# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email roubeau@unizar.es _publ_contact_author_name 'O. Roubeau' loop_ _publ_author_name 'A. Escuer' 'B. Cordero' 'O. Roubeau' 'S. J. Teat' data_bc799 _database_code_depnum_ccdc_archive 'CCDC 804307' #TrackingRef '3424_web_deposit_cif_file_0_OlivierRoubeau_1291913919.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H88 Mn12 N24 O36, 4(C H4 O), 2(H2 O)' _chemical_formula_sum 'C94 H108 Mn12 N24 O42' _chemical_formula_weight 2905.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Mn Mn 0.2237 0.8587 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3924(4) _cell_length_b 14.1267(4) _cell_length_c 18.9933(6) _cell_angle_alpha 85.3010(10) _cell_angle_beta 73.1710(10) _cell_angle_gamma 66.3400(10) _cell_volume 2912.89(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 34.50 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'SADABS v2.10 Bruker AXS Madison WI US' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 38408 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 32.06 _reflns_number_total 15429 _reflns_number_gt 14116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.56a' _computing_data_reduction 'Bruker SAINT v7.56a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non hydrogens were refined anisotropically. Hydrogens were found in difference Fourier maps except those on the methyl groups of the methanol molecules. Hydrogens of the water molecules and of the hydroxyl groups of the methanol molecules, both coordinated and in the lattice, were refined freely with their thermal parameter 1.5 times that of their carrier oxygen. 1,3 H H distance restrains were used in the case of the water molecules, and a distance restrains was also used for the O8-H8 methanol hydroxyl group. The rest of hydrogens were placed geometrically on their carrier atom and refined with a riding model. ; _vrf_PLAT601_bc799 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 144.00 A**3 RESPONSE: The remaining void present in the structure at the end of the refinement was analyzed by PLATON/SQUEEZE that detected one void per cell of 143 cubic angstrom. However it only recovered 1 electron per void indicating this void in the structure is actually empty. Therefore the model was left as it was and the data was not treated with SQUEEZE. ; _vrf_PLAT042_bc799 ; PROBLEM: Calc. and Reported MoietyFormula Strings Differ ? RESPONSE: The calculated moeity formula seems to consider that one of the lattice methanol molecule of the asymmetric unit pertains to the complex which is not the case. We give the correct moeity formula with four lattice methanol molecules per cell (2 per asymmetric unit). ; _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^)+(0.0530P)^2^+1.5853P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15429 _refine_ls_number_parameters 804 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.59028(2) 0.55893(2) 0.452928(14) 0.01183(6) Uani 1 1 d . . . Mn2 Mn 0.39318(2) 0.75111(2) 0.391584(15) 0.01330(6) Uani 1 1 d . . . Mn3 Mn 0.45267(2) 0.51700(2) 0.343544(14) 0.01288(6) Uani 1 1 d . . . Mn4 Mn 0.81550(2) 0.63788(2) 0.281565(14) 0.01319(6) Uani 1 1 d . . . Mn5 Mn 0.61805(2) 0.66891(2) 0.190186(14) 0.01332(6) Uani 1 1 d . . . Mn6 Mn 0.89837(2) 0.49551(2) 0.133235(14) 0.01365(6) Uani 1 1 d . . . O1 O 0.47950(11) 0.60827(9) 0.39569(7) 0.0133(2) Uani 1 1 d . . . O2 O 0.67813(12) 0.50946(10) 0.52331(7) 0.0157(2) Uani 1 1 d . . . O3 O 0.46771(12) 0.78253(10) 0.45725(7) 0.0167(2) Uani 1 1 d . . . O4 O 0.31482(13) 0.89336(10) 0.38378(8) 0.0190(3) Uani 1 1 d . . . O5 O 0.31161(12) 0.62397(10) 0.32436(8) 0.0180(3) Uani 1 1 d . . . O6 O 0.41404(12) 0.42127(10) 0.30441(7) 0.0171(3) Uani 1 1 d . . . O7 O 0.59565(12) 0.42033(10) 0.44637(7) 0.0141(2) Uani 1 1 d . . . O8 O 0.24220(14) 0.74419(12) 0.49019(9) 0.0277(3) Uani 1 1 d D . . H8 H 0.264(3) 0.6887(17) 0.5118(16) 0.042 Uiso 1 1 d D . . O9 O 0.77797(11) 0.60149(10) 0.20094(7) 0.0142(2) Uani 1 1 d . . . O10 O 0.55842(11) 0.74119(10) 0.28696(7) 0.0149(2) Uani 1 1 d . . . O11 O 0.86628(12) 0.69819(10) 0.34311(8) 0.0184(3) Uani 1 1 d . . . O12 O 0.46515(12) 0.74032(11) 0.17387(7) 0.0198(3) Uani 1 1 d . . . O13 O 0.80031(12) 0.52714(10) 0.06753(7) 0.0178(3) Uani 1 1 d . . . O14 O 1.01900(12) 0.38525(10) 0.06752(7) 0.0176(3) Uani 1 1 d . . . H14 H 0.724(3) 0.812(2) 0.1552(15) 0.026 Uiso 1 1 d . . . O15 O 0.98030(12) 0.53773(10) 0.25196(7) 0.0174(3) Uani 1 1 d . . . O16 O 0.66636(14) 0.80731(11) 0.14529(8) 0.0210(3) Uani 1 1 d . . . O17 O 0.81534(14) 0.38484(12) 0.19342(8) 0.0222(3) Uani 1 1 d . . . H17 H 0.741(3) 0.421(2) 0.2132(16) 0.033 Uiso 1 1 d . . . O18 O 0.99682(13) 0.60142(11) 0.07540(8) 0.0187(3) Uani 1 1 d . . . H18B H 0.995(2) 0.608(2) 0.0292(16) 0.028 Uiso 1 1 d D . . H18C H 1.067(3) 0.581(2) 0.0740(15) 0.028 Uiso 1 1 d D . . N1 N 0.56236(14) 0.70307(12) 0.47608(8) 0.0146(3) Uani 1 1 d . . . N2 N 0.29624(14) 0.72469(12) 0.33329(8) 0.0153(3) Uani 1 1 d . . . N3 N 0.57205(14) 0.39873(12) 0.38352(8) 0.0136(3) Uani 1 1 d . . . N4 N 0.75419(14) 0.53120(12) 0.35940(9) 0.0169(3) Uani 1 1 d . . . N5 N 0.82196(14) 0.44023(12) 0.35448(9) 0.0168(3) Uani 1 1 d . . . N6 N 0.88338(16) 0.35334(14) 0.35097(11) 0.0260(4) Uani 1 1 d . . . N7 N 0.57120(15) 0.52936(13) 0.23300(9) 0.0187(3) Uani 1 1 d . . . N8 N 0.53161(17) 0.50675(15) 0.18500(10) 0.0249(4) Uani 1 1 d . . . N9 N 0.4958(2) 0.48707(19) 0.14123(12) 0.0381(5) Uani 1 1 d . . . N10 N 0.65117(14) 0.75408(12) 0.30703(8) 0.0143(3) Uani 1 1 d . . . N11 N 0.68694(14) 0.60796(12) 0.08673(8) 0.0152(3) Uani 1 1 d . . . N12 N 1.00736(14) 0.46311(12) 0.19968(8) 0.0151(3) Uani 1 1 d . . . C1 C 0.74966(16) 0.55056(15) 0.53972(10) 0.0159(3) Uani 1 1 d . . . C2 C 0.84899(17) 0.48526(16) 0.56526(10) 0.0193(4) Uani 1 1 d . . . H2A H 0.8693 0.4129 0.5659 0.023 Uiso 1 1 calc R . . C3 C 0.91782(19) 0.52502(18) 0.58956(11) 0.0243(4) Uani 1 1 d . . . H3A H 0.9850 0.4799 0.6067 0.029 Uiso 1 1 calc R . . C4 C 0.8888(2) 0.63156(19) 0.58901(12) 0.0276(4) Uani 1 1 d . . . H4A H 0.9350 0.6591 0.6067 0.033 Uiso 1 1 calc R . . C5 C 0.7927(2) 0.69631(17) 0.56262(11) 0.0235(4) Uani 1 1 d . . . H5A H 0.7737 0.7685 0.5618 0.028 Uiso 1 1 calc R . . C6 C 0.72214(17) 0.65750(15) 0.53689(10) 0.0175(3) Uani 1 1 d . . . C7 C 0.62234(17) 0.72981(14) 0.51063(10) 0.0171(3) Uani 1 1 d . . . H7A H 0.5992 0.8015 0.5193 0.021 Uiso 1 1 calc R . . C8 C 0.23173(17) 0.94779(14) 0.34888(10) 0.0179(3) Uani 1 1 d . . . C9 C 0.1975(2) 1.05564(15) 0.34715(11) 0.0232(4) Uani 1 1 d . . . H9A H 0.2363 1.0865 0.3687 0.028 Uiso 1 1 calc R . . C10 C 0.1081(2) 1.11695(16) 0.31441(12) 0.0265(4) Uani 1 1 d . . . H10A H 0.0868 1.1895 0.3134 0.032 Uiso 1 1 calc R . . C11 C 0.0483(2) 1.07416(17) 0.28278(12) 0.0285(5) Uani 1 1 d . . . H11A H -0.0146 1.1170 0.2614 0.034 Uiso 1 1 calc R . . C12 C 0.08243(19) 0.96878(16) 0.28316(12) 0.0252(4) Uani 1 1 d . . . H12A H 0.0426 0.9391 0.2614 0.030 Uiso 1 1 calc R . . C13 C 0.17499(17) 0.90336(14) 0.31494(11) 0.0190(4) Uani 1 1 d . . . C14 C 0.20965(17) 0.79298(14) 0.30938(10) 0.0179(3) Uani 1 1 d . . . H14A H 0.1658 0.7691 0.2866 0.021 Uiso 1 1 calc R . . C15 C 0.48466(17) 0.32372(14) 0.28277(10) 0.0163(3) Uani 