# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_comp _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C280 H200 Mn19 O80' _chemical_formula_weight 5888.26 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 38.8251(2) _cell_length_b 17.6702(2) _cell_length_c 19.4001(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13309.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'claret ' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5990 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.766 _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29808 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.49 _reflns_number_total 29808 _reflns_number_gt 27733 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+71.8346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(4) _refine_ls_number_reflns 29808 _refine_ls_number_parameters 1684 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1549 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 2.263 _refine_ls_shift/su_max 0.006 _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 C1 C 0.3814(4) 0.2361(9) 0.9049(8) 0.037(3) Uani 1 1 d . . . C2 C 0.3478(4) 0.2715(9) 0.9214(7) 0.034(3) Uani 1 1 d . . . C3 C 0.3463(4) 0.3402(10) 0.9564(8) 0.042(4) Uani 1 1 d . . . H3 H 0.3669 0.3656 0.9689 0.051 Uiso 1 1 calc R . . C4 C 0.3146(5) 0.3719(11) 0.9730(8) 0.047(4) Uani 1 1 d . . . H4 H 0.3134 0.4182 0.9978 0.056 Uiso 1 1 calc R . . C5 C 0.2843(5) 0.3349(10) 0.9531(8) 0.043(4) Uani 1 1 d . . . H5 H 0.2626 0.3565 0.9641 0.052 Uiso 1 1 calc R . . C6 C 0.2858(4) 0.2665(10) 0.9169(9) 0.043(4) Uani 1 1 d . . . H6 H 0.2652 0.2415 0.9038 0.052 Uiso 1 1 calc R . . C7 C 0.3172(4) 0.2357(8) 0.9005(7) 0.033(3) Uani 1 1 d . . . H7 H 0.3182 0.1899 0.8749 0.040 Uiso 1 1 calc R . . C8 C 0.3224(5) 0.2976(8) 0.7074(7) 0.038(4) Uani 1 1 d . . . C9 C 0.3089(4) 0.3737(8) 0.7291(8) 0.035(3) Uani 1 1 d . . . C10 C 0.3215(5) 0.4062(9) 0.7890(8) 0.046(4) Uani 1 1 d . . . H10 H 0.3388 0.3811 0.8150 0.056 Uiso 1 1 calc R . . C11 C 0.3088(5) 0.4752(10) 0.8106(9) 0.052(5) Uani 1 1 d . . . H11 H 0.3174 0.4973 0.8518 0.063 Uiso 1 1 calc R . . C12 C 0.2842(5) 0.5120(10) 0.7738(9) 0.055(5) Uani 1 1 d . . . H12 H 0.2757 0.5594 0.7891 0.066 Uiso 1 1 calc R . . C13 C 0.2717(5) 0.4796(10) 0.7135(10) 0.052(5) Uani 1 1 d . . . H13 H 0.2546 0.5053 0.6872 0.063 Uiso 1 1 calc R . . C14 C 0.2839(4) 0.4097(9) 0.6916(9) 0.041(4) Uani 1 1 d . . . H14 H 0.2750 0.3871 0.6509 0.049 Uiso 1 1 calc R . . C15 C 0.4319(3) 0.0424(9) 0.7796(7) 0.030(3) Uani 1 1 d . . . C16 C 