -0.1551 0.069 Uiso 1 1 d R . . H8B H -0.0725 0.7685 -0.1515 0.069 Uiso 1 1 d R . . N9 N 0.3438(8) 0.5823(8) -0.0531(4) 0.023(2) Uani 1 1 d . . . N10 N 0.5017(9) 0.5446(12) -0.0559(5) 0.045(3) Uani 1 1 d . . . H10A H 0.5105 0.5780 -0.0191 0.068 Uiso 1 1 d R . . H10B H 0.5587 0.5394 -0.0695 0.068 Uiso 1 1 d R . . N11 N 0.1341(7) 0.5808(8) 0.0865(4) 0.022(2) Uani 1 1 d . . . N12 N 0.0617(9) 0.6118(10) 0.1694(5) 0.040(3) Uani 1 1 d . . . H12A H -0.0055 0.5918 0.1569 0.059 Uiso 1 1 d R . . H12B H 0.0808 0.6124 0.2045 0.059 Uiso 1 1 d R . . C35 C -0.1471(9) 0.7042(10) -0.0127(6) 0.027(3) Uani 1 1 d . . . C36 C -0.2259(10) 0.7390(11) 0.0174(6) 0.034(3) Uani 1 1 d . . . H36 H -0.2552 0.7022 0.0421 0.041 Uiso 1 1 calc R . . C37 C -0.2607(12) 0.8276(10) 0.0107(6) 0.035(3) Uani 1 1 d . . . H37 H -0.3135 0.8489 0.0300 0.042 Uiso 1 1 calc R . . C38 C -0.2144(11) 0.8817(11) -0.0250(6) 0.034(3) Uiso 1 1 d . . . H38 H -0.2327 0.9437 -0.0279 0.041 Uiso 1 1 calc R . . C39 C -0.1407(10) 0.8461(11) -0.0570(7) 0.035(3) Uani 1 1 d . . . H39 H -0.1138 0.8809 -0.0830 0.042 Uiso 1 1 calc R . . C40 C -0.1076(9) 0.7581(9) -0.0499(6) 0.025(3) Uani 1 1 d . . . C41 C -0.0339(10) 0.7212(11) -0.0886(6) 0.029(3) Uani 1 1 d . . . C42 C 0.3769(10) 0.6740(10) -0.1483(5) 0.026(3) Uani 1 1 d . . . C43 C 0.4058(12) 0.7332(14) -0.1857(7) 0.045(4) Uani 1 1 d . . . H43 H 0.3543 0.7418 -0.2107 0.054 Uiso 1 1 calc R . . C44 C 0.5077(14) 0.7789(14) -0.1869(8) 0.052(5) Uani 1 1 d . . . H44 H 0.5248 0.8207 -0.2115 0.062 Uiso 1 1 calc R . . C45 C 0.5844(11) 0.7646(13) -0.1529(7) 0.043(4) Uani 1 1 d . . . H45 H 0.6540 0.7960 -0.1544 0.052 Uiso 1 1 calc R . . C46 C 0.5601(11) 0.7035(12) -0.1159(6) 0.036(3) Uani 1 1 d . . . H46 H 0.6132 0.6942 -0.0923 0.043 Uiso 1 1 calc R . . C47 C 0.4551(9) 0.6553(10) -0.1139(5) 0.025(3) Uani 1 1 d . . . C48 C 0.4325(9) 0.5930(10) -0.0739(5) 0.025(3) Uani 1 1 d . . . C49 C 0.3254(10) 0.5766(11) 0.1488(6) 0.029(3) Uani 1 1 d . . . C50 C 0.4205(11) 0.5933(13) 0.1828(6) 0.042(4) Uani 1 1 d . . . H50 H 0.4708 0.5598 0.1677 0.050 Uiso 1 1 calc R . . C51 C 0.4408(13) 0.6575(15) 0.2373(7) 0.053(5) Uani 1 1 d . . . H51 H 0.5050 0.6684 0.2590 0.064 Uiso 1 1 calc R . . C52 C 0.3661(14) 0.7072(16) 0.2611(7) 0.061(5) Uani 1 1 d . . . H52 H 0.3802 0.7529 0.2981 0.073 Uiso 1 1 calc R . . C53 C 0.2704(12) 0.6866(13) 0.2282(6) 0.044(4) Uani 1 1 d . . . H53 H 0.2198 0.7185 0.2441 0.053 Uiso 1 1 calc R . . C54 C 0.2470(10) 0.6212(11) 0.1730(6) 0.030(3) Uani 1 1 d . . . C55 C 0.1444(10) 0.6038(10) 0.1422(5) 0.025(3) Uani 1 1 d . . . C56 C 0.1405(11) 0.8536(10) 0.0794(6) 0.030(3) Uani 1 1 d . . . C57 C 0.1217(11) 0.9376(9) 0.1293(6) 0.029(3) Uani 1 1 d . . . C58 C 0.0173(14) 0.9435(13) 0.1348(7) 0.049(4) Uani 1 1 d . . . H58 H -0.0389 0.8957 0.1090 0.059 Uiso 1 1 calc R . . C59 C 0.0024(16) 1.0237(15) 0.1802(8) 0.059(5) Uani 1 1 d . . . H59 H -0.0653 1.0277 0.1857 0.071 Uiso 1 1 calc R . . C60 C 0.0847(19) 1.0969(14) 0.2171(8) 0.064(6) Uani 1 1 d . . . H60 H 0.0728 1.1513 0.2464 0.077 Uiso 1 1 calc R . . C61 C 0.1872(16) 1.0894(12) 0.2103(7) 0.054(5) Uani 1 1 d . . . H61 H 0.2441 1.1370 0.2357 0.064 Uiso 1 1 calc R . . C62 C 0.2013(12) 1.0095(11) 0.1651(6) 0.038(3) Uani 1 1 d . . . H62 H 0.2691 1.0059 0.1594 0.045 Uiso 1 1 calc R . . C63 C 0.2765(14) 0.8713(12) -0.0689(8) 0.057(5) Uani 1 1 d D . . H63A H 0.2211 0.9076 -0.0621 0.069 Uiso 0.50 1 calc PR E 1 H63B H 0.2734 0.8405 -0.1096 0.069 Uiso 0.50 1 calc PR E 1 H63C H 0.2287 0.9147 -0.0556 0.069 Uiso 0.50 1 d PR E 2 H63D H 0.2543 0.8360 -0.1093 0.069 Uiso 0.50 1 d PR E 2 C64A C 0.384(2) 0.948(3) -0.0425(19) 0.072(9) Uiso 0.50 1 d PD F 1 H64A H 0.3969 0.9516 -0.0030 0.109 Uiso 0.50 1 calc PR F 1 H64B H 0.3853 1.0184 -0.0459 0.109 Uiso 0.50 1 calc PR F 1 H64C H 0.4371 0.9218 -0.0620 0.109 Uiso 0.50 1 calc PR F 1 C64B C 0.383(2) 0.943(4) -0.067(2) 0.072(9) Uiso 0.50 1 d PD F 2 H64D H 0.4212 0.9622 -0.0289 0.109 Uiso 0.50 1 calc PR F 2 H64E H 0.3759 1.0075 -0.0755 0.109 Uiso 0.50 1 calc PR F 2 H64F H 0.4206 0.9063 -0.0936 0.109 Uiso 0.50 1 calc PR F 2 C65 C 0.4449(13) 0.7634(16) 0.0764(9) 0.071(6) Uani 1 1 d D . . H65A H 0.4610 0.7843 0.0424 0.086 Uiso 0.60 1 calc PR G 3 H65B H 0.4833 0.7116 0.0811 0.086 Uiso 0.60 1 calc PR G 3 H65C H 0.4550 0.8024 0.0481 0.086 Uiso 0.40 1 d PR G 4 H65D H 0.4752 0.7027 0.0647 0.086 Uiso 0.40 1 d PR G 4 C66A C 0.471(3) 0.862(3) 0.1292(13) 0.077(11) Uiso 0.60 1 d PD H 3 H66A H 0.4209 0.9038 0.1274 0.115 Uiso 0.60 1 calc PR H 3 H66B H 0.5398 0.9053 0.1302 0.115 Uiso 0.60 1 calc PR H 3 H66C H 0.4673 0.8385 0.1629 0.115 Uiso 0.60 1 calc PR H 3 C66B C 0.510(5) 0.839(5) 0.1314(19) 0.10(2) Uiso 0.40 1 d PD H 4 H66D H 0.4924 0.9072 0.1390 0.148 Uiso 0.40 1 calc PR H 4 H66E H 0.5826 0.8492 0.1280 0.148 Uiso 0.40 1 calc PR H 4 H66F H 0.4946 0.8085 0.1622 0.148 Uiso 0.40 1 calc PR H 4 O24 O 0.1551(7) 0.4204(7) -0.1175(4) 0.031(2) Uani 1 1 d . . . H24C H 0.1486 0.3998 -0.0877 0.046 Uiso 0.70 1 d PR I 1 H24D H 0.1571 0.3986 -0.0879 0.046 Uiso 0.30 1 d PR I 2 C67A C 0.216(2) 0.3500(19) -0.1448(10) 0.044(5) Uiso 0.70 1 d P J 1 H67A H 0.2808 0.3628 -0.1201 0.053 Uiso 0.70 1 calc PR J 1 H67B H 0.1774 0.2757 -0.1511 0.053 Uiso 0.70 1 calc PR J 1 C67B C 0.161(4) 0.333(4) -0.163(2) 0.041(12) Uiso 0.30 1 d P J 2 H67C H 0.0931 0.3025 -0.1863 0.049 Uiso 0.30 1 calc PR J 2 H67D H 0.1795 0.2783 -0.1481 0.049 Uiso 0.30 1 calc PR J 2 C68 C 0.239(2) 0.367(2) -0.1983(11) 0.103(8) Uiso 1 1 d . . . H68A H 0.2793 0.3194 -0.2156 0.154 Uiso 0.70 1 calc PR J 1 H68B H 0.2780 0.4404 -0.1921 0.154 Uiso 0.70 1 calc PR J 1 H68C H 0.1747 0.3535 -0.2231 0.154 Uiso 0.70 1 calc PR J 1 H68D H 0.2722 0.3105 -0.2123 0.154 Uiso 0.30 1 d PR J 2 H68E H 0.2905 0.4307 -0.1759 0.154 Uiso 0.30 1 d PR J 2 H68F H 0.2050 0.3827 -0.2299 0.154 Uiso 0.30 1 d PR J 2 O25 O 0.2228(9) 0.8592(10) 0.7380(5) 0.055(3) Uani 1 1 d . . . H25C H 0.2678 0.8409 0.7173 0.083 Uiso 1 1 d R . . C69 C 0.2848(16) 0.9581(15) 0.7789(8) 0.062(5) Uani 1 1 d . . . H69A H 0.3562 0.9534 0.7861 0.075 Uiso 1 1 calc R . . H69B H 0.2564 0.9682 0.8147 0.075 Uiso 1 1 calc R . . C70 C 0.2835(17) 1.051(2) 0.7565(11) 0.093(8) Uani 1 1 d . . . H70A H 0.2849 1.0303 0.7161 0.140 Uiso 1 1 calc R . . H70B H 0.3438 1.1094 0.7747 0.140 Uiso 1 1 calc R . . H70C H 0.2211 1.0743 0.7641 0.140 Uiso 1 1 calc R . . O100 O 0.1229(8) 0.6919(10) 0.7805(4) 0.050(3) Uani 1 1 d . . . H1WA H 0.1553 0.7434 0.7689 0.074 Uiso 1 1 d R . . H1WB H 0.1669 0.6778 0.8025 0.074 Uiso 1 1 d 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 0.0151(9) 0.0168(9) 0.0235(10) 0.0015(7) 0.0006(7) 0.0060(7) Mn2 0.0153(9) 0.0212(9) 0.0229(10) -0.0016(7) -0.0017(7) 0.0067(7) Mn3 0.0164(9) 0.0213(9) 0.0233(10) -0.0005(7) 0.0001(7) 0.0089(7) O1 0.013(4) 0.024(4) 0.023(4) 0.001(3) 0.001(3) 0.007(3) O2 0.014(4) 0.019(4) 0.030(5) 0.003(3) -0.002(3) 0.008(3) O3 0.034(5) 0.028(5) 0.022(5) 0.001(4) -0.001(4) 0.015(4) O4 0.023(5) 0.029(5) 0.025(5) -0.003(4) -0.005(4) 0.004(4) O5 0.025(5) 0.026(5) 0.028(5) -0.011(4) -0.014(4) 0.012(4) O6 0.011(4) 0.035(5) 0.020(4) -0.010(4) 0.000(3) 0.012(3) O7 0.014(4) 0.016(4) 0.023(4) 0.002(3) 0.002(3) 0.006(3) O8 0.037(6) 0.037(6) 0.048(6) 0.024(5) 0.018(5) 0.015(4) O9 0.027(5) 0.038(5) 0.041(6) 0.019(5) -0.001(4) 0.003(4) O10 0.056(6) 0.015(4) 0.039(6) 0.010(4) -0.001(5) 0.010(4) O11 0.022(5) 0.030(5) 0.057(7) 0.010(5) 0.008(4) 0.009(4) O12 0.023(5) 0.039(5) 0.035(5) 0.013(4) 0.000(4) 0.013(4) N1 0.013(5) 0.020(5) 0.026(5) 0.007(4) 0.000(4) 0.011(4) N2 0.042(7) 0.057(8) 0.036(7) -0.006(6) -0.003(6) 0.031(6) N3 0.024(6) 0.020(5) 0.029(6) 0.005(4) 0.000(4) 0.006(4) N4 0.036(8) 0.109(13) 0.055(9) -0.006(9) -0.010(7) 0.053(9) N5 0.026(5) 0.014(5) 0.021(5) 0.004(4) 0.008(4) 0.008(4) N6 0.022(6) 0.052(7) 0.020(6) 0.007(5) -0.002(4) 0.010(5) C1 0.016(6) 0.024(6) 0.019(6) 0.005(5) 0.001(4) 0.009(5) C2 0.031(8) 0.024(7) 0.046(9) -0.002(6) -0.004(6) 0.010(6) C3 0.039(8) 0.029(7) 0.040(8) 0.024(6) 0.001(6) 0.007(6) C4 0.045(9) 0.014(6) 0.057(10) 0.005(6) 0.005(7) 0.018(6) C5 0.027(7) 0.016(6) 0.049(9) -0.004(6) -0.001(6) 0.011(5) C6 0.014(6) 0.017(6) 0.062(9) 0.013(6) 0.006(6) 0.006(5) C7 0.022(6) 0.024(6) 0.025(7) -0.005(5) 0.007(5) 0.008(5) C8 0.022(6) 0.021(6) 0.026(7) 0.003(5) -0.009(5) 0.004(5) C9 0.035(8) 0.029(7) 0.048(9) -0.004(7) 0.007(7) 0.001(6) C10 0.030(8) 0.032(8) 0.068(12) 0.002(8) -0.007(8) -0.004(6) C11 0.023(8) 0.064(12) 0.074(13) 0.023(10) -0.003(8) -0.005(8) C12 0.031(8) 0.042(9) 0.036(8) 0.005(7) -0.001(6) -0.001(6) C13 0.015(6) 0.035(7) 0.031(7) 0.008(6) -0.001(5) 0.005(5) C14 0.015(6) 0.040(8) 0.040(8) 0.014(6) -0.005(5) 0.009(5) C15 0.028(7) 0.022(6) 0.034(7) 0.003(5) 0.011(6) 0.008(5) C16 0.026(7) 0.046(9) 0.037(8) 0.002(7) 0.004(6) 0.016(6) C17 0.030(8) 0.069(11) 0.030(8) -0.008(7) 0.010(6) 0.015(7) C18 0.041(9) 0.069(12) 0.034(9) 0.010(8) 0.011(7) 0.004(8) C19 0.040(8) 0.049(9) 0.031(8) 0.019(7) 0.017(6) 0.016(7) C20 0.019(6) 0.022(6) 0.025(6) 0.004(5) 0.007(5) -0.002(5) C21 0.018(6) 0.017(6) 0.020(6) 0.002(5) 0.007(5) 0.003(4) C22 0.033(8) 0.031(7) 0.032(7) 0.008(6) 0.003(6) 0.015(6) C23 0.034(7) 0.011(5) 0.030(7) 0.008(5) 0.006(5) -0.001(5) C24 0.043(9) 0.032(8) 0.032(8) 0.007(6) -0.008(6) 0.006(6) C25 0.037(9) 0.050(10) 0.053(10) 0.019(8) -0.005(7) 0.007(7) C26 0.056(11) 0.039(9) 0.046(10) 0.021(7) -0.012(8) 0.001(7) C27 0.055(10) 0.035(8) 0.026(7) 0.010(6) -0.001(7) 0.013(7) C28 0.038(8) 0.030(7) 0.030(7) 0.005(6) -0.001(6) 0.008(6) C31 0.056(14) 0.13(2) 0.23(3) 0.11(2) 0.076(19) 0.035(14) C33 0.14(2) 0.098(18) 0.047(12) 0.023(12) -0.025(13) 0.063(17) C34 0.32(7) 0.24(5) 0.14(4) 0.10(4) 0.09(4) 0.13(5) Mn4 0.0158(9) 0.0217(9) 0.0250(10) 0.0117(7) 0.0060(7) 0.0076(7) Mn5 0.0174(9) 0.0286(10) 0.0251(10) 0.0142(8) 0.0085(7) 0.0105(7) Mn6 0.0171(9) 0.0267(10) 0.0225(10) 0.0129(8) 0.0068(7) 0.0102(7) O13 0.017(4) 0.029(5) 0.025(4) 0.016(4) 0.010(3) 0.009(3) O14 0.026(4) 0.015(4) 0.026(4) 0.011(3) 0.011(4) 0.009(3) O15 0.037(5) 0.036(5) 0.024(5) 0.014(4) 0.015(4) 0.018(4) O16 0.024(5) 0.044(5) 0.024(5) 0.018(4) 0.012(4) 0.012(4) O17 0.037(5) 0.034(5) 0.031(5) 0.024(4) 0.022(4) 0.021(4) O18 0.012(4) 0.041(5) 0.021(4) 0.013(4) 0.007(3) 0.015(4) O19 0.016(4) 0.022(4) 0.021(4) 0.010(3) 0.005(3) 0.007(3) O20 0.036(6) 0.029(5) 0.050(6) 0.006(5) -0.006(5) 0.010(4) O21 0.028(5) 0.036(5) 0.046(6) 0.008(5) 0.007(4) 0.009(4) O22 0.048(6) 0.022(4) 0.033(5) 0.011(4) 0.017(4) 0.017(4) O23 0.026(5) 0.034(5) 0.044(6) 0.019(4) 0.007(4) 0.007(4) N7 0.012(5) 0.028(5) 0.032(6) 0.013(5) 0.008(4) 0.009(4) N8 0.049(8) 0.079(10) 0.035(7) 0.030(7) 0.019(6) 0.046(7) N9 0.019(5) 0.028(5) 0.028(6) 0.010(4) 0.009(4) 0.010(4) N10 0.030(7) 0.091(10) 0.037(7) 0.026(7) 0.018(5) 0.047(7) N11 0.018(5) 0.030(6) 0.020(5) 0.007(4) -0.001(4) 0.012(4) N12 0.024(6) 0.062(8) 0.024(6) -0.004(6) 0.011(5) 0.011(6) C35 0.019(6) 0.032(7) 0.031(7) 0.006(6) 0.004(5) 0.014(5) C36 0.028(7) 0.039(8) 0.042(8) 0.017(7) 0.016(6) 0.012(6) C37 0.047(9) 0.024(7) 0.030(7) 0.001(6) 0.011(6) 0.007(6) C39 0.029(7) 0.035(8) 0.052(9) 0.023(7) 0.015(6) 0.017(6) C40 0.020(6) 0.020(6) 0.035(7) 0.009(5) -0.001(5) 0.007(5) C41 0.019(6) 0.034(7) 0.041(8) 0.022(6) 0.009(5) 0.008(5) C42 0.028(7) 0.028(7) 0.030(7) 0.014(5) 0.018(5) 0.016(5) C43 0.041(9) 0.069(11) 0.050(10) 0.042(9) 0.021(7) 0.032(8) C44 0.058(11) 0.057(11) 0.063(11) 0.040(9) 0.040(9) 0.021(8) C45 0.025(8) 0.062(10) 0.045(9) 0.025(8) 0.017(7) -0.003(7) C46 0.029(7) 0.049(9) 0.036(8) 0.026(7) 0.014(6) 0.005(6) C47 0.016(6) 0.036(7) 0.027(7) 0.012(5) 0.005(5) 0.008(5) C48 0.018(6) 0.029(7) 0.027(7) 0.005(5) 0.007(5) 0.009(5) C49 0.023(7) 0.038(7) 0.033(7) 0.020(6) 0.004(5) 0.013(6) C50 0.030(8) 0.060(10) 0.034(8) 0.009(7) 0.001(6) 0.014(7) C51 0.042(9) 0.075(12) 0.033(9) -0.001(8) -0.016(7) 0.022(9) C52 0.060(11) 0.081(13) 0.027(8) -0.017(8) -0.013(8) 0.037(10) C53 0.031(8) 0.057(10) 0.036(8) 0.000(7) -0.007(6) 0.012(7) C54 0.030(7) 0.037(7) 0.032(7) 0.015(6) 0.009(6) 0.019(6) C55 0.023(6) 0.029(7) 0.024(6) 0.009(5) 0.000(5) 0.005(5) C56 0.033(8) 0.023(7) 0.032(7) 0.009(6) 0.010(6) 0.005(6) C57 0.047(8) 0.011(6) 0.029(7) 0.008(5) 0.009(6) 0.005(5) C58 0.058(11) 0.041(9) 0.056(11) 0.023(8) 0.029(9) 0.010(8) C59 0.077(13) 0.053(11) 0.067(13) 0.024(10) 0.047(11) 0.035(10) C60 0.125(19) 0.038(10) 0.049(11) 0.022(8) 0.046(12) 0.037(11) C61 0.088(14) 0.029(8) 0.031(8) -0.004(6) 0.012(9) 0.000(8) C62 0.048(9) 0.036(8) 0.033(8) 0.017(6) 0.003(7) 0.011(7) C63 0.090(14) 0.032(8) 0.065(12) 0.024(8) 0.047(11) 0.024(9) C65 0.034(10) 0.079(14) 0.083(15) 0.023(12) -0.016(9) -0.011(9) O24 0.025(5) 0.032(5) 0.032(5) 0.004(4) 0.007(4) 0.005(4) O25 0.053(7) 0.060(8) 0.040(6) -0.003(6) 0.009(5) 0.012(6) C69 0.077(14) 0.058(12) 0.052(11) 0.020(9) 0.004(10) 0.015(10) C70 0.062(14) 0.103(19) 0.11(2) 0.011(15) -0.022(13) 0.040(13) O100 0.037(6) 0.077(8) 0.036(6) 0.022(6) 0.003(5) 0.012(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 O1 1.882(8) . ? Mn1 O7 1.921(8) . ? Mn1 O2 1.941(8) . ? Mn1 N1 1.958(10) . ? Mn1 O8 2.137(9) . ? Mn1 O7 2.328(8) 2_566 ? Mn1 Mn1 3.191(4) 2_566 ? Mn2 O1 1.870(8) . ? Mn2 O4 1.879(8) . ? Mn2 O3 1.893(9) . ? Mn2 N3 1.972(10) . ? Mn2 O10 2.227(9) . ? Mn2 O12 2.408(9) . ? Mn3 O1 1.891(8) . ? Mn3 O6 1.900(8) . ? Mn3 O5 1.903(8) . ? Mn3 N5 1.945(10) . ? Mn3 O11 2.241(10) . ? Mn3 O2 2.426(8) 2_566 ? O2 C1 1.355(13) . ? O2 Mn3 2.426(8) 2_566 ? O3 N1 1.398(12) . ? O4 C8 1.348(15) . ? O5 N3 1.411(13) . ? O6 C15 1.381(16) . ? O7 N5 1.423(12) . ? O7 Mn1 2.328(8) 2_566 ? O8 C22 1.247(16) . ? O9 C22 1.256(16) . ? O10 C29 1.406(15) . ? O10 H10C 0.8460 . ? O11 C31 1.31(2) . ? O11 H11C 0.8497 . ? O12 C33 1.43(2) . ? O12 H12C 0.8472 . ? N1 C7 1.311(14) . ? N2 C7 1.294(16) . ? N2 H2A 0.8765 . ? N2 H2B 0.8790 . ? N3 C14 1.295(16) . ? N4 C14 1.338(18) . ? N4 H4A 0.8632 . ? N4 H4B 0.9033 . ? N5 C21 1.304(15) . ? N6 C21 1.328(15) . ? N6 H6A 0.8778 . ? N6 H6B 0.8753 . ? C1 C6 1.375(17) . ? C1 C2 1.375(17) . ? C2 C3 1.435(18) . ? C2 H2 0.9300 . ? C3 C4 1.351(19) . ? C3 H3 0.9300 . ? C4 C5 1.385(19) . ? C4 H4 0.9300 . ? C5 C6 1.407(16) . ? C5 H5 0.9300 . ? C6 C7 1.479(18) . ? C8 C9 1.391(18) . ? C8 C13 1.419(18) . ? C9 C10 1.35(2) . ? C9 H9 0.9300 . ? C10 C11 1.33(2) . ? C10 H10 0.9300 . ? C11 C12 1.37(2) . ? C11 H11 0.9300 . ? C12 C13 1.392(18) . ? C12 H12 0.9300 . ? C13 C14 1.433(19) . ? C15 C16 1.391(18) . ? C15 C20 1.396(18) . ? C16 C17 1.36(2) . ? C16 H16 0.9300 . ? C17 C18 1.36(2) . ? C17 H17 0.9300 . ? C18 C19 1.36(2) . ? C18 H18 0.9300 . ? C19 C20 1.396(18) . ? C19 H19 0.9300 . ? C20 C21 1.469(16) . ? C22 C23 1.494(18) . ? C23 C28 1.363(18) . ? C23 C24 1.393(19) . ? C24 C25 1.41(2) . ? C24 H24 0.9300 . ? C25 C26 1.37(2) . ? C25 H25 0.9300 . ? C26 C27 1.36(2) . ? C26 H26 0.9300 . ? C27 C28 1.400(19) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30A 1.504(19) . ? C29 C30B 1.51(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C29 H29D 0.9700 . ? C30A H29D 0.9556 . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31 C32A 1.477(19) . ? C31 C32B 1.49(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C31 H31D 0.9700 . ? C32A H31D 0.9669 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33 C34 1.492(19) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? Mn4 O13 1.888(8) . ? Mn4 O19 1.933(8) . ? Mn4 N7 1.936(10) . ? Mn4 O14 1.944(8) . ? Mn4 O20 2.135(10) . ? Mn4 O19 2.313(8) 2_565 ? Mn4 Mn4 3.170(4) 2_565 ? Mn5 O13 1.876(8) . ? Mn5 O15 1.882(9) . ? Mn5 O16 1.885(8) . ? Mn5 N9 1.972(10) . ? Mn5 O22 2.214(9) . ? Mn5 O24 2.439(9) . ? Mn6 O13 1.885(8) . ? Mn6 O17 1.898(8) . ? Mn6 O18 1.913(8) . ? Mn6 N11 1.962(10) . ? Mn6 O23 2.200(9) . ? Mn6 O14 2.384(8) 2_565 ? O14 C35 1.347(14) . ? O14 Mn6 2.384(8) 2_565 ? O15 N7 1.394(12) . ? O16 C42 1.356(15) . ? O17 N9 1.384(12) . ? O18 C49 1.364(16) . ? O19 N11 1.407(12) . ? O19 Mn4 2.313(8) 2_565 ? O20 C56 1.233(16) . ? O21 C56 1.258(16) . ? O22 C63 1.415(17) . ? O22 H22C 0.8606 . ? O23 C65 1.425(19) . ? O23 H23C 0.8440 . ? N7 C41 1.323(15) . ? N8 C41 1.297(17) . ? N8 H8A 0.8771 . ? N8 H8B 0.8761 . ? N9 C48 1.310(15) . ? N10 C48 1.345(16) . ? N10 H10A 0.8821 . ? N10 H10B 0.8590 . ? N11 C55 1.310(15) . ? N12 C55 1.337(16) . ? N12 H12A 0.8766 . ? N12 H12B 0.8780 . ? C35 C40 1.367(18) . ? C35 C36 1.417(17) . ? C36 C37 1.403(19) . ? C36 H36 0.9300 . ? C37 C38 1.371(19) . ? C37 H37 0.9300 . ? C38 C39 1.388(19) . ? C38 H38 0.9300 . ? C39 C40 1.388(17) . ? C39 H39 0.9300 . ? C40 C41 1.487(18) . ? C42 C43 1.382(18) . ? C42 C47 1.397(17) . ? C43 C44 1.36(2) . ? C43 H43 0.9300 . ? C44 C45 1.35(2) . ? C44 H44 0.9300 . ? C45 C46 1.381(19) . ? C45 H45 0.9300 . ? C46 C47 1.404(17) . ? C46 H46 0.9300 . ? C47 C48 1.450(17) . ? C49 C50 1.398(18) . ? C49 C54 1.406(17) . ? C50 C51 1.36(2) . ? C50 H50 0.9300 . ? C51 C52 1.39(2) . ? C51 H51 0.9300 . ? C52 C53 1.38(2) . ? C52 H52 0.9300 . ? C53 C54 1.37(2) . ? C53 H53 0.9300 . ? C54 C55 1.446(18) . ? C56 C57 1.507(17) . ? C57 C62 1.328(19) . ? C57 C58 1.42(2) . ? C58 C59 1.39(2) . ? C58 H58 0.9300 . ? C59 C60 1.37(3) . ? C59 H59 0.9300 . ? C60 C61 1.40(3) . ? C60 H60 0.9300 . ? C61 C62 1.38(2) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64B 1.505(19) . ? C63 C64A 1.532(19) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? C63 H63D 0.9700 . ? C64A H64A 0.9600 . ? C64A H64B 0.9600 . ? C64A H64C 0.9600 . ? C64B H64D 0.9600 . ? C64B H64E 0.9600 . ? C64B H64F 0.9600 . ? C65 C66B 1.52(2) . ? C65 C66A 1.537(19) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C65 H65C 0.9700 . ? C65 H65D 0.9700 . ? C66A H66A 0.9600 . ? C66A H66B 0.9600 . ? C66A H66C 0.9600 . ? C66B H66D 0.9600 . ? C66B H66E 0.9600 . ? C66B H66F 0.9600 . ? O24 C67B 1.41(5) . ? O24 C67A 1.44(2) . ? O24 H24C 0.8496 . ? O24 H24D 0.8504 . ? C67A C68 1.44(3) . ? C67A H67A 0.9700 . ? C67A H67B 0.9700 . ? C67B C68 1.47(6) . ? C67B H67C 0.9700 . ? C67B H67D 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C68 H68D 0.9600 . ? C68 H68E 0.9600 . ? C68 H68F 0.9600 . ? O25 C69 1.45(2) . ? O25 H25C 0.8496 . ? C69 C70 1.49(3) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? O100 H1WA 0.8501 . ? O100 H1WB 0.8499 . ? 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 O7 89.3(3) . . ? O1 Mn1 O2 170.8(4) . . ? O7 Mn1 O2 91.9(3) . . ? O1 Mn1 N1 88.0(4) . . ? O7 Mn1 N1 171.4(4) . . ? O2 Mn1 N1 89.6(4) . . ? O1 Mn1 O8 101.3(4) . . ? O7 Mn1 O8 93.0(4) . . ? O2 Mn1 O8 87.8(4) . . ? N1 Mn1 O8 95.5(4) . . ? O1 Mn1 O7 85.6(3) . 2_566 ? O7 Mn1 O7 83.1(3) . 2_566 ? O2 Mn1 O7 85.5(3) . 2_566 ? N1 Mn1 O7 88.6(3) . 2_566 ? O8 Mn1 O7 172.1(3) . 2_566 ? O1 Mn1 Mn1 86.4(3) . 2_566 ? O7 Mn1 Mn1 46.4(2) . 2_566 ? O2 Mn1 Mn1 87.8(2) . 2_566 ? N1 Mn1 Mn1 125.2(3) . 2_566 ? O8 Mn1 Mn1 139.0(3) . 2_566 ? O7 Mn1 Mn1 36.70(19) 2_566 2_566 ? O1 Mn2 O4 178.5(4) . . ? O1 Mn2 O3 92.4(4) . . ? O4 Mn2 O3 89.1(4) . . ? O1 Mn2 N3 89.2(4) . . ? O4 Mn2 N3 89.3(4) . . ? O3 Mn2 N3 172.2(4) . . ? O1 Mn2 O10 88.1(4) . . ? O4 Mn2 O10 92.3(4) . . ? O3 Mn2 O10 92.9(4) . . ? N3 Mn2 O10 94.7(4) . . ? O1 Mn2 O12 86.5(3) . . ? O4 Mn2 O12 93.1(4) . . ? O3 Mn2 O12 89.9(4) . . ? N3 Mn2 O12 82.6(4) . . ? O10 Mn2 O12 174.0(3) . . ? O1 Mn3 O6 175.5(3) . . ? O1 Mn3 O5 91.7(4) . . ? O6 Mn3 O5 92.3(3) . . ? O1 Mn3 N5 86.5(4) . . ? O6 Mn3 N5 89.3(4) . . ? O5 Mn3 N5 175.4(4) . . ? O1 Mn3 O11 90.7(4) . . ? O6 Mn3 O11 91.1(4) . . ? O5 Mn3 O11 92.1(4) . . ? N5 Mn3 O11 92.2(4) . . ? O1 Mn3 O2 87.4(3) . 2_566 ? O6 Mn3 O2 90.4(3) . 