1 1 d . . . C16 C 0.45535(19) 0.27680(15) 0.23226(11) 0.0213(4) Uani 1 1 d . . . H16A H 0.3885 0.3165 0.2131 0.026 Uiso 1 1 calc R . . C17 C 0.5227(2) 0.17400(17) 0.21042(12) 0.0265(4) Uani 1 1 d . . . H17A H 0.5011 0.1439 0.1766 0.032 Uiso 1 1 calc R . . C18 C 0.6218(2) 0.11356(16) 0.23706(13) 0.0281(4) Uani 1 1 d . . . H18A H 0.6679 0.0430 0.2213 0.034 Uiso 1 1 calc R . . C19 C 0.6523(2) 0.15740(15) 0.28665(11) 0.0235(4) Uani 1 1 d . . . H19A H 0.7190 0.1162 0.3056 0.028 Uiso 1 1 calc R . . C20 C 0.58589(17) 0.26257(14) 0.30969(10) 0.0168(3) Uani 1 1 d . . . C21 C 0.61737(17) 0.30198(14) 0.36492(10) 0.0162(3) Uani 1 1 d . . . H21A H 0.6740 0.2545 0.3887 0.019 Uiso 1 1 calc R . . C22 C 0.1185(2) 0.8107(2) 0.51462(15) 0.0375(6) Uani 1 1 d . . . H22A H 0.0785 0.7849 0.5597 0.056 Uiso 1 1 calc R . . H22B H 0.0782 0.8140 0.4765 0.056 Uiso 1 1 calc R . . H22C H 0.1120 0.8800 0.5248 0.056 Uiso 1 1 calc R . . C23 C 0.81657(17) 0.79300(14) 0.37280(10) 0.0171(3) Uani 1 1 d . . . C24 C 0.88470(19) 0.82332(16) 0.40737(11) 0.0214(4) Uani 1 1 d . . . H24A H 0.9659 0.7771 0.4064 0.026 Uiso 1 1 calc R . . C25 C 0.8349(2) 0.91948(16) 0.44276(12) 0.0248(4) Uani 1 1 d . . . H25A H 0.8827 0.9384 0.4655 0.030 Uiso 1 1 calc R . . C26 C 0.7154(2) 0.98950(16) 0.44568(12) 0.0251(4) Uani 1 1 d . . . H26A H 0.6808 1.0545 0.4714 0.030 Uiso 1 1 calc R . . C27 C 0.64904(19) 0.96198(15) 0.41034(11) 0.0214(4) Uani 1 1 d . . . H27A H 0.5685 1.0095 0.4111 0.026 Uiso 1 1 calc R . . C28 C 0.69751(17) 0.86518(14) 0.37303(10) 0.0168(3) Uani 1 1 d . . . C29 C 0.61886(17) 0.84099(14) 0.34088(10) 0.0161(3) Uani 1 1 d . . . H29 H 0.5387 0.8920 0.3449 0.019 Uiso 1 1 calc R . . C30 C 0.43565(17) 0.76477(15) 0.11092(10) 0.0183(3) Uani 1 1 d . . . C31 C 0.31990(19) 0.84255(16) 0.11313(12) 0.0242(4) Uani 1 1 d . . . H31A H 0.2672 0.8779 0.1585 0.029 Uiso 1 1 calc R . . C32 C 0.2818(2) 0.86824(18) 0.04984(13) 0.0287(4) Uani 1 1 d . . . H32A H 0.2030 0.9208 0.0524 0.034 Uiso 1 1 calc R . . C33 C 0.3573(2) 0.8181(2) -0.01748(13) 0.0323(5) Uani 1 1 d . . . H33A H 0.3300 0.8350 -0.0605 0.039 Uiso 1 1 calc R . . C34 C 0.4722(2) 0.74350(18) -0.02088(12) 0.0273(4) Uani 1 1 d . . . H34A H 0.5243 0.7097 -0.0669 0.033 Uiso 1 1 calc R . . C35 C 0.51408(18) 0.71622(15) 0.04229(11) 0.0195(4) Uani 1 1 d . . . C36 C 0.63568(18) 0.63662(15) 0.03395(10) 0.0183(3) Uani 1 1 d . . . H36A H 0.6806 0.6034 -0.0132 0.022 Uiso 1 1 calc R . . C37 C 1.10953(17) 0.30181(14) 0.08203(10) 0.0183(3) Uani 1 1 d . . . C38 C 1.1675(2) 0.21678(16) 0.03150(12) 0.0257(4) Uani 1 1 d . . . H38A H 1.1414 0.2199 -0.0113 0.031 Uiso 1 1 calc R . . C39 C 1.2620(2) 0.12881(18) 0.04340(14) 0.0340(5) Uani 1 1 d . . . H39A H 1.3002 0.0722 0.0086 0.041 Uiso 1 1 calc R . . C40 C 1.3017(2) 0.12195(17) 0.10547(15) 0.0340(5) Uani 1 1 d . . . H40A H 1.3657 0.0606 0.1137 0.041 Uiso 1 1 calc R . . C41 C 1.2477(2) 0.20471(16) 0.15511(13) 0.0260(4) Uani 1 1 d . . . H41A H 1.2759 0.2003 0.1972 0.031 Uiso 1 1 calc R . . C42 C 1.15139(17) 0.29579(14) 0.14471(11) 0.0192(4) Uani 1 1 d . . . C43 C 1.10221(17) 0.37995(15) 0.19878(10) 0.0183(3) Uani 1 1 d . . . H43A H 1.1425 0.3732 0.2357 0.022 Uiso 1 1 calc R . . C44 C 0.5748(2) 0.90899(18) 0.15669(17) 0.0377(6) Uani 1 1 d . . . H44A H 0.6116 0.9579 0.1340 0.057 Uiso 1 1 calc R . . H44B H 0.5387 0.9256 0.2096 0.057 Uiso 1 1 calc R . . H44C H 0.5108 0.9140 0.1343 0.057 Uiso 1 1 calc R . . C45 C 0.8169(2) 0.30279(19) 0.15299(15) 0.0355(5) Uani 1 1 d . . . H45A H 0.7775 0.2624 0.1869 0.053 Uiso 1 1 calc R . . H45B H 0.9020 0.2578 0.1283 0.053 Uiso 1 1 calc R . . H45C H 0.7723 