0.4383(3) -0.0351(8) 0.7513(8) 0.031(3) Uani 1 1 d . . . C17 C 0.4155(5) -0.0643(10) 0.7028(10) 0.051(5) Uani 1 1 d . . . H17 H 0.3963 -0.0354 0.6877 0.062 Uiso 1 1 calc R . . C18 C 0.4213(6) -0.1371(11) 0.6764(13) 0.075(7) Uani 1 1 d . . . H18 H 0.4056 -0.1585 0.6442 0.090 Uiso 1 1 calc R . . C19 C 0.4497(6) -0.1774(11) 0.6973(14) 0.077(8) Uani 1 1 d . . . H19 H 0.4537 -0.2266 0.6790 0.093 Uiso 1 1 calc R . . C20 C 0.4722(5) -0.1482(11) 0.7435(13) 0.067(6) Uani 1 1 d . . . H20 H 0.4918 -0.1767 0.7573 0.081 Uiso 1 1 calc R . . C21 C 0.4666(4) -0.0766(10) 0.7708(9) 0.046(4) Uani 1 1 d . . . H21 H 0.4825 -0.0562 0.8032 0.055 Uiso 1 1 calc R . . C22 C 0.3929(3) 0.2203(8) 0.5878(7) 0.027(3) Uani 1 1 d . . . C23 C 0.4305(4) 0.2048(11) 0.5742(8) 0.045(4) Uani 1 1 d . . . C24 C 0.4483(5) 0.2539(17) 0.5325(10) 0.078(8) Uani 1 1 d . . . H24 H 0.4370 0.2959 0.5118 0.094 Uiso 1 1 calc R . . C25 C 0.4829(6) 0.241(3) 0.5213(15) 0.149(19) Uani 1 1 d . . . H25 H 0.4956 0.2754 0.4934 0.179 Uiso 1 1 calc R . . C26 C 0.4991(8) 0.181(3) 0.5492(17) 0.18(2) Uani 1 1 d . . . H26 H 0.5232 0.1752 0.5431 0.214 Uiso 1 1 calc R . . C27 C 0.4801(7) 0.127(2) 0.5878(15) 0.126(15) Uani 1 1 d . . . H27 H 0.4909 0.0817 0.6038 0.151 Uiso 1 1 calc R . . C28 C 0.4455(5) 0.1406(15) 0.6015(11) 0.072(7) Uani 1 1 d . . . H28 H 0.4324 0.1067 0.6290 0.087 Uiso 1 1 calc R . . C36 C 0.2808(3) 0.1717(7) 0.5217(7) 0.026(3) Uani 1 1 d . . . C37 C 0.2565(4) 0.1812(8) 0.4641(7) 0.030(3) Uani 1 1 d . . . C38 C 0.2219(4) 0.1612(9) 0.4710(9) 0.042(4) Uani 1 1 d . . . H38 H 0.2135 0.1431 0.5139 0.050 Uiso 1 1 calc R . . C39 C 0.2002(4) 0.1676(11) 0.4158(10) 0.050(4) Uani 1 1 d . . . H39 H 0.1766 0.1545 0.4209 0.060 Uiso 1 1 calc R . . C40 C 0.2119(5) 0.1924(10) 0.3544(9) 0.047(4) Uani 1 1 d . . . H40 H 0.1965 0.1960 0.3164 0.057 Uiso 1 1 calc R . . C41 C 0.2462(5) 0.2127(10) 0.3462(8) 0.045(4) Uani 1 1 d . . . H41 H 0.2544 0.2296 0.3027 0.054 Uiso 1 1 calc R . . C42 C 0.2681(4) 0.2082(8) 0.4015(7) 0.033(3) Uani 1 1 d . . . H42 H 0.2914 0.2238 0.3966 0.039 Uiso 1 1 calc R . . C43 C 0.3615(3) 0.3375(7) 0.3874(6) 0.023(3) Uani 1 1 d . . . C44 C 0.3842(3) 0.2708(8) 0.3789(7) 0.028(3) Uani 1 1 d . . . C45 C 0.3751(4) 0.2007(8) 0.4066(7) 0.029(3) Uani 1 1 d . . . H45 H 0.3549 0.1961 0.4338 0.035 Uiso 1 1 calc R . . C46 C 0.3956(4) 0.1375(8) 0.3945(9) 0.040(4) Uani 1 1 d . . . H46 H 0.3890 0.0896 0.4122 0.048 Uiso 1 1 calc R . . C47 C 0.4259(4) 0.1446(10) 0.3564(11) 0.053(5) Uani 1 1 d . . . H47 H 0.4402 0.1018 0.3483 0.064 Uiso 1 1 calc R . . C48 C 0.4349(5) 