2_566 ? O5 Mn3 O2 94.9(4) . 2_566 ? N5 Mn3 O2 80.8(3) . 2_566 ? O11 Mn3 O2 172.9(3) . 2_566 ? Mn2 O1 Mn1 119.6(4) . . ? Mn2 O1 Mn3 119.1(4) . . ? Mn1 O1 Mn3 121.1(4) . . ? C1 O2 Mn1 117.6(7) . . ? C1 O2 Mn3 115.6(7) . 2_566 ? Mn1 O2 Mn3 116.2(4) . 2_566 ? N1 O3 Mn2 113.3(6) . . ? C8 O4 Mn2 124.5(8) . . ? N3 O5 Mn3 113.5(6) . . ? C15 O6 Mn3 117.7(7) . . ? N5 O7 Mn1 111.7(6) . . ? N5 O7 Mn1 112.0(5) . 2_566 ? Mn1 O7 Mn1 96.9(3) . 2_566 ? C22 O8 Mn1 141.0(9) . . ? C29 O10 Mn2 127.4(11) . . ? C29 O10 H10C 104.4 . . ? Mn2 O10 H10C 126.7 . . ? C31 O11 Mn3 133.6(13) . . ? C31 O11 H11C 108.2 . . ? Mn3 O11 H11C 107.9 . . ? C33 O12 Mn2 119.1(12) . . ? C33 O12 H12C 103.1 . . ? Mn2 O12 H12C 102.2 . . ? C7 N1 O3 112.4(9) . . ? C7 N1 Mn1 128.0(8) . . ? O3 N1 Mn1 118.6(6) . . ? C7 N2 H2A 115.8 . . ? C7 N2 H2B 125.4 . . ? H2A N2 H2B 117.4 . . ? C14 N3 O5 114.2(10) . . ? C14 N3 Mn2 128.4(9) . . ? O5 N3 Mn2 116.1(7) . . ? C14 N4 H4A 132.1 . . ? C14 N4 H4B 108.0 . . ? H4A N4 H4B 115.5 . . ? C21 N5 O7 115.1(9) . . ? C21 N5 Mn3 128.9(8) . . ? O7 N5 Mn3 115.4(7) . . ? C21 N6 H6A 125.1 . . ? C21 N6 H6B 118.6 . . ? H6A N6 H6B 115.9 . . ? O2 C1 C6 123.6(10) . . ? O2 C1 C2 117.7(11) . . ? C6 C1 C2 118.7(11) . . ? C1 C2 C3 122.8(12) . . ? C1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C4 C3 C2 116.2(13) . . ? C4 C3 H3 121.9 . . ? C2 C3 H3 121.9 . . ? C3 C4 C5 122.5(12) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C4 C5 C6 119.8(12) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 119.7(12) . . ? C1 C6 C7 123.3(10) . . ? C5 C6 C7 117.0(12) . . ? N2 C7 N1 120.4(12) . . ? N2 C7 C6 122.4(11) . . ? N1 C7 C6 117.3(11) . . ? O4 C8 C9 119.3(12) . . ? O4 C8 C13 122.3(11) . . ? C9 C8 C13 118.4(12) . . ? C10 C9 C8 120.6(14) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 121.0(15) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 121.8(15) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C13 119.6(15) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C8 118.6(12) . . ? C12 C13 C14 119.2(12) . . ? C8 C13 C14 122.2(11) . . ? N3 C14 N4 116.9(13) . . ? N3 C14 C13 121.1(12) . . ? N4 C14 C13 122.0(12) . . ? O6 C15 C16 118.3(12) . . ? O6 C15 C20 123.3(11) . . ? C16 C15 C20 118.3(13) . . ? C17 C16 C15 121.4(13) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 120.7(13) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.4(15) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.7(14) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C15 118.5(12) . . ? C19 C20 C21 118.9(12) . . ? C15 C20 C21 122.6(11) . . ? N5 C21 N6 121.1(10) . . ? N5 C21 C20 118.4(10) . . ? N6 C21 C20 120.5(11) . . ? O8 C22 O9 125.5(13) . . ? O8 C22 C23 116.4(12) . . ? O9 C22 C23 118.0(12) . . ? C28 C23 C24 120.5(13) . . ? C28 C23 C22 120.2(12) . . ? C24 C23 C22 119.3(12) . . ? C23 C24 C25 117.3(14) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? C26 C25 C24 120.7(15) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C25 122.2(15) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 117.0(14) . . ? C26 C27 H27 121.5 . . ? C28 C27 H27 121.5 . . ? C23 C28 C27 122.1(14) . . ? C23 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? O10 C29 C30A 125(3) . . ? O10 C29 C30B 115(3) . . ? C30A C29 C30B 117(3) . . ? O10 C29 H29A 106.1 . . ? C30A C29 H29A 106.1 . . ? O10 C29 H29B 106.1 . . ? C30A C29 H29B 106.1 . . ? C30B C29 H29B 71.6 . . ? H29A C29 H29B 106.3 . . ? O10 C29 H29C 108.3 . . ? C30A C29 H29C 69.4 . . ? C30B C29 H29C 109.7 . . ? H29A C29 H29C 139.9 . . ? O10 C29 H29D 108.3 . . ? C30B C29 H29D 107.8 . . ? H29A C29 H29D 80.0 . . ? H29B C29 H29D 141.6 . . ? H29C C29 H29D 107.5 . . ? H29C C30A H29D 76.8 . . ? C29 C30A H30A 109.5 . . ? H29C C30A H30A 145.6 . . ? H29D C30A H30A 72.9 . . ? C29 C30A H30B 109.5 . . ? H29C C30A H30B 81.8 . . ? H29D C30A H30B 136.2 . . ? C29 C30A H30C 109.5 . . ? H29C C30A H30C 96.1 . . ? H29D C30A H30C 110.4 . . ? C29 C30B H30D 109.5 . . ? C29 C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29 C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? O11 C31 C32A 135(3) . . ? O11 C31 C32B 135(3) . . ? C32A C31 C32B 88(3) . . ? O11 C31 H31A 103.5 . . ? C32A C31 H31A 103.5 . . ? O11 C31 H31B 103.5 . . ? C32A C31 H31B 103.5 . . ? C32B C31 H31B 70.7 . . ? H31A C31 H31B 105.3 . . ? O11 C31 H31C 102.7 . . ? C32A C31 H31C 73.8 . . ? C32B C31 H31C 101.9 . . ? H31A C31 H31C 144.1 . . ? O11 C31 H31D 104.3 . . ? C32B C31 H31D 104.0 . . ? H31A C31 H31D 90.5 . . ? H31B C31 H31D 143.6 . . ? H31C C31 H31D 106.3 . . ? H31C C32A H31D 73.3 . . ? C31 C32A H32A 109.5 . . ? C31 C32A H32B 109.5 . . ? C31 C32A H32C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? O12 C33 C34 115(3) . . ? O12 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? O12 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O13 Mn4 O19 89.4(3) . . ? O13 Mn4 N7 87.6(4) . . ? O19 Mn4 N7 172.2(4) . . ? O13 Mn4 O14 169.2(4) . . ? O19 Mn4 O14 92.8(3) . . ? N7 Mn4 O14 88.9(4) . . ? O13 Mn4 O20 102.9(4) . . ? O19 Mn4 O20 90.1(4) . . ? N7 Mn4 O20 97.5(4) . . ? O14 Mn4 O20 87.7(4) . . ? O13 Mn4 O19 84.1(3) . 2_565 ? O19 Mn4 O19 83.8(3) . 2_565 ? N7 Mn4 O19 88.7(4) . 2_565 ? O14 Mn4 O19 85.6(3) . 2_565 ? O20 Mn4 O19 170.7(3) . 2_565 ? O13 Mn4 Mn4 85.4(2) . 2_565 ? O19 Mn4 Mn4 46.5(2) . 2_565 ? N7 Mn4 Mn4 126.0(3) . 2_565 ? O14 Mn4 Mn4 88.5(2) . 2_565 ? O20 Mn4 Mn4 136.2(3) . 2_565 ? O19 Mn4 Mn4 37.33(19) 2_565 2_565 ? O13 Mn5 O15 91.7(4) . . ? O13 Mn5 O16 178.4(4) . . ? O15 Mn5 O16 89.7(4) . . ? O13 Mn5 N9 87.9(4) . . ? O15 Mn5 N9 172.5(4) . . ? O16 Mn5 N9 90.5(4) . . ? O13 Mn5 O22 89.0(3) . . ? O15 Mn5 O22 91.8(4) . . ? O16 Mn5 O22 91.6(4) . . ? N9 Mn5 O22 95.7(4) . . ? O13 Mn5 O24 84.7(3) . . ? O15 Mn5 O24 90.0(4) . . ? O16 Mn5 O24 94.6(4) . . ? N9 Mn5 O24 82.5(4) . . ? O22 Mn5 O24 173.6(3) . . ? O13 Mn6 O17 91.4(3) . . ? O13 Mn6 O18 174.8(3) . . ? O17 Mn6 O18 93.8(3) . . ? O13 Mn6 N11 86.1(4) . . ? O17 Mn6 N11 175.4(4) . . ? O18 Mn6 N11 88.7(4) . . ? O13 Mn6 O23 90.0(4) . . ? O17 Mn6 O23 92.8(4) . . ? O18 Mn6 O23 90.3(4) . . ? N11 Mn6 O23 91.1(4) . . ? O13 Mn6 O14 87.8(3) . 2_565 ? O17 Mn6 O14 94.9(3) . 2_565 ? O18 Mn6 O14 91.2(3) . 2_565 ? N11 Mn6 O14 81.0(4) . 2_565 ? O23 Mn6 O14 172.0(3) . 2_565 ? Mn5 O13 Mn6 119.4(4) . . ? Mn5 O13 Mn4 119.6(4) . . ? Mn6 O13 Mn4 121.0(4) . . ? C35 O14 Mn4 117.2(7) . . ? C35 O14 Mn6 118.6(7) . 2_565 ? Mn4 O14 Mn6 116.2(3) . 2_565 ? N7 O15 Mn5 113.5(7) . . ? C42 O16 Mn5 123.4(8) . . ? N9 O17 Mn6 113.0(6) . . ? C49 O18 Mn6 117.2(7) . . ? N11 O19 Mn4 110.5(6) . . ? N11 O19 Mn4 112.5(6) . 2_565 ? Mn4 O19 Mn4 96.2(3) . 2_565 ? C56 O20 Mn4 141.0(9) . . ? C63 O22 Mn5 124.4(9) . . ? C63 O22 H22C 103.5 . . ? Mn5 O22 H22C 131.2 . . ? C65 O23 Mn6 129.3(10) . . ? C65 O23 H23C 102.5 . . ? Mn6 O23 H23C 118.7 . . ? C41 N7 O15 113.5(10) . . ? C41 N7 Mn4 127.0(9) . . ? O15 N7 Mn4 119.5(7) . . ? C41 N8 H8A 121.9 . . ? C41 N8 H8B 120.1 . . ? H8A N8 H8B 117.3 . . ? C48 N9 O17 114.4(10) . . ? C48 N9 Mn5 126.7(9) . . ? O17 N9 Mn5 117.4(7) . . ? C48 N10 H10A 98.8 . . ? C48 N10 H10B 125.1 . . ? H10A N10 H10B 114.3 . . ? C55 N11 O19 115.7(9) . . ? C55 N11 Mn6 127.9(8) . . ? O19 N11 Mn6 115.8(7) . . ? C55 N12 H12A 131.3 . . ? C55 N12 H12B 106.3 . . ? H12A N12 H12B 117.2 . . ? O14 C35 C40 124.5(11) . . ? O14 C35 C36 117.7(12) . . ? C40 C35 C36 117.8(12) . . ? C37 C36 C35 121.6(13) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C38 C37 C36 117.9(13) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? C37 C38 C39 121.5(13) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C38 C39 C40 119.5(13) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C35 C40 C39 121.6(12) . . ? C35 C40 C41 122.4(11) . . ? C39 C40 C41 115.8(12) . . ? N8 C41 N7 119.2(12) . . ? N8 C41 C40 122.5(11) . . ? N7 C41 C40 118.3(11) . . ? O16 C42 C43 118.9(12) . . ? O16 C42 C47 122.3(11) . . ? C43 C42 C47 118.8(12) . . ? C44 C43 C42 121.3(14) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C45 C44 C43 120.9(14) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 120.2(13) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 120.0(13) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C42 C47 C46 118.7(12) . . ? C42 C47 C48 122.8(11) . . ? C46 C47 C48 118.4(11) . . ? N9 C48 N10 116.9(12) . . ? N9 C48 C47 121.3(11) . . ? N10 C48 C47 121.8(11) . . ? O18 C49 C50 118.5(11) . . ? O18 C49 C54 122.2(11) . . ? C50 C49 C54 119.1(13) . . ? C51 C50 C49 121.2(14) . . ? C51 C50 H50 119.4 . . ? C49 C50 H50 119.4 . . ? C50 C51 C52 120.5(14) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C53 C52 C51 118.1(14) . . ? C53 C52 H52 120.9 . . ? C51 C52 H52 120.9 . . ? C54 C53 C52 122.9(14) . . ? C54 C53 H53 118.6 . . ? C52 C53 H53 118.6 . . ? C53 C54 C49 118.0(13) . . ? C53 C54 C55 118.8(12) . . ? C49 C54 C55 123.1(12) . . ? N11 C55 N12 120.3(11) . . ? N11 C55 C54 118.5(11) . . ? N12 C55 C54 121.2(12) . . ? O20 C56 O21 125.6(13) . . ? O20 C56 C57 116.9(12) . . ? O21 C56 C57 117.4(12) . . ? C62 C57 C58 120.5(14) . . ? C62 C57 C56 120.9(13) . . ? C58 C57 C56 118.5(13) . . ? C59 C58 C57 117.3(17) . . ? C59 C58 H58 121.4 . . ? C57 C58 H58 121.4 . . ? C60 C59 C58 121.8(17) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? C59 C60 C61 119.6(16) . . ? C59 C60 H60 120.2 . . ? C61 C60 H60 120.2 . . ? C62 C61 C60 118.2(17) . . ? C62 C61 H61 120.9 . . ? C60 C61 H61 120.9 . . ? C57 C62 C61 122.6(16) . . ? C57 C62 H62 118.7 . . ? C61 C62 H62 118.7 . . ? O22 C63 C64B 117(2) . . ? O22 C63 C64A 102(2) . . ? O22 C63 H63A 111.3 . . ? C64B C63 H63A 115.3 . . ? C64A C63 H63A 111.3 . . ? O22 C63 H63B 111.3 . . ? C64B C63 H63B 90.3 . . ? C64A C63 H63B 111.3 . . ? H63A C63 H63B 109.2 . . ? O22 C63 H63C 109.0 . . ? C64B C63 H63C 109.7 . . ? C64A C63 H63C 102.8 . . ? H63B C63 H63C 118.6 . . ? O22 C63 H63D 108.8 . . ? C64B C63 H63D 103.9 . . ? C64A C63 H63D 125.4 . . ? H63A C63 H63D 97.8 . . ? H63C C63 H63D 107.7 . . ? C63 C64A H64A 109.5 . . ? C63 C64A H64B 109.5 . . ? H64A C64A H64B 109.5 . . ? C63 C64A H64C 109.5 . . ? H64A C64A H64C 109.5 . . ? H64B C64A H64C 109.5 . . ? C63 C64B H64D 109.5 . . ? C63 C64B H64E 109.5 . . ? H64D C64B H64E 109.5 . . ? C63 C64B H64F 109.5 . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? O23 C65 C66B 121(3) . . ? O23 C65 C66A 103(2) . . ? O23 C65 H65A 111.1 . . ? C66B C65 H65A 114.8 . . ? C66A C65 H65A 111.1 . . ? O23 C65 H65B 111.1 . . ? C66B C65 H65B 87.2 . . ? C66A C65 H65B 111.1 . . ? H65A C65 H65B 109.1 . . ? O23 C65 H65C 107.7 . . ? C66B C65 H65C 106.0 . . ? C66A C65 H65C 97.2 . . ? H65B C65 H65C 123.9 . . ? O23 C65 H65D 107.1 . . ? C66B C65 H65D 107.9 . . ? C66A C65 H65D 132.7 . . ? H65A C65 H65D 90.7 . . ? H65C C65 H65D 106.9 . . ? C65 C66A H66A 109.5 . . ? C65 C66A H66B 109.5 . . ? H66A C66A H66B 109.5 . . ? C65 C66A H66C 109.5 . . ? H66A C66A H66C 109.5 . . ? H66B C66A H66C 109.5 . . ? C65 C66B H66D 109.5 . . ? C65 C66B H66E 109.5 . . ? H66D C66B H66E 109.5 . . ? C65 C66B H66F 109.5 . . ? H66D C66B H66F 109.5 . . ? H66E C66B H66F 109.5 . . ? C67B O24 Mn5 141(2) . . ? C67A O24 Mn5 125.0(11) . . ? C67B O24 H24C 109.4 . . ? C67A O24 H24C 98.9 . . ? Mn5 O24 H24C 104.5 . . ? C67B O24 H24D 106.0 . . ? C67A O24 H24D 92.4 . . ? Mn5 O24 H24D 104.9 . . ? C68 C67A O24 111(2) . . ? C68 C67A H67A 109.4 . . ? O24 C67A H67A 109.4 . . ? C68 C67A H67B 109.4 . . ? O24 C67A H67B 109.4 . . ? H67A C67A H67B 108.0 . . ? O24 C67B C68 112(4) . . ? O24 C67B H67C 109.3 . . ? C68 C67B H67C 109.3 . . ? O24 C67B H67D 109.3 . . ? C68 C67B H67D 109.3 . . ? H67C C67B H67D 108.0 . . ? C67A C68 H68A 109.5 . . ? C67B C68 H68A 119.9 . . ? C67A C68 H68B 109.5 . . ? C67B C68 H68B 123.9 . . ? H68A C68 H68B 109.5 . . ? C67A C68 H68C 109.5 . . ? C67B C68 H68C 78.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67A C68 H68D 100.6 . . ? C67B C68 H68D 109.5 . . ? H68B C68 H68D 118.7 . . ? H68C C68 H68D 108.7 . . ? C67A C68 H68E 85.7 . . ? C67B C68 H68E 109.5 . . ? H68A C68 H68E 104.0 . . ? H68C C68 H68E 135.1 . . ? H68D C68 H68E 109.5 . . ? C67A C68 H68F 138.5 . . ? C67B C68 H68F 109.5 . . ? H68A C68 H68F 104.0 . . ? H68B C68 H68F 80.7 . . ? H68D C68 H68F 109.5 . . ? H68E C68 H68F 109.5 . . ? C69 O25 H25C 101.6 . . ? O25 C69 C70 109.9(16) . . ? O25 C69 H69A 109.7 . . ? C70 C69 H69A 109.7 . . ? O25 C69 H69B 109.7 . . ? C70 C69 H69B 109.7 . . ? H69A C69 H69B 108.2 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? H1WA O100 H1WB 107.7 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.851 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.207 data_pg200608 _database_code_depnum_ccdc_archive 'CCDC 888449' #TrackingRef 'web_deposit_cif_file_1_Lise-MarieChamoreau_1340629901.pg200608 - publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H82 Mn6 N12 O24, 4(C2 H6 O)' _chemical_formula_sum 'C76 H106 Mn6 N12 O28' _chemical_formula_weight 1965.37 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.384(5) _cell_length_b 14.457(4) _cell_length_c 15.499(4) _cell_angle_alpha 75.42(3) _cell_angle_beta 76.68(3) _cell_angle_gamma 66.86(2) _cell_volume 2245.1(13) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 14.4 _exptl_crystal_description parallelepipped _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35968 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10214 _reflns_number_gt 5816 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0537P)^2^+1.9331P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10214 _refine_ls_number_parameters 567 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1217 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.39451(5) -0.06416(4) 0.21803(3) 0.02266(15) Uani 1 1 d . . . Mn2 Mn 0.33887(5) 0.04882(4) 0.01280(3) 0.02138(14) Uani 1 1 d . . . Mn3 Mn 0.26351(6) 0.18573(4) 0.17078(3) 0.02466(15) Uani 1 1 d . . . O1 O 0.3374(2) 0.05699(16) 0.13269(14) 0.0218(5) Uani 1 1 d . . . O2 O 0.4886(3) -0.18146(18) 0.29552(16) 0.0292(6) Uani 1 1 d . . . O3 O 0.4663(2) -0.08993(17) 0.03056(15) 0.0221(5) Uani 1 1 d . . . O4 O 0.3486(2) 0.03977(18) -0.10902(15) 0.0270(6) Uani 1 1 d . . . O5 O 0.2254(3) 0.25535(17) 0.05286(16) 0.0284(6) Uani 1 1 d . . . O6 O 0.2236(3) 0.31616(18) 0.19869(16) 0.0328(6) Uani 1 1 d . . . O7 O 0.3762(3) 0.01112(18) 0.30672(16) 0.0365(7) Uani 1 1 d . . . O8 O 0.2110(3) -0.0852(2) 0.24607(17) 0.0364(7) Uani 1 1 d . . . O9 O 0.0346(3) 0.0191(2) 0.3203(2) 0.0652(11) Uani 1 1 d . . . O10 O 0.1749(3) -0.01137(19) 0.06633(17) 0.0331(6) Uani 1 1 d . . . H10B H 0.1753 -0.0338 0.1204 0.040 Uiso 1 1 d R . . O11 O 0.0670(3) 0.1825(2) 0.21750(19) 0.0443(8) Uani 1 1 d . . . H11B H 0.0535 0.1173 0.2443 0.053 Uiso 1 1 d R . . O12 O 0.5011(3) 0.17242(19) 0.13423(16) 0.0348(7) Uani 1 1 d . B . H12B H 0.5483 0.1145 0.1288 0.042 Uiso 1 1 d R . . N1 N 0.4586(3) -0.1455(2) 0.12046(18) 0.0205(6) Uani 1 1 d . . . N2 N 0.5266(3) -0.2860(2) 0.05061(19) 0.0258(7) Uani 1 1 d . . . H2B H 0.5291 -0.2453 -0.0032 0.031 Uiso 1 1 d R . . H2C H 0.5768 -0.3525 0.0564 0.031 Uiso 1 1 d R . . N3 N 0.2362(3) 0.1981(2) -0.01208(18) 0.0234(7) Uani 1 1 d . . . N4 N 0.1584(3) 0.3608(2) -0.0968(2) 0.0322(8) Uani 1 1 d . . . H4A H 0.1741 0.3870 -0.0506 0.039 Uiso 1 1 d R . . H4B H 0.1553 0.3956 -0.1574 0.039 Uiso 1 1 d R . . N5 N 0.3114(3) 0.1182(2) 0.29241(19) 0.0279(7) Uani 1 1 d . . . N6 N 0.3825(3) 0.0967(2) 0.4271(2) 0.0371(9) Uani 1 1 d . . . H6A H 0.4165 0.0234 0.4253 0.045 Uiso 1 1 d R . . H6B H 0.4149 0.1255 0.4590 0.045 Uiso 1 1 d R . . C1 C 0.5188(4) -0.2805(3) 0.2925(2) 0.0259(8) Uani 1 1 d . . . C2 C 0.5550(4) -0.3538(3) 0.3705(3) 0.0368(10) Uani 1 1 d . . . H2 H 0.5626 -0.3324 0.4214 0.044 Uiso 1 1 calc R . . C3 C 0.5796(4) -0.4561(3) 0.3741(3) 0.0421(11) Uani 1 1 d . . . H3 H 0.6025 -0.5038 0.4276 0.051 Uiso 1 1 calc R . . C4 C 0.5711(5) -0.4900(3) 0.2998(3) 0.0455(12) Uani 1 1 d . . . H4 H 0.5859 -0.5601 0.3031 0.055 Uiso 1 1 calc R . . C5 C 0.5408(4) -0.4204(3) 0.2214(3) 0.0360(10) Uani 1 1 d . . . H5 H 0.5359 -0.4437 0.1707 0.043 Uiso 1 1 calc R . . C6 C 0.5168(4) -0.3145(3) 0.2148(2) 0.0258(8) Uani 1 1 d . . . C7 C 0.4996(4) -0.2460(3) 0.1255(2) 0.0232(8) Uani 1 1 d . . . C8 C 0.2753(4) 0.1076(3) -0.1716(2) 0.0247(8) Uani 1 1 d . . . C9 C 0.2736(4) 0.0719(3) -0.2476(2) 0.0341(10) Uani 1 1 d . . . H9 H 0.3223 0.0025 -0.2525 0.041 Uiso 1 1 calc R . . C10 C 0.2028(4) 0.1352(3) -0.3154(3) 0.0422(11) Uani 1 1 d . . . H10 H 0.2030 0.1088 -0.3658 0.051 Uiso 1 1 calc R . . C11 C 0.1319(5) 0.2368(3) -0.3099(3) 0.0448(11) Uani 1 1 d . . . H11 H 0.0829 0.2805 -0.3561 0.054 Uiso 1 1 calc R . . C12 C 0.1332(4) 0.2740(3) -0.2361(3) 0.0355(10) Uani 1 1 d . . . H12 H 0.0845 0.3439 -0.2327 0.043 Uiso 1 1 calc R . . C13 C 0.2043(4) 0.2117(3) -0.1658(2) 0.0247(8) Uani 1 1 d . . . C14 C 0.2019(3) 0.2570(3) -0.0885(2) 0.0232(8) Uani 1 1 d . . . C15 C 0.2050(4) 0.3412(3) 0.2806(2) 0.0306(9) Uani 1 1 d . . . C16 C 0.1363(4) 0.4448(3) 0.2880(3) 0.0414(11) Uani 1 1 d . . . H16 H 0.0998 0.4923 0.2379 0.050 Uiso 1 1 calc R . . C17 C 0.1216(5) 0.4777(3) 0.3676(3) 0.0497(13) Uani 1 1 d . . . H17 H 0.0766 0.5480 0.3711 0.060 Uiso 1 1 calc R . . C18 C 0.1716(5) 0.4098(3) 0.4423(3) 0.0510(13) Uani 1 1 d . . . H18 H 0.1619 0.4333 0.4965 0.061 Uiso 1 1 calc R . . C19 C 0.2359(4) 0.3072(3) 0.4372(3) 0.0406(11) Uani 1 1 d . . . H19 H 0.2681 0.2606 0.4890 0.049 Uiso 1 1 calc R . . C20 C 0.2550(4) 0.2700(3) 0.3571(2) 0.0310(9) Uani 1 1 d . . . C21 C 0.3204(4) 0.1578(3) 0.3575(2) 0.0268(8) Uani 1 1 d . . . C22 C 0.1188(4) -0.0668(3) 0.3135(3) 0.0379(10) Uani 1 1 d . . . C23 C 0.1144(4) -0.1569(3) 0.3878(2) 0.0320(9) Uani 1 1 d . . . C24 C 0.1933(4) -0.2561(3) 0.3772(3) 0.0364(10) Uani 1 1 d . . . H24 H 0.2483 -0.2683 0.3218 0.044 Uiso 1 1 calc R . . C25 C 0.1922(5) -0.3386(3) 0.4480(3) 0.0475(12) Uani 1 1 d . . . H25 H 0.2465 -0.4064 0.4406 0.057 Uiso 1 1 calc R . . C26 C 0.1123(5) -0.3210(4) 0.5281(3) 0.0573(14) Uani 1 1 d . . . H26 H 0.1109 -0.3769 0.5757 0.069 Uiso 1 1 calc R . . C27 C 0.0337(5) -0.2222(4) 0.5401(3) 0.0562(14) Uani 1 1 d . . . H27 H -0.0198 -0.2106 0.5961 0.067 Uiso 1 1 calc R . . C28 C 0.0332(4) -0.1397(3) 0.4697(3) 0.0415(11) Uani 1 1 d . . . H28 H -0.0220 -0.0722 0.4773 0.050 Uiso 1 1 calc R . . C29 C 0.1748(4) -0.0994(3) 0.0356(3) 0.0408(10) Uani 1 1 d . . . H29A H 0.2604 -0.1545 0.0393 0.049 Uiso 1 1 calc R . . H29B H 0.1618 -0.0790 -0.0284 0.049 Uiso 1 1 calc R . . C30 C 0.0731(5) -0.1400(4) 0.0889(4) 0.0656(15) Uani 1 1 d . . . H30A H 0.0987 -0.1781 0.1476 0.098 Uiso 1 1 calc R . . H30B H 0.0625 -0.1855 0.0564 0.098 Uiso 1 1 calc R . . H30C H -0.0087 -0.0830 0.0978 0.098 Uiso 1 1 calc R . . C31 C -0.0470(5) 0.2444(4) 0.1753(4) 0.0558(13) Uani 1 1 d . . . H31A H -0.1160 0.2155 0.2010 0.067 Uiso 1 1 calc R . . H31B H -0.0265 0.2432 0.1098 0.067 Uiso 1 1 calc R . . C32 C -0.0936(6) 0.3524(4) 0.1899(4) 0.088(2) Uani 1 1 d . . . H32A H -0.1190 0.3539 0.2545 0.132 Uiso 1 1 calc R . . H32B H -0.1681 0.3939 0.1584 0.132 Uiso 1 1 calc R . . H32C H -0.0242 0.3801 0.1662 0.132 Uiso 1 1 calc R . . C33 C 0.5676(7) 0.2060(4) 0.1819(4) 0.0730(18) Uani 1 1 d . . . H33A H 0.5400 0.1886 0.2474 0.088 Uiso 0.67 1 calc PR A 1 H33B H 0.6614 0.1677 0.1693 0.088 Uiso 0.67 1 calc PR A 1 H33C H 0.5007 0.2533 0.2199 0.088 Uiso 0.33 1 d PR A 2 H33D H 0.6152 0.1453 0.2234 0.088 Uiso 0.33 1 d PR A 2 C34A C 0.5457(9) 0.3138(5) 0.1588(6) 0.055(2) Uani 0.67 1 d P B 1 H34A H 0.5977 0.3297 0.1914 0.082 Uiso 0.67 1 calc PR B 1 H34B H 0.4540 0.3527 0.1756 0.082 Uiso 0.67 1 