0.3320 0.1161 0.053 Uiso 1 1 calc R . . O1S O 0.22215(15) 0.54331(13) 0.09130(9) 0.0268(3) Uani 1 1 d . . . H1S H 0.216(3) 0.552(2) 0.1337(18) 0.040 Uiso 1 1 d . . . C1S C 0.2864(3) 0.6000(2) 0.04543(15) 0.0396(6) Uani 1 1 d . . . H1S1 H 0.2515 0.6712 0.0652 0.059 Uiso 1 1 calc R . . H1S2 H 0.2786 0.6002 -0.0045 0.059 Uiso 1 1 calc R . . H1S3 H 0.3733 0.5674 0.0440 0.059 Uiso 1 1 calc R . . O1W O 0.17785(17) 0.59509(16) 0.23387(9) 0.0338(4) Uani 1 1 d . . . H1W H 0.224(3) 0.583(3) 0.2627(19) 0.051 Uiso 1 1 d D . . H2W H 0.121(3) 0.575(3) 0.2546(19) 0.051 Uiso 1 1 d D . . O2S O 0.87964(14) 0.75847(12) 0.17917(9) 0.0242(3) Uani 1 1 d . . . H2S H 0.917(3) 0.719(2) 0.1464(17) 0.036 Uiso 1 1 d . . . C2S C 0.9519(3) 0.8142(2) 0.18393(16) 0.0388(6) Uani 1 1 d . . . H2S1 H 0.9064 0.8662 0.2245 0.058 Uiso 1 1 calc R . . H2S2 H 0.9697 0.8485 0.1376 0.058 Uiso 1 1 calc R . . H2S3 H 1.0291 0.7660 0.1929 0.058 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 0.01227(12) 0.01072(12) 0.01268(12) -0.00009(9) -0.00534(9) -0.00338(9) Mn2 0.01262(13) 0.01055(12) 0.01531(13) -0.00037(9) -0.00527(10) -0.00207(10) Mn3 0.01304(13) 0.01130(12) 0.01464(13) -0.00049(9) -0.00638(10) -0.00325(10) Mn4 0.01202(12) 0.01278(13) 0.01412(13) -0.00141(9) -0.00487(9) -0.00307(10) Mn5 0.01146(12) 0.01419(13) 0.01280(13) -0.00080(9) -0.00431(9) -0.00268(10) Mn6 0.01217(13) 0.01330(13) 0.01309(13) -0.00124(9) -0.00370(9) -0.00221(10) O1 0.0135(6) 0.0122(6) 0.0141(6) 0.0003(4) -0.0059(4) -0.0036(5) O2 0.0162(6) 0.0161(6) 0.0180(6) 0.0017(5) -0.0092(5) -0.0068(5) O3 0.0178(6) 0.0107(6) 0.0193(6) -0.0017(5) -0.0086(5) -0.0005(5) O4 0.0197(6) 0.0136(6) 0.0220(7) 0.0004(5) -0.0096(5) -0.0023(5) O5 0.0190(6) 0.0129(6) 0.0243(7) 0.0000(5) -0.0109(5) -0.0052(5) O6 0.0180(6) 0.0139(6) 0.0200(6) -0.0020(5) -0.0083(5) -0.0046(5) O7 0.0168(6) 0.0141(6) 0.0133(6) -0.0005(4) -0.0075(5) -0.0055(5) O8 0.0168(7) 0.0245(7) 0.0262(8) 0.0100(6) 0.0001(6) 0.0016(6) O9 0.0126(6) 0.0141(6) 0.0144(6) -0.0012(4) -0.0045(4) -0.0029(5) O10 0.0121(6) 0.0178(6) 0.0158(6) -0.0019(5) -0.0053(5) -0.0054(5) O11 0.0179(6) 0.0156(6) 0.0209(6) -0.0044(5) -0.0081(5) -0.0029(5) O12 0.0140(6) 0.0250(7) 0.0167(6) 0.0003(5) -0.0064(5) -0.0025(5) O13 0.0128(6) 0.0187(6) 0.0166(6) -0.0042(5) -0.0043(5) 0.0001(5) O14 0.0175(6) 0.0151(6) 0.0155(6) -0.0012(5) -0.0039(5) -0.0017(5) O15 0.0143(6) 0.0185(6) 0.0183(6) -0.0043(5) -0.0050(5) -0.0040(5) O16 0.0216(7) 0.0168(6) 0.0246(7) 0.0034(5) -0.0093(6) -0.0061(5) O17 0.0204(7) 0.0222(7) 0.0227(7) -0.0005(5) -0.0034(5) -0.0087(6) O18 0.0173(6) 0.0202(7) 0.0168(6) 0.0010(5) -0.0043(5) -0.0059(5) N1 0.0156(7) 0.0133(7) 0.0143(7) 0.0004(5) -0.0050(5) -0.0047(5) N2 0.0146(7) 0.0127(7) 0.0173(7) 0.0003(5) -0.0046(5) -0.0039(5) N3 0.0158(7) 0.0141(7) 0.0114(6) -0.0002(5) -0.0053(5) -0.0052(5) N4 0.0136(7) 0.0145(7) 0.0180(7) 0.0004(5) -0.0020(6) -0.0027(6) N5 0.0134(7) 0.0192(8) 0.0170(7) 0.0004(6) -0.0044(6) -0.0054(6) N6 0.0191(8) 0.0173(8) 0.0360(10) 0.0011(7) -0.0087(7) -0.0012(6) N7 0.0168(7) 0.0192(7) 0.0172(7) 0.0013(6) -0.0017(6) -0.0065(6) N8 0.0277(9) 0.0281(9) 0.0221(8) 0.0019(7) -0.0066(7) -0.0147(7) N9 0.0518(13) 0.0507(13) 0.0273(10) 0.0046(9) -0.0160(9) -0.0330(11) N10 0.0131(7) 0.0161(7) 0.0146(7) 0.0010(5) -0.0050(5) -0.0058(5) N11 0.0129(7) 0.0147(7) 0.0164(7) -0.0002(5) -0.0040(5) -0.0039(5) N12 0.0144(7) 0.0147(7) 0.0149(7) -0.0012(5) -0.0031(5) -0.0049(6) C1 0.0149(8) 0.0210(9) 0.0132(8) 0.0013(6) -0.0046(6) -0.0082(7) C2 0.0155(8) 0.0247(9) 0.0174(8) 0.0024(7) -0.0057(7) -0.0072(7) C3 0.0198(9) 0.0361(11) 0.0205(9) 