0.2148(11) 0.3309(11) 0.054(5) Uani 1 1 d . . . H48 H 0.4558 0.2201 0.3061 0.065 Uiso 1 1 calc R . . C49 C 0.4141(4) 0.2776(9) 0.3404(8) 0.036(3) Uani 1 1 d . . . H49 H 0.4203 0.3249 0.3208 0.043 Uiso 1 1 calc R . . C50 C 0.2598(3) 0.4139(8) 0.5121(7) 0.027(3) Uani 1 1 d . . . C51 C 0.2278(3) 0.4238(8) 0.5527(7) 0.028(3) Uani 1 1 d . . . C52 C 0.2125(4) 0.3621(9) 0.5861(8) 0.037(3) Uani 1 1 d . . . H52 H 0.2226 0.3133 0.5821 0.044 Uiso 1 1 calc R . . C53 C 0.1829(4) 0.3708(11) 0.6246(10) 0.054(5) Uani 1 1 d . . . H53 H 0.1720 0.3280 0.6446 0.065 Uiso 1 1 calc R . . C54 C 0.1695(4) 0.4426(11) 0.6338(9) 0.051(4) Uani 1 1 d . . . H54 H 0.1492 0.4491 0.6604 0.061 Uiso 1 1 calc R . . C55 C 0.1852(4) 0.5048(10) 0.6047(8) 0.043(4) Uani 1 1 d . . . H55 H 0.1763 0.5540 0.6129 0.052 Uiso 1 1 calc R . . C56 C 0.2141(4) 0.4956(9) 0.5636(7) 0.032(3) Uani 1 1 d . . . H56 H 0.2246 0.5385 0.5428 0.038 Uiso 1 1 calc R . . C57 C 0.3524(3) 0.4847(8) 0.5455(7) 0.029(3) Uani 1 1 d . . . C58 C 0.3688(4) 0.5415(9) 0.5921(8) 0.039(4) Uani 1 1 d . . . C59 C 0.3881(5) 0.6016(10) 0.5666(10) 0.050(4) Uani 1 1 d . . . H59 H 0.3923 0.6055 0.5184 0.061 Uiso 1 1 calc R . . C60 C 0.4012(6) 0.6551(12) 0.6105(11) 0.071(7) Uani 1 1 d . . . H60 H 0.4153 0.6945 0.5928 0.085 Uiso 1 1 calc R . . C61 C 0.3941(8) 0.6525(17) 0.6805(13) 0.102(11) Uani 1 1 d . . . H61 H 0.4020 0.6911 0.7106 0.123 Uiso 1 1 calc R . . C62 C 0.3751(9) 0.5921(19) 0.7050(13) 0.125(14) Uani 1 1 d . . . H62 H 0.3709 0.5882 0.7531 0.150 Uiso 1 1 calc R . . C63 C 0.3621(6) 0.5368(11) 0.6611(9) 0.060(6) Uani 1 1 d . . . H63 H 0.3488 0.4962 0.6790 0.072 Uiso 1 1 calc R . . C64 C 0.1677(4) 0.4861(8) 0.4278(7) 0.030(3) Uani 1 1 d . . . C65 C 0.1436(4) 0.4291(8) 0.4567(8) 0.034(3) Uani 1 1 d . . . C66 C 0.1528(4) 0.3524(9) 0.4613(10) 0.048(4) Uani 1 1 d . . . H66 H 0.1742 0.3357 0.4435 0.057 Uiso 1 1 calc R . . C67 C 0.1305(5) 0.3014(12) 0.4917(14) 0.076(8) Uani 1 1 d . . . H67 H 0.1371 0.2499 0.4967 0.091 Uiso 1 1 calc R . . C68 C 0.0988(6) 0.3253(17) 0.5149(16) 0.098(10) Uani 1 1 d . . . H68 H 0.0830 0.2893 0.5329 0.118 Uiso 1 1 calc R . . C69 C 0.0897(6) 0.4001(15) 0.5123(15) 0.086(8) Uani 1 1 d . . . H69 H 0.0682 0.4163 0.5308 0.103 Uiso 1 1 calc R . . C70 C 0.1120(4) 0.4522(11) 0.4825(10) 0.049(4) Uani 1 1 d . . . H70 H 0.1055 0.5039 0.4798 0.059 Uiso 1 1 calc R . . C71 C 0.3127(3) 0.5810(7) 0.3227(6) 0.023(2) Uani 1 1 d . . . C72 C 0.3116(4) 0.6491(8) 0.2764(7) 0.032(3) Uani 1 1 d . . . C73 C 0.2835(4) 0.6984(9) 0.2797(10) 0.043(4) Uani 1 1 d . . . H73 H 0.2656 