calc PR B 1 H34C H 0.5705 0.3324 0.0938 0.082 Uiso 0.67 1 calc PR B 1 C34B C 0.644(2) 0.249(2) 0.1404(12) 0.091(7) Uani 0.33 1 d P B 2 H34D H 0.6211 0.2826 0.0802 0.136 Uiso 0.33 1 calc PR B 2 H34E H 0.7319 0.1977 0.1346 0.136 Uiso 0.33 1 calc PR B 2 H34F H 0.6409 0.2996 0.1733 0.136 Uiso 0.33 1 calc PR B 2 O13 O 0.2473(3) 0.4589(2) 0.02514(19) 0.0473(8) Uani 1 1 d . . . H13 H 0.2251 0.4221 0.0723 0.071 Uiso 1 1 calc R . . C35 C 0.2132(5) 0.5606(3) 0.0419(3) 0.0503(12) Uani 1 1 d D . . H35A H 0.1264 0.5811 0.0783 0.060 Uiso 1 1 calc R . . H35B H 0.2091 0.6090 -0.0162 0.060 Uiso 1 1 calc R . . C36 C 0.3097(6) 0.5676(4) 0.0913(4) 0.0675(15) Uani 1 1 d D . . H36A H 0.3117 0.5216 0.1500 0.101 Uiso 1 1 calc R . . H36B H 0.2837 0.6380 0.1005 0.101 Uiso 1 1 calc R . . H36C H 0.3958 0.5476 0.0555 0.101 Uiso 1 1 calc R . . O14 O 0.4744(3) -0.1419(2) 0.46804(18) 0.0402(7) Uani 1 1 d . . . H14 H 0.4884 -0.1459 0.4132 0.060 Uiso 1 1 calc R . . C37 C 0.3487(6) -0.1449(5) 0.5065(4) 0.0833(19) Uani 1 1 d . . . H37A H 0.2843 -0.0805 0.4803 0.100 Uiso 1 1 calc R . . H37B H 0.3393 -0.2014 0.4869 0.100 Uiso 1 1 calc R . . C38 C 0.3177(9) -0.1569(10) 0.5961(5) 0.177(5) Uani 1 1 d . . . H38A H 0.3714 -0.2251 0.6234 0.265 Uiso 1 1 calc R . . H38B H 0.2265 -0.1495 0.6128 0.265 Uiso 1 1 calc R . . H38C H 0.3326 -0.1049 0.6178 0.265 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 0.0317(3) 0.0168(3) 0.0163(3) -0.0048(2) -0.0038(2) -0.0040(2) Mn2 0.0280(3) 0.0170(3) 0.0172(3) -0.0049(2) -0.0046(2) -0.0041(2) Mn3 0.0348(4) 0.0173(3) 0.0183(3) -0.0061(2) -0.0046(2) -0.0034(2) O1 0.0307(15) 0.0157(12) 0.0150(12) -0.0031(9) -0.0040(10) -0.0036(11) O2 0.0455(17) 0.0180(13) 0.0216(13) -0.0038(10) -0.0110(12) -0.0051(12) O3 0.0301(15) 0.0172(12) 0.0160(12) -0.0031(9) -0.0033(10) -0.0051(11) O4 0.0352(16) 0.0229(13) 0.0210(13) -0.0075(10) -0.0097(11) -0.0031(12) O5 0.0426(17) 0.0186(13) 0.0221(13) -0.0073(10) -0.0067(12) -0.0058(12) O6 0.0501(18) 0.0206(13) 0.0230(14) -0.0084(11) -0.0058(12) -0.0046(13) O7 0.061(2) 0.0183(13) 0.0235(14) -0.0061(11) -0.0153(13) -0.0008(13) O8 0.0378(17) 0.0381(16) 0.0321(16) -0.0068(12) 0.0041(13) -0.0171(14) O9 0.062(2) 0.0390(19) 0.061(2) 0.0008(16) 0.0245(18) -0.0084(18) O10 0.0373(17) 0.0334(15) 0.0297(15) -0.0051(12) -0.0037(12) -0.0148(13) O11 0.0347(18) 0.0337(16) 0.0493(18) 0.0021(13) -0.0008(14) -0.0052(14) O12 0.0504(19) 0.0264(14) 0.0308(15) -0.0108(11) -0.0115(13) -0.0105(13) N1 0.0276(17) 0.0179(15) 0.0144(14) -0.0004(11) -0.0026(12) -0.0081(13) N2 0.038(2) 0.0163(15) 0.0209(16) -0.0038(12) -0.0051(14) -0.0066(14) N3 0.0283(18) 0.0220(16) 0.0172(15) -0.0062(12) -0.0021(13) -0.0054(14) N4 0.045(2) 0.0207(16) 0.0289(18) -0.0018(13) -0.0152(15) -0.0057(15) N5 0.042(2) 0.0178(15) 0.0214(16) -0.0070(12) -0.0062(14) -0.0046(14) N6 0.058(2) 0.0202(17) 0.0311(18) -0.0083(14) -0.0200(17) -0.0017(16) C1 0.028(2) 0.0212(19) 0.0228(19) -0.0030(15) -0.0011(16) -0.0045(16) C2 0.048(3) 0.026(2) 0.025(2) -0.0037(16) -0.0095(19) 0.0000(19) C3 0.060(3) 0.024(2) 0.030(2) 0.0024(17) -0.012(2) -0.004(2) C4 0.074(3) 0.017(2) 0.041(3) 0.0007(17) -0.012(2) -0.012(2) C5 0.058(3) 0.023(2) 0.029(2) -0.0029(16) -0.008(2) -0.015(2) C6 0.030(2) 0.0222(19) 0.0222(19) -0.0050(15) -0.0022(16) -0.0062(16) C7 0.028(2) 0.0224(19) 0.0195(18) -0.0037(14) -0.0052(15) -0.0087(16) C8 0.025(2) 0.032(2) 0.0181(18) -0.0054(15) -0.0032(15) -0.0106(17) C9 0.042(3) 0.030(2) 0.026(2) -0.0082(17) -0.0096(18) -0.0049(19) C10 0.053(3) 0.042(3) 0.029(2) -0.0126(19) -0.019(2) -0.003(2) C11 0.052(3) 0.042(3) 0.031(2) -0.0047(19) -0.022(2) 0.000(2) C12 0.042(3) 0.027(2) 0.029(2) -0.0055(17) -0.0152(19) 0.0014(19) C13 0.026(2) 0.027(2) 0.0202(19) -0.0041(15) -0.0043(16) -0.0078(17) C14 0.022(2) 0.0204(18) 0.0237(19) -0.0037(15) -0.0025(15) -0.0042(15) C15 0.040(2) 0.024(2) 0.027(2) -0.0119(16) -0.0029(18) -0.0076(18) C16 0.057(3) 0.021(2) 0.037(2) -0.0113(17) -0.012(2) 0.001(2) C17 0.073(4) 0.026(2) 0.042(3) -0.019(2) -0.006(2) -0.004(2) C18 0.081(4) 0.035(2) 0.035(3) -0.020(2) -0.007(2) -0.012(2) C19 0.059(3) 0.032(2) 0.026(2) -0.0128(17) -0.006(2) -0.008(2) C20 0.043(3) 0.023(2) 0.025(2) -0.0103(16) -0.0032(18) -0.0074(18) C21 0.033(2) 0.0232(19) 0.0230(19) -0.0095(15) -0.0034(16) -0.0064(17) C22 0.037(3) 0.037(2) 0.035(2) -0.0084(19) 0.0029(19) -0.011(2) C23 0.034(2) 0.039(2) 0.025(2) -0.0056(17) 0.0009(17) -0.019(2) C24 0.037(3) 0.041(3) 0.034(2) -0.0063(19) -0.0050(19) -0.017(2) C25 0.052(3) 0.038(3) 0.051(3) 0.001(2) -0.015(2) -0.016(2) C26 0.071(4) 0.056(3) 0.044(3) 0.013(2) -0.009(3) -0.034(3) C27 0.066(4) 0.079(4) 0.025(2) -0.003(2) 0.006(2) -0.039(3) C28 0.039(3) 0.045(3) 0.042(3) -0.013(2) 0.002(2) -0.018(2) C29 0.038(3) 0.043(3) 0.051(3) -0.014(2) -0.008(2) -0.021(2) C30 0.055(4) 0.049(3) 0.099(4) -0.012(3) -0.006(3) -0.028(3) C31 0.031(3) 0.056(3) 0.067(3) -0.004(3) -0.012(2) -0.004(2) C32 0.074(4) 0.066(4) 0.105(5) -0.037(4) -0.046(4) 0.025(3) C33 0.131(6) 0.071(4) 0.052(3) -0.004(3) -0.041(4) -0.061(4) C34A 0.069(6) 0.036(4) 0.072(6) -0.012(4) -0.024(5) -0.022(4) C34B 0.090(16) 0.17(2) 0.047(11) -0.031(13) 0.017(11) -0.085(17) O13 0.069(2) 0.0314(16) 0.0402(17) -0.0084(13) -0.0084(16) -0.0145(16) C35 0.067(3) 0.028(2) 0.056(3) -0.008(2) -0.014(3) -0.014(2) C36 0.075(4) 0.066(4) 0.075(4) -0.015(3) -0.015(3) -0.036(3) O14 0.054(2) 0.0427(17) 0.0257(15) -0.0093(13) -0.0110(14) -0.0141(15) C37 0.090(5) 0.104(5) 0.052(4) -0.005(3) 0.006(3) -0.044(4) C38 0.117(7) 0.365(17) 0.072(6) -0.005(7) -0.017(5) -0.128(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O7 1.887(2) . ? Mn1 O1 1.891(2) . ? Mn1 O2 1.898(3) . ? Mn1 N1 1.979(3) . ? Mn1 O8 2.158(3) . ? Mn2 O1 1.887(2) . ? Mn2 O4 1.900(2) . ? Mn2 O3 1.955(2) . ? Mn2 N3 1.995(3) . ? Mn2 O10 2.265(3) . ? Mn2 O3 2.423(3) 2_655 ? Mn3 O6 1.896(2) . ? Mn3 O1 1.901(2) . ? Mn3 O5 1.907(3) . ? Mn3 N5 1.983(3) . ? Mn3 O11 2.202(3) . ? O2 C1 1.346(4) . ? O3 N1 1.425(3) . ? O3 Mn2 2.423(3) 2_655 ? O4 C8 1.360(4) . ? O5 N3 1.412(3) . ? O6 C15 1.354(4) . ? O7 N5 1.412(4) . ? O8 C22 1.296(5) . ? O9 C22 1.247(5) . ? O10 C29 1.466(5) . ? O10 H10B 0.8192 . ? O11 C31 1.448(5) . ? O11 H11B 0.9855 . ? O12 C33 1.443(5) . ? O12 H12B 0.8112 . ? N1 C7 1.326(4) . ? N2 C7 1.346(4) . ? N2 H2B 0.8931 . ? N2 H2C 0.8987 . ? N3 C14 1.313(4) . ? N4 C14 1.365(4) . ? N4 H4A 0.9676 . ? N4 H4B 0.9487 . ? N5 C21 1.320(4) . ? N6 C21 1.350(5) . ? N6 H6A 0.9810 . ? N6 H6B 0.9281 . ? C1 C2 1.413(5) . ? C1 C6 1.418(5) . ? C2 C3 1.381(5) . ? C2 H2 0.9500 . ? C3 C4 1.395(6) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.426(5) . ? C5 H5 0.9500 . ? C6 C7 1.489(5) . ? C8 C9 1.406(5) . ? C8 C13 1.416(5) . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.385(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(5) . ? C11 H11 0.9500 . ? C12 C13 1.412(5) . ? C12 H12 0.9500 . ? C13 C14 1.492(5) . ? C15 C16 1.411(5) . ? C15 C20 1.423(5) . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 C19 1.385(6) . ? C18 H18 0.9500 . ? C19 C20 1.414(5) . ? C19 H19 0.9500 . ? C20 C21 1.495(5) . ? C22 C23 1.515(5) . ? C23 C24 1.389(6) . ? C23 C28 1.401(5) . ? C24 C25 1.404(6) . ? C24 H24 0.9500 . ? C25 C26 1.375(7) . ? C25 H25 0.9500 . ? C26 C27 1.388(7) . ? C26 H26 0.9500 . ? C27 C28 1.399(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.489(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.497(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34B 1.234(17) . ? C33 C34A 1.440(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 H33C 0.9900 . ? C33 H33D 0.9900 . ? C34A H33C 1.2787 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? O13 C35 1.442(5) . ? O13 H13 0.8400 . ? C35 C36 1.522(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O14 C37 1.431(6) . ? O14 H14 0.8400 . ? C37 C38 1.335(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 O7 Mn1 O1 91.55(10) . . ? O7 Mn1 O2 86.76(11) . . ? O1 Mn1 O2 166.91(11) . . ? O7 Mn1 N1 165.84(13) . . ? O1 Mn1 N1 90.04(10) . . ? O2 Mn1 N1 88.51(11) . . ? O7 Mn1 O8 101.82(12) . . ? O1 Mn1 O8 93.45(11) . . ? O2 Mn1 O8 99.61(11) . . ? N1 Mn1 O8 92.12(11) . . ? O1 Mn2 O4 177.34(11) . . ? O1 Mn2 O3 89.67(10) . . ? O4 Mn2 O3 89.05(10) . . ? O1 Mn2 N3 90.17(11) . . ? O4 Mn2 N3 90.68(11) . . ? O3 Mn2 N3 169.74(12) . . ? O1 Mn2 O10 87.28(10) . . ? O4 Mn2 O10 95.08(11) . . ? O3 Mn2 O10 91.03(10) . . ? N3 Mn2 O10 99.21(11) . . ? O1 Mn2 O3 88.81(10) . 2_655 ? O4 Mn2 O3 88.69(10) . 2_655 ? O3 Mn2 O3 81.16(10) . 2_655 ? N3 Mn2 O3 88.58(11) . 2_655 ? O10 Mn2 O3 171.29(9) . 2_655 ? O6 Mn3 O1 168.17(11) . . ? O6 Mn3 O5 86.94(11) . . ? O1 Mn3 O5 91.55(10) . . ? O6 Mn3 N5 90.74(11) . . ? O1 Mn3 N5 90.09(11) . . ? O5 Mn3 N5 176.10(12) . . ? O6 Mn3 O11 95.06(12) . . ? O1 Mn3 O11 96.73(11) . . ? O5 Mn3 O11 92.77(12) . . ? N5 Mn3 O11 90.55(13) . . ? Mn2 O1 Mn1 119.83(12) . . ? Mn2 O1 Mn3 120.21(12) . . ? Mn1 O1 Mn3 119.68(11) . . ? C1 O2 Mn1 128.2(2) . . ? N1 O3 Mn2 115.06(17) . . ? N1 O3 Mn2 111.41(18) . 2_655 ? Mn2 O3 Mn2 98.84(10) . 2_655 ? C8 O4 Mn2 128.3(2) . . ? N3 O5 Mn3 119.29(18) . . ? C15 O6 Mn3 128.4(2) . . ? N5 O7 Mn1 120.27(19) . . ? C22 O8 Mn1 130.4(3) . . ? C29 O10 Mn2 120.6(2) . . ? C29 O10 H10B 100.5 . . ? Mn2 O10 H10B 108.7 . . ? C31 O11 Mn3 126.9(3) . . ? C31 O11 H11B 103.8 . . ? Mn3 O11 H11B 120.6 . . ? C33 O12 H12B 104.7 . . ? C7 N1 O3 113.7(3) . . ? C7 N1 Mn1 129.8(2) . . ? O3 N1 Mn1 116.47(18) . . ? C7 N2 H2B 119.1 . . ? C7 N2 H2C 114.6 . . ? H2B N2 H2C 119.6 . . ? C14 N3 O5 112.1(3) . . ? C14 N3 Mn2 129.2(2) . . ? O5 N3 Mn2 116.6(2) . . ? C14 N4 H4A 116.6 . . ? C14 N4 H4B 113.2 . . ? H4A N4 H4B 123.1 . . ? C21 N5 O7 111.0(3) . . ? C21 N5 Mn3 129.9(2) . . ? O7 N5 Mn3 117.10(19) . . ? C21 N6 H6A 115.1 . . ? C21 N6 H6B 118.1 . . ? H6A N6 H6B 123.0 . . ? O2 C1 C2 118.1(3) . . ? O2 C1 C6 123.2(3) . . ? C2 C1 C6 118.8(3) . . ? C3 C2 C1 121.2(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.6(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 118.3(3) . . ? C1 C6 C7 122.8(3) . . ? C5 C6 C7 118.8(3) . . ? N1 C7 N2 120.5(3) . . ? N1 C7 C6 119.5(3) . . ? N2 C7 C6 120.0(3) . . ? O4 C8 C9 117.4(3) . . ? O4 C8 C13 124.0(3) . . ? C9 C8 C13 118.6(3) . . ? C10 C9 C8 121.8(4) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.2(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C13 122.3(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C12 C13 C8 118.0(3) . . ? C12 C13 C14 119.5(3) . . ? C8 C13 C14 122.5(3) . . ? N3 C14 N4 120.0(3) . . ? N3 C14 C13 120.7(3) . . ? N4 C14 C13 119.3(3) . . ? O6 C15 C16 117.2(3) . . ? O6 C15 C20 123.6(3) . . ? C16 C15 C20 119.2(3) . . ? C17 C16 C15 120.6(4) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 121.0(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 121.9(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 118.1(3) . . ? C19 C20 C21 119.0(3) . . ? C15 C20 C21 122.9(3) . . ? N5 C21 N6 120.3(3) . . ? N5 C21 C20 119.9(3) . . ? N6 C21 C20 119.8(3) . . ? O9 C22 O8 124.3(4) . . ? O9 C22 C23 118.9(4) . . ? O8 C22 C23 116.8(4) . . ? C24 C23 C28 119.4(4) . . ? C24 C23 C22 121.0(3) . . ? C28 C23 C22 119.6(4) . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.6(4) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 119.8(4) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? O10 C29 C30 113.4(4) . . ? O10 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? O10 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O11 C31 C32 110.5(4) . . ? O11 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? O11 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34B C33 C34A 51.5(12) . . ? C34B C33 O12 120.7(10) . . ? C34A C33 O12 114.5(5) . . ? C34B C33 H33A 130.7 . . ? C34A C33 H33A 108.6 . . ? O12 C33 H33A 108.6 . . ? C34B C33 H33B 58.0 . . ? C34A C33 H33B 108.6 . . ? O12 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C34B C33 H33C 107.1 . . ? C34A C33 H33C 60.2 . . ? O12 C33 H33C 107.2 . . ? H33A C33 H33C 54.2 . . ? H33B C33 H33C 143.7 . . ? C34B C33 H33D 107.2 . . ? C34A C33 H33D 138.3 . . ? O12 C33 H33D 107.2 . . ? H33A C33 H33D 54.2 . . ? H33B C33 H33D 56.5 . . ? H33C C33 H33D 106.8 . . ? C33 C34A H34A 109.5 . . ? H33C C34A H34A 102.1 . . ? C33 C34A H34B 109.5 . . ? H33C C34A H34B 73.6 . . ? C33 C34A H34C 109.5 . . ? H33C C34A H34C 144.4 . . ? C33 C34B H34D 109.5 . . ? C33 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C35 O13 H13 109.5 . . ? O13 C35 C36 112.2(4) . . ? O13 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? O13 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C37 O14 H14 109.5 . . ? C38 C37 O14 118.0(6) . . ? C38 C37 H37A 107.8 . . ? O14 C37 H37A 107.8 . . ? C38 C37 H37B 107.8 . . ? O14 C37 H37B 107.8 . . ? H37A C37 H37B 107.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.615 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.093 data_jml050209 _database_code_depnum_ccdc_archive 'CCDC 888450' #TrackingRef 'web_deposit_cif_file_2_Lise-MarieChamoreau_1340629901.jml050209_publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H90 Mn6 N12 O24, 4(C3 H8 O)' _chemical_formula_sum 'C84 H122 Mn6 N12 O28' _chemical_formula_weight 2077.58 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6828(16) _cell_length_b 14.0471(16) _cell_length_c 15.9646(17) _cell_angle_alpha 89.104(8) _cell_angle_beta 71.940(9) _cell_angle_gamma 66.627(9) _cell_volume 2463.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 67 _cell_measurement_theta_min 4.9 _cell_measurement_theta_max 14.9 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43150 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.1494 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 29.99 _reflns_number_total 14150 _reflns_number_gt 6044 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Distances C35-C36 and C40-C42 were restrained to be 1.54 A. 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^ > 2\s(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^)+(0.0898P)^2^+1.3151P] 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 14150 _refine_ls_number_parameters 594 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2001 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.045 _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 0.62775(6) 0.43487(5) 0.78176(4) 0.03064(19) Uani 1 1 d . . . Mn2 Mn 0.59727(6) 0.55727(5) 0.96835(4) 0.02801(18) Uani 1 1 d . . . Mn3 Mn 0.51347(6) 0.69167(5) 0.81277(4) 0.02977(19) Uani 1 1 d . . . O1 O 0.5829(3) 0.5605(2) 0.85344(18) 0.0278(7) Uani 1 1 d . . . O2 O 0.6386(3) 0.3103(2) 0.7263(2) 0.0421(8) Uani 1 1 d . . . O3 O 0.6151(3) 0.4128(2) 0.96651(19) 0.0301(7) Uani 1 1 d . . . O4 O 0.6112(3) 0.5527(2) 1.0841(2) 0.0351(8) Uani 1 1 d . . . O5 O 0.4879(3) 0.7658(2) 0.9211(2) 0.0338(7) Uani 1 1 d . . . O6 O 0.4209(3) 0.8220(2) 0.7813(2) 0.0376(8) Uani 1 1 d . . . O7 O 0.5504(3) 0.5107(2) 0.7024(2) 0.0437(9) Uani 1 1 d . . . O8 O 0.8088(4) 0.3928(3) 0.7067(3) 0.0743(14) Uani 1 1 d . . . O9 O 0.8784(4) 0.5120(4) 0.7115(4) 0.0853(16) Uani 1 1 d . . . O10 O 0.7923(3) 0.5194(3) 0.8974(2) 0.0459(9) Uani 1 1 d . . . H10A H 0.8186 0.5080 0.8336 0.069 Uiso 1 1 d R . . O11 O 0.6909(3) 0.7044(3) 0.7442(2) 0.0437(9) Uani 1 1 d . . . H11A H 0.7399 0.6445 0.7289 0.066 Uiso 1 1 d R . . O12 O 0.3199(3) 0.6653(3) 0.8733(2) 0.0390(8) Uani 1 1 d . . . H12A H 0.3373 0.6053 0.8816 0.058 Uiso 1 1 d R . . N1 N 0.6670(3) 0.3563(3) 0.8805(2) 0.0290(8) Uani 1 1 d . . . N2 N 0.7562(3) 0.2150(3) 0.9499(3) 0.0414(10) Uani 1 1 d . . . H2A H 0.7204 0.2549 0.9981 0.050 Uiso 1 1 d R . . H2B H 0.7711 0.1496 0.9515 0.050 Uiso 1 1 d R . . N3 N 0.5425(3) 0.7116(3) 0.9820(2) 0.0303(8) Uani 1 1 d . . . N4 N 0.4765(4) 0.8795(3) 1.0464(3) 0.0506(12) Uani 1 1 d . . . H4A H 0.4432 0.9024 1.0041 0.061 Uiso 1 1 d R . . H4B H 0.4558 0.9197 1.0928 0.061 Uiso 1 1 d R . . N5 N 0.5285(3) 0.6175(3) 0.7021(2) 0.0313(9) Uani 1 1 d . . . N6 N 0.4955(4) 0.5941(3) 0.5719(3) 0.0499(12) Uani 1 1 d . . . H6A H 0.5193 0.5206 0.5774 0.060 Uiso 1 1 d R . . H6B H 0.4663 0.6203 0.5316 0.060 Uiso 1 1 d R . . C1 C 0.7241(5) 0.2133(4) 0.7258(3) 0.0402(12) Uani 1 1 d . . . C2 C 0.7604(6) 0.1374(4) 0.6548(4) 0.0551(15) Uani 1 1 d . . . H2 H 0.7213 0.1535 0.6112 0.066 Uiso 1 1 calc R . . C3 C 0.8534(6) 0.0385(4) 0.6470(4) 0.0672(19) Uani 1 1 d . . . H3 H 0.8776 -0.0118 0.5980 0.081 Uiso 1 1 calc R . . C4 C 0.9106(6) 0.0135(4) 0.7109(4) 0.0624(17) Uani 1 1 d . . . H4 H 0.9763 -0.0526 0.7043 0.075 Uiso 1 1 calc R . . C5 C 0.8714(5) 0.0851(4) 0.7836(4) 0.0482(14) Uani 1 1 d . . . H5 H 0.9092 0.0667 0.8279 0.058 Uiso 1 1 calc R . . C6 C 0.7764(4) 0.1854(3) 0.7944(3) 0.0350(11) Uani 1 1 d . . . C7 C 0.7323(4) 0.2549(4) 0.8773(3) 0.0331(11) Uani 1 1 d . . . C8 C 0.6193(4) 0.6259(4) 1.1338(3) 0.0307(10) Uani 1 1 d . . . C9 C 0.6633(5) 0.5931(4) 1.2048(3) 0.0421(12) Uani 1 1 d . . . H9 H 0.6892 0.5216 1.2140 0.051 Uiso 1 1 calc R . . C10 C 0.6695(6) 0.6624(5) 1.2612(4) 0.0601(16) Uani 1 1 d . . . H10 H 0.6982 0.6388 1.3094 0.072 Uiso 1 1 calc R . . C11 C 0.6335(7) 0.7677(5) 1.2474(4) 0.073(2) Uani 1 1 d . . . H11 H 0.6381 0.8156 1.2860 0.088 Uiso 1 1 calc R . . C12 C 0.5914(6) 0.8018(5) 1.1778(4) 0.0580(16) Uani 1 1 d . . . H12 H 0.5666 0.8736 1.1697 0.070 Uiso 1 1 calc R . . C13 C 0.5840(4) 0.7328(4) 1.1177(3) 0.0342(11) Uani 1 1 d . . . C14 C 0.5323(4) 0.7746(3) 1.0464(3) 0.0328(10) Uani 1 1 d . . . C15 C 0.4244(4) 0.8459(4) 0.6991(3) 0.0358(11) Uani 1 1 d . . . C16 C 0.3892(6) 0.9517(4) 0.6843(4) 0.0524(15) Uani 1 1 d . . . H16 H 0.3675 1.0026 0.7322 0.063 Uiso 1 1 calc R . . C17 C 0.3850(6) 0.9837(5) 0.6035(4) 0.0613(17) Uani 1 1 d . . . H17 H 0.3601 1.0558 0.5963 0.074 Uiso 1 1 calc R . . C18 C 0.4176(6) 0.9102(5) 0.5313(4) 0.0587(16) Uani 1 1 d . . . H18 H 0.4145 0.9320 0.4751 0.070 Uiso 1 1 calc R . . C19 C 0.4541(5) 0.8054(4) 0.5431(3) 0.0443(13) Uani 1 1 d . . . H19 H 0.4780 0.7554 0.4939 0.053 Uiso 1 1 calc R . . C20 C 0.4570(4) 0.7709(4) 0.6262(3) 0.0337(11) Uani 1 1 d . . . C21 C 0.4948(4) 0.6568(4) 0.6344(3) 0.0334(11) Uani 1 1 d . . . C22 C 0.8898(5) 0.4266(4) 0.6792(4) 0.0485(14) Uani 1 1 d . . . C23 C 1.0105(4) 0.3532(4) 0.6138(3) 0.0435(13) Uani 1 1 d . . . C28 C 1.0939(6) 0.3910(6) 0.5665(5) 0.093(3) Uani 1 1 d . . . H28 H 1.0766 0.4630 0.5760 0.112 Uiso 1 1 calc R . . C27 C 1.2034(7) 0.3231(9) 0.5050(6) 0.125(4) Uani 1 1 d . . . H27 H 1.2595 0.3502 0.4721 0.150 Uiso 1 1 calc R . . C26 C 1.2322(6) 0.2203(8) 0.4906(5) 0.091(3) Uani 1 1 d . . . H26 H 1.3084 0.1756 0.4490 0.109 Uiso 1 1 calc R . . C25 C 1.1510(6) 0.1801(6) 0.5363(6) 0.093(3) Uani 1 1 d . . . H25 H 1.1700 0.1078 0.5258 0.111 Uiso 1 1 calc R . . C24 C 1.0364(5) 0.2491(5) 0.6005(5) 0.0646(18) Uani 1 1 d . . . H24 H 0.9797 0.2225 0.6331 0.078 Uiso 1 1 calc R . . C29 C 0.8988(5) 0.4792(6) 0.9221(4) 0.071(2) Uani 1 1 d . . . H29 H 0.8745 0.4909 0.9882 0.085 Uiso 1 1 calc R . . C30 C 0.9718(8) 0.3679(6) 0.8922(7) 0.123(3) Uani 1 1 d . . . H30A H 0.9246 0.3283 0.9207 0.184 Uiso 1 1 calc R . . H30B H 1.0459 0.3452 0.9083 0.184 Uiso 1 1 calc R . . H30C H 0.9939 0.3553 0.8276 0.184 Uiso 1 1 calc R . . C31 C 0.9809(8) 0.5376(9) 0.8804(8) 0.132(4) Uani 1 1 d . . . H31A H 1.0053 0.5265 0.8155 0.198 Uiso 1 1 calc R . . H31B H 1.0536 0.5105 0.8984 0.198 Uiso 1 1 calc R . . H31C H 0.9354 0.6125 0.9010 0.198 Uiso 1 1 calc R . . C32 C 0.7380(5) 0.7699(4) 0.7766(4) 0.0539(15) Uani 1 1 d . . . H32 H 0.7355 0.7561 0.8386 0.065 Uiso 1 1 calc R . . C33 C 0.8654(7) 0.7465(6) 