0.0050(8) -0.0096(7) -0.0127(8) C4 0.0290(11) 0.0378(12) 0.0272(10) 0.0030(9) -0.0148(9) -0.0200(9) C5 0.0313(11) 0.0262(10) 0.0213(9) 0.0019(7) -0.0116(8) -0.0170(9) C6 0.0186(8) 0.0209(9) 0.0153(8) 0.0011(6) -0.0059(6) -0.0094(7) C7 0.0211(9) 0.0168(8) 0.0148(8) -0.0004(6) -0.0058(7) -0.0081(7) C8 0.0163(8) 0.0130(8) 0.0181(8) 0.0011(6) -0.0031(6) -0.0010(6) C9 0.0253(10) 0.0147(9) 0.0241(9) -0.0006(7) -0.0059(8) -0.0031(7) C10 0.0263(10) 0.0157(9) 0.0251(10) 0.0016(7) -0.0043(8) 0.0020(8) C11 0.0247(10) 0.0212(10) 0.0288(11) 0.0053(8) -0.0100(8) 0.0025(8) C12 0.0219(10) 0.0224(10) 0.0279(10) 0.0040(8) -0.0119(8) -0.0025(8) C13 0.0158(8) 0.0151(8) 0.0212(9) 0.0025(6) -0.0057(7) -0.0011(7) C14 0.0163(8) 0.0178(8) 0.0196(9) 0.0031(6) -0.0076(7) -0.0055(7) C15 0.0179(8) 0.0161(8) 0.0153(8) -0.0013(6) -0.0040(6) -0.0073(7) C16 0.0258(9) 0.0188(9) 0.0215(9) -0.0021(7) -0.0117(7) -0.0070(7) C17 0.0332(11) 0.0236(10) 0.0261(10) -0.0054(8) -0.0133(9) -0.0099(9) C18 0.0363(12) 0.0161(9) 0.0320(11) -0.0064(8) -0.0147(9) -0.0057(8) C19 0.0304(10) 0.0148(8) 0.0241(9) -0.0015(7) -0.0121(8) -0.0044(7) C20 0.0203(8) 0.0142(8) 0.0166(8) -0.0006(6) -0.0065(7) -0.0063(7) C21 0.0182(8) 0.0134(8) 0.0164(8) 0.0010(6) -0.0073(6) -0.0042(6) C22 0.0201(10) 0.0371(13) 0.0371(13) 0.0112(10) 0.0000(9) -0.0005(9) C23 0.0187(8) 0.0164(8) 0.0167(8) -0.0006(6) -0.0050(6) -0.0072(7) C24 0.0232(9) 0.0220(9) 0.0221(9) -0.0014(7) -0.0100(7) -0.0091(8) C25 0.0290(10) 0.0231(10) 0.0282(10) -0.0030(8) -0.0130(8) -0.0121(8) C26 0.0326(11) 0.0178(9) 0.0270(10) -0.0045(7) -0.0112(8) -0.0092(8) C27 0.0239(9) 0.0160(8) 0.0233(9) -0.0016(7) -0.0075(7) -0.0058(7) C28 0.0194(8) 0.0159(8) 0.0165(8) -0.0006(6) -0.0056(6) -0.0079(7) C29 0.0161(8) 0.0145(8) 0.0167(8) 0.0011(6) -0.0046(6) -0.0051(6) C30 0.0170(8) 0.0190(8) 0.0193(9) 0.0028(7) -0.0082(7) -0.0055(7) C31 0.0189(9) 0.0248(10) 0.0241(10) 0.0014(7) -0.0079(7) -0.0027(8) C32 0.0234(10) 0.0273(11) 0.0310(11) 0.0042(8) -0.0143(8) -0.0017(8) C33 0.0302(11) 0.0388(13) 0.0253(11) 0.0078(9) -0.0161(9) -0.0066(10) C34 0.0251(10) 0.0323(11) 0.0203(10) 0.0034(8) -0.0100(8) -0.0050(9) C35 0.0180(9) 0.0211(9) 0.0190(9) 0.0029(7) -0.0078(7) -0.0060(7) C36 0.0189(9) 0.0193(8) 0.0152(8) -0.0004(6) -0.0044(6) -0.0063(7) C37 0.0171(8) 0.0140(8) 0.0194(9) 0.0012(6) -0.0025(7) -0.0038(7) C38 0.0286(10) 0.0196(9) 0.0221(10) -0.0020(7) -0.0067(8) -0.0024(8) C39 0.0335(12) 0.0198(10) 0.0363(12) -0.0072(9) -0.0094(10) 0.0031(9) C40 0.0301(11) 0.0185(10) 0.0435(13) -0.0043(9) -0.0147(10) 0.0042(8) C41 0.0231(10) 0.0187(9) 0.0325(11) 0.0022(8) -0.0124(8) -0.0015(8) C42 0.0169(8) 0.0141(8) 0.0224(9) 0.0011(7) -0.0048(7) -0.0023(7) C43 0.0164(8) 0.0187(8) 0.0194(9) 0.0022(7) -0.0071(7) -0.0055(7) C44 0.0379(13) 0.0188(10) 0.0607(17) 0.0065(10) -0.0251(12) -0.0088(9) C45 0.0384(13) 0.0284(11) 0.0397(13) -0.0058(10) -0.0016(10) -0.0182(10) O1S 0.0262(8) 0.0348(8) 0.0215(7) -0.0020(6) -0.0067(6) -0.0136(7) C1S 0.0440(15) 0.0505(16) 0.0341(13) 0.0029(11) -0.0101(11) -0.0294(13) O1W 0.0300(9) 0.0574(12) 0.0255(8) 0.0028(7) -0.0119(7) -0.0262(8) O2S 0.0219(7) 0.0242(7) 0.0256(7) -0.0058(6) -0.0040(6) -0.0087(6) C2S 0.0372(13) 0.0376(13) 0.0474(15) -0.0033(11) -0.0114(11) -0.0200(11) _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 1.8772(12) . ? Mn1 O2 1.8814(13) . ? Mn1 O7 1.9452(13) . ? Mn1 N1 1.9882(15) . ? Mn1 N4 2.1957(15) . ? Mn1 O7 2.4599(13) 2_666 ? Mn2 O4 1.8633(13) . ? Mn2 O1 1.8740(13) . ? Mn2 O3 1.9215(13) . ? Mn2 N2 2.0014(16) . ? Mn2 O8 2.2595(15) . ? Mn2 O10 2.3708(13) . ? Mn2 Mn3 3.2344(4) . ? Mn3 O1 1.8703(13) . ? Mn3 O6 