0.6890 0.3118 0.052 Uiso 1 1 calc R . . C74 C 0.2816(5) 0.7597(10) 0.2374(12) 0.058(5) Uani 1 1 d . . . H74 H 0.2625 0.7931 0.2399 0.070 Uiso 1 1 calc R . . C75 C 0.3074(7) 0.7724(11) 0.1913(10) 0.072(7) Uani 1 1 d . . . H75 H 0.3058 0.8142 0.1608 0.086 Uiso 1 1 calc R . . C76 C 0.3365(7) 0.7245(11) 0.1883(11) 0.072(7) Uani 1 1 d . . . H76 H 0.3550 0.7355 0.1578 0.087 Uiso 1 1 calc R . . C77 C 0.3377(5) 0.6617(9) 0.2298(9) 0.051(5) Uani 1 1 d . . . H77 H 0.3564 0.6272 0.2264 0.061 Uiso 1 1 calc R . . C78 C 0.1951(4) 0.5697(7) 0.2508(7) 0.029(3) Uani 1 1 d . . . C79 C 0.1929(4) 0.5411(8) 0.1788(7) 0.030(3) Uani 1 1 d . . . C80 C 0.1608(4) 0.5322(7) 0.1471(7) 0.032(3) Uani 1 1 d . . . H80 H 0.1404 0.5428 0.1722 0.039 Uiso 1 1 calc R . . C81 C 0.1587(5) 0.5081(9) 0.0796(8) 0.042(4) Uani 1 1 d . . . H81 H 0.1368 0.5025 0.0582 0.051 Uiso 1 1 calc R . . C82 C 0.1886(6) 0.4919(10) 0.0426(9) 0.057(5) Uani 1 1 d . . . H82 H 0.1873 0.4752 -0.0039 0.069 Uiso 1 1 calc R . . C83 C 0.2205(5) 0.5005(10) 0.0747(8) 0.047(4) Uani 1 1 d . . . H83 H 0.2410 0.4895 0.0499 0.056 Uiso 1 1 calc R . . C84 C 0.2225(4) 0.5249(9) 0.1421(7) 0.036(3) Uani 1 1 d . . . H84 H 0.2444 0.5305 0.1635 0.043 Uiso 1 1 calc R . . C85 C 0.2786(3) 0.3945(7) 0.2796(7) 0.025(3) Uani 1 1 d . . . C86 C 0.2487(3) 0.3675(7) 0.2362(7) 0.026(3) Uani 1 1 d . . . C87 C 0.2151(3) 0.3708(7) 0.2612(8) 0.029(3) Uani 1 1 d . . . H87 H 0.2106 0.3911 0.3056 0.035 Uiso 1 1 calc R . . C88 C 0.1880(4) 0.3439(8) 0.2206(9) 0.040(4) Uani 1 1 d . . . H88 H 0.1652 0.3453 0.2379 0.048 Uiso 1 1 calc R . . C89 C 0.1942(4) 0.3156(9) 0.1563(9) 0.043(4) Uani 1 1 d . . . H89 H 0.1757 0.2977 0.1289 0.052 Uiso 1 1 calc R . . C90 C 0.2280(4) 0.3132(10) 0.1307(9) 0.046(4) Uani 1 1 d . . . H90 H 0.2323 0.2944 0.0857 0.055 Uiso 1 1 calc R . . C91 C 0.2552(4) 0.3384(8) 0.1717(7) 0.034(3) Uani 1 1 d . . . H91 H 0.2782 0.3356 0.1550 0.041 Uiso 1 1 calc R . . C92 C 0.3547(4) 0.5131(9) 0.1052(7) 0.037(3) Uani 1 1 d . . . C93 C 0.3374(4) 0.5570(8) 0.0500(7) 0.035(3) Uani 1 1 d . . . C94 C 0.3044(4) 0.5855(10) 0.0600(9) 0.045(4) Uani 1 1 d . . . H94 H 0.2936 0.5788 0.1035 0.054 Uiso 1 1 calc R . . C95 C 0.2867(6) 0.6238(11) 0.0078(11) 0.059(5) Uani 1 1 d . . . H95 H 0.2637 0.6407 0.0139 0.070 Uiso 1 1 calc R . . C96 C 0.3043(6) 0.6359(9) -0.0531(9) 0.051(5) Uani 1 1 d . . . H96 H 0.2933 0.6634 -0.0890 0.061 Uiso 1 1 calc R . . C97 C 0.3366(6) 0.6101(10) -0.0634(9) 0.052(5) Uani 1 1 d . . . H97 H 0.3477 0.6189 -0.1063 0.062 Uiso 1 1 calc R . . C98 C 0.3536(5) 0.5708(9) -0.0122(8) 