0.7229(6) 0.095(3) Uani 1 1 d . . . H33A H 0.9146 0.6711 0.7163 0.142 Uiso 1 1 calc R . . H33B H 0.8976 0.7836 0.7527 0.142 Uiso 1 1 calc R . . H33C H 0.8686 0.7693 0.6642 0.142 Uiso 1 1 calc R . . C34 C 0.6557(6) 0.8827(4) 0.7796(5) 0.0694(19) Uani 1 1 d . . . H34A H 0.6525 0.8971 0.7199 0.104 Uiso 1 1 calc R . . H34B H 0.6873 0.9275 0.8007 0.104 Uiso 1 1 calc R . . H34C H 0.5737 0.8971 0.8200 0.104 Uiso 1 1 calc R . . C35 C 0.2214(9) 0.6910(8) 0.8358(7) 0.115(3) Uiso 1 1 d D . . H35A H 0.2566 0.6508 0.7761 0.138 Uiso 1 1 calc R . . H35B H 0.1623 0.6652 0.8730 0.138 Uiso 1 1 calc R . . C36 C 0.1564(13) 0.7958(11) 0.8274(10) 0.193(6) Uiso 1 1 d D . . H36A H 0.0940 0.8010 0.8015 0.289 Uiso 1 1 calc R . . H36B H 0.2123 0.8227 0.7888 0.289 Uiso 1 1 calc R . . H36C H 0.1175 0.8371 0.8861 0.289 Uiso 1 1 calc R . . C37 C 0.2095(6) 1.0645(5) 0.9411(5) 0.0692(19) Uani 1 1 d . . . H37A H 0.2196 1.1152 0.8979 0.083 Uiso 0.50 1 calc PR A 1 H37B H 0.2644 1.0850 0.8940 0.083 Uiso 0.50 1 d PR A 2 O13A O 0.3285(18) 0.9905(12) 0.9248(12) 0.083(6) Uani 0.50 1 d P B 1 H13A H 0.3413 0.9296 0.9121 0.125 Uiso 0.50 1 d PR B 1 C38A C 0.166(3) 1.130(3) 1.033(2) 0.119(12) Uani 0.50 1 d P B 1 H38A H 0.2326 1.1445 1.0396 0.178 Uiso 0.50 1 calc PR B 1 H38B H 0.1416 1.0900 1.0806 0.178 Uiso 0.50 1 calc PR B 1 H38C H 0.0964 1.1957 1.0368 0.178 Uiso 0.50 1 calc PR B 1 C39A C 0.113(2) 1.0447(17) 0.9289(18) 0.078(6) Uani 0.50 1 d P B 1 H39A H 0.1415 1.0047 0.8706 0.117 Uiso 0.50 1 calc PR B 1 H39B H 0.0443 1.1112 0.9325 0.117 Uiso 0.50 1 calc PR B 1 H39C H 0.0869 1.0045 0.9754 0.117 Uiso 0.50 1 calc PR B 1 O13B O 0.2928(17) 0.9629(12) 0.9470(12) 0.060(4) Uani 0.50 1 d P B 2 H13B H 0.3164 0.9158 0.9074 0.090 Uiso 0.50 1 d PR B 2 C38B C 0.1897(19) 1.1390(13) 1.0172(14) 0.050(5) Uani 0.50 1 d P B 2 H38D H 0.2646 1.1172 1.0322 0.075 Uiso 0.50 1 calc PR B 2 H38E H 0.1236 1.1384 1.0690 0.075 Uiso 0.50 1 calc PR B 2 H38F H 0.1680 1.2097 1.0000 0.075 Uiso 0.50 1 calc PR B 2 C39B C 0.121(3) 1.082(2) 0.900(2) 0.136(14) Uani 0.50 1 d P B 2 H39D H 0.1518 1.0268 0.8511 0.204 Uiso 0.50 1 calc PR B 2 H39E H 0.1026 1.1500 0.8768 0.204 Uiso 0.50 1 calc PR B 2 H39F H 0.0466 1.0828 0.9436 0.204 Uiso 0.50 1 calc PR B 2 O14 O 0.3526(3) 0.6537(3) 0.4546(2) 0.0521(10) Uani 1 1 d . . . H14A H 0.3753 0.6525 0.3889 0.078 Uiso 1 1 d R . . C40 C 0.2284(7) 0.6764(6) 0.4920(6) 0.087(2) Uiso 1 1 d D . . H40 H 0.1887 0.7000 0.4456 0.104 Uiso 1 1 calc R . . C41 C 0.1663(10) 0.7635(9) 0.5706(8) 0.145(4) Uiso 1 1 d . . . H41A H 0.0800 0.7773 0.5960 0.217 Uiso 1 1 calc R . . H41B H 0.1741 0.8272 0.5499 0.217 Uiso 1 1 calc R . . H41C H 0.2054 0.7414 0.6160 0.217 Uiso 1 1 calc R . . C42 C 0.2091(11) 0.5904(9) 0.5235(9) 0.166(5) Uiso 1 1 d D . . H42A H 0.2628 0.5287 0.4797 0.248 Uiso 1 1 calc R . . H42B H 0.1241 0.6029 0.5338 0.248 Uiso 1 1 calc R . . H42C H 0.2266 0.5787 0.5793 0.248 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 0.0365(4) 0.0230(3) 0.0255(4) -0.0032(3) -0.0074(3) -0.0074(3) Mn2 0.0333(4) 0.0219(3) 0.0259(4) -0.0022(3) -0.0099(3) -0.0082(3) Mn3 0.0385(4) 0.0225(3) 0.0244(4) -0.0011(3) -0.0099(3) -0.0089(3) O1 0.0375(17) 0.0218(15) 0.0237(16) 0.0001(12) -0.0139(13) -0.0089(13) O2 0.058(2) 0.0239(16) 0.0393(19) -0.0055(15) -0.0216(17) -0.0067(15) O3 0.0371(17) 0.0231(15) 0.0226(15) -0.0018(13) -0.0063(13) -0.0076(13) O4 0.051(2) 0.0273(16) 0.0311(17) 0.0027(14) -0.0220(15) -0.0143(15) O5 0.0459(19) 0.0212(15) 0.0290(17) 0.0003(13) -0.0158(15) -0.0058(14) O6 0.054(2) 0.0249(16) 0.0286(17) 0.0017(14) -0.0151(16) -0.0102(15) O7 0.074(2) 0.0218(16) 0.0372(19) -0.0005(14) -0.0273(18) -0.0145(16) O8 0.046(2) 0.060(3) 0.080(3) 0.015(2) 0.015(2) -0.012(2) O9 0.054(3) 0.056(3) 0.123(4) -0.029(3) -0.003(3) -0.019(2) O10 0.0275(17) 0.061(2) 0.041(2) -0.0005(18) -0.0091(15) -0.0113(16) O11 0.0449(19) 0.0306(18) 0.048(2) -0.0065(16) -0.0047(17) -0.0153(16) O12 0.0423(18) 0.0351(18) 0.0403(19) 0.0064(15) -0.0199(16) -0.0121(15) N1 0.0306(19) 0.0225(18) 0.0238(19) -0.0062(15) -0.0023(16) -0.0056(15) N2 0.044(2) 0.025(2) 0.038(2) -0.0012(18) -0.0112(19) 0.0009(18) N3 0.036(2) 0.0256(19) 0.028(2) 0.0011(16) -0.0114(17) -0.0112(16) N4 0.082(3) 0.026(2) 0.041(3) -0.0032(19) -0.029(2) -0.013(2) N5 0.043(2) 0.0204(18) 0.027(2) -0.0009(16) -0.0104(17) -0.0103(17) N6 0.079(3) 0.033(2) 0.034(2) 0.0029(19) -0.030(2) -0.010(2) C1 0.048(3) 0.024(2) 0.039(3) -0.007(2) -0.006(2) -0.011(2) C2 0.083(4) 0.028(3) 0.047(3) -0.006(2) -0.027(3) -0.011(3) C3 0.098(5) 0.027(3) 0.055(4) -0.014(3) -0.024(4) -0.004(3) C4 0.070(4) 0.030(3) 0.059(4) -0.010(3) -0.021(3) 0.008(3) C5 0.044(3) 0.034(3) 0.051(3) -0.009(3) -0.012(3) -0.002(2) C6 0.038(3) 0.021(2) 0.036(3) -0.005(2) -0.006(2) -0.007(2) C7 0.027(2) 0.031(2) 0.036(3) -0.001(2) -0.007(2) -0.0084(19) C8 0.033(2) 0.034(2) 0.029(2) -0.002(2) -0.011(2) -0.018(2) C9 0.053(3) 0.037(3) 0.042(3) 0.000(2) -0.025(3) -0.016(2) C10 0.094(5) 0.056(4) 0.052(4) 0.011(3) -0.047(4) -0.036(4) C11 0.129(6) 0.055(4) 0.071(4) 0.007(3) -0.062(4) -0.052(4) C12 0.098(5) 0.042(3) 0.053(4) 0.009(3) -0.041(4) -0.036(3) C13 0.047(3) 0.034(3) 0.028(2) 0.003(2) -0.015(2) -0.021(2) C14 0.043(3) 0.023(2) 0.030(2) 0.0036(19) -0.013(2) -0.011(2) C15 0.044(3) 0.028(2) 0.032(3) 0.005(2) -0.011(2) -0.012(2) C16 0.087(4) 0.032(3) 0.047(3) 0.015(2) -0.036(3) -0.023(3) C17 0.105(5) 0.038(3) 0.052(4) 0.020(3) -0.038(4) -0.031(3) C18 0.093(5) 0.055(4) 0.044(3) 0.024(3) -0.030(3) -0.041(3) C19 0.060(3) 0.041(3) 0.038(3) 0.005(2) -0.020(3) -0.024(3) C20 0.039(3) 0.036(3) 0.028(2) 0.010(2) -0.010(2) -0.018(2) C21 0.036(2) 0.027(2) 0.026(2) -0.005(2) -0.007(2) -0.005(2) C22 0.044(3) 0.043(3) 0.048(3) -0.008(3) -0.008(3) -0.013(3) C23 0.032(3) 0.054(3) 0.033(3) -0.004(2) -0.004(2) -0.010(2) C28 0.051(4) 0.082(5) 0.111(6) 0.015(5) 0.012(4) -0.021(4) C27 0.054(5) 0.137(9) 0.106(7) 0.037(7) 0.035(5) -0.008(5) C26 0.044(4) 0.121(7) 0.061(5) -0.041(5) 0.000(3) 0.000(5) C25 0.053(4) 0.066(5) 0.138(7) -0.044(5) -0.032(5) -0.001(4) C24 0.042(3) 0.060(4) 0.087(5) -0.006(4) -0.021(3) -0.016(3) C29 0.042(3) 0.098(5) 0.056(4) 0.008(4) -0.017(3) -0.012(4) C30 0.119(7) 0.078(6) 0.136(8) 0.024(6) -0.055(7) 0.002(5) C31 0.097(7) 0.172(10) 0.171(10) 0.038(8) -0.063(7) -0.084(7) C32 0.055(3) 0.044(3) 0.063(4) -0.008(3) -0.008(3) -0.028(3) C33 0.089(6) 0.074(5) 0.124(7) -0.006(5) -0.030(5) -0.039(4) C34 0.079(4) 0.041(3) 0.085(5) -0.006(3) -0.015(4) -0.031(3) C37 0.073(4) 0.053(4) 0.064(4) -0.007(3) -0.027(4) -0.004(3) O13A 0.131(16) 0.032(8) 0.071(11) -0.011(6) -0.070(11) 0.010(7) C38A 0.083(14) 0.14(2) 0.12(2) -0.039(16) 0.013(14) -0.074(14) C39A 0.074(11) 0.072(15) 0.091(14) 0.009(11) -0.050(10) -0.016(12) O13B 0.082(8) 0.029(7) 0.052(7) -0.002(5) -0.028(6) -0.002(5) C38B 0.059(11) 0.028(6) 0.036(7) -0.005(6) -0.014(8) 0.009(7) C39B 0.15(2) 0.070(17) 0.17(3) 0.022(15) -0.11(3) 0.007(15) O14 0.060(2) 0.048(2) 0.036(2) -0.0085(17) -0.0179(18) -0.0086(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O7 1.898(3) . ? Mn1 O1 1.900(3) . ? Mn1 O2 1.910(3) . ? Mn1 N1 1.986(4) . ? Mn1 O8 2.073(4) . ? Mn2 O1 1.897(3) . ? Mn2 O4 1.907(3) . ? Mn2 O3 1.950(3) . ? Mn2 N3 1.989(4) . ? Mn2 O10 2.218(3) . ? Mn2 O3 2.427(3) 2_667 ? Mn3 O6 1.900(3) . ? Mn3 O1 1.903(3) . ? Mn3 O5 1.903(3) . ? Mn3 N5 1.983(4) . ? Mn3 O11 2.254(3) . ? Mn3 O12 2.517(3) . ? O2 C1 1.362(5) . ? O3 N1 1.418(4) . ? O3 Mn2 2.427(3) 2_667 ? O4 C8 1.364(5) . ? O5 N3 1.407(5) . ? O6 C15 1.342(5) . ? O7 N5 1.413(5) . ? O8 C22 1.255(6) . ? O9 C22 1.250(7) . ? O10 C29 1.420(7) . ? O10 H10A 0.9626 . ? O11 C32 1.454(6) . ? O11 H11A 0.8070 . ? O12 C35 1.466(10) . ? O12 H12A 0.8017 . ? N1 C7 1.326(5) . ? N2 C7 1.346(6) . ? N2 H2A 0.8403 . ? N2 H2B 0.8641 . ? N3 C14 1.309(6) . ? N4 C14 1.357(6) . ? N4 H4A 0.8947 . ? N4 H4B 0.8436 . ? N5 C21 1.317(6) . ? N6 C21 1.337(6) . ? N6 H6A 0.9646 . ? N6 H6B 0.8489 . ? C1 C2 1.399(7) . ? C1 C6 1.421(7) . ? C2 C3 1.397(7) . ? C2 H2 0.9500 . ? C3 C4 1.391(8) . ? C3 H3 0.9500 . ? C4 C5 1.374(7) . ? C4 H4 0.9500 . ? C5 C6 1.414(6) . ? C5 H5 0.9500 . ? C6 C7 1.471(6) . ? C8 C9 1.407(6) . ? C8 C13 1.430(6) . ? C9 C10 1.378(7) . ? C9 H9 0.9500 . ? C10 C11 1.401(8) . ? C10 H10 0.9500 . ? C11 C12 1.377(8) . ? C11 H11 0.9500 . ? C12 C13 1.424(7) . ? C12 H12 0.9500 . ? C13 C14 1.484(6) . ? C15 C16 1.411(7) . ? C15 C20 1.425(7) . ? C16 C17 1.369(7) . ? C16 H16 0.9500 . ? C17 C18 1.404(8) . ? C17 H17 0.9500 . ? C18 C19 1.386(7) . ? C18 H18 0.9500 . ? C19 C20 1.412(7) . ? C19 H19 0.9500 . ? C20 C21 1.497(6) . ? C22 C23 1.512(7) . ? C23 C24 1.369(8) . ? C23 C28 1.382(8) . ? C28 C27 1.391(10) . ? C28 H28 0.9500 . ? C27 C26 1.347(12) . ? C27 H27 0.9500 . ? C26 C25 1.377(11) . ? C26 H26 0.9500 . ? C25 C24 1.447(9) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? C29 C30 1.459(10) . ? C29 C31 1.560(11) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.477(9) . ? C32 C34 1.504(8) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.402(12) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O13A 1.40(2) . ? C37 C39B 1.41(3) . ? C37 O13B 1.422(18) . ? C37 C39A 1.43(3) . ? C37 C38B 1.51(2) . ? C37 C38A 1.56(3) . ? C37 H37A 1.0000 . ? C37 H37B 0.9800 . ? O13A H13A 0.8212 . ? O13A H13B 1.1687 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? O13B H13A 0.6893 . ? O13B H13B 0.8164 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? O14 C40 1.401(8) . ? O14 H14A 0.9967 . ? C40 C42 1.382(11) . ? C40 C41 1.537(12) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O7 Mn1 O1 91.26(13) . . ? O7 Mn1 O2 88.50(14) . . ? O1 Mn1 O2 167.26(14) . . ? O7 Mn1 N1 165.39(16) . . ? O1 Mn1 N1 88.60(13) . . ? O2 Mn1 N1 88.44(14) . . ? O7 Mn1 O8 100.36(17) . . ? O1 Mn1 O8 104.64(17) . . ? O2 Mn1 O8 87.91(17) . . ? N1 Mn1 O8 93.80(16) . . ? O1 Mn2 O4 179.34(13) . . ? O1 Mn2 O3 89.97(12) . . ? O4 Mn2 O3 89.41(13) . . ? O1 Mn2 N3 90.36(14) . . ? O4 Mn2 N3 90.20(14) . . ? O3 Mn2 N3 168.08(14) . . ? O1 Mn2 O10 85.12(13) . . ? O4 Mn2 O10 95.17(14) . . ? O3 Mn2 O10 95.73(13) . . ? N3 Mn2 O10 96.17(14) . . ? O1 Mn2 O3 90.20(12) . 2_667 ? O4 Mn2 O3 89.47(12) . 2_667 ? O3 Mn2 O3 80.54(12) . 2_667 ? N3 Mn2 O3 87.54(13) . 2_667 ? O10 Mn2 O3 174.03(12) . 2_667 ? O6 Mn3 O1 171.27(14) . . ? O6 Mn3 O5 87.46(13) . . ? O1 Mn3 O5 91.77(12) . . ? O6 Mn3 N5 90.75(14) . . ? O1 Mn3 N5 89.50(13) . . ? O5 Mn3 N5 176.29(15) . . ? O6 Mn3 O11 92.67(14) . . ? O1 Mn3 O11 96.06(13) . . ? O5 Mn3 O11 93.02(13) . . ? N5 Mn3 O11 90.31(14) . . ? O6 Mn3 O12 87.97(13) . . ? O1 Mn3 O12 83.40(12) . . ? O5 Mn3 O12 93.49(12) . . ? N5 Mn3 O12 83.19(13) . . ? O11 Mn3 O12 173.48(12) . . ? Mn2 O1 Mn1 120.77(15) . . ? Mn2 O1 Mn3 119.38(14) . . ? Mn1 O1 Mn3 119.73(15) . . ? C1 O2 Mn1 123.5(3) . . ? N1 O3 Mn2 114.4(2) . . ? N1 O3 Mn2 111.1(2) . 2_667 ? Mn2 O3 Mn2 99.46(12) . 2_667 ? C8 O4 Mn2 128.5(3) . . ? N3 O5 Mn3 119.5(2) . . ? C15 O6 Mn3 126.8(3) . . ? N5 O7 Mn1 117.9(3) . . ? C22 O8 Mn1 143.7(4) . . ? C29 O10 Mn2 134.1(3) . . ? C29 O10 H10A 106.9 . . ? Mn2 O10 H10A 116.4 . . ? C32 O11 Mn3 126.5(3) . . ? C32 O11 H11A 113.0 . . ? Mn3 O11 H11A 104.0 . . ? C35 O12 Mn3 128.1(4) . . ? C35 O12 H12A 104.5 . . ? Mn3 O12 H12A 108.4 . . ? C7 N1 O3 114.5(4) . . ? C7 N1 Mn1 128.1(3) . . ? O3 N1 Mn1 117.3(2) . . ? C7 N2 H2A 117.5 . . ? C7 N2 H2B 115.5 . . ? H2A N2 H2B 118.2 . . ? C14 N3 O5 112.4(3) . . ? C14 N3 Mn2 130.4(3) . . ? O5 N3 Mn2 116.4(2) . . ? C14 N4 H4A 118.0 . . ? C14 N4 H4B 119.3 . . ? H4A N4 H4B 120.2 . . ? C21 N5 O7 112.2(4) . . ? C21 N5 Mn3 129.0(3) . . ? O7 N5 Mn3 116.9(3) . . ? C21 N6 H6A 119.6 . . ? C21 N6 H6B 119.7 . . ? H6A N6 H6B 120.2 . . ? O2 C1 C2 118.0(5) . . ? O2 C1 C6 123.2(4) . . ? C2 C1 C6 118.8(4) . . ? C3 C2 C1 121.0(5) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.9(5) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 118.4(4) . . ? C5 C6 C7 118.9(5) . . ? C1 C6 C7 122.7(4) . . ? N1 C7 N2 120.3(4) . . ? N1 C7 C6 119.6(4) . . ? N2 C7 C6 120.0(4) . . ? O4 C8 C9 117.2(4) . . ? O4 C8 C13 123.2(4) . . ? C9 C8 C13 119.6(4) . . ? C10 C9 C8 121.5(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.8(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.0(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 122.0(5) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C12 C13 C8 117.1(4) . . ? C12 C13 C14 119.8(4) . . ? C8 C13 C14 123.0(4) . . ? N3 C14 N4 119.3(4) . . ? N3 C14 C13 120.8(4) . . ? N4 C14 C13 119.9(4) . . ? O6 C15 C16 118.5(4) . . ? O6 C15 C20 123.7(4) . . ? C16 C15 C20 117.8(4) . . ? C17 C16 C15 122.5(5) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.0(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 121.8(5) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 118.8(4) . . ? C19 C20 C21 118.8(4) . . ? C15 C20 C21 122.4(4) . . ? N5 C21 N6 119.8(4) . . ? N5 C21 C20 120.6(4) . . ? N6 C21 C20 119.5(4) . . ? O9 C22 O8 122.2(5) . . ? O9 C22 C23 120.1(5) . . ? O8 C22 C23 117.2(5) . . ? C24 C23 C28 119.9(6) . . ? C24 C23 C22 119.9(5) . . ? C28 C23 C22 120.2(6) . . ? C23 C28 C27 119.7(8) . . ? C23 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C26 C27 C28 121.9(8) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C27 C26 C25 119.8(6) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C25 C24 119.3(7) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C23 C24 C25 119.3(6) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? O10 C29 C30 112.9(7) . . ? O10 C29 C31 109.7(6) . . ? C30 C29 C31 107.4(7) . . ? O10 C29 H29 108.9 . . ? C30 C29 H29 108.9 . . ? C31 C29 H29 108.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O11 C32 C33 112.4(5) . . ? O11 C32 C34 108.9(5) . . ? C33 C32 C34 111.6(5) . . ? O11 C32 H32 107.9 . . ? C33 C32 H32 107.9 . . ? C34 C32 H32 107.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 O12 118.6(10) . . ? C36 C35 H35A 107.7 . . ? O12 C35 H35A 107.7 . . ? C36 C35 H35B 107.7 . . ? O12 C35 H35B 107.7 . . ? H35A C35 H35B 107.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O13A C37 C39B 134.6(17) . . ? C39B C37 O13B 123.2(15) . . ? O13A C37 C39A 125.5(13) . . ? O13B C37 C39A 102.3(12) . . ? O13A C37 C38B 103.4(11) . . ? C39B C37 C38B 121.9(16) . . ? O13B C37 C38B 109.0(11) . . ? C39A C37 C38B 122.4(15) . . ? O13A C37 C38A 108.4(15) . . ? C39B C37 C38A 116(2) . . ? O13B C37 C38A 106.3(16) . . ? C39A C37 C38A 110.5(17) . . ? O13A C37 H37A 103.2 . . ? C39B C37 H37A 74.1 . . ? O13B C37 H37A 130.6 . . ? C39A C37 H37A 103.2 . . ? C38B C37 H37A 91.5 . . ? C38A C37 H37A 103.2 . . ? O13A C37 H37B 71.5 . . ? C39B C37 H37B 96.7 . . ? O13B C37 H37B 99.4 . . ? C39A C37 H37B 122.8 . . ? C38B C37 H37B 98.3 . . ? C38A C37 H37B 112.8 . . ? C37 O13A H13A 116.2 . . ? H37B O13A H13A 131.5 . . ? C37 O13A H13B 99.1 . . ? H37B O13A H13B 117.8 . . ? C37 C38A H38A 109.5 . . ? C37 C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C37 C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? C37 C39A H39A 109.5 . . ? C37 C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C37 C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? C37 O13B H13A 125.4 . . ? C37 O13B H13B 119.4 . . ? C37 C38B H38D 109.5 . . ? C37 C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37 C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C37 C39B H39D 109.5 . . ? C37 C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C37 C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C40 O14 H14A 110.0 . . ? C42 C40 O14 112.0(8) . . ? C42 C40 C41 107.2(9) . . ? O14 C40 C41 111.0(7) . . ? C42 C40 H40 108.9 . . ? O14 C40 H40 108.9 . . ? C41 C40 H40 108.9 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.117 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.107 data_pg180510 _database_code_depnum_ccdc_archive 'CCDC 888451' #TrackingRef 'web_deposit_cif_file_3_Lise-MarieChamoreau_1340629901.pg180510-publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H90 Mn6 N12 O24, 4(C2 H6 O), C2 H6 O' _chemical_formula_sum 'C74 H120 Mn6 N12 O29' _chemical_formula_weight 1971.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.177(2) _cell_length_b 15.5532(13) _cell_length_c 27.8361(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.768(8) _cell_angle_gamma 90.00 _cell_volume 9035.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 205 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 22.4 _exptl_crystal_description parallelepipped _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4120 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ; SADABS Sheldrick, G. M. (1996). University of G\=ottingen, Germany. ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51967 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13029 _reflns_number_gt 8749 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Models of disorder were introduced for the pivalate moiety, a coordinated ethanol molecule and a "free" ethanol molecule. The site occupation factors of each part was refined and then fixed to the rounded obtained value for further refinements. The Uij's of C22a and C22b were constrained to be equal. 