1.8710(13) . ? Mn3 O5 1.9054(13) . ? Mn3 N3 2.0038(15) . ? Mn3 N7 2.2263(16) . ? Mn4 O11 1.8729(14) . ? Mn4 O9 1.8865(13) . ? Mn4 O15 1.9065(13) . ? Mn4 N10 1.9880(15) . ? Mn4 N4 2.2221(16) . ? Mn5 O12 1.8598(14) . ? Mn5 O9 1.8878(13) . ? Mn5 O10 1.9704(13) . ? Mn5 N11 2.0117(15) . ? Mn5 N7 2.2951(16) . ? Mn5 O16 2.2975(15) . ? Mn6 O9 1.8796(13) . ? Mn6 O13 1.8933(13) . ? Mn6 O14 1.8942(13) . ? Mn6 N12 2.0056(16) . ? Mn6 O17 2.2642(15) . ? Mn6 O18 2.3138(14) . ? O2 C1 1.350(2) . ? O3 N1 1.3725(19) . ? O4 C8 1.329(2) . ? O5 N2 1.3759(19) . ? O6 C15 1.323(2) . ? O7 N3 1.3917(18) . ? O7 Mn1 2.4599(13) 2_666 ? O8 C22 1.397(3) . ? O8 H8 0.836(18) . ? O10 N10 1.3902(19) . ? O11 C23 1.323(2) . ? O12 C30 1.329(2) . ? O13 N11 1.3764(19) . ? O14 C37 1.337(2) . ? O15 N12 1.3801(19) . ? O16 C44 1.413(3) . ? O16 H14 0.82(3) . ? O17 C45 1.433(3) . ? O17 H17 0.84(3) . ? O18 H18B 0.88(3) . ? O18 H18C 0.80(3) . ? N1 C7 1.294(2) . ? N2 C14 1.292(2) . ? N3 C21 1.287(2) . ? N4 N5 1.214(2) . ? N5 N6 1.151(2) . ? N7 N8 1.267(2) . ? N8 N9 1.147(3) . ? N10 C29 1.291(2) . ? N11 C36 1.292(2) . ? N12 C43 1.283(2) . ? C1 C2 1.401(2) . ? C1 C6 1.409(3) . ? C2 C3 1.382(3) . ? C2 H2A 0.9500 . ? C3 C4 1.400(3) . ? C3 H3A 0.9500 . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 C6 1.407(3) . ? C5 H5A 0.9500 . ? C6 C7 1.443(3) . ? C7 H7A 0.9500 . ? C8 C9 1.408(3) . ? C8 C13 1.410(3) . ? C9 C10 1.380(3) . ? C9 H9A 0.9500 . ? C10 C11 1.397(3) . ? C10 H10A 0.9500 . ? C11 C12 1.375(3) . ? C11 H11A 0.9500 . ? C12 C13 1.412(3) . ? C12 H12A 0.9500 . ? C13 C14 1.446(3) . ? C14 H14A 0.9500 . ? C15 C16 1.411(3) . ? C15 C20 1.418(3) . ? C16 C17 1.380(3) . ? C16 H16A 0.9500 . ? C17 C18 1.393(3) . ? C17 H17A 0.9500 . ? C18 C19 1.379(3) . ? C18 H18A 0.9500 . ? C19 C20 1.412(3) . ? C19 H19A 0.9500 . ? C20 C21 1.439(2) . ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.409(3) . ? C23 C28 1.416(3) . ? C24 C25 1.384(3) . ? C24 H24A 0.9500 . ? C25 C26 1.401(3) . ? C25 H25A 0.9500 . ? C26 C27 1.377(3) . ? C26 H26A 0.9500 . ? C27 C28 1.409(3) . ? C27 H27A 0.9500 . ? C28 C29 1.444(3) . ? C29 H29 0.9500 . ? C30 C31 1.405(3) . ? C30 C35 1.411(3) . ? C31 C32 1.385(3) . ? C31 H31A 0.9500 . ? C32 C33 1.392(3) . ? C32 H32A 0.9500 . ? C33 C34 1.376(3) . ? C33 H33A 0.9500 . ? C34 C35 1.408(3) . ? C34 H34A 0.9500 . ? C35 C36 1.446(3) . ? C36 H36A 0.9500 . ? C37 C38 1.406(3) . ? C37 C42 1.414(3) . ? C38 C39 1.380(3) . ? C38 H38A 0.9500 . ? C39 C40 1.386(4) . ? C39 H39A 0.9500 . ? C40 C41 1.375(3) . ? C40 H40A 0.9500 . ? C41 C42 1.407(3) . ? C41 H41A 0.9500 . ? C42 C43 1.448(3) . ? C43 H43A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O1S C1S 1.424(3) . ? O1S H1S 0.80(3) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O1W H1W 0.86(3) . ? O1W H2W 0.84(4) . ? O2S C2S 1.433(3) . ? O2S H2S 0.78(3) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 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 O1 Mn1 O2 170.24(6) . . ? O1 Mn1 O7 90.43(5) . . ? O2 Mn1 O7 87.20(5) . . ? O1 Mn1 N1 90.37(6) . . ? O2 Mn1 N1 90.34(6) . . ? O7 Mn1 N1 170.02(6) . . ? O1 Mn1 N4 94.82(6) . . ? O2 Mn1 N4 94.79(6) . . ? O7 Mn1 N4 94.05(6) . . ? N1 Mn1 N4 95.80(6) . . ? O1 Mn1 O7 83.41(5) . 2_666 ? O2 Mn1 O7 86.88(5) . 2_666 ? O7 Mn1 O7 82.04(5) . 2_666 ? N1 Mn1 O7 88.17(5) . 2_666 ? N4 Mn1 O7 175.68(5) . 