0.038(3) Uani 1 1 d . . . H98 H 0.3765 0.5534 -0.0197 0.046 Uiso 1 1 calc R . . C99 C 0.4353(3) 0.5109(7) 0.2447(7) 0.028(3) Uani 1 1 d . . . C100 C 0.4452(5) 0.5721(13) 0.2924(10) 0.061(6) Uani 1 1 d . . . C101 C 0.4789(4) 0.5944(10) 0.3032(9) 0.042(4) Uani 1 1 d . . . H101 H 0.4971 0.5689 0.2799 0.051 Uiso 1 1 calc R . . C102 C 0.4864(6) 0.6516(17) 0.3460(13) 0.093(10) Uani 1 1 d . . . H102 H 0.5098 0.6623 0.3566 0.111 Uiso 1 1 calc R . . C103 C 0.4597(6) 0.697(2) 0.376(2) 0.146(18) Uani 1 1 d . . . H103 H 0.4648 0.7411 0.4019 0.175 Uiso 1 1 calc R . . C104 C 0.4260(7) 0.673(2) 0.3660(17) 0.126(14) Uani 1 1 d . . . H104 H 0.4078 0.6989 0.3886 0.152 Uiso 1 1 calc R . . C105 C 0.4180(6) 0.6122(14) 0.3242(13) 0.078(7) Uani 1 1 d . . . H105 H 0.3947 0.5977 0.3168 0.093 Uiso 1 1 calc R . . C106 C 0.3733(4) 0.3041(10) 0.1456(8) 0.039(4) Uani 1 1 d . . . C107 C 0.3484(4) 0.2423(9) 0.1553(7) 0.032(3) Uani 1 1 d . . . C108 C 0.3353(4) 0.2043(10) 0.0983(8) 0.046(4) Uani 1 1 d . . . H108 H 0.3423 0.2195 0.0534 0.056 Uiso 1 1 calc R . . C109 C 0.3125(5) 0.1453(11) 0.1053(9) 0.054(5) Uani 1 1 d . . . H109 H 0.3033 0.1212 0.0656 0.064 Uiso 1 1 calc R . . C110 C 0.3030(5) 0.1207(11) 0.1717(11) 0.054(5) Uani 1 1 d . . . H110 H 0.2876 0.0794 0.1771 0.064 Uiso 1 1 calc R . . C111 C 0.3163(4) 0.1575(10) 0.2293(9) 0.047(4) Uani 1 1 d . . . H111 H 0.3102 0.1414 0.2744 0.057 Uiso 1 1 calc R . . C112 C 0.3387(4) 0.2182(9) 0.2202(7) 0.036(3) Uani 1 1 d . . . H112 H 0.3476 0.2436 0.2596 0.043 Uiso 1 1 calc R . . C113 C 0.4476(4) 0.4600(10) 0.0041(7) 0.036(4) Uani 1 1 d . . . C120 C 0.4884(4) 0.3245(9) 0.1469(8) 0.037(3) Uani 1 1 d . . . C121 C 0.5051(5) 0.2538(9) 0.1742(10) 0.047(4) Uani 1 1 d . . . C122 C 0.5398(5) 0.2550(11) 0.1923(12) 0.064(6) Uani 1 1 d . . . H122 H 0.5529 0.2999 0.1864 0.077 Uiso 1 1 calc R . . C123 C 0.5549(7) 0.1913(12) 0.2185(16) 0.093(9) Uani 1 1 d . . . H123 H 0.5786 0.1925 0.2309 0.111 Uiso 1 1 calc R . . C124 C 0.5366(8) 0.1266(15) 0.227(2) 0.125(14) Uani 1 1 d . . . H124 H 0.5477 0.0824 0.2441 0.150 Uiso 1 1 calc R . . C125 C 0.5026(8) 0.1246(11) 0.2119(18) 0.105(11) Uani 1 1 d . . . H125 H 0.4896 0.0802 0.2215 0.126 Uiso 1 1 calc R . . C126 C 0.4860(5) 0.1889(9) 0.1814(10) 0.054(5) Uani 1 1 d . . . H126 H 0.4627 0.1866 0.1667 0.065 Uiso 1 1 calc R . . C127 C 0.4203(4) 0.1068(11) 0.0371(12) 0.062(6) Uani 1 1 d . . . C128 C 0.4062(4) 0.0481(11) 0.0858(11) 0.052(5) Uani 1 1 d . . . C129 C 0.4011(6) -0.0262(13) 0.0667(14) 0.080(8) Uani 1 1 d . . . H129 H 0.4076 -0.0416 0.0216 0.096 Uiso 1 