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^ > 2\s(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^)+(0.0557P)^2^+8.2172P] 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 13029 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.002 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 0.379736(15) 0.22115(2) 0.077013(11) 0.02413(9) Uani 1 1 d . A . Mn2 Mn 0.244451(15) 0.15115(2) 0.015932(11) 0.02209(8) Uani 1 1 d . . . Mn3 Mn 0.268375(16) 0.15887(2) 0.134995(11) 0.02524(9) Uani 1 1 d . . . O1 O 0.29800(7) 0.17398(10) 0.07532(5) 0.0236(3) Uani 1 1 d . . . O2 O 0.45850(7) 0.27673(11) 0.07598(5) 0.0290(3) Uani 1 1 d . . . O3 O 0.30206(7) 0.21322(10) -0.01800(5) 0.0236(3) Uani 1 1 d . . . O4 O 0.18545(7) 0.13550(10) -0.04350(5) 0.0267(3) Uani 1 1 d . . . O5 O 0.18705(8) 0.12462(11) 0.10165(5) 0.0319(4) Uani 1 1 d . . . O6 O 0.23158(8) 0.16552(11) 0.19176(5) 0.0329(4) Uani 1 1 d . . . O7 O 0.38606(8) 0.25469(11) 0.14258(5) 0.0314(4) Uani 1 1 d . . . O8 O 0.42466(8) 0.09606(11) 0.09114(6) 0.0395(4) Uani 1 1 d . . . H8A H 0.3918 0.0605 0.0862 0.059 Uiso 1 1 d R A . O9 O 0.28833(9) 0.02619(11) 0.00791(6) 0.0381(4) Uani 1 1 d . C . H9A H 0.3040 0.0033 0.0355 0.057 Uiso 1 1 d R . . O10 O 0.30424(10) 0.03233(12) 0.15096(7) 0.0449(5) Uani 1 1 d . . . O11 O 0.34358(9) -0.03610(12) 0.09301(7) 0.0438(5) Uani 1 1 d . . . O12 O 0.24019(8) 0.31449(11) 0.12276(6) 0.0340(4) Uani 1 1 d . . . H12A H 0.2606 0.3385 0.0992 0.051 Uiso 1 1 d R . . N1 N 0.36617(8) 0.21158(12) 0.00581(6) 0.0237(4) Uani 1 1 d . . . N2 N 0.38982(10) 0.21656(15) -0.07161(7) 0.0366(5) Uani 1 1 d . . . H2A H 0.4155 0.2377 -0.0894 0.044 Uiso 1 1 d R A . H2B H 0.3467 0.2130 -0.0836 0.044 Uiso 1 1 d R . . N3 N 0.18256(9) 0.10143(12) 0.05325(6) 0.0263(4) Uani 1 1 d . . . N4 N 0.08950(11) 0.04039(17) 0.06644(8) 0.0507(7) Uani 1 1 d . . . H4A H 0.0528 0.0218 0.0570 0.061 Uiso 1 1 d R . . H4B H 0.0889 0.0747 0.0930 0.061 Uiso 1 1 d R . . N5 N 0.34745(9) 0.21039(12) 0.17017(6) 0.0264(4) Uani 1 1 d . . . N6 N 0.42030(10) 0.26119(15) 0.23362(7) 0.0397(5) Uani 1 1 d . . . H6A H 0.4315 0.2796 0.2654 0.048 Uiso 1 1 d R . . H6B H 0.4394 0.2876 0.2113 0.048 Uiso 1 1 d R . . C1 C 0.49768(11) 0.25575(15) 0.04515(8) 0.0279(5) Uani 1 1 d . A . C2 C 0.56371(11) 0.26403(17) 0.06103(9) 0.0359(6) Uani 1 1 d . . . H2 H 0.5791 0.2852 0.0929 0.043 Uiso 1 1 calc R . . C3 C 0.60669(12) 0.2419(2) 0.03114(10) 0.0445(7) Uani 1 1 d . . . H3 H 0.6513 0.2486 0.0426 0.053 Uiso 1 1 calc R . . C4 C 0.58616(13) 0.2102(2) -0.01484(11) 0.0475(7) Uani 1 1 d . . . H4 H 0.6162 0.1934 -0.0348 0.057 Uiso 1 1 calc R . . C5 C 0.52121(12) 0.20292(18) -0.03167(9) 0.0384(6) Uani 1 1 d . A . H5 H 0.5068 0.1818 -0.0637 0.046 Uiso 1 1 calc R . . C6 C 0.47623(11) 0.22601(15) -0.00257(8) 0.0281(5) Uani 1 1 d . . . C7 C 0.40802(11) 0.21839(15) -0.02338(8) 0.0266(5) Uani 1 1 d . A . C8 C 0.14548(11) 0.06769(15) -0.05112(8) 0.0269(5) Uani 1 1 d . . . C9 C 0.12949(12) 0.03668(17) -0.09844(9) 0.0365(6) Uani 1 1 d . . . H9 H 0.1452 0.0654 -0.1241 0.044 Uiso 1 1 calc R . . C10 C 0.09147(14) -0.03458(19) -0.10879(10) 0.0472(7) Uani 1 1 d . . . H10 H 0.0818 -0.0552 -0.1413 0.057 Uiso 1 1 calc R . . C11 C 0.06740(15) -0.07624(19) -0.07236(10) 0.0489(7) Uani 1 1 d . . . H11 H 0.0422 -0.1266 -0.0794 0.059 Uiso 1 1 calc R . . C12 C 0.08004(13) -0.04452(18) -0.02560(10) 0.0424(6) Uani 1 1 d . . . H12 H 0.0622 -0.0725 -0.0007 0.051 Uiso 1 1 calc R . . C13 C 0.11873(11) 0.02809(15) -0.01392(8) 0.0301(5) Uani 1 1 d . . . C14 C 0.13047(11) 0.05894(16) 0.03652(8) 0.0298(5) Uani 1 1 d . . . C15 C 0.26379(11) 0.15679(15) 0.23703(8) 0.0276(5) Uani 1 1 d . . . C16 C 0.23034(13) 0.12442(16) 0.27218(8) 0.0337(5) Uani 1 1 d . . . H16 H 0.1867 0.1083 0.2629 0.040 Uiso 1 1 calc R . . C17 C 0.25952(14) 0.11541(17) 0.32004(9) 0.0390(6) Uani 1 1 d . . . H17 H 0.2358 0.0937 0.3434 0.047 Uiso 1 1 calc R . . C18 C 0.32268(14) 0.13766(18) 0.33412(9) 0.0410(6) Uani 1 1 d . . . H18 H 0.3428 0.1310 0.3671 0.049 Uiso 1 1 calc R . . C19 C 0.35651(13) 0.16961(17) 0.30014(8) 0.0366(6) Uani 1 1 d . . . H19 H 0.4002 0.1849 0.3100 0.044 Uiso 1 1 calc R . . C20 C 0.32822(11) 0.18030(15) 0.25124(7) 0.0263(5) Uani 1 1 d . . . C21 C 0.36634(11) 0.21849(15) 0.21707(8) 0.0262(5) Uani 1 1 d . . . C22A C 0.4873(13) 0.0649(17) 0.1091(9) 0.082(4) Uani 0.40 1 d P A 1 H22A H 0.4846 0.0224 0.1352 0.098 Uiso 0.40 1 calc PR A 1 H22B H 0.5140 0.1134 0.1239 0.098 Uiso 0.40 1 calc PR A 1 C23A C 0.5186(6) 0.0253(7) 0.0730(5) 0.096(4) Uani 0.40 1 d P A 1 H23A H 0.4865 -0.0012 0.0479 0.145 Uiso 0.40 1 calc PR A 1 H23B H 0.5483 -0.0188 0.0884 0.145 Uiso 0.40 1 calc PR A 1 H23C H 0.5424 0.0690 0.0580 0.145 Uiso 0.40 1 calc PR A 1 C22B C 0.4783(8) 0.0850(10) 0.1284(5) 0.082(4) Uani 0.60 1 d P A 2 H22C H 0.4640 0.0873 0.1605 0.098 Uiso 0.60 1 calc PR A 2 H22D H 0.5087 0.1329 0.1271 0.098 Uiso 0.60 1 calc PR A 2 C23B C 0.5109(4) 0.0043(6) 0.1242(5) 0.159(5) Uani 0.60 1 d P A 2 H23D H 0.4802 -0.0382 0.1082 0.239 Uiso 0.60 1 calc PR A 2 H23E H 0.5296 -0.0164 0.1568 0.239 Uiso 0.60 1 calc PR A 2 H23F H 0.5449 0.0127 0.1049 0.239 Uiso 0.60 1 calc PR A 2 C24 C 0.29861(17) -0.0246(2) -0.03264(10) 0.0557(8) Uani 1 1 d . . . H24A H 0.3444 -0.0407 -0.0290 0.067 Uiso 0.80 1 calc PR B 1 H24B H 0.2873 0.0090 -0.0631 0.067 Uiso 0.80 1 calc PR B 1 H24C H 0.2710 -0.0066 -0.0623 0.067 Uiso 0.20 1 d PR B 2 H24D H 0.2915 -0.0852 -0.0271 0.067 Uiso 0.20 1 d PR B 2 C25 C 0.2566(2) -0.1072(3) -0.03553(16) 0.0664(13) Uani 0.80 1 d P C 1 H25A H 0.2681 -0.1404 -0.0054 0.100 Uiso 0.80 1 calc PR C 1 H25B H 0.2640 -0.1423 -0.0633 0.100 Uiso 0.80 1 calc PR C 1 H25C H 0.2113 -0.0910 -0.0397 0.100 Uiso 0.80 1 calc PR C 1 C25B C 0.3765(9) -0.0043(9) -0.0352(6) 0.056(4) Uani 0.20 1 d P C 2 H25D H 0.4029 -0.0189 -0.0038 0.085 Uiso 0.20 1 calc PR C 2 H25E H 0.3817 0.0568 -0.0422 0.085 Uiso 0.20 1 calc PR C 2 H25F H 0.3899 -0.0391 -0.0610 0.085 Uiso 0.20 1 calc PR C 2 C26 C 0.31343(12) -0.03403(17) 0.12843(9) 0.0337(6) Uani 1 1 d . D . C27 C 0.28718(15) -0.11787(19) 0.14475(11) 0.0481(7) Uani 1 1 d . . . C28A C 0.3143(5) -0.1976(4) 0.1210(4) 0.081(3) Uani 0.50 1 d P D 1 H28A H 0.2935 -0.2499 0.1303 0.122 Uiso 0.50 1 calc PR D 1 H28B H 0.3606 -0.2015 0.1324 0.122 Uiso 0.50 1 calc PR D 1 H28C H 0.3058 -0.1915 0.0855 0.122 Uiso 0.50 1 calc PR D 1 C29A C 0.2154(5) -0.1144(8) 0.1228(6) 0.121(6) Uani 0.50 1 d P D 1 H29A H 0.2105 -0.1101 0.0872 0.182 Uiso 0.50 1 calc PR D 1 H29B H 0.1959 -0.0641 0.1356 0.182 Uiso 0.50 1 calc PR D 1 H29C H 0.1943 -0.1668 0.1316 0.182 Uiso 0.50 1 calc PR D 1 C30A C 0.2961(9) -0.1283(6) 0.1971(3) 0.120(6) Uani 0.50 1 d P D 1 H30A H 0.2750 -0.0809 0.2113 0.181 Uiso 0.50 1 calc PR D 1 H30B H 0.3420 -0.1279 0.2104 0.181 Uiso 0.50 1 calc PR D 1 H30C H 0.2774 -0.1830 0.2049 0.181 Uiso 0.50 1 calc PR D 1 C28B C 0.3411(5) -0.1723(7) 0.1659(7) 0.141(6) Uani 0.50 1 d P D 2 H28D H 0.3249 -0.2274 0.1758 0.212 Uiso 0.50 1 calc PR D 2 H28E H 0.3657 -0.1436 0.1944 0.212 Uiso 0.50 1 calc PR D 2 H28F H 0.3688 -0.1824 0.1416 0.212 Uiso 0.50 1 calc PR D 2 C29B C 0.2424(6) -0.1545(7) 0.1045(4) 0.107(5) Uani 0.50 1 d P D 2 H29D H 0.2298 -0.2122 0.1134 0.161 Uiso 0.50 1 calc PR D 2 H29E H 0.2629 -0.1581 0.0755 0.161 Uiso 0.50 1 calc PR D 2 H29F H 0.2043 -0.1179 0.0975 0.161 Uiso 0.50 1 calc PR D 2 C30B C 0.2480(8) -0.0989(8) 0.1845(5) 0.122(5) Uani 0.50 1 d P D 2 H30D H 0.2201 -0.0493 0.1749 0.183 Uiso 0.50 1 calc PR D 2 H30E H 0.2769 -0.0860 0.2150 0.183 Uiso 0.50 1 calc PR D 2 H30F H 0.2217 -0.1491 0.1891 0.183 Uiso 0.50 1 calc PR D 2 C31 C 0.24264(16) 0.3761(2) 0.16157(11) 0.0548(8) Uani 1 1 d . . . H31A H 0.2718 0.3546 0.1907 0.066 Uiso 1 1 calc R . . H31B H 0.2606 0.4307 0.1515 0.066 Uiso 1 1 calc R . . C32 C 0.1812(2) 0.3925(3) 0.17421(15) 0.0840(13) Uani 1 1 d . . . H32A H 0.1525 0.4157 0.1458 0.126 Uiso 1 1 calc R . . H32B H 0.1855 0.4341 0.2010 0.126 Uiso 1 1 calc R . . H32C H 0.1633 0.3387 0.1845 0.126 Uiso 1 1 calc R . . O13 O 0.09168(10) 0.17498(15) 0.15905(7) 0.0565(6) Uani 1 1 d . . . H13A H 0.1319 0.1787 0.1674 0.085 Uiso 1 1 d R . . C33 C 0.06499(17) 0.2074(3) 0.19855(12) 0.0664(10) Uani 1 1 d . . . H33A H 0.0956 0.2473 0.2180 0.080 Uiso 1 1 calc R . . H33B H 0.0566 0.1594 0.2200 0.080 Uiso 1 1 calc R . . C34 C 0.0056(2) 0.2522(4) 0.18059(14) 0.0937(15) Uani 1 1 d . . . H34A H 0.0148 0.3046 0.1635 0.141 Uiso 1 1 calc R . . H34B H -0.0157 0.2674 0.2081 0.141 Uiso 1 1 calc R . . H34C H -0.0226 0.2148 0.1580 0.141 Uiso 1 1 calc R . . O14 O 0.48132(9) 0.33131(12) 0.32802(6) 0.0415(4) Uani 1 1 d . . . H14A H 0.4994 0.3060 0.3579 0.062 Uiso 1 1 d R . . C35 C 0.4538(2) 0.4108(2) 0.33693(14) 0.0740(11) Uani 1 1 d . . . H35A H 0.4209 0.4007 0.3577 0.089 Uiso 1 1 calc R . . H35B H 0.4874 0.4476 0.3556 0.089 Uiso 1 1 calc R . . C36 C 0.4254(4) 0.4556(3) 0.29506(19) 0.162(3) Uani 1 1 d . . . H36A H 0.4576 0.4670 0.2744 0.243 Uiso 1 1 calc R . . H36B H 0.4080 0.5102 0.3046 0.243 Uiso 1 1 calc R . . H36C H 0.3907 0.4209 0.2769 0.243 Uiso 1 1 calc R . . O15 O 0.4313(6) -0.0120(8) 0.2176(5) 0.210(5) Uiso 0.50 1 d P . . C37 C 0.4772(8) 0.0511(11) 0.2327(6) 0.169(6) Uiso 0.50 1 d P . . C38 C 0.5401(8) -0.0044(10) 0.2440(6) 0.151(5) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01946(16) 0.03414(19) 0.01805(15) 0.00102(13) 0.00106(12) -0.00576(14) Mn2 0.02028(17) 0.02807(18) 0.01687(15) 0.00113(13) 0.00011(12) -0.00498(14) Mn3 0.02156(17) 0.0366(2) 0.01678(15) 0.00148(13) 0.00116(12) -0.00534(14) O1 0.0210(7) 0.0325(8) 0.0165(7) -0.0002(6) 0.0007(6) -0.0062(6) O2 0.0203(8) 0.0407(9) 0.0256(8) -0.0014(7) 0.0029(6) -0.0076(7) O3 0.0190(7) 0.0310(8) 0.0194(7) 0.0026(6) -0.0004(6) -0.0030(6) O4 0.0277(8) 0.0300(8) 0.0205(7) 0.0008(6) -0.0014(6) -0.0082(7) O5 0.0253(8) 0.0517(10) 0.0180(7) -0.0026(7) 0.0017(6) -0.0100(7) O6 0.0248(8) 0.0546(11) 0.0194(7) 0.0005(7) 0.0037(6) -0.0033(8) O7 0.0290(9) 0.0444(10) 0.0206(7) -0.0006(7) 0.0030(6) -0.0134(7) O8 0.0284(9) 0.0423(10) 0.0449(10) 0.0094(8) -0.0023(8) -0.0001(8) O9 0.0507(11) 0.0351(10) 0.0273(8) 0.0001(7) 0.0026(8) 0.0088(8) O10 0.0603(13) 0.0343(10) 0.0385(10) 0.0074(8) 0.0035(9) 0.0009(9) O11 0.0468(11) 0.0470(11) 0.0382(10) 0.0123(8) 0.0088(9) 0.0011(9) O12 0.0334(9) 0.0422(10) 0.0251(8) -0.0054(7) 0.0012(7) 0.0007(8) N1 0.0184(9) 0.0320(10) 0.0193(8) 0.0030(7) -0.0012(7) -0.0028(8) N2 0.0240(10) 0.0667(15) 0.0193(9) 0.0007(9) 0.0044(8) 0.0013(10) N3 0.0252(10) 0.0347(11) 0.0181(8) 0.0011(7) 0.0010(7) -0.0060(8) N4 0.0343(12) 0.0878(19) 0.0307(11) -0.0053(12) 0.0072(10) -0.0323(13) N5 0.0266(10) 0.0341(11) 0.0184(8) 0.0009(8) 0.0036(7) -0.0044(8) N6 0.0356(12) 0.0611(15) 0.0204(9) -0.0035(9) -0.0008(8) -0.0166(11) C1 0.0238(11) 0.0298(12) 0.0304(11) 0.0050(9) 0.0054(9) -0.0001(9) C2 0.0248(12) 0.0440(15) 0.0373(13) 0.0025(11) 0.0006(10) -0.0036(11) C3 0.0195(12) 0.0627(19) 0.0506(16) 0.0048(14) 0.0037(11) 0.0028(12) C4 0.0257(13) 0.072(2) 0.0467(16) 0.0023(14) 0.0108(12) 0.0097(13) C5 0.0307(13) 0.0536(17) 0.0315(13) 0.0002(11) 0.0067(10) 0.0063(12) C6 0.0225(11) 0.0339(13) 0.0277(11) 0.0054(10) 0.0043(9) 0.0028(10) C7 0.0239(11) 0.0312(12) 0.0248(11) 0.0013(9) 0.0046(9) 0.0027(9) C8 0.0250(11) 0.0281(12) 0.0252(11) 0.0006(9) -0.0024(9) -0.0034(9) C9 0.0387(14) 0.0415(15) 0.0272(12) -0.0023(11) -0.0006(10) -0.0079(12) C10 0.0536(18) 0.0505(17) 0.0344(14) -0.0132(12) -0.0017(12) -0.0158(14) C11 0.0566(19) 0.0400(16) 0.0478(16) -0.0098(13) 0.0024(14) -0.0231(14) C12 0.0421(15) 0.0440(16) 0.0395(14) 0.0015(12) 0.0022(12) -0.0192(12) C13 0.0269(12) 0.0322(13) 0.0292(11) 0.0011(10) -0.0011(9) -0.0052(10) C14 0.0236(11) 0.0374(13) 0.0276(11) 0.0053(10) 0.0021(9) -0.0080(10) C15 0.0330(12) 0.0292(12) 0.0212(10) -0.0008(9) 0.0058(9) 0.0018(10) C16 0.0373(14) 0.0365(13) 0.0282(12) -0.0002(10) 0.0082(10) -0.0026(11) C17 0.0549(17) 0.0397(15) 0.0251(12) 0.0068(10) 0.0145(11) 0.0020(13) C18 0.0529(17) 0.0472(16) 0.0208(11) 0.0084(11) 0.0004(11) 0.0001(13) C19 0.0368(14) 0.0466(16) 0.0244(11) 0.0051(10) -0.0008(10) 0.0015(12) C20 0.0299(12) 0.0308(12) 0.0176(10) -0.0004(9) 0.0020(9) 0.0019(10) C21 0.0259(11) 0.0294(12) 0.0214(10) 0.0007(9) -0.0011(8) 0.0020(9) C22A 0.051(5) 0.066(8) 0.116(12) 0.025(7) -0.020(7) 0.000(5) C23A 0.094(9) 0.065(7) 0.141(11) 0.026(7) 0.052(8) 0.025(6) C22B 0.051(5) 0.066(8) 0.116(12) 0.025(7) -0.020(7) 0.000(5) C23B 0.086(6) 0.082(6) 0.277(15) 0.006(8) -0.063(8) 0.045(5) C24 0.072(2) 0.059(2) 0.0373(15) -0.0004(14) 0.0138(15) 0.0258(17) C25 0.070(3) 0.059(3) 0.063(3) -0.021(2) -0.012(2) 0.021(2) C25B 0.083(12) 0.034(8) 0.061(10) -0.005(7) 0.038(9) -0.006(8) C26 0.0298(13) 0.0387(14) 0.0290(12) 0.0104(11) -0.0055(10) -0.0011(11) C27 0.0561(19) 0.0399(16) 0.0497(16) 0.0052(13) 0.0133(14) -0.0106(14) C28A 0.118(8) 0.027(3) 0.118(7) 0.002(4) 0.078(6) -0.007(4) C29A 0.063(6) 0.087(9) 0.218(19) 0.011(9) 0.033(8) -0.038(6) C30A 0.27(2) 0.047(5) 0.040(4) 0.018(4) 0.008(8) -0.015(8) C28B 0.078(7) 0.072(7) 0.256(18) 0.097(10) -0.021(9) -0.005(5) C29B 0.133(12) 0.085(8) 0.082(7) 0.012(6) -0.046(7) -0.061(7) C30B 0.182(14) 0.096(9) 0.110(10) 0.025(7) 0.085(10) -0.054(9) C31 0.063(2) 0.0524(18) 0.0472(17) -0.0174(14) 0.0025(15) 0.0069(16) C32 0.086(3) 0.094(3) 0.080(3) -0.041(2) 0.036(2) -0.013(2) O13 0.0462(12) 0.0817(16) 0.0458(12) -0.0041(11) 0.0201(10) -0.0022(11) C33 0.062(2) 0.099(3) 0.0435(17) 0.0037(18) 0.0241(16) 0.007(2) C34 0.086(3) 0.141(4) 0.057(2) -0.005(2) 0.018(2) 0.048(3) O14 0.0426(11) 0.0500(11) 0.0283(9) -0.0058(8) -0.0038(8) 0.0112(9) C35 0.077(3) 0.068(2) 0.073(2) -0.013(2) 0.002(2) 0.019(2) C36 0.294(9) 0.093(4) 0.094(4) 0.019(3) 0.019(5) 0.102(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.8732(15) . ? Mn1 O7 1.8810(15) . ? Mn1 O2 1.8832(15) . ? Mn1 N1 1.9595(17) . ? Mn1 O8 2.1721(18) . ? Mn1 Mn3 3.2243(5) . ? Mn2 O1 1.8731(14) . ? Mn2 O4 1.9120(15) . ? Mn2 O3 1.9245(15) . ? Mn2 N3 1.9639(18) . ? Mn2 O9 2.1820(17) . ? Mn2 O3 2.3330(15) 7 ? Mn2 Mn2 3.2199(7) 7 ? Mn3 O6 1.8796(16) . ? Mn3 O1 1.8874(14) . ? Mn3 O5 1.8892(16) . ? Mn3 N5 1.9619(19) . ? Mn3 O10 2.1291(19) . ? Mn3 O12 2.5023(18) . ? O2 C1 1.332(3) . ? O3 N1 1.406(2) . ? O3 Mn2 2.3330(15) 7 ? O4 C8 1.346(3) . ? O5 N3 1.382(2) . ? O6 C15 1.334(3) . ? O7 N5 1.395(2) . ? O8 C22B 1.413(16) . ? O8 C22A 1.42(3) . ? O8 H8A 0.8820 . ? O9 C24 1.425(3) . ? O9 H9A 0.8595 . ? O10 C26 1.240(3) . ? O11 C26 1.263(3) . ? O12 C31 1.439(3) . ? O12 H12A 0.9226 . ? N1 C7 1.304(3) . ? N2 C7 1.333(3) . ? N2 H2A 0.8608 . ? N2 H2B 0.9199 . ? N3 C14 1.302(3) . ? N4 C14 1.332(3) . ? N4 H4A 0.8287 . ? N4 H4B 0.9130 . ? N5 C21 1.305(3) . ? N6 C21 1.334(3) . ? N6 H6A 0.9223 . ? N6 H6B 0.8960 . ? C1 C2 1.399(3) . ? C1 C6 1.407(3) . ? C2 C3 1.377(4) . ? C2 H2 0.9500 . ? C3 C4 1.372(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.398(3) . ? C5 H5 0.9500 . ? C6 C7 1.467(3) . ? C8 C9 1.390(3) . ? C8 C13 1.404(3) . ? C9 C10 1.371(4) . ? C9 H9 0.9500 . ? C10 C11 1.372(4) . ? C10 H10 0.9500 . ? C11 C12 1.375(4) . ? C11 H11 0.9500 . ? C12 C13 1.401(3) . ? C12 H12 0.9500 . ? C13 C14 1.465(3) . ? C15 C16 1.396(3) . ? C15 C20 1.403(3) . ? C16 C17 1.377(3) . ? C16 H16 0.9500 . ? C17 C18 1.373(4) . ? C17 H17 0.9500 . ? C18 C19 1.373(4) . ? C18 H18 0.9500 . ? C19 C20 1.401(3) . ? C19 H19 0.9500 . ? C20 C21 1.473(3) . ? C22A C23A 1.43(2) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C22B C23B 1.447(15) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24 C25 1.557(5) . ? C24 C25B 1.692(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9700 . ? C24 H24D 0.9700 . ? C25 H24D 0.8133 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26 C27 1.517(4) . ? C27 C30A 1.446(9) . ? C27 C29B 1.456(9) . ? C27 C28B 1.463(9) . ? C27 C30B 1.519(12) . ? C27 C29A 1.539(12) . ? C27 C28A 1.559(7) . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31 C32 1.427(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O13 C33 1.412(4) . ? O13 H13A 0.8469 . ? C33 C34 1.451(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O14 C35 1.407(4) . ? O14 H14A 0.9401 . ? C35 C36 1.403(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O15 C38 1.142(17) 2_655 ? O15 C37 1.396(18) . ? C37 C38 1.18(2) 2_655 ? C37 C37 1.24(3) 2_655 ? C37 C38 1.573(19) . ? C38 O15 1.142(17) 2_655 ? C38 C37 1.18(2) 2_655 ? C38 C38 1.78(3) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O7 92.66(7) . . ? O1 Mn1 O2 175.16(7) . . ? O7 Mn1 O2 88.28(7) . . ? O1 Mn1 N1 88.19(7) . . ? O7 Mn1 N1 167.57(8) . . ? O2 Mn1 N1 89.87(7) . . ? O1 Mn1 O8 91.62(7) . . ? O7 Mn1 O8 96.65(7) . . ? O2 Mn1 O8 92.98(7) . . ? N1 Mn1 O8 95.72(7) . . ? O1 Mn1 Mn3 31.10(4) . . ? O7 Mn1 Mn3 62.31(5) . . ? O2 Mn1 Mn3 150.51(5) . . ? N1 Mn1 Mn3 119.29(5) . . ? O8 Mn1 Mn3 88.59(5) . . ? O1 Mn2 O4 175.29(7) . . ? O1 Mn2 O3 89.93(6) . . ? O4 Mn2 O3 90.85(6) . . ? O1 Mn2 N3 88.07(7) . . ? O4 Mn2 N3 90.62(7) . . ? O3 Mn2 N3 173.06(8) . . ? O1 Mn2 O9 93.13(7) . . ? O4 Mn2 O9 91.44(7) . . ? O3 Mn2 O9 94.60(7) . . ? N3 Mn2 O9 92.15(8) . . ? O1 Mn2 O3 90.10(6) . 7 ? O4 Mn2 O3 85.40(6) . 7 ? O3 Mn2 O3 82.19(6) . 7 ? N3 Mn2 O3 91.17(7) . 7 ? O9 Mn2 O3 175.44(6) . 7 ? O1 Mn2 Mn2 90.03(5) . 7 ? O4 Mn2 Mn2 87.18(5) . 7 ? O3 Mn2 Mn2 45.88(5) . 7 ? N3 Mn2 Mn2 127.46(6) . 7 ? O9 Mn2 Mn2 140.37(5) . 7 ? O3 Mn2 Mn2 36.31(4) 7 7 ? O6 Mn3 O1 168.60(7) . . ? O6 Mn3 O5 87.43(7) . . ? O1 Mn3 O5 90.80(6) . . ? O6 Mn3 N5 89.91(7) . . ? O1 Mn3 N5 90.31(7) . . ? O5 Mn3 N5 171.98(8) . . ? O6 Mn3 O10 93.41(8) . . ? O1 Mn3 O10 97.97(7) . . ? O5 Mn3 O10 96.03(8) . . ? N5 Mn3 O10 91.68(8) . . ? O6 Mn3 O12 86.44(7) . . ? O1 Mn3 O12 82.36(6) . . ? O5 Mn3 O12 91.68(7) . . ? N5 Mn3 O12 80.59(7) . . ? O10 Mn3 O12 172.27(7) . . ? O6 Mn3 Mn1 147.90(5) . . ? O1 Mn3 Mn1 30.84(4) . . ? O5 Mn3 Mn1 121.46(5) . . ? N5 Mn3 Mn1 59.48(5) . . ? O10 Mn3 Mn1 96.71(6) . . ? O12 Mn3 Mn1 79.58(4) . . ? Mn2 O1 Mn1 121.00(8) . . ? Mn2 O1 Mn3 120.75(8) . . ? Mn1 O1 Mn3 118.05(7) . . ? C1 O2 Mn1 123.21(14) . . ? N1 O3 Mn2 113.65(11) . . ? N1 O3 Mn2 112.50(11) . 7 ? Mn2 O3 Mn2 97.81(6) . 7 ? C8 O4 Mn2 122.49(13) . . ? N3 O5 Mn3 117.31(12) . . ? C15 O6 Mn3 124.75(15) . . ? N5 O7 Mn1 116.45(12) . . ? C22B O8 Mn1 121.0(6) . . ? C22A O8 Mn1 136.4(11) . . ? C22B O8 H8A 123.6 . . ? C22A O8 H8A 120.4 . . ? Mn1 O8 H8A 102.9 . . ? C24 O9 Mn2 134.45(16) . . ? C24 O9 H9A 112.9 . . ? Mn2 O9 H9A 112.6 . . ? C26 O10 Mn3 138.15(16) . . ? C31 O12 Mn3 124.40(17) . . ? C31 O12 H12A 107.6 . . ? Mn3 O12 H12A 111.0 . . ? C7 N1 O3 114.11(16) . . ? C7 N1 Mn1 128.71(15) . . ? O3 N1 Mn1 116.08(12) . . ? C7 N2 H2A 117.9 . . ? C7 N2 H2B 117.8 . . ? H2A N2 H2B 120.1 . . ? C14 N3 O5 113.26(18) . . ? C14 N3 Mn2 127.70(15) . . ? O5 N3 Mn2 118.10(13) . . ? C14 N4 H4A 123.6 . . ? C14 N4 H4B 118.6 . . ? H4A N4 H4B 108.6 . . ? C21 N5 O7 113.23(17) . . ? C21 N5 Mn3 129.01(16) . . ? O7 N5 Mn3 117.22(12) . . ? C21 N6 H6A 123.5 . . ? C21 N6 H6B 116.7 . . ? H6A N6 H6B 116.7 . . ? O2 C1 C2 118.2(2) . . ? O2 C1 C6 123.5(2) . . ? C2 C1 C6 118.3(2) . . ? C3 C2 C1 120.9(2) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 121.1(2) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 121.3(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.3(2) . . ? C5 C6 C7 118.2(2) . . ? C1 C6 C7 122.5(2) . . ? N1 C7 N2 121.0(2) . . ? N1 C7 C6 119.21(19) . . ? N2 C7 C6 119.8(2) . . ? O4 C8 C9 117.8(2) . . ? O4 C8 C13 123.3(2) . . ? C9 C8 C13 118.9(2) . . ? C10 C9 C8 121.3(2) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 120.3(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 119.5(2) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 121.4(2) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 118.4(2) . . ? C12 C13 C14 119.0(2) . . ? C8 C13 C14 122.6(2) . . ? N3 C14 N4 119.2(2) . . ? N3 C14 C13 120.3(2) . . ? N4 C14 C13 120.4(2) . . ? O6 C15 C16 117.4(2) . . ? O6 C15 C20 123.8(2) . . ? C16 C15 C20 118.8(2) . . ? C17 C16 C15 121.1(2) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 119.4(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.7(2) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C15 118.6(2) . . ? C19 C20 C21 119.0(2) . . ? C15 C20 C21 122.42(19) . . ? N5 C21 N6 119.5(2) . . ? N5 C21 C20 119.9(2) . . ? N6 C21 C20 120.58(19) . . ? O8 C22A C23A 114.6(17) . . ? O8 C22A H22A 108.6 . . ? C23A C22A H22A 108.6 . . ? O8 C22A H22B 108.6 . . ? C23A C22A H22B 108.6 . . ? H22A C22A H22B 107.6 . . ? O8 C22B C23B 112.4(9) . . ? O8 C22B H22C 109.1 . . ? C23B C22B H22C 109.1 . . ? O8 C22B H22D 109.1 . . ? C23B C22B H22D 109.1 . . ? H22C C22B H22D 107.9 . . ? C22B C23B H23D 109.5 . . ? C22B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C22B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? O9 C24 C25 109.6(3) . . ? O9 C24 C25B 102.2(6) . . ? C25 C24 C25B 134.8(6) . . ? O9 C24 H24A 109.7 . . ? C25 C24 H24A 109.7 . . ? O9 C24 H24B 109.7 . . ? C25 C24 H24B 109.7 . . ? C25B C24 H24B 87.8 . . ? H24A C24 H24B 108.2 . . ? O9 C24 H24C 111.3 . . ? C25 C24 H24C 86.4 . . ? C25B C24 H24C 111.2 . . ? H24A C24 H24C 126.9 . . ? O9 C24 H24D 111.3 . . ? C25B C24 H24D 111.5 . . ? H24A C24 H24D 85.0 . . ? H24B C24 H24D 128.9 . . ? H24C C24 H24D 109.2 . . ? C24 C25 H25A 109.5 . . ? H24D C25 H25A 83.8 . . ? C24 C25 H25B 109.5 . . ? H24D C25 H25B 101.8 . . ? C24 C25 H25C 109.5 . . ? H24D C25 H25C 138.6 . . ? C24 C25B H25D 109.5 . . ? C24 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? O10 C26 O11 124.0(2) . . ? O10 C26 C27 117.8(2) . . ? O11 C26 C27 118.1(2) . . ? C30A C27 C29B 133.5(8) . . ? C30A C27 C28B 64.5(8) . . ? C29B C27 C28B 116.5(8) . . ? C30A C27 C26 113.9(5) . . ? C29B C27 C26 109.3(5) . . ? C28B C27 C26 108.5(4) . . ? C29B C27 C30B 105.7(8) . . ? C28B C27 C30B 107.8(9) . . ? C26 C27 C30B 108.9(5) . . ? C30A C27 C29A 110.8(9) . . ? C28B C27 C29A 146.2(6) . . ? C26 C27 C29A 103.8(5) . . ? C30B C27 C29A 70.0(8) . . ? C30A C27 C28A 110.1(6) . . ? C29B C27 C28A 66.5(7) . . ? C28B C27 C28A 52.6(7) . . ? C26 C27 C28A 112.1(3) . . ? C30B C27 C28A 138.5(5) . . ? C29A C27 C28A 105.6(7) . . ? C27 C28A H28A 109.5 . . ? C27 C28A H28B 109.5 . . ? C27 C28A H28C 109.5 . . ? C27 C29A H29A 109.5 . . ? C27 C29A H29B 109.5 . . ? C27 C29A H29C 109.5 . . ? C27 C30A H30A 109.5 . . ? C27 C30A H30B 109.5 . . ? C27 C30A H30C 109.5 . . ? C27 C28B H28D 109.5 . . ? C27 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27 C29B H29D 109.5 . . ? C27 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C27 C30B H30D 109.5 . . ? C27 C30B H30E 109.4 . . ? H30D C30B H30E 109.5 . . ? C27 C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C32 C31 O12 112.7(3) . . ? C32 C31 H31A 109.1 . . ? O12 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? O12 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O13 H13A 106.2 . . ? O13 C33 C34 110.0(3) . . ? O13 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? O13 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O14 H14A 109.3 . . ? C36 C35 O14 115.0(3) . . ? C36 C35 H35A 108.5 . . ? O14 C35 H35A 108.5 . . ? C36 C35 H35B 108.5 . . ? O14 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 O15 C37 54.1(11) 2_655 . ? C38 C37 C37 81.1(16) 2_655 2_655 ? C38 C37 O15 51.9(11) 2_655 . ? C37 C37 O15 130.0(14) 2_655 . ? C38 C37 C38 79.5(16) 2_655 . ? C37 C37 C38 47.6(11) 2_655 . ? O15 C37 C38 101.3(13) . . ? O15 C38 C37 74.1(14) 2_655 2_655 ? O15 C38 C37 122.8(18) 2_655 . ? C37 C38 C37 51.3(15) 2_655 . ? O15 C38 C38 101.3(17) 2_655 2_655 ? C37 C38 C38 60.1(12) 2_655 2_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.627 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.071 data_frart86 _database_code_depnum_ccdc_archive 'CCDC 888452' #TrackingRef 'web_deposit_cif_file_4_Lise-MarieChamoreau_1340629901.frart86 - publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H80 Mn6 N14 O24, 4(H2O)' _chemical_formula_sum 'C68 H88 Mn6 N14 O26' _chemical_formula_weight 1847.