2_666 ? O4 Mn2 O1 176.92(6) . . ? O4 Mn2 O3 86.93(6) . . ? O1 Mn2 O3 92.61(5) . . ? O4 Mn2 N2 90.88(6) . . ? O1 Mn2 N2 89.93(6) . . ? O3 Mn2 N2 172.92(6) . . ? O4 Mn2 O8 93.61(6) . . ? O1 Mn2 O8 89.43(6) . . ? O3 Mn2 O8 88.97(6) . . ? N2 Mn2 O8 84.44(6) . . ? O4 Mn2 O10 91.61(5) . . ? O1 Mn2 O10 85.37(5) . . ? O3 Mn2 O10 92.70(5) . . ? N2 Mn2 O10 94.09(5) . . ? O8 Mn2 O10 174.60(5) . . ? O4 Mn2 Mn3 150.18(4) . . ? O1 Mn2 Mn3 30.22(4) . . ? O3 Mn2 Mn3 122.82(4) . . ? N2 Mn2 Mn3 59.85(4) . . ? O8 Mn2 Mn3 89.35(4) . . ? O10 Mn2 Mn3 85.43(3) . . ? O1 Mn3 O6 171.87(6) . . ? O1 Mn3 O5 92.40(6) . . ? O6 Mn3 O5 88.43(6) . . ? O1 Mn3 N3 88.87(6) . . ? O6 Mn3 N3 88.49(6) . . ? O5 Mn3 N3 166.64(6) . . ? O1 Mn3 N7 97.89(6) . . ? O6 Mn3 N7 90.17(6) . . ? O5 Mn3 N7 91.73(6) . . ? N3 Mn3 N7 101.27(6) . . ? O1 Mn3 Mn2 30.29(4) . . ? O6 Mn3 Mn2 151.20(4) . . ? O5 Mn3 Mn2 62.80(4) . . ? N3 Mn3 Mn2 119.14(4) . . ? N7 Mn3 Mn2 91.94(4) . . ? O11 Mn4 O9 164.34(6) . . ? O11 Mn4 O15 87.15(6) . . ? O9 Mn4 O15 92.35(5) . . ? O11 Mn4 N10 90.14(6) . . ? O9 Mn4 N10 88.66(6) . . ? O15 Mn4 N10 173.49(6) . . ? O11 Mn4 N4 99.73(6) . . ? O9 Mn4 N4 95.93(6) . . ? O15 Mn4 N4 92.15(6) . . ? N10 Mn4 N4 94.14(6) . . ? O12 Mn5 O9 175.81(6) . . ? O12 Mn5 O10 90.49(6) . . ? O9 Mn5 O10 91.27(5) . . ? O12 Mn5 N11 90.24(6) . . ? O9 Mn5 N11 87.56(6) . . ? O10 Mn5 N11 173.18(6) . . ? O12 Mn5 N7 92.05(6) . . ? O9 Mn5 N7 91.55(6) . . ? O10 Mn5 N7 95.76(6) . . ? N11 Mn5 N7 90.99(6) . . ? O12 Mn5 O16 87.97(6) . . ? O9 Mn5 O16 88.39(5) . . ? O10 Mn5 O16 85.23(5) . . ? N11 Mn5 O16 88.01(6) . . ? N7 Mn5 O16 179.00(6) . . ? O9 Mn6 O13 92.25(6) . . ? O9 Mn6 O14 177.98(6) . . ? O13 Mn6 O14 88.64(6) . . ? O9 Mn6 N12 88.90(6) . . ? O13 Mn6 N12 177.73(6) . . ? O14 Mn6 N12 90.28(6) . . ? O9 Mn6 O17 88.91(6) . . ? O13 Mn6 O17 91.68(6) . . ? O14 Mn6 O17 89.25(6) . . ? N12 Mn6 O17 90.30(6) . . ? O9 Mn6 O18 92.69(5) . . ? O13 Mn6 O18 92.64(6) . . ? O14 Mn6 O18 89.08(5) . . ? N12 Mn6 O18 85.36(6) . . ? O17 Mn6 O18 175.34(6) . . ? Mn3 O1 Mn2 119.49(7) . . ? Mn3 O1 Mn1 121.00(7) . . ? Mn2 O1 Mn1 119.50(7) . . ? C1 O2 Mn1 125.31(11) . . ? N1 O3 Mn2 118.08(10) . . ? C8 O4 Mn2 131.01(12) . . ? N2 O5 Mn3 117.74(10) . . ? C15 O6 Mn3 128.41(12) . . ? N3 O7 Mn1 114.68(10) . . ? N3 O7 Mn1 105.13(9) . 2_666 ? Mn1 O7 Mn1 97.96(5) . 2_666 ? C22 O8 Mn2 130.68(13) . . ? C22 O8 H8 117(2) . . ? Mn2 O8 H8 112(2) . . ? Mn6 O9 Mn4 119.95(7) . . ? Mn6 O9 Mn5 120.20(7) . . ? Mn4 O9 Mn5 119.82(7) . . ? N10 O10 Mn5 112.40(10) . . ? N10 O10 Mn2 111.10(9) . . ? Mn5 O10 Mn2 131.58(6) . . ? C23 O11 Mn4 130.27(12) . . ? C30 O12 Mn5 129.80(12) . . ? N11 O13 Mn6 118.15(10) . . ? C37 O14 Mn6 128.01(12) . . ? N12 O15 Mn4 117.19(10) . . ? C44 O16 Mn5 120.58(14) . . ? C44 O16 H14 105(2) . . ? Mn5 O16 H14 117(2) . . ? C45 O17 Mn6 119.67(13) . . ? C45 O17 H17 106(2) . . ? Mn6 O17 H17 106(2) . . ? Mn6 O18 H18B 109.6(18) . . ? Mn6 O18 H18C 115(2) . . ? H18B O18 H18C 106(2) . . ? C7 N1 O3 115.91(15) . . ? C7 N1 Mn1 125.87(13) . . ? O3 N1 Mn1 118.14(11) . . ? C14 N2 O5 114.83(15) . . ? C14 N2 Mn2 127.01(13) . . ? O5 N2 Mn2 117.69(11) . . ? C21 N3 O7 114.56(14) . . ? C21 N3 Mn3 128.17(13) . . ? O7 N3 Mn3 116.52(10) . . ? N5 N4 Mn1 109.71(12) . . ? N5 N4 Mn4 118.33(12) . . ? Mn1 N4 Mn4 131.87(7) . . ? N6 N5 N4 178.0(2) . . ? N8 N7 Mn3 107.91(12) . . ? N8 N7 Mn5 105.95(12) . . ? Mn3 N7 Mn5 126.75(8) . . ? N9 N8 N7 179.4(2) . . ? C29 N10 O10 115.16(15) . . ? C29 N10 Mn4 127.85(13) . . ? O10 N10 Mn4 116.99(11) . . ? C36 N11 O13 114.20(15) . . ? C36 N11 Mn5 126.79(13) . . ? O13 N11 Mn5 119.00(11) . . ? C43 N12 O15 115.13(15) . . ? C43 N12 Mn6 127.13(13) . . ? O15 N12 Mn6 117.74(11) . . ? O2 C1 C2 118.43(16) . . ? O2 C1 C6 121.98(16) . . ? C2 C1 C6 119.43(17) . . ? C3 C2 C1 120.71(19) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 120.22(19) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 119.52(19) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 121.27(19) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 118.80(18) . . ? C5 C6 C7 118.25(17) . . ? C1 C6 C7 122.92(17) . . ? N1 C7 C6 124.09(17) . . ? N1 C7 H7A 118.0 . . ? C6 C7 H7A 118.0 . . ? O4 C8 C9 117.91(18) . . ? O4 C8 C13 123.41(16) . . ? C9 C8 C13 118.67(18) . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 121.10(19) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C12 C11 C10 118.65(19) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? C11 C12 C13 121.9(2) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C8 C13 C12 118.94(18) . . ? C8 C13 C14 122.86(17) . . ? C12 C13 C14 118.18(19) . . ? N2 C14 C13 124.34(18) . . ? N2 C14 H14A 117.8 . . ? C13 C14 H14A 117.8 . . ? O6 C15 C16 118.42(17) . . ? O6 C15 C20 123.40(16) . . ? C16 C15 C20 118.13(17) . . ? C17 C16 C15 120.75(19) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 121.26(19) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C18 C17 119.20(19) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 120.98(19) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C19 C20 C15 119.66(17) . . ? C19 C20 C21 118.24(17) . . ? C15 C20 C21 121.88(16) . . ? N3 C21 C20 122.84(16) . . ? N3 C21 H21A 118.6 . . ? C20 C21 H21A 118.6 . . ? 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 . . ? O11 C23 C24 118.31(17) . . ? O11 C23 C28 123.62(17) . . ? C24 C23 C28 118.05(17) . . ? C25 C24 C23 120.88(19) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 121.21(19) . . ? C24 C25 H25A 119.4 . . ? C26 C25 H25A 119.4 . . ? C27 C26 C25 118.48(18) . . ? C27 C26 H26A 120.8 . . ? C25 C26 H26A 120.8 . . ? C26 C27 C28 121.73(19) . . ? C26 C27 H27A 119.1 . . ? C28 C27 H27A 119.1 . . ? C27 C28 C23 119.56(17) . . ? C27 C28 C29 117.79(17) . . ? C23 C28 C29 122.49(16) . . ? N10 C29 C28 123.80(17) . . ? N10 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? O12 C30 C31 118.09(18) . . ? O12 C30 C35 123.43(17) . . ? C31 C30 C35 118.47(18) . . ? C32 C31 C30 120.7(2) . . ? C32 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? C31 C32 C33 120.9(2) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C34 C33 C32 119.1(2) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 C35 121.5(2) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C34 C35 C30 119.31(18) . . ? C34 C35 C36 117.90(18) . . ? C30 C35 C36 122.76(17) . . ? N11 C36 C35 123.96(17) . . ? N11 C36 H36A 118.0 . . ? C35 C36 H36A 118.0 . . ? O14 C37 C38 118.17(18) . . ? O14 C37 C42 123.29(17) . . ? C38 C37 C42 118.53(18) . . ? C39 C38 C37 120.7(2) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C38 C39 C40 120.9(2) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? C41 C40 C39 119.5(2) . . ? C41 C40 H40A 120.3 . . ? C39 C40 H40A 120.3 . . ? C40 C41 C42 121.3(2) . . ? C40 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C41 C42 C37 119.13(18) . . ? C41 C42 C43 117.45(18) . . ? C37 C42 C43 123.40(17) . . ? N12 C43 C42 123.71(18) . . ? N12 C43 H43A 118.1 . . ? C42 C43 H43A 118.1 . . ? O16 C44 H44A 109.5 . . ? O16 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O16 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O17 C45 H45A 109.5 . . ? O17 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O17 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C1S O1S H1S 111(2) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? H1W O1W H2W 108(3) . . ? C2S O2S H2S 107(2) . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 32.06 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.004 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.096