1 calc R . . C130 C 0.3869(7) -0.0791(12) 0.1108(14) 0.090(10) Uani 1 1 d . . . H130 H 0.3829 -0.1295 0.0957 0.108 Uiso 1 1 calc R . . C131 C 0.3786(6) -0.0573(11) 0.1775(13) 0.073(7) Uani 1 1 d . . . H131 H 0.3689 -0.0932 0.2085 0.088 Uiso 1 1 calc R . . C132 C 0.3842(6) 0.0159(11) 0.1990(12) 0.064(5) Uani 1 1 d . . . H132 H 0.3784 0.0304 0.2447 0.077 Uiso 1 1 calc R . . C133 C 0.3983(5) 0.0686(11) 0.1539(11) 0.058(5) Uani 1 1 d . . . H133 H 0.4027 0.1187 0.1693 0.069 Uiso 1 1 calc R . . O40 O 0.4893(3) 0.1746(9) -0.0758(6) 0.062(4) Uani 1 1 d . . . C135 C 0.5407(5) 0.2289(15) -0.0325(10) 0.066(6) Uani 1 1 d . . . C136 C 0.5564(5) 0.2750(16) 0.0157(11) 0.076(8) Uani 1 1 d . . . H136 H 0.5425 0.3049 0.0454 0.092 Uiso 1 1 calc R . . C137 C 0.5923(5) 0.2785(16) 0.0215(11) 0.071(7) Uani 1 1 d . . . H137 H 0.6029 0.3112 0.0541 0.085 Uiso 1 1 calc R . . C138 C 0.6116(5) 0.2340(17) -0.0202(13) 0.082(8) Uani 1 1 d . . . H138 H 0.6360 0.2359 -0.0167 0.099 Uiso 1 1 calc R . . C139 C 0.5967(6) 0.1862(16) -0.0678(14) 0.081(8) Uani 1 1 d . . . H139 H 0.6105 0.1555 -0.0970 0.098 Uiso 1 1 calc R . . C140 C 0.5612(5) 0.1841(14) -0.0718(11) 0.064(6) Uani 1 1 d . . . H140 H 0.5508 0.1500 -0.1033 0.076 Uiso 1 1 calc R . . O1 O 0.3831(3) 0.1837(6) 0.8607(5) 0.036(2) Uani 1 1 d . . . O2 O 0.3418(4) 0.2641(7) 0.7474(6) 0.076(5) Uani 1 1 d . . . O3 O 0.3137(3) 0.2714(5) 0.6484(5) 0.032(2) Uani 1 1 d . . . O4 O 0.4088(3) 0.0810(6) 0.7525(5) 0.037(2) Uani 1 1 d . . . O5 O 0.4501(3) 0.0641(6) 0.8303(5) 0.038(2) Uani 1 1 d . . . O6 O 0.3312(3) 0.1049(6) 0.7248(5) 0.037(2) Uani 1 1 d . . . O7 O 0.3781(2) 0.1793(5) 0.6342(5) 0.0282(19) Uani 1 1 d . . . O8 O 0.3784(2) 0.2706(5) 0.5537(5) 0.029(2) Uani 1 1 d . . . O9 O 0.4125(7) 0.2662(11) 0.7407(9) 0.106(7) Uani 1 1 d . . . O10 O 0.4573(5) 0.2466(13) 0.7989(12) 0.112(7) Uani 1 1 d . . . O11 O 0.3421(3) 0.0528(5) 0.5717(5) 0.034(2) Uani 1 1 d . . . O12 O 0.3103(2) 0.2018(5) 0.5193(5) 0.0239(19) Uani 1 1 d . . . O13 O 0.3363(2) 0.3366(5) 0.4294(4) 0.0227(18) Uani 1 1 d . . . O14 O 0.3670(2) 0.3969(5) 0.3528(4) 0.026(2) Uani 1 1 d . . . O15 O 0.2766(2) 0.3536(5) 0.5200(5) 0.029(2) Uani 1 1 d . . . O16 O 0.2692(2) 0.4659(5) 0.4705(4) 0.0248(19) Uani 1 1 d . . . O17 O 0.3434(3) 0.4234(6) 0.5705(5) 0.038(2) Uani 1 1 d . . . O18 O 0.3493(2) 0.5040(5) 0.4824(5) 0.030(2) Uani 1 1 d . . . O19 O 0.1963(2) 0.4627(5) 0.4048(5) 0.0245(18) Uani 1 1 d . . . O20 O 0.2270(2) 0.6320(5) 0.4252(4) 0.0251(19) Uani 1 1 d . . . O21 O 0.2913(2) 0.5762(5) 0.3717(5) 0.029(2) Uani 1 1 d . . . O22 O 