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4165(14) _cell_length_b 13.6528(14) _cell_length_c 13.7425(10) _cell_angle_alpha 81.732(7) _cell_angle_beta 81.276(8) _cell_angle_gamma 63.784(7) _cell_volume 2058.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 133 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 21.2 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 250(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39735 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11940 _reflns_number_gt 7810 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0285P)^2^+3.9264P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11940 _refine_ls_number_parameters 563 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.104 _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 0.40427(4) 0.07572(4) 0.22748(3) 0.02143(11) Uani 1 1 d . . . Mn2 Mn 0.37917(5) -0.01845(4) 0.02777(3) 0.02277(11) Uani 1 1 d . . . Mn3 Mn 0.41718(5) -0.16777(4) 0.24012(3) 0.02386(11) Uani 1 1 d . A . O1 O 0.4068(2) -0.03830(16) 0.16274(14) 0.0236(5) Uani 1 1 d . . . O2 O 0.4144(2) 0.19029(18) 0.28293(15) 0.0274(5) Uani 1 1 d . . . O3 O 0.4140(2) 0.10994(16) 0.01243(14) 0.0236(5) Uani 1 1 d . . . O4 O 0.3625(2) -0.00481(19) -0.10970(15) 0.0314(5) Uani 1 1 d . . . O5 O 0.4067(2) -0.22822(18) 0.12876(15) 0.0329(6) Uani 1 1 d . A . O6 O 0.4388(2) -0.30173(19) 0.31526(16) 0.0329(5) Uani 1 1 d . . . O7 O 0.4801(2) -0.02661(17) 0.33590(15) 0.0258(5) Uani 1 1 d . B . O8 O 0.2101(2) 0.12576(19) 0.27410(17) 0.0321(5) Uani 1 1 d . . . O9 O 0.1835(2) 0.0943(2) 0.0720(2) 0.0474(7) Uani 1 1 d . . . H9A H 0.1752 0.1160 0.1262 0.071 Uiso 1 1 d R A . O10 O 0.2182(2) -0.0806(2) 0.2838(2) 0.0487(7) Uani 1 1 d D . . H10A H 0.1995 -0.0112 0.2896 0.073 Uiso 1 1 d R B . O11 O 0.6339(2) -0.2196(2) 0.19600(17) 0.0385(6) Uani 1 1 d . . . H11A H 0.6443 -0.1656 0.1707 0.058 Uiso 1 1 d R B . N1 N 0.3772(2) 0.1658(2) 0.09914(17) 0.0228(5) Uani 1 1 d . . . N2 N 0.3311(3) 0.3218(2) -0.0096(2) 0.0403(8) Uani 1 1 d . . . H2A H 0.3216 0.3848 -0.0168 0.048 Uiso 1 1 d R . . H2B H 0.3518 0.2741 -0.0518 0.048 Uiso 1 1 d R . . N3 N 0.3632(3) -0.1577(2) 0.04479(18) 0.0261(6) Uani 1 1 d . . . N4 N 0.3375(3) -0.3038(2) 0.0077(2) 0.0419(8) Uani 1 1 d . . . H4A H 0.3284 -0.3347 -0.0353 0.050 Uiso 1 1 d R A . H4B H 0.3777 -0.3441 0.0578 0.050 Uiso 1 1 d R . . N5 N 0.4459(2) -0.1135(2) 0.35612(17) 0.0228(5) Uani 1 1 d . . . N6 N 0.5050(3) -0.1221(2) 0.5088(2) 0.0365(7) Uani 1 1 d . . . H6A H 0.5017 -0.1394 0.5706 0.044 Uiso 1 1 d R B . H6B H 0.5318 -0.0712 0.4788 0.044 Uiso 1 1 d R . . N7 N -0.0688(4) 0.3485(4) 0.1952(3) 0.0699(12) Uani 1 1 d . . . C1 C 0.3396(3) 0.2959(2) 0.2625(2) 0.0239(6) Uani 1 1 d . . . C2 C 0.2986(3) 0.3675(3) 0.3392(2) 0.0327(8) Uani 1 1 d . . . H2 H 0.3258 0.3399 0.4020 0.039 Uiso 1 1 calc R . . C3 C 0.2206(3) 0.4759(3) 0.3237(3) 0.0384(8) Uani 1 1 d . . . H3 H 0.1948 0.5211 0.3760 0.046 Uiso 1 1 calc R . . C4 C 0.1790(4) 0.5198(3) 0.2311(3) 0.0454(10) Uani 1 1 d . . . H4 H 0.1252 0.5941 0.2208 0.054 Uiso 1 1 calc R . . C5 C 0.2183(4) 0.4521(3) 0.1548(3) 0.0414(9) Uani 1 1 d . . . H5 H 0.1907 0.4814 0.0923 0.050 Uiso 1 1 calc R . . C6 C 0.2979(3) 0.3412(2) 0.1680(2) 0.0271(7) Uani 1 1 d . . . C7 C 0.3383(3) 0.2732(3) 0.0827(2) 0.0252(6) Uani 1 1 d . . . C8 C 0.3043(3) -0.0485(3) -0.1523(2) 0.0260(7) Uani 1 1 d . A . C9 C 0.2656(3) 0.0000(3) -0.2462(2) 0.0316(7) Uani 1 1 d . . . H9 H 0.2833 0.0583 -0.2762 0.038 Uiso 1 1 calc R . . C10 C 0.2022(3) -0.0362(3) -0.2949(2) 0.0382(9) Uani 1 1 d . . . H10 H 0.1762 -0.0018 -0.3568 0.046 Uiso 1 1 calc R . . C11 C 0.1770(3) -0.1238(3) -0.2524(3) 0.0373(8) Uani 1 1 d . . . H11 H 0.1318 -0.1473 -0.2843 0.045 Uiso 1 1 calc R . . C12 C 0.2194(3) -0.1757(3) -0.1623(2) 0.0317(7) Uani 1 1 d . A . H12 H 0.2045 -0.2362 -0.1347 0.038 Uiso 1 1 calc R . . C13 C 0.2841(3) -0.1407(3) -0.1109(2) 0.0258(6) Uani 1 1 d . . . C14 C 0.3306(3) -0.2028(3) -0.0169(2) 0.0263(7) Uani 1 1 d . A . C15 C 0.4100(3) -0.3124(3) 0.4138(2) 0.0274(7) Uani 1 1 d . B . C16 C 0.3709(4) -0.3942(3) 0.4508(3) 0.0387(8) Uani 1 1 d . . . H16 H 0.3632 -0.4370 0.4069 0.046 Uiso 1 1 calc R . . C17 C 0.3437(4) -0.4119(3) 0.5521(3) 0.0464(10) Uani 1 1 d . . . H17 H 0.3146 -0.4648 0.5759 0.056 Uiso 1 1 calc R . . C18 C 0.3591(4) -0.3524(3) 0.6177(3) 0.0457(10) Uani 1 1 d . . . H18 H 0.3426 -0.3665 0.6860 0.055 Uiso 1 1 calc R . . C19 C 0.3984(4) -0.2725(3) 0.5834(2) 0.0381(8) Uani 1 1 d . B . H19 H 0.4082 -0.2322 0.6287 0.046 Uiso 1 1 calc R . . C20 C 0.4244(3) -0.2504(3) 0.4803(2) 0.0268(7) Uani 1 1 d . . . C21 C 0.4607(3) -0.1605(2) 0.4473(2) 0.0239(6) Uani 1 1 d . B . C22 C 0.1581(3) 0.1824(3) 0.3519(2) 0.0307(7) Uani 1 1 d . . . C23 C 0.2086(3) 0.1487(3) 0.4431(3) 0.0383(8) Uani 1 1 d . . . H23 H 0.2781 0.0823 0.4496 0.046 Uiso 1 1 calc R . . C24 C 0.1584(4) 0.2110(4) 0.5231(3) 0.0511(11) Uani 1 1 d . . . H24 H 0.1949 0.1864 0.5825 0.061 Uiso 1 1 calc R . . C25 C 0.0548(4) 0.3094(4) 0.5175(3) 0.0597(13) Uani 1 1 d . . . H25 H 0.0227 0.3520 0.5717 0.072 Uiso 1 1 calc R . . C26 C 0.0006(4) 0.3428(4) 0.4312(3) 0.0558(12) Uani 1 1 d . . . H26 H -0.0704 0.4082 0.4266 0.067 Uiso 1 1 calc R . . C27 C 0.0504(3) 0.2798(3) 0.3496(3) 0.0380(8) Uani 1 1 d . . . C28 C -0.0124(4) 0.3168(3) 0.2610(3) 0.0478(10) Uani 1 1 d . . . C29A C 0.0811(9) 0.0954(10) 0.0487(8) 0.066(3) Uani 0.50 1 d PD A 1 H29A H 0.0223 0.1070 0.1072 0.080 Uiso 0.50 1 calc PR A 1 H29B H 0.0983 0.0252 0.0248 0.080 Uiso 0.50 1 calc PR A 1 C30A C 0.029(3) 0.191(2) -0.0341(18) 0.190(18) Uani 0.50 1 d PD A 1 H30A H 0.0279 0.2576 -0.0153 0.285 Uiso 0.50 1 calc PR A 1 H30B H -0.0527 0.2039 -0.0421 0.285 Uiso 0.50 1 calc PR A 1 H30C H 0.0791 0.1717 -0.0960 0.285 Uiso 0.50 1 calc PR A 1 C29B C 0.1006(12) 0.1807(15) 0.0146(10) 0.119(6) Uani 0.50 1 d PD A 2 H29C H 0.1458 0.2102 -0.0359 0.143 Uiso 0.50 1 calc PR A 2 H29D H 0.0494 0.2392 0.0574 0.143 Uiso 0.50 1 calc PR A 2 C30B C 0.0219(18) 0.153(2) -0.0350(15) 0.096(6) Uani 0.50 1 d PD A 2 H30D H 0.0709 0.0908 -0.0732 0.144 Uiso 0.50 1 calc PR A 2 H30E H -0.0245 0.2153 -0.0787 0.144 Uiso 0.50 1 calc PR A 2 H30F H -0.0326 0.1345 0.0141 0.144 Uiso 0.50 1 calc PR A 2 C31A C 0.1293(6) -0.1122(6) 0.3345(6) 0.0574(18) Uani 0.50 1 d PD B 1 H31A H 0.1622 -0.1923 0.3387 0.069 Uiso 0.50 1 calc PR B 1 H31B H 0.0602 -0.0826 0.2954 0.069 Uiso 0.50 1 calc PR B 1 C32A C 0.0853(11) -0.0761(12) 0.4364(8) 0.101(4) Uani 0.50 1 d PD B 1 H32A H 0.1066 -0.0175 0.4443 0.151 Uiso 0.50 1 calc PR B 1 H32B H 0.1224 -0.1374 0.4844 0.151 Uiso 0.50 1 calc PR B 1 H32C H -0.0016 -0.0498 0.4466 0.151 Uiso 0.50 1 calc PR B 1 C31B C 0.1293(6) -0.1122(6) 0.3345(6) 0.0574(18) Uani 0.20 1 d P B 2 H31C H 0.0516 -0.0474 0.3379 0.069 Uiso 0.20 1 calc PR B 2 H31D H 0.1496 -0.1397 0.4024 0.069 Uiso 0.20 1 calc PR B 2 C32B C 0.1170(10) -0.1943(8) 0.2899(10) 0.080(4) Uani 0.20 1 d PD B 2 H32D H 0.1548 -0.1983 0.2225 0.120 Uiso 0.20 1 calc PR B 2 H32E H 0.0321 -0.1757 0.2896 0.120 Uiso 0.20 1 calc PR B 2 H32F H 0.1557 -0.2646 0.3271 0.120 Uiso 0.20 1 calc PR B 2 C31C C 0.1248(17) -0.0926(14) 0.2595(19) 0.080(6) Uani 0.30 1 d PD B 3 H31E H 0.1257 -0.0808 0.1874 0.096 Uiso 0.30 1 calc PR B 3 H31F H 0.0507 -0.0339 0.2869 0.096 Uiso 0.30 1 calc PR B 3 C32C C 0.1170(10) -0.1943(8) 0.2899(10) 0.080(4) Uani 0.30 1 d P B 3 H32G H 0.1512 -0.2416 0.2362 0.120 Uiso 0.30 1 calc PR B 3 H32H H 0.0331 -0.1805 0.3069 0.120 Uiso 0.30 1 calc PR B 3 H32I H 0.1614 -0.2296 0.3470 0.120 Uiso 0.30 1 calc PR B 3 C33 C 0.7229(6) -0.2833(6) 0.2609(5) 0.111(3) Uani 1 1 d D B . H33A H 0.7936 -0.2692 0.2368 0.133 Uiso 1 1 calc R C 1 H33B H 0.6924 -0.2528 0.3250 0.133 Uiso 1 1 calc R C 1 C34A C 0.7617(12) -0.3873(8) 0.2780(11) 0.093(4) Uani 0.50 1 d PD B 1 H34A H 0.8263 -0.4231 0.2277 0.140 Uiso 0.50 1 calc PR B 1 H34B H 0.6965 -0.4078 0.2766 0.140 Uiso 0.50 1 calc PR B 1 H34C H 0.7919 -0.4099 0.3424 0.140 Uiso 0.50 1 calc PR B 1 C34B C 0.8410(11) -0.3429(12) 0.2246(11) 0.104(5) Uani 0.50 1 d PD B 2 H34D H 0.8729 -0.4146 0.2608 0.157 Uiso 0.50 1 calc PR B 2 H34E H 0.8887 -0.3048 0.2325 0.157 Uiso 0.50 1 calc PR B 2 H34F H 0.8444 -0.3510 0.1551 0.157 Uiso 0.50 1 calc PR B 2 O1W O 0.2956(3) 0.5428(2) -0.09612(19) 0.0433(7) Uani 1 1 d . . . H1WA H 0.2382 0.5633 -0.1286 0.065 Uiso 1 1 d R . . H1WB H 0.3609 0.5212 -0.1307 0.065 Uiso 1 1 d R . . O2W O 0.4695(3) 0.5350(2) 0.1902(2) 0.0536(8) Uani 1 1 d . . . H2WA H 0.4338 0.4945 0.2201 0.080 Uiso 1 1 d R . . H2WB H 0.4570 0.5774 0.2288 0.080 Uiso 1 1 d 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 0.0318(3) 0.0188(2) 0.0143(2) -0.00053(17) -0.00562(18) -0.0107(2) Mn2 0.0353(3) 0.0204(2) 0.0150(2) 0.00025(17) -0.00701(19) -0.0132(2) Mn3 0.0375(3) 0.0215(2) 0.0154(2) 0.00139(17) -0.00661(19) -0.0148(2) O1 0.0382(13) 0.0207(10) 0.0139(9) 0.0003(8) -0.0051(9) -0.0141(10) O2 0.0385(14) 0.0239(11) 0.0222(10) -0.0017(9) -0.0105(10) -0.0132(10) O3 0.0377(13) 0.0184(10) 0.0147(9) -0.0040(8) -0.0030(9) -0.0112(10) O4 0.0496(15) 0.0365(13) 0.0183(10) 0.0040(9) -0.0120(10) -0.0271(12) O5 0.0585(17) 0.0258(12) 0.0199(10) 0.0050(9) -0.0161(11) -0.0214(12) O6 0.0553(16) 0.0274(12) 0.0200(11) 0.0049(9) -0.0085(10) -0.0220(12) O7 0.0366(13) 0.0254(11) 0.0196(10) 0.0025(8) -0.0080(9) -0.0167(10) O8 0.0318(13) 0.0337(13) 0.0294(12) -0.0088(10) 0.0004(10) -0.0122(11) O9 0.0370(16) 0.0521(17) 0.0435(15) -0.0077(13) -0.0078(12) -0.0083(13) O10 0.0362(15) 0.0368(15) 0.075(2) -0.0097(14) 0.0035(14) -0.0184(13) O11 0.0431(16) 0.0337(13) 0.0279(12) -0.0020(10) -0.0089(11) -0.0051(12) N1 0.0339(15) 0.0193(12) 0.0134(11) -0.0034(9) -0.0022(10) -0.0092(11) N2 0.075(2) 0.0158(13) 0.0233(14) 0.0018(11) -0.0064(14) -0.0138(15) N3 0.0417(17) 0.0244(13) 0.0154(11) 0.0008(10) -0.0083(11) -0.0162(13) N4 0.073(2) 0.0299(16) 0.0350(16) 0.0022(13) -0.0281(16) -0.0269(16) N5 0.0317(15) 0.0198(12) 0.0165(11) 0.0012(10) -0.0051(10) -0.0106(11) N6 0.059(2) 0.0375(16) 0.0196(13) 0.0038(12) -0.0136(13) -0.0261(16) N7 0.065(3) 0.067(3) 0.069(3) -0.004(2) -0.035(2) -0.013(2) C1 0.0278(17) 0.0223(15) 0.0233(14) -0.0068(12) -0.0001(12) -0.0115(13) C2 0.040(2) 0.0340(18) 0.0253(16) -0.0118(14) -0.0031(14) -0.0139(16) C3 0.041(2) 0.0336(19) 0.0381(19) -0.0185(16) -0.0007(16) -0.0104(17) C4 0.052(3) 0.0263(18) 0.045(2) -0.0142(16) -0.0057(19) -0.0016(17) C5 0.053(3) 0.0251(17) 0.0340(19) -0.0033(15) -0.0107(17) -0.0040(17) C6 0.0347(19) 0.0197(15) 0.0243(15) -0.0041(12) -0.0029(13) -0.0087(14) C7 0.0316(18) 0.0220(15) 0.0205(14) -0.0018(12) -0.0017(13) -0.0104(14) C8 0.0308(18) 0.0299(16) 0.0188(14) -0.0056(12) -0.0033(12) -0.0130(14) C9 0.038(2) 0.0361(18) 0.0233(15) 0.0017(14) -0.0081(14) -0.0175(16) C10 0.045(2) 0.048(2) 0.0239(16) 0.0030(15) -0.0165(15) -0.0200(19) C11 0.043(2) 0.045(2) 0.0323(18) -0.0034(16) -0.0160(16) -0.0227(18) C12 0.037(2) 0.0321(18) 0.0297(17) -0.0037(14) -0.0083(14) -0.0163(16) C13 0.0298(17) 0.0283(16) 0.0199(14) -0.0044(12) -0.0060(12) -0.0113(14) C14 0.0323(18) 0.0262(16) 0.0227(15) -0.0023(12) -0.0056(13) -0.0136(14) C15 0.0319(18) 0.0228(15) 0.0237(15) 0.0065(12) -0.0055(13) -0.0101(14) C16 0.048(2) 0.037(2) 0.0360(19) 0.0060(16) -0.0071(17) -0.0247(18) C17 0.051(3) 0.041(2) 0.044(2) 0.0137(18) 0.0010(19) -0.024(2) C18 0.055(3) 0.050(2) 0.0246(17) 0.0090(17) 0.0038(17) -0.022(2) C19 0.048(2) 0.040(2) 0.0217(16) 0.0024(14) 0.0001(15) -0.0172(18) C20 0.0275(17) 0.0280(16) 0.0202(14) 0.0026(12) -0.0034(12) -0.0087(14) C21 0.0280(17) 0.0234(15) 0.0165(13) -0.0011(11) -0.0048(12) -0.0069(13) C22 0.0273(18) 0.0322(18) 0.0314(17) -0.0061(14) 0.0017(14) -0.0122(15) C23 0.037(2) 0.042(2) 0.0284(17) -0.0007(15) -0.0058(15) -0.0094(17) C24 0.049(3) 0.067(3) 0.0275(19) -0.0124(19) 0.0004(17) -0.015(2) C25 0.054(3) 0.072(3) 0.037(2) -0.026(2) 0.006(2) -0.010(2) C26 0.038(2) 0.054(3) 0.055(3) -0.022(2) -0.003(2) 0.003(2) C27 0.030(2) 0.040(2) 0.040(2) -0.0055(16) -0.0053(16) -0.0097(16) C28 0.038(2) 0.040(2) 0.058(3) -0.0072(19) -0.012(2) -0.0072(18) C29A 0.039(5) 0.096(9) 0.078(7) -0.028(6) -0.002(5) -0.037(6) C30A 0.111(18) 0.30(4) 0.089(15) 0.06(2) -0.078(13) -0.03(2) C29B 0.070(9) 0.154(15) 0.067(8) -0.023(9) -0.026(7) 0.022(10) C30B 0.038(8) 0.170(16) 0.063(10) -0.044(10) 0.003(7) -0.023(9) C31A 0.033(3) 0.058(4) 0.072(5) 0.014(4) -0.004(3) -0.018(3) C32A 0.074(9) 0.139(13) 0.081(9) 0.005(8) 0.014(7) -0.050(9) C31B 0.033(3) 0.058(4) 0.072(5) 0.014(4) -0.004(3) -0.018(3) C32B 0.066(7) 0.062(7) 0.130(10) -0.001(7) -0.016(7) -0.044(6) C31C 0.058(12) 0.073(13) 0.122(18) 0.016(13) -0.032(13) -0.038(10) C32C 0.066(7) 0.062(7) 0.130(10) -0.001(7) -0.016(7) -0.044(6) C33 0.077(5) 0.126(6) 0.085(4) -0.010(4) -0.047(4) 0.010(4) C34A 0.090(9) 0.040(6) 0.142(12) 0.040(7) -0.064(9) -0.018(6) C34B 0.078(10) 0.103(11) 0.119(12) -0.036(9) 0.007(8) -0.025(9) O1W 0.0633(19) 0.0301(13) 0.0403(14) 0.0042(11) -0.0210(13) -0.0207(13) O2W 0.077(2) 0.0417(16) 0.0457(16) -0.0053(13) -0.0024(15) -0.0292(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.887(2) . ? Mn1 O2 1.894(2) . ? Mn1 O7 1.930(2) . ? Mn1 N1 1.982(2) . ? Mn1 O8 2.212(2) . ? Mn1 Mn3 3.2371(7) . ? Mn2 O1 1.8968(19) . ? Mn2 O4 1.905(2) . ? Mn2 O3 1.960(2) . ? Mn2 N3 1.975(3) . ? Mn2 O9 2.271(3) . ? Mn2 O3 2.322(2) 2_655 ? Mn2 Mn2 3.2201(10) 2_655 ? Mn3 O5 1.887(2) . ? Mn3 O1 1.890(2) . ? Mn3 O6 1.895(2) . ? Mn3 N5 1.991(2) . ? Mn3 O10 2.245(3) . ? Mn3 O11 2.460(3) . ? O2 C1 1.341(4) . ? O3 N1 1.414(3) . ? O3 Mn2 2.322(2) 2_655 ? O4 C8 1.352(4) . ? O5 N3 1.400(3) . ? O6 C15 1.351(4) . ? O7 N5 1.407(3) . ? O8 C22 1.321(4) . ? O9 C29A 1.351(9) . ? O9 C29B 1.407(13) . ? O9 H9A 0.8170 . ? O10 C31C 1.335(16) . ? O10 C31A 1.410(7) . ? O10 H10A 0.8837 . ? O11 C33 1.414(6) . ? O11 H11A 0.8235 . ? N1 C7 1.322(4) . ? N2 C7 1.341(4) . ? N2 H2A 0.8081 . ? N2 H2B 0.8612 . ? N3 C14 1.317(4) . ? N4 C14 1.339(4) . ? N4 H4A 0.8209 . ? N4 H4B 0.8821 . ? N5 C21 1.323(4) . ? N6 C21 1.348(4) . ? N6 H6A 0.8476 . ? N6 H6B 0.9177 . ? N7 C28 1.144(5) . ? C1 C2 1.422(4) . ? C1 C6 1.423(4) . ? C2 C3 1.370(5) . ? C2 H2 0.9400 . ? C3 C4 1.397(5) . ? C3 H3 0.9400 . ? C4 C5 1.386(5) . ? C4 H4 0.9400 . ? C5 C6 1.398(5) . ? C5 H5 0.9400 . ? C6 C7 1.487(4) . ? C8 C9 1.413(4) . ? C8 C13 1.415(4) . ? C9 C10 1.383(5) . ? C9 H9 0.9400 . ? C10 C11 1.394(5) . ? C10 H10 0.9400 . ? C11 C12 1.389(5) . ? C11 H11 0.9400 . ? C12 C13 1.407(4) . ? C12 H12 0.9400 . ? C13 C14 1.484(4) . ? C15 C16 1.408(5) . ? C15 C20 1.409(4) . ? C16 C17 1.394(5) . ? C16 H16 0.9400 . ? C17 C18 1.382(6) . ? C17 H17 0.9400 . ? C18 C19 1.380(5) . ? C18 H18 0.9400 . ? C19 C20 1.425(4) . ? C19 H19 0.9400 . ? C20 C21 1.478(4) . ? C22 C27 1.410(5) . ? C22 C23 1.412(5) . ? C23 C24 1.383(5) . ? C23 H23 0.9400 . ? C24 C25 1.392(6) . ? C24 H24 0.9400 . ? C25 C26 1.373(6) . ? C25 H25 0.9400 . ? C26 C27 1.406(5) . ? C26 H26 0.9400 . ? C27 C28 1.452(5) . ? C29A C30A 1.574(17) . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C30A H30C 0.9700 . ? C29B C30B 1.473(17) . ? C29B H29C 0.9800 . ? C29B H29D 0.9800 . ? C30B H30D 0.9700 . ? C30B H30E 0.9700 . ? C30B H30F 0.9700 . ? C31A C32A 1.493(12) . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C32A H32A 0.9700 . ? C32A H32B 0.9700 . ? C32A H32C 0.9700 . ? C32B H32D 0.9700 . ? C32B H32E 0.9700 . ? C32B H32F 0.9700 . ? C31C H31E 0.9800 . ? C31C H31F 0.9800 . ? C33 C34A 1.279(10) . ? C33 C34B 1.379(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C34A H34C 0.9700 . ? C34B H34D 0.9700 . ? C34B H34E 0.9700 . ? C34B H34F 0.9700 . ? O1W H1WA 0.8184 . ? O1W H1WB 0.8261 . ? O2W H2WA 0.8751 . ? O2W H2WB 0.7898 . ? 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 O2 174.28(10) . . ? O1 Mn1 O7 90.99(9) . . ? O2 Mn1 O7 90.62(9) . . ? O1 Mn1 N1 87.44(9) . . ? O2 Mn1 N1 89.40(10) . . ? O7 Mn1 N1 162.83(11) . . ? O1 Mn1 O8 89.24(9) . . ? O2 Mn1 O8 95.77(9) . . ? O7 Mn1 O8 102.65(9) . . ? N1 Mn1 O8 94.43(10) . . ? O1 Mn1 Mn3 31.04(6) . . ? O2 Mn1 Mn3 152.20(7) . . ? O7 Mn1 Mn3 62.48(6) . . ? N1 Mn1 Mn3 118.35(7) . . ? O8 Mn1 Mn3 84.34(6) . . ? O1 Mn2 O4 176.18(11) . . ? O1 Mn2 O3 88.72(8) . . ? O4 Mn2 O3 91.37(9) . . ? O1 Mn2 N3 89.14(9) . . ? O4 Mn2 N3 90.37(10) . . ? O3 Mn2 N3 173.67(11) . . ? O1 Mn2 O9 88.20(10) . . ? O4 Mn2 O9 95.62(11) . . ? O3 Mn2 O9 88.00(10) . . ? N3 Mn2 O9 97.89(11) . . ? O1 Mn2 O3 88.95(8) . 2_655 ? O4 Mn2 O3 87.27(9) . 2_655 ? O3 Mn2 O3 82.83(9) . 2_655 ? N3 Mn2 O3 91.17(10) . 2_655 ? O9 Mn2 O3 170.46(9) . 2_655 ? O1 Mn2 Mn2 88.47(7) . 2_655 ? O4 Mn2 Mn2 88.87(7) . 2_655 ? O3 Mn2 Mn2 45.68(7) . 2_655 ? N3 Mn2 Mn2 128.29(9) . 2_655 ? O9 Mn2 Mn2 133.63(8) . 2_655 ? O3 Mn2 Mn2 37.15(5) 2_655 2_655 ? O5 Mn3 O1 91.31(9) . . ? O5 Mn3 O6 88.42(9) . . ? O1 Mn3 O6 176.17(11) . . ? O5 Mn3 N5 174.27(12) . . ? O1 Mn3 N5 89.89(9) . . ? O6 Mn3 N5 90.02(10) . . ? O5 Mn3 O10 97.03(11) . . ? O1 Mn3 O10 88.07(10) . . ? O6 Mn3 O10 95.76(11) . . ? N5 Mn3 O10 88.62(11) . . ? O5 Mn3 O11 92.01(10) . . ? O1 Mn3 O11 81.09(9) . . ? O6 Mn3 O11 95.10(10) . . ? N5 Mn3 O11 82.63(10) . . ? O10 Mn3 O11 166.04(9) . . ? O5 Mn3 Mn1 122.27(7) . . ? O1 Mn3 Mn1 31.00(6) . . ? O6 Mn3 Mn1 149.25(7) . . ? N5 Mn3 Mn1 59.25(7) . . ? O10 Mn3 Mn1 83.34(7) . . ? O11 Mn3 Mn1 82.84(6) . . ? Mn1 O1 Mn3 117.95(10) . . ? Mn1 O1 Mn2 121.59(10) . . ? Mn3 O1 Mn2 119.97(10) . . ? C1 O2 Mn1 121.94(18) . . ? N1 O3 Mn2 112.26(15) . . ? N1 O3 Mn2 116.02(16) . 2_655 ? Mn2 O3 Mn2 97.17(9) . 2_655 ? C8 O4 Mn2 125.92(19) . . ? N3 O5 Mn3 118.42(17) . . ? C15 O6 Mn3 124.8(2) . . ? N5 O7 Mn1 113.29(16) . . ? C22 O8 Mn1 120.3(2) . . ? C29A O9 C29B 56.3(8) . . ? C29A O9 Mn2 129.9(5) . . ? C29B O9 Mn2 128.6(7) . . ? C29A O9 H9A 112.4 . . ? C29B O9 H9A 106.8 . . ? Mn2 O9 H9A 111.4 . . ? C31C O10 C31A 44.0(10) . . ? C31C O10 Mn3 131.5(11) . . ? C31A O10 Mn3 135.1(3) . . ? C31C O10 H10A 111.5 . . ? C31A O10 H10A 111.8 . . ? Mn3 O10 H10A 108.7 . . ? C33 O11 Mn3 123.4(4) . . ? C33 O11 H11A 110.2 . . ? Mn3 O11 H11A 109.9 . . ? C7 N1 O3 114.2(2) . . ? C7 N1 Mn1 128.0(2) . . ? O3 N1 Mn1 117.48(17) . . ? C7 N2 H2A 117.2 . . ? C7 N2 H2B 110.5 . . ? H2A N2 H2B 131.1 . . ? C14 N3 O5 112.5(2) . . ? C14 N3 Mn2 129.9(2) . . ? O5 N3 Mn2 117.10(17) . . ? C14 N4 H4A 117.6 . . ? C14 N4 H4B 119.4 . . ? H4A N4 H4B 118.8 . . ? C21 N5 O7 113.5(2) . . ? C21 N5 Mn3 128.7(2) . . ? O7 N5 Mn3 116.35(16) . . ? C21 N6 H6A 121.9 . . ? C21 N6 H6B 114.1 . . ? H6A N6 H6B 123.8 . . ? O2 C1 C2 118.6(3) . . ? O2 C1 C6 123.9(3) . . ? C2 C1 C6 117.5(3) . . ? C3 C2 C1 121.6(3) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 120.8(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C7 119.2(3) . . ? C1 C6 C7 121.3(3) . . ? N1 C7 N2 120.9(3) . . ? N1 C7 C6 119.4(3) . . ? N2 C7 C6 119.7(3) . . ? O4 C8 C9 116.8(3) . . ? O4 C8 C13 124.5(3) . . ? C9 C8 C13 118.6(3) . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.1(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 122.1(3) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C12 C13 C8 118.5(3) . . ? C12 C13 C14 119.0(3) . . ? C8 C13 C14 122.5(3) . . ? N3 C14 N4 119.1(3) . . ? N3 C14 C13 120.0(3) . . ? N4 C14 C13 120.9(3) . . ? O6 C15 C16 117.4(3) . . ? O6 C15 C20 123.0(3) . . ? C16 C15 C20 119.4(3) . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 118.7(3) . . ? C15 C20 C21 122.8(3) . . ? C19 C20 C21 118.5(3) . . ? N5 C21 N6 118.7(3) . . ? N5 C21 C20 119.5(3) . . ? N6 C21 C20 121.8(3) . . ? O8 C22 C27 122.8(3) . . ? O8 C22 C23 121.5(3) . . ? C27 C22 C23 115.7(3) . . ? C24 C23 C22 121.7(4) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 121.3(4) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C26 C25 C24 118.7(4) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 120.4(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 122.0(3) . . ? C26 C27 C28 118.4(4) . . ? C22 C27 C28 119.6(3) . . ? N7 C28 C27 175.5(5) . . ? O9 C29A C30A 108.0(14) . . ? O9 C29A H29A 110.1 . . ? C30A C29A H29A 110.1 . . ? O9 C29A H29B 110.1 . . ? C30A C29A H29B 110.1 . . ? H29A C29A H29B 108.4 . . ? O9 C29B C30B 116.1(18) . . ? O9 C29B H29C 108.3 . . ? C30B C29B H29C 108.3 . . ? O9 C29B H29D 108.3 . . ? C30B C29B H29D 108.3 . . ? H29C C29B H29D 107.4 . . ? C29B C30B H30D 109.5 . . ? C29B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? O10 C31A C32A 115.3(7) . . ? O10 C31A H31A 108.5 . . ? C32A C31A H31A 108.5 . . ? O10 C31A H31B 108.5 . . ? C32A C31A H31B 108.5 . . ? H31A C31A H31B 107.5 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? H32D C32B H32E 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? O10 C31C H31E 107.7 . . ? O10 C31C H31F 107.7 . . ? H31E C31C H31F 107.1 . . ? C34A C33 C34B 65.1(9) . . ? C34A C33 O11 123.3(8) . . ? C34B C33 O11 120.7(9) . . ? C34A C33 H33A 106.5 . . ? C34B C33 H33A 42.9 . . ? O11 C33 H33A 106.5 . . ? C34A C33 H33B 106.5 . . ? C34B C33 H33B 128.2 . . ? O11 C33 H33B 106.5 . . ? H33A C33 H33B 106.5 . . ? C33 C34A H34A 109.5 . . ? C33 C34A H34B 109.5 . . ? C33 C34A H34C 109.5 . . ? C33 C34B H34D 109.5 . . ? C33 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? H1WA O1W H1WB 112.5 . . ? H2WA O2W H2WB 103.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.562 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.085 data_jml12b _database_code_depnum_ccdc_archive 'CCDC 888453' #TrackingRef 'web_deposit_cif_file_5_Lise-MarieChamoreau_1340629901.jml12b-publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C50 H68 Mn6 N12 O22)2+, 2 Cl-, 9(C H4 O)' _chemical_formula_sum 'C59 H104 Cl2 Mn6 N12 O31' _chemical_formula_weight 1878.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.1601(11) _cell_length_b 15.108(2) _cell_length_c 23.331(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.260(10) _cell_angle_gamma 90.00 _cell_volume 4533.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 177 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 22.3 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.527 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70249 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12881 _reflns_number_gt 8689 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; MeOH molecules are disordered, thus there is no short contact between O16 and O17. It was not possible to locate correctly H atoms of hydroxyde groups for O15, O16 and O17, neither from Fourier difmap, nor with softwares. 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^ > 2\s(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^)+(0.0616P)^2^+13.2276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12881 _refine_ls_number_parameters 510 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.88851(4) 0.69036(4) 0.47911(2) 0.02449(13) Uani 1 1 d . . . Mn2 Mn 1.02065(4) 0.53809(3) 0.56611(2) 0.02305(12) Uani 1 1 d . . . Mn3 Mn 0.78540(4) 0.59598(4) 0.57948(2) 0.02757(13) Uani 1 1 d . . . O1 O 0.9034(2) 0.61428(17) 0.54559(10) 0.0265(5) Uani 1 1 d . . . O2 O 0.8745(2) 0.76126(18) 0.41057(11) 0.0297(5) Uani 1 1 d . . . O3 O 1.06695(19) 0.57445(16) 0.49537(10) 0.0248(5) Uani 1 1 d . . . O4 O 1.13575(19) 0.45538(17) 0.58585(10) 0.0269(5) Uani 1 1 d . . . O5 O 0.8507(2) 0.49804(18) 0.62401(11) 0.0312(6) Uani 1 1 d . . . O6 O 0.6630(2) 0.5774(2) 0.60919(13) 0.0397(7) Uani 1 1 d . . . O7 O 0.7441(2) 0.70717(19) 0.47585(11) 0.0332(6) Uani 1 1 d . . . O8 O 0.9383(3) 0.8113(2) 0.53340(12) 0.0430(7) Uani 1 1 d . . . H8A H 0.9719 0.8106 0.5699 0.065 Uiso 1 1 d R . . O9 O 1.1203(2) 0.6374(2) 0.62083(14) 0.0419(7) Uani 1 1 d . . . H9A H 1.0913 0.6870 0.6329 0.063 Uiso 1 1 d R . . O10 O 0.8412(3) 0.6906(2) 0.65563(12) 0.0403(7) Uani 1 1 d . . . H10A H 0.8989 0.7303 0.6578 0.060 Uiso 1 1 d R . . O11 O 0.7249(2) 0.50104(19) 0.49726(12) 0.0347(6) Uani 1 1 d . . . H11A H 0.7615 0.5154 0.4669 0.052 Uiso 1 1 d R . . N1 N 1.0319(2) 0.66021(19) 0.47428(13) 0.0255(6) Uani 1 1 d . . . N2 N 1.1908(3) 0.6706(2) 0.44632(16) 0.0372(8) Uani 1 1 d . . . H2A H 1.2231 0.6888 0.4209 0.045 Uiso 1 1 d R . . H2B H 1.2125 0.6162 0.4630 0.045 Uiso 1 1 d R . . N3 N 0.9591(2) 0.4911(2) 0.63039(13) 0.0275(6) Uani 1 1 d . . . N4 N 0.9432(3) 0.3993(3) 0.70649(16) 0.0441(9) Uani 1 1 d . . . H4A H 0.9691 0.3737 0.7386 0.053 Uiso 1 1 d R . . H4B H 0.8748 0.4162 0.6975 0.053 Uiso 1 1 d R . . N5 N 0.7121(2) 0.6914(2) 0.52877(13) 0.0303(7) Uani 1 1 d . . . N6 N 0.5880(3) 0.7977(3) 0.49353(19) 0.0570(12) Uani 1 1 d . . . H6A H 0.5409 0.8382 0.4951 0.068 Uiso 1 1 d R . . H6B H 0.6182 0.8032 0.4607 0.068 Uiso 1 1 d R . . C1 C 0.9532(3) 0.8097(2) 0.39762(14) 0.0276(7) Uani 1 1 d . . . C2 C 0.9268(3) 0.8874(3) 0.36431(17) 0.0347(8) Uani 1 1 d . . . H2 H 0.8556 0.9028 0.3519 0.042 Uiso 1 1 calc R . . C3 C 1.0016(4) 0.9421(3) 0.3491(2) 0.0431(10) Uani 1 1 d . . . H3 H 0.9815 0.9936 0.3261 0.052 Uiso 1 1 calc R . . C4 C 1.1074(4) 0.9206(3) 0.3682(2) 0.0467(11) Uani 1 1 d . . . H4 H 1.1593 0.9585 0.3590 0.056 Uiso 1 1 calc R . . C5 C 1.1359(4) 0.8438(3) 0.4004(2) 0.0395(9) Uani 1 1 d . . . H5 H 1.2075 0.8294 0.4126 0.047 Uiso 1 1 calc R . . C6 C 1.0604(3) 0.7867(2) 0.41545(15) 0.0285(7) Uani 1 1 d . . . C7 C 1.0957(3) 0.7022(2) 0.44638(16) 0.0270(7) Uani 1 1 d . . . C8 C 1.1773(3) 0.4327(3) 0.64294(15) 0.0290(7) Uani 1 1 d . . . C9 C 1.2842(3) 0.4157(3) 0.65833(19) 0.0407(10) Uani 1 1 d . . . H9 H 1.3254 0.4211 0.6296 0.049 Uiso 1 1 calc R . . C10 C 1.3312(4) 0.3909(4) 0.7157(2) 0.0513(12) Uani 1 1 d . . . H10 H 1.4038 0.3796 0.7255 0.062 Uiso 1 1 calc R . . C11 C 1.2732(4) 0.3826(4) 0.7581(2) 0.0539(13) Uani 1 1 d . . . H11 H 1.3059 0.3665 0.7970 0.065 Uiso 1 1 calc R . . C12 C 1.1666(4) 0.3979(3) 0.74372(17) 0.0433(10) Uani 1 1 d . . . H12 H 1.1268 0.3913 0.7730 0.052 Uiso 1 1 calc R . . C13 C 1.1164(3) 0.4232(3) 0.68612(16) 0.0314(8) Uani 1 1 d . . . C14 C 1.0028(3) 0.4377(3) 0.67339(15) 0.0302(8) Uani 1 1 d . . . C15 C 0.6015(3) 0.6438(3) 0.62035(17) 0.0355(9) Uani 1 1 d . . . C16 C 0.5523(3) 0.6343(4) 0.66817(19) 0.0442(11) Uani 1 1 d . . . H16 H 0.5639 0.5820 0.6912 0.053 Uiso 1 1 calc R . . C17 C 0.4875(4) 0.6992(4) 0.6823(2) 0.0540(14) Uani 1 1 d . . . H17 H 0.4541 0.6904 0.7142 0.065 Uiso 1 1 calc R . . C18 C 0.4711(4) 0.7778(4) 0.6498(2) 0.0504(12) Uani 1 1 d . . . H18 H 0.4289 0.8234 0.6603 0.061 Uiso 1 1 calc R . . C19 C 0.5170(3) 0.7881(3) 0.6022(2) 0.0445(10) Uani 1 1 d . . . H19 H 0.5036 0.8404 0.5792 0.053 Uiso 1 1 calc R . . C20 C 0.5837(3) 0.7228(3) 0.58681(18) 0.0354(8) Uani 1 1 d . . . C21 C 0.6300(3) 0.7374(3) 0.53449(18) 0.0355(9) Uani 1 1 d . . . C22 C 0.8796(6) 0.8914(4) 0.5278(3) 0.080(2) Uani 1 1 d . . . H22A H 0.8435 0.8993 0.4869 0.120 Uiso 1 1 calc R . . H22B H 0.9265 0.9415 0.5400 0.120 Uiso 1 1 calc R . . H22C H 0.8285 0.8884 0.5528 0.120 Uiso 1 1 calc R . . C23 C 1.2238(4) 0.6611(4) 0.6157(3) 0.0713(18) Uani 1 1 d . . . H23A H 1.2697 0.6096 0.6251 0.107 Uiso 1 1 calc R . . H23B H 1.2496 0.7094 0.6430 0.107 Uiso 1 1 calc R . . H23C H 1.2228 0.6804 0.5755 0.107 Uiso 1 1 calc R . . C24 C 0.8586(5) 0.6601(4) 0.71601(19) 0.0536(13) Uani 1 1 d . . . H24A H 0.8144 0.6087 0.7184 0.080 Uiso 1 1 calc R . . H24B H 0.8416 0.7077 0.7409 0.080 Uiso 1 1 calc R . . H24C H 0.9318 0.6434 0.7294 0.080 Uiso 1 1 calc R . . C25 C 0.6182(4) 0.4908(5) 0.4703(3) 0.0678(17) Uani 1 1 d . . . H25A H 0.5799 0.4698 0.4994 0.102 Uiso 1 1 calc R . . H25B H 0.6112 0.4477 0.4383 0.102 Uiso 1 1 calc R . . H25C H 0.5897 0.5479 0.4546 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.96019(9) 0.30795(7) 0.83490(4) 0.0424(2) Uani 1 1 d . . . O12 O 0.6898(4) 0.4648(3) 0.9367(2) 0.0847(14) Uani 1 1 d . . . H12A H 0.7048 0.5215 0.9295 0.127 Uiso 1 1 d R . . C26 C 0.7794(6) 0.4152(5) 0.9326(3) 0.082(2) Uani 1 1 d . . . H26A H 0.8403 0.4542 0.9397 0.123 Uiso 1 1 calc R . . H26B H 0.7701 0.3893 0.8933 0.123 Uiso 1 1 calc R . . H26C H 0.7898 0.3679 0.9619 0.123 Uiso 1 1 calc R . . O13 O 0.6838(3) 0.6389(2) 0.89129(14) 0.0468(8) Uani 1 1 d . . . H13A H 0.7421 0.6613 0.8938 0.070 Uiso 1 1 d R . . C27 C 0.6219(6) 0.6609(5) 0.8360(3) 0.079(2) Uani 1 1 d . . . H27A H 0.5893 0.7187 0.8384 0.118 Uiso 1 1 calc R . . H27B H 0.5679 0.6158 0.8244 0.118 Uiso 1 1 calc R . . H27C H 0.6656 0.6634 0.8069 0.118 Uiso 1 1 calc R . . O14 O 0.3985(4) 0.5972(3) 0.9742(2) 0.0857(15) Uani 1 1 d . . . H14A H 0.3609 0.5676 0.9963 0.128 Uiso 1 1 d R . . C28 C 0.4004(6) 0.5379(6) 0.9282(4) 0.092(2) Uani 1 1 d . . . H28A H 0.3988 0.5711 0.8920 0.139 Uiso 1 1 calc R . . H28B H 0.3396 0.4989 0.9230 0.139 Uiso 1 1 calc R . . H28C H 0.4640 0.5024 0.9376 0.139 Uiso 1 1 calc R . . O15 O 0.7076(8) 0.4362(6) 0.7003(4) 0.081(3) Uani 0.50 1 d P . . C29 C 0.7032(10) 0.4449(8) 0.7616(5) 0.060(3) Uani 0.50 1 d P . . H29A H 0.7492 0.4931 0.7793 0.089 Uiso 0.50 1 calc PR . . H29B H 0.7257 0.3895 0.7822 0.089 Uiso 0.50 1 calc PR . . H29C H 0.6317 0.4582 0.7648 0.089 Uiso 0.50 1 calc PR . . O16 O 0.3230(7) 0.7116(6) 0.3605(4) 0.070(2) Uiso 0.50 1 d P . . C30 C 0.4113(16) 0.6576(15) 0.3836(9) 0.123(7) Uiso 0.50 1 d P . . H30A H 0.4720 0.6801 0.3700 0.185 Uiso 0.50 1 calc PR . . H30B H 0.3973 0.5965 0.3701 0.185 Uiso 0.50 1 calc PR . . H30C H 0.4253 0.6593 0.4266 0.185 Uiso 0.50 1 calc PR . . O17 O 0.2689(17) 0.7750(15) 0.2617(9) 0.206(9) Uiso 0.50 1 d PD . . C31 C 0.2575(18) 0.8669(15) 0.2626(10) 0.136(8) Uiso 0.50 1 d PD . . H31A H 0.1975 0.8819 0.2794 0.203 Uiso 0.50 1 calc PR . . H31B H 0.2466 0.8899 0.2225 0.203 Uiso 0.50 1 calc PR . . H31C H 0.3204 0.8933 0.2865 0.203 Uiso 0.50 1 calc PR . . 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 0.0283(3) 0.0221(3) 0.0240(2) 0.00523(19) 0.00760(19) 0.0052(2) Mn2 0.0269(3) 0.0196(2) 0.0228(2) 0.00345(18) 0.00561(19) 0.0032(2) Mn3 0.0301(3) 0.0263(3) 0.0285(3) 0.0059(2) 0.0112(2) 0.0053(2) O1 0.0299(13) 0.0258(13) 0.0256(11) 0.0061(9) 0.0096(9) 0.0071(10) O2 0.0343(14) 0.0285(14) 0.0264(12) 0.0065(10) 0.0068(10) 0.0022(11) O3 0.0311(13) 0.0174(11) 0.0267(11) 0.0055(9) 0.0081(9) 0.0040(10) O4 0.0292(13) 0.0242(13) 0.0259(11) 0.0041(9) 0.0029(9) 0.0049(10) O5 0.0309(13) 0.0302(14) 0.0344(13) 0.0092(11) 0.0112(11) 0.0049(11) O6 0.0372(15) 0.0375(16) 0.0497(17) 0.0107(13) 0.0208(13) 0.0026(13) O7 0.0322(14) 0.0399(16) 0.0298(13) 0.0108(11) 0.0122(10) 0.0104(12) O8 0.065(2) 0.0285(15) 0.0323(14) -0.0040(11) 0.0021(13) 0.0113(14) O9 0.0396(16) 0.0304(15) 0.0527(18) -0.0114(13) 0.0027(13) -0.0015(13) O10 0.0531(18) 0.0398(17) 0.0299(13) 0.0011(12) 0.0130(12) -0.0027(14) O11 0.0300(14) 0.0336(15) 0.0401(15) 0.0024(12) 0.0064(11) 0.0034(11) N1 0.0332(16) 0.0168(13) 0.0269(14) 0.0049(10) 0.0073(12) 0.0026(12) N2 0.0299(17) 0.0317(18) 0.054(2) 0.0095(15) 0.0167(15) 0.0020(14) N3 0.0302(15) 0.0252(15) 0.0278(14) 0.0043(11) 0.0076(12) 0.0029(12) N4 0.045(2) 0.049(2) 0.0398(19) 0.0249(17) 0.0132(15) 0.0073(17) N5 0.0295(15) 0.0342(17) 0.0291(15) 0.0062(13) 0.0103(12) 0.0063(13) N6 0.054(2) 0.065(3) 0.059(2) 0.031(2) 0.028(2) 0.038(2) C1 0.041(2) 0.0212(16) 0.0213(15) -0.0018(12) 0.0091(14) 0.0010(15) C2 0.044(2) 0.028(2) 0.0328(18) 0.0063(15) 0.0080(16) 0.0051(17) C3 0.062(3) 0.025(2) 0.044(2) 0.0108(17) 0.014(2) 0.0021(19) C4 0.053(3) 0.029(2) 0.061(3) 0.013(2) 0.020(2) -0.004(2) C5 0.041(2) 0.026(2) 0.053(2) 0.0070(17) 0.0127(19) -0.0047(17) C6 0.041(2) 0.0179(16) 0.0283(16) 0.0009(12) 0.0115(14) -0.0016(14) C7 0.0309(18) 0.0187(16) 0.0324(17) 0.0000(13) 0.0093(14) -0.0021(14) C8 0.0322(18) 0.0256(18) 0.0269(16) 0.0014(13) 0.0009(13) 0.0026(14) C9 0.035(2) 0.049(3) 0.036(2) 0.0051(18) 0.0028(16) 0.0093(19) C10 0.039(2) 0.064(3) 0.043(2) 0.008(2) -0.0067(19) 0.007(2) C11 0.053(3) 0.071(4) 0.031(2) 0.011(2) -0.0057(19) 0.011(3) C12 0.052(3) 0.050(3) 0.0249(18) 0.0063(17) 0.0014(17) 0.004(2) C13 0.037(2) 0.0272(19) 0.0272(17) 0.0047(14) 0.0017(14) 0.0023(15) C14 0.039(2) 0.0252(18) 0.0261(16) 0.0035(13) 0.0064(14) 0.0052(15) C15 0.0236(17) 0.047(2) 0.037(2) 0.0034(17) 0.0090(15) 0.0000(17) C16 0.032(2) 0.062(3) 0.039(2) 0.010(2) 0.0107(17) 0.001(2) C17 0.033(2) 0.095(4) 0.037(2) 0.004(2) 0.0150(18) 0.009(3) C18 0.032(2) 0.073(4) 0.049(3) -0.011(2) 0.0122(19) 0.009(2) C19 0.034(2) 0.052(3) 0.051(3) 0.000(2) 0.0164(19) 0.010(2) C20 0.0301(19) 0.042(2) 0.0357(19) 0.0019(17) 0.0115(15) 0.0043(17) C21 0.032(2) 0.038(2) 0.038(2) 0.0042(16) 0.0107(16) 0.0094(17) C22 0.119(6) 0.037(3) 0.070(4) -0.018(3) -0.014(4) 0.033(3) C23 0.045(3) 0.050(3) 0.116(5) -0.025(3) 0.010(3) -0.015(2) C24 0.084(4) 0.048(3) 0.031(2) 0.0019(19) 0.016(2) 0.000(3) C25 0.038(3) 0.097(5) 0.068(4) -0.003(3) 0.009(2) -0.006(3) Cl1 0.0614(7) 0.0341(5) 0.0322(5) 0.0106(4) 0.0108(4) 0.0032(5) O12 0.085(3) 0.055(3) 0.125(4) 0.003(3) 0.048(3) -0.010(2) C26 0.090(5) 0.057(4) 0.101(5) -0.015(4) 0.026(4) -0.007(4) O13 0.0444(18) 0.0476(19) 0.0475(17) -0.0069(14) 0.0076(14) -0.0160(15) C27 0.084(5) 0.076(5) 0.065(4) 0.003(3) -0.012(3) -0.016(4) O14 0.071(3) 0.090(4) 0.101(4) -0.016(3) 0.028(3) -0.040(3) C28 0.072(5) 0.096(6) 0.105(6) -0.025(5) 0.010(4) -0.002(4) O15 0.114(8) 0.060(5) 0.085(6) 0.029(5) 0.056(6) 0.019(5) C29 0.073(7) 0.059(7) 0.053(6) -0.002(5) 0.027(5) -0.009(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.901(2) . ? Mn1 O7 1.903(3) . ? Mn1 O1 1.907(2) . ? Mn1 N1 1.967(3) . ? Mn1 O8 2.241(3) . ? Mn2 O1 1.903(2) . ? Mn2 O4 1.942(2) . ? Mn2 O3 1.956(2) . ? Mn2 N3 1.982(3) . ? Mn2 O9 2.211(3) . ? Mn2 O3 2.361(3) 3_766 ? Mn2 Mn2 3.2289(11) 3_766 ? Mn3 O6 1.905(3) . ? Mn3 O5 1.905(3) . ? Mn3 O1 1.906(3) . ? Mn3 N5 1.980(3) . ? Mn3 O10 2.277(3) . ? Mn3 O11 2.392(3) . ? O2 C1 1.354(5) . ? O3 N1 1.427(4) . ? O3 Mn2 2.361(3) 3_766 ? O4 C8 1.372(4) . ? O5 N3 1.406(4) . ? O6 C15 1.349(5) . ? O7 N5 1.407(4) . ? O8 C22 1.426(6) . ? O8 H8A 0.8725 . ? O9 C23 1.439(6) . ? O9 H9A 0.9117 . ? O10 C24 1.453(5) . ? O10 H10A 0.9606 . ? O11 C25 1.420(6) . ? O11 H11A 0.9633 . ? N1 C7 1.328(5) . ? N2 C7 1.341(5) . ? N2 H2A 0.8457 . ? N2 H2B 0.9291 . ? N3 C14 1.320(5) . ? N4 C14 1.345(5) . ? N4 H4A 0.8475 . ? N4 H4B 0.9160 . ? N5 C21 1.316(5) . ? N6 C21 1.350(5) . ? N6 H6A 0.8778 . ? N6 H6B 0.9376 . ? C1 C2 1.411(5) . ? C1 C6 1.425(5) . ? C2 C3 1.387(6) . ? C2 H2 0.9500 . ? C3 C4 1.407(7) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.415(5) . ? C5 H5 0.9500 . ? C6 C7 1.492(5) . ? C8 C9 1.401(5) . ? C8 C13 1.421(5) . ? C9 C10 1.401(6) . ? C9 H9 0.9500 . ? C10 C11 1.377(7) . ? C10 H10 0.9500 . ? C11 C12 1.391(7) . ? C11 H11 0.9500 . ? C12 C13 1.418(5) . ? C12 H12 0.9500 . ? C13 C14 1.477(6) . ? C15 C16 1.411(6) . ? C15 C20 1.420(6) . ? C16 C17 1.384(7) . ? C16 H16 0.9500 . ? C17 C18 1.402(8) . ? C17 H17 0.9500 . ? C18 C19 1.380(6) . ? C18 H18 0.9500 . ? C19 C20 1.417(6) . ? C19 H19 0.9500 . ? C20 C21 1.492(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O12 C26 1.418(8) . ? O12 H12A 0.9028 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O13 C27 1.411(7) . ? O13 H13A 0.8283 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O14 C28 1.401(8) . ? O14 H14A 0.9051 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O15 C29 1.450(13) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O16 C30 1.43(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O17 C31 1.396(16) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 O2 Mn1 O7 88.49(11) . . ? O2 Mn1 O1 177.18(12) . . ? O7 Mn1 O1 92.40(11) . . ? O2 Mn1 N1 90.29(12) . . ? O7 Mn1 N1 172.09(13) . . ? O1 Mn1 N1 88.46(11) . . ? O2 Mn1 O8 88.88(11) . . ? O7 Mn1 O8 94.78(13) . . ? O1 Mn1 O8 93.71(11) . . ? N1 Mn1 O8 93.01(13) . . ? O1 Mn2 O4 177.15(12) . . ? O1 Mn2 O3 89.95(10) . . ? O4 Mn2 O3 90.78(10) . . ? O1 Mn2 N3 88.12(12) . . ? O4 Mn2 N3 90.78(12) . . ? O3 Mn2 N3 171.99(12) . . ? O1 Mn2 O9 94.84(12) . . ? O4 Mn2 O9 87.88(11) . . ? O3 Mn2 O9 92.51(12) . . ? N3 Mn2 O9 95.40(13) . . ? O1 Mn2 O3 91.00(10) . 3_766 ? O4 Mn2 O3 86.34(10) . 3_766 ? O3 Mn2 O3 83.62(10) . 3_766 ? N3 Mn2 O3 88.64(11) . 3_766 ? O9 Mn2 O3 173.00(10) . 3_766 ? O1 Mn2 Mn2 90.70(8) . 3_766 ? O4 Mn2 Mn2 87.80(8) . 3_766 ? O3 Mn2 Mn2 46.61(7) . 3_766 ? N3 Mn2 Mn2 125.62(10) . 3_766 ? O9 Mn2 Mn2 138.80(9) . 3_766 ? O3 Mn2 Mn2 37.01(6) 3_766 3_766 ? O6 Mn3 O5 90.33(12) . . ? O6 Mn3 O1 176.91(12) . . ? O5 Mn3 O1 91.48(11) . . ? O6 Mn3 N5 89.00(13) . . ? O5 Mn3 N5 175.70(14) . . ? O1 Mn3 N5 89.01(12) . . ? O6 Mn3 O10 88.05(13) . . ? O5 Mn3 O10 91.66(12) . . ? O1 Mn3 O10 94.40(11) . . ? N5 Mn3 O10 92.55(13) . . ? O6 Mn3 O11 92.29(12) . . ? O5 Mn3 O11 90.37(11) . . ? O1 Mn3 O11 85.19(11) . . ? N5 Mn3 O11 85.42(12) . . ? O10 Mn3 O11 177.94(11) . . ? Mn2 O1 Mn3 119.76(13) . . ? Mn2 O1 Mn1 120.45(13) . . ? Mn3 O1 Mn1 118.23(13) . . ? C1 O2 Mn1 123.4(2) . . ? N1 O3 Mn2 114.19(19) . . ? N1 O3 Mn2 111.33(18) . 3_766 ? Mn2 O3 Mn2 96.38(10) . 3_766 ? C8 O4 Mn2 121.4(2) . . ? N3 O5 Mn3 116.5(2) . . ? C15 O6 Mn3 123.3(3) . . ? N5 O7 Mn1 115.1(2) . . ? C22 O8 Mn1 123.5(3) . . ? C22 O8 H8A 104.6 . . ? Mn1 O8 H8A 124.6 . . ? C23 O9 Mn2 125.2(3) . . ? C23 O9 H9A 106.7 . . ? Mn2 O9 H9A 120.1 . . ? C24 O10 Mn3 121.0(3) . . ? C24 O10 H10A 100.7 . . ? Mn3 O10 H10A 123.6 . . ? C25 O11 Mn3 123.4(3) . . ? C25 O11 H11A 107.5 . . ? Mn3 O11 H11A 108.8 . . ? C7 N1 O3 114.3(3) . . ? C7 N1 Mn1 129.1(2) . . ? O3 N1 Mn1 115.8(2) . . ? C7 N2 H2A 119.6 . . ? C7 N2 H2B 121.2 . . ? H2A N2 H2B 115.3 . . ? C14 N3 O5 113.3(3) . . ? C14 N3 Mn2 127.7(3) . . ? O5 N3 Mn2 117.5(2) . . ? C14 N4 H4A 122.0 . . ? C14 N4 H4B 114.3 . . ? H4A N4 H4B 121.5 . . ? C21 N5 O7 113.9(3) . . ? C21 N5 Mn3 129.1(3) . . ? O7 N5 Mn3 116.7(2) . . ? C21 N6 H6A 128.8 . . ? C21 N6 H6B 117.2 . . ? H6A N6 H6B 113.5 . . ? O2 C1 C2 117.5(3) . . ? O2 C1 C6 124.0(3) . . ? C2 C1 C6 118.4(4) . . ? C3 C2 C1 122.1(4) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.9(3) . . ? C5 C6 C7 118.6(4) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 N2 121.2(3) . . ? N1 C7 C6 118.8(3) . . ? N2 C7 C6 120.0(3) . . ? O4 C8 C9 117.8(3) . . ? O4 C8 C13 123.1(3) . . ? C9 C8 C13 119.1(3) . . ? C8 C9 C10 120.6(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 121.1(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 118.7(4) . . ? C12 C13 C14 118.6(4) . . ? C8 C13 C14 122.8(3) . . ? N3 C14 N4 119.1(4) . . ? N3 C14 C13 120.2(3) . . ? N4 C14 C13 120.7(3) . . ? O6 C15 C16 118.2(4) . . ? O6 C15 C20 123.7(4) . . ? C16 C15 C20 118.1(4) . . ? C17 C16 C15 121.7(5) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 121.7(5) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 119.0(4) . . ? C19 C20 C21 119.2(4) . . ? C15 C20 C21 121.8(4) . . ? N5 C21 N6 120.4(4) . . ? N5 C21 C20 119.5(4) . . ? N6 C21 C20 120.1(4) . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 C23 H23A 109.5 . . ? O9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O10 C24 H24A 109.5 . . ? O10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O11 C25 H25A 109.5 . . ? O11 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O11 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 O12 H12A 105.7 . . ? O12 C26 H26A 109.5 . . ? O12 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O12 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 O13 H13A 108.4 . . ? O13 C27 H27A 109.5 . . ? O13 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O13 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 O14 H14A 102.7 . . ? O14 C28 H28A 109.5 . . ? O14 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O14 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O15 C29 H29A 109.5 . . ? O15 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O15 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O16 C30 H30A 109.5 . . ? O16 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O16 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O17 C31 H31A 109.5 . . ? O17 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O17 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.361 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.103 data_jml19 _database_code_depnum_ccdc_archive 'CCDC 888454' #TrackingRef 'web_deposit_cif_file_6_Lise-MarieChamoreau_1340629901.jml19 - publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H64 Cl2 Mn6 N12 O20, 5(C2 H6 O)' _chemical_formula_sum 'C60 H94 Cl2 Mn6 N12 O25' _chemical_formula_weight 1784.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 30.713(9) _cell_length_b 30.713(9) _cell_length_c 17.092(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16122(8) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 144 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 17.6 _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7376 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77072 _diffrn_reflns_av_R_equivalents 0.1713 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9248 _reflns_number_gt 4937 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Geometrical restraints were introduced on disordered EtOH molecules. No H atoms were placed for these moities. There is a litlle residual density near these EtOH and not so far from the center of the void. 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^ > 2\s(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^)+(0.0677P)^2^+22.9613P] 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 9248 _refine_ls_number_parameters 469 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.005 _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 0.42442(2) 0.05523(2) 0.41100(4) 0.02015(17) Uani 1 1 d . . . Mn2 Mn 0.49770(2) 0.04457(2) 0.55168(4) 0.01764(17) Uani 1 1 d . . . Mn3 Mn 0.39427(2) 0.05484(2) 0.59430(4) 0.01921(17) Uani 1 1 d . . . Cl1 Cl 0.40460(4) 0.14104(4) 0.60049(8) 0.0382(3) Uani 1 1 d . . . O1 O 0.43962(9) 0.05230(9) 0.51848(17) 0.0192(7) Uani 1 1 d . . . O2 O 0.41092(10) 0.05355(10) 0.30293(18) 0.0261(7) Uani 1 1 d . . . O3 O 0.51457(9) 0.03271(9) 0.44373(17) 0.0180(7) Uani 1 1 d . . . O4 O 0.55589(9) 0.03240(10) 0.58469(17) 0.0225(7) Uani 1 1 d . . . O5 O 0.43336(9) 0.04271(10) 0.67875(17) 0.0227(7) Uani 1 1 d . . . O6 O 0.34765(9) 0.05345(9) 0.66675(17) 0.0213(7) Uani 1 1 d . . . O7 O 0.36399(9) 0.04740(10) 0.43366(17) 0.0235(7) Uani 1 1 d . . . O8 O 0.42314(11) 0.12937(11) 0.4209(2) 0.0370(9) Uani 1 1 d . . . H8A H 0.4210 0.1327 0.4763 0.055 Uiso 1 1 d R . . O9 O 0.50477(11) 0.11862(10) 0.5480(2) 0.0356(9) Uani 1 1 d . . . H9A H 0.4809 0.1273 0.5606 0.053 Uiso 1 1 d R . . O10 O 0.39035(9) -0.02299(10) 0.56275(18) 0.0259(7) Uani 1 1 d . . . H10A H 0.4087 -0.0224 0.5242 0.039 Uiso 1 1 d R . . H10B H 0.3682 -0.0371 0.5499 0.039 Uiso 1 1 d R . . N1 N 0.48728(11) 0.05197(11) 0.3850(2) 0.0187(8) Uani 1 1 d . . . N2 N 0.55073(12) 0.05547(13) 0.3115(2) 0.0291(10) Uani 1 1 d . . . H2A H 0.5604 0.0590 0.2631 0.035 Uiso 1 1 d R . . H2B H 0.5676 0.0467 0.3494 0.035 Uiso 1 1 d R . . N3 N 0.47816(11) 0.04800(11) 0.6627(2) 0.0203(8) Uani 1 1 d . . . N4 N 0.48355(14) 0.04307(19) 0.7968(3) 0.0593(16) Uani 1 1 d . . . H4A H 0.4993 0.0407 0.8480 0.071 Uiso 1 1 d R . . H4B H 0.4558 0.0368 0.7916 0.071 Uiso 1 1 d R . . N5 N 0.35160(11) 0.06186(12) 0.5093(2) 0.0200(8) Uani 1 1 d . . . N6 N 0.28585(12) 0.07527(14) 0.4472(2) 0.0342(10) Uani 1 1 d . . . H6A H 0.3014 0.0659 0.4033 0.041 Uiso 1 1 d R . . H6B H 0.2603 0.0914 0.4434 0.041 Uiso 1 1 d R . . C1 C 0.43589(15) 0.07064(15) 0.2451(3) 0.0255(11) Uani 1 1 d . . . C2 C 0.41444(17) 0.08356(18) 0.1760(3) 0.0363(13) Uani 1 1 d . . . H2 H 0.3839 0.0793 0.1713 0.044 Uiso 1 1 calc R . . C3 C 0.43735(18) 0.1024(2) 0.1149(3) 0.0474(15) Uani 1 1 d . . . H3 H 0.4223 0.1105 0.0686 0.057 Uiso 1 1 calc R . . C4 C 0.48199(18) 0.1097(2) 0.1201(3) 0.0509(16) Uani 1 1 d . . . H4 H 0.4973 0.1237 0.0789 0.061 Uiso 1 1 calc R . . C5 C 0.50353(17) 0.09612(18) 0.1873(3) 0.0383(13) Uani 1 1 d . . . H5 H 0.5341 0.1004 0.1911 0.046 Uiso 1 1 calc R . . C6 C 0.48142(15) 0.07605(14) 0.2502(3) 0.0240(10) Uani 1 1 d . . . C7 C 0.50726(14) 0.06043(14) 0.3186(3) 0.0218(10) Uani 1 1 d . . . C8 C 0.57407(14) 0.04881(13) 0.6514(3) 0.0198(10) Uani 1 1 d . . . C9 C 0.61900(14) 0.05818(14) 0.6505(3) 0.0252(11) Uani 1 1 d . . . H9 H 0.6356 0.0530 0.6045 0.030 Uiso 1 1 calc R . . C10 C 0.63927(15) 0.07511(16) 0.7172(3) 0.0321(12) Uani 1 1 d . . . H10 H 0.6696 0.0813 0.7160 0.039 Uiso 1 1 calc R . . C11 C 0.61591(16) 0.08295(18) 0.7850(3) 0.0373(13) Uani 1 1 d . . . H11 H 0.6299 0.0947 0.8298 0.045 Uiso 1 1 calc R . . C12 C 0.57198(17) 0.07345(18) 0.7868(3) 0.0400(14) Uani 1 1 d . . . H12 H 0.5561 0.0785 0.8336 0.048 Uiso 1 1 calc R . . C13 C 0.54988(15) 0.05629(16) 0.7207(3) 0.0265(11) Uani 1 1 d . . . C14 C 0.50216(15) 0.04842(16) 0.7268(3) 0.0286(11) Uani 1 1 d . . . C15 C 0.31140(14) 0.07856(14) 0.6614(3) 0.0212(10) Uani 1 1 d . . . C16 C 0.29142(15) 0.09253(15) 0.7315(3) 0.0287(11) Uani 1 1 d . . . H16 H 0.3040 0.0849 0.7803 0.034 Uiso 1 1 calc R . . C17 C 0.25394(16) 0.11710(17) 0.7299(3) 0.0370(13) Uani 1 1 d . . . H17 H 0.2412 0.1263 0.7778 0.044 Uiso 1 1 calc R . . C18 C 0.23449(16) 0.12868(17) 0.6595(3) 0.0360(13) Uani 1 1 d . . . H18 H 0.2088 0.1459 0.6590 0.043 Uiso 1 1 calc R . . C19 C 0.25329(14) 0.11465(15) 0.5893(3) 0.0295(11) Uani 1 1 d . . . H19 H 0.2397 0.1221 0.5411 0.035 Uiso 1 1 calc R . . C20 C 0.29178(14) 0.08985(14) 0.5883(3) 0.0212(10) Uani 1 1 d . . . C21 C 0.31025(14) 0.07516(14) 0.5130(3) 0.0211(10) Uani 1 1 d . . . C22 C 0.4058(2) 0.15921(18) 0.3666(4) 0.0580(18) Uani 1 1 d . . . H22A H 0.3737 0.1564 0.3653 0.070 Uiso 1 1 calc R . . H22B H 0.4171 0.1527 0.3137 0.070 Uiso 1 1 calc R . . C23 C 0.4180(2) 0.20513(19) 0.3893(4) 0.066(2) Uani 1 1 d . . . H23A H 0.4073 0.2113 0.4421 0.099 Uiso 1 1 calc R . . H23B H 0.4050 0.2257 0.3522 0.099 Uiso 1 1 calc R . . H23C H 0.4498 0.2082 0.3883 0.099 Uiso 1 1 calc R . . C24 C 0.5332(2) 0.14729(19) 0.5897(4) 0.065(2) Uani 1 1 d . . . H24A H 0.5635 0.1418 0.5725 0.077 Uiso 1 1 calc R . . H24B H 0.5315 0.1403 0.6462 0.077 Uiso 1 1 calc R . . C25 C 0.5233(3) 0.1949(2) 0.5789(5) 0.087(3) Uani 1 1 d . . . H25A H 0.5256 0.2024 0.5233 0.131 Uiso 1 1 calc R . . H25B H 0.5441 0.2123 0.6091 0.131 Uiso 1 1 calc R . . H25C H 0.4936 0.2009 0.5972 0.131 Uiso 1 1 calc R . . O11 O 0.31374(10) -0.06753(11) 0.52707(19) 0.0327(8) Uani 1 1 d . . . H11A H 0.3131 -0.0939 0.5324 0.050(19) Uiso 1 1 d R . . C26 C 0.27412(19) -0.0445(2) 0.5078(4) 0.0524(16) Uani 1 1 d . . . H26A H 0.2798 -0.0128 0.5108 0.063 Uiso 1 1 calc R . . H26B H 0.2518 -0.0516 0.5476 0.063 Uiso 1 1 calc R . . C27 C 0.2563(2) -0.0546(2) 0.4295(4) 0.065(2) Uani 1 1 d . . . H27A H 0.2767 -0.0446 0.3892 0.098 Uiso 1 1 calc R . . H27B H 0.2283 -0.0399 0.4227 0.098 Uiso 1 1 calc R . . H27C H 0.2522 -0.0862 0.4245 0.098 Uiso 1 1 calc R . . O12 O 0.5156(5) 0.0575(4) -0.0425(8) 0.126(5) Uiso 0.50 1 d PD . . C28 C 0.5263(9) 0.0138(7) -0.0320(19) 0.158(11) Uiso 0.50 1 d PD . . C29 C 0.5072(9) 0.0189(7) 0.0072(15) 0.132(9) Uiso 0.50 1 d PD . . O13 O 0.5748(4) 0.1217(4) -0.0152(7) 0.105(4) Uiso 0.50 1 d PD . . C30 C 0.5662(8) 0.1631(7) -0.0392(14) 0.136(8) Uiso 0.50 1 d PD . . C31 C 0.5981(7) 0.1886(7) -0.0620(13) 0.243(8) Uiso 1 1 d D . . C32 C 0.5873(15) 0.2086(14) -0.140(2) 0.28(2) Uiso 0.50 1 d PD . . O14 O 0.6318(6) 0.1538(6) -0.0526(11) 0.182(7) Uiso 0.50 1 d PD . . 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 0.0165(3) 0.0280(4) 0.0160(4) 0.0030(3) -0.0004(3) 0.0011(3) Mn2 0.0155(3) 0.0222(4) 0.0152(3) -0.0003(3) -0.0011(3) 0.0007(3) Mn3 0.0159(3) 0.0247(4) 0.0171(4) 0.0020(3) 0.0001(3) 0.0026(3) Cl1 0.0455(8) 0.0295(7) 0.0398(8) -0.0028(6) 0.0057(6) 0.0037(6) O1 0.0168(15) 0.0247(16) 0.0162(16) 0.0011(13) 0.0004(13) 0.0035(12) O2 0.0252(17) 0.0365(19) 0.0168(17) 0.0053(15) -0.0013(14) -0.0004(14) O3 0.0162(15) 0.0227(16) 0.0151(15) 0.0006(13) -0.0028(13) 0.0061(12) O4 0.0169(16) 0.0319(18) 0.0186(17) -0.0060(14) -0.0011(13) -0.0002(13) O5 0.0148(16) 0.0346(18) 0.0186(16) 0.0024(14) 0.0001(13) 0.0000(13) O6 0.0179(16) 0.0269(17) 0.0190(17) 0.0045(14) 0.0021(13) 0.0045(13) O7 0.0175(16) 0.0382(19) 0.0147(16) -0.0008(14) 0.0013(13) 0.0010(13) O8 0.039(2) 0.046(2) 0.0261(19) 0.0186(17) -0.0012(16) 0.0072(16) O9 0.0326(19) 0.0241(18) 0.050(2) -0.0022(17) -0.0040(18) -0.0051(15) O10 0.0185(16) 0.0315(18) 0.0277(19) 0.0004(15) 0.0011(14) -0.0025(13) N1 0.0189(19) 0.0211(19) 0.0161(19) 0.0059(16) -0.0042(16) 0.0018(15) N2 0.023(2) 0.044(3) 0.021(2) 0.0157(19) 0.0019(17) 0.0052(18) N3 0.0153(19) 0.025(2) 0.021(2) 0.0004(17) 0.0000(17) -0.0015(15) N4 0.022(2) 0.139(5) 0.017(2) 0.001(3) -0.004(2) -0.010(3) N5 0.0168(19) 0.027(2) 0.016(2) 0.0006(16) 0.0010(16) 0.0016(16) N6 0.023(2) 0.057(3) 0.022(2) 0.003(2) -0.0037(19) 0.016(2) C1 0.030(3) 0.031(3) 0.015(2) 0.004(2) 0.000(2) 0.002(2) C2 0.028(3) 0.053(3) 0.028(3) 0.010(3) -0.004(2) 0.000(2) C3 0.043(3) 0.073(4) 0.026(3) 0.022(3) -0.003(3) 0.003(3) C4 0.040(3) 0.080(5) 0.033(3) 0.031(3) 0.000(3) -0.006(3) C5 0.031(3) 0.054(4) 0.029(3) 0.010(3) 0.000(2) -0.002(3) C6 0.025(3) 0.028(3) 0.020(2) 0.006(2) -0.001(2) 0.006(2) C7 0.023(3) 0.021(2) 0.022(3) 0.002(2) 0.001(2) 0.0011(18) C8 0.024(2) 0.017(2) 0.019(2) 0.0042(19) -0.006(2) -0.0013(18) C9 0.023(2) 0.031(3) 0.022(3) 0.002(2) -0.004(2) -0.003(2) C10 0.022(3) 0.038(3) 0.037(3) 0.000(2) -0.011(2) -0.007(2) C11 0.030(3) 0.053(3) 0.030(3) -0.008(3) -0.011(2) -0.003(2) C12 0.034(3) 0.061(4) 0.026(3) -0.009(3) -0.004(2) 0.001(3) C13 0.024(3) 0.039(3) 0.017(2) -0.001(2) -0.005(2) -0.002(2) C14 0.021(3) 0.045(3) 0.020(3) -0.002(2) 0.002(2) 0.001(2) C15 0.021(2) 0.019(2) 0.023(2) 0.004(2) 0.001(2) -0.0023(18) C16 0.027(3) 0.036(3) 0.024(3) -0.001(2) 0.002(2) 0.003(2) C17 0.028(3) 0.054(3) 0.029(3) -0.003(3) 0.012(2) 0.008(2) C18 0.023(3) 0.048(3) 0.037(3) 0.003(3) 0.003(2) 0.012(2) C19 0.022(2) 0.033(3) 0.033(3) 0.003(2) 0.002(2) 0.006(2) C20 0.019(2) 0.020(2) 0.024(2) 0.005(2) 0.003(2) -0.0009(18) C21 0.020(2) 0.020(2) 0.023(3) 0.008(2) 0.000(2) -0.0004(18) C22 0.079(5) 0.039(4) 0.056(4) 0.004(3) -0.008(4) 0.015(3) C23 0.078(5) 0.046(4) 0.073(5) 0.017(4) 0.019(4) 0.011(3) C24 0.068(4) 0.042(4) 0.083(5) -0.003(4) -0.019(4) -0.008(3) C25 0.098(6) 0.038(4) 0.125(8) -0.004(4) -0.008(6) -0.005(4) O11 0.034(2) 0.029(2) 0.036(2) 0.0013(16) -0.0040(17) -0.0061(15) C26 0.043(3) 0.046(4) 0.068(5) -0.004(3) -0.002(3) -0.001(3) C27 0.044(4) 0.103(6) 0.049(4) 0.022(4) -0.001(3) 0.000(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.894(3) . ? Mn1 O1 1.898(3) . ? Mn1 O7 1.911(3) . ? Mn1 N1 1.983(4) . ? Mn1 O8 2.284(4) . ? Mn2 O1 1.887(3) . ? Mn2 O4 1.911(3) . ? Mn2 O3 1.951(3) . ? Mn2 N3 1.994(4) . ? Mn2 O9 2.285(3) . ? Mn2 O3 2.404(3) 9_656 ? Mn3 O6 1.894(3) . ? Mn3 O1 1.904(3) . ? Mn3 O5 1.914(3) . ? Mn3 N5 1.969(4) . ? Mn3 O10 2.453(3) . ? Mn3 Cl1 2.6686(16) . ? O2 C1 1.357(5) . ? O3 N1 1.435(4) . ? O3 Mn2 2.404(3) 9_656 ? O4 C8 1.366(5) . ? O5 N3 1.412(4) . ? O6 C15 1.357(5) . ? O7 N5 1.419(4) . ? O8 C22 1.409(6) . ? O8 H8A 0.9555 . ? O9 C24 1.431(7) . ? O9 H9A 0.8098 . ? O10 H10A 0.8665 . ? O10 H10B 0.8378 . ? N1 C7 1.316(5) . ? N2 C7 1.349(6) . ? N2 H2A 0.8864 . ? N2 H2B 0.8726 . ? N3 C14 1.319(6) . ? N4 C14 1.337(6) . ? N4 H4A 1.0016 . ? N4 H4B 0.8788 . ? N5 C21 1.335(5) . ? N6 C21 1.352(6) . ? N6 H6A 0.9344 . ? N6 H6B 0.9307 . ? C1 C2 1.409(6) . ? C1 C6 1.411(6) . ? C2 C3 1.386(7) . ? C2 H2 0.9500 . ? C3 C4 1.392(8) . ? C3 H3 0.9500 . ? C4 C5 1.390(7) . ? C4 H4 0.9500 . ? C5 C6 1.413(7) . ? C5 H5 0.9500 . ? C6 C7 1.492(6) . ? C8 C9 1.410(6) . ? C8 C13 1.417(6) . ? C9 C10 1.400(6) . ? C9 H9 0.9500 . ? C10 C11 1.383(7) . ? C10 H10 0.9500 . ? C11 C12 1.381(7) . ? C11 H11 0.9500 . ? C12 C13 1.419(7) . ? C12 H12 0.9500 . ? C13 C14 1.489(6) . ? C15 C16 1.412(6) . ? C15 C20 1.431(6) . ? C16 C17 1.376(7) . ? C16 H16 0.9500 . ? C17 C18 1.390(7) . ? C17 H17 0.9500 . ? C18 C19 1.400(7) . ? C18 H18 0.9500 . ? C19 C20 1.406(6) . ? C19 H19 0.9500 . ? C20 C21 1.476(6) . ? C22 C23 1.510(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.505(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O11 C26 1.445(6) . ? O11 H11A 0.8142 . ? C26 C27 1.479(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O12 C28 1.393(17) . ? O12 C29 1.480(16) . ? C28 C29 0.91(3) . ? C28 C29 1.50(3) 9_655 ? C29 C29 1.26(4) 9_655 ? C29 C28 1.50(3) 9_655 ? O13 C30 1.365(16) . ? C30 C31 1.31(3) . ? C31 O14 1.495(15) . ? C31 C32 1.509(19) . ? 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 175.43(13) . . ? O2 Mn1 O7 88.94(13) . . ? O1 Mn1 O7 92.11(12) . . ? O2 Mn1 N1 89.64(14) . . ? O1 Mn1 N1 88.54(13) . . ? O7 Mn1 N1 169.81(14) . . ? O2 Mn1 O8 95.48(13) . . ? O1 Mn1 O8 88.86(12) . . ? O7 Mn1 O8 95.38(13) . . ? N1 Mn1 O8 94.80(13) . . ? O1 Mn2 O4 175.95(13) . . ? O1 Mn2 O3 89.44(12) . . ? O4 Mn2 O3 89.68(12) . . ? O1 Mn2 N3 89.72(13) . . ? O4 Mn2 N3 90.61(14) . . ? O3 Mn2 N3 172.05(14) . . ? O1 Mn2 O9 87.50(12) . . ? O4 Mn2 O9 96.54(12) . . ? O3 Mn2 O9 97.76(13) . . ? N3 Mn2 O9 90.11(14) . . ? O1 Mn2 O3 89.19(11) . 9_656 ? O4 Mn2 O3 86.78(11) . 9_656 ? O3 Mn2 O3 83.58(11) . 9_656 ? N3 Mn2 O3 88.51(12) . 9_656 ? O9 Mn2 O3 176.41(11) . 9_656 ? O6 Mn3 O1 175.81(13) . . ? O6 Mn3 O5 88.67(13) . . ? O1 Mn3 O5 92.66(12) . . ? O6 Mn3 N5 88.95(14) . . ? O1 Mn3 N5 89.38(14) . . ? O5 Mn3 N5 174.57(14) . . ? O6 Mn3 O10 94.86(12) . . ? O1 Mn3 O10 81.16(11) . . ? O5 Mn3 O10 90.40(12) . . ? N5 Mn3 O10 84.94(13) . . ? O6 Mn3 Cl1 94.94(9) . . ? O1 Mn3 Cl1 88.89(9) . . ? O5 Mn3 Cl1 95.08(10) . . ? N5 Mn3 Cl1 89.98(11) . . ? O10 Mn3 Cl1 168.87(8) . . ? Mn2 O1 Mn1 121.99(15) . . ? Mn2 O1 Mn3 119.48(15) . . ? Mn1 O1 Mn3 118.48(14) . . ? C1 O2 Mn1 125.2(3) . . ? N1 O3 Mn2 115.4(2) . . ? N1 O3 Mn2 109.8(2) . 9_656 ? Mn2 O3 Mn2 96.42(11) . 9_656 ? C8 O4 Mn2 123.8(3) . . ? N3 O5 Mn3 116.3(2) . . ? C15 O6 Mn3 124.3(3) . . ? N5 O7 Mn1 113.9(2) . . ? C22 O8 Mn1 127.3(3) . . ? C22 O8 H8A 123.9 . . ? Mn1 O8 H8A 100.4 . . ? C24 O9 Mn2 131.1(3) . . ? C24 O9 H9A 102.5 . . ? Mn2 O9 H9A 103.6 . . ? Mn3 O10 H10A 96.7 . . ? Mn3 O10 H10B 127.1 . . ? H10A O10 H10B 109.8 . . ? C7 N1 O3 114.3(3) . . ? C7 N1 Mn1 129.5(3) . . ? O3 N1 Mn1 115.7(2) . . ? C7 N2 H2A 113.8 . . ? C7 N2 H2B 123.8 . . ? H2A N2 H2B 122.0 . . ? C14 N3 O5 112.6(3) . . ? C14 N3 Mn2 128.5(3) . . ? O5 N3 Mn2 118.1(2) . . ? C14 N4 H4A 125.7 . . ? C14 N4 H4B 110.5 . . ? H4A N4 H4B 122.8 . . ? C21 N5 O7 113.3(3) . . ? C21 N5 Mn3 129.1(3) . . ? O7 N5 Mn3 117.4(2) . . ? C21 N6 H6A 112.6 . . ? C21 N6 H6B 121.9 . . ? H6A N6 H6B 122.5 . . ? O2 C1 C2 117.1(4) . . ? O2 C1 C6 124.1(4) . . ? C2 C1 C6 118.9(4) . . ? C3 C2 C1 120.8(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 121.3(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 118.7(4) . . ? C1 C6 C7 122.5(4) . . ? C5 C6 C7 118.7(4) . . ? N1 C7 N2 121.1(4) . . ? N1 C7 C6 119.4(4) . . ? N2 C7 C6 119.5(4) . . ? O4 C8 C9 117.8(4) . . ? O4 C8 C13 122.9(4) . . ? C9 C8 C13 119.3(4) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 121.1(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 119.3(5) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 121.9(5) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C8 118.3(4) . . ? C12 C13 C14 118.4(4) . . ? C8 C13 C14 123.2(4) . . ? N3 C14 N4 120.2(4) . . ? N3 C14 C13 119.6(4) . . ? N4 C14 C13 120.2(4) . . ? O6 C15 C16 118.2(4) . . ? O6 C15 C20 122.8(4) . . ? C16 C15 C20 119.0(4) . . ? C17 C16 C15 120.9(5) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 121.1(5) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 121.6(5) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C15 118.4(4) . . ? C19 C20 C21 119.9(4) . . ? C15 C20 C21 121.7(4) . . ? N5 C21 N6 119.2(4) . . ? N5 C21 C20 120.1(4) . . ? N6 C21 C20 120.7(4) . . ? O8 C22 C23 110.1(5) . . ? O8 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? O8 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O9 C24 C25 114.3(6) . . ? O9 C24 H24A 108.7 . . ? C25 C24 H24A 108.7 . . ? O9 C24 H24B 108.7 . . ? C25 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 O11 H11A 119.4 . . ? O11 C26 C27 114.5(5) . . ? O11 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? O11 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O12 76.9(17) . . ? C29 C28 C29 57(3) . 9_655 ? O12 C28 C29 121(3) . 9_655 ? C28 C29 C29 86(3) . 9_655 ? C28 C29 O12 66.5(16) . . ? C29 C29 O12 133(3) 9_655 . ? C28 C29 C28 123(3) . 9_655 ? O12 C29 C28 145(2) . 9_655 ? C31 C30 O13 120(2) . . ? C30 C31 O14 93.4(19) . . ? C30 C31 C32 110(3) . . ? O14 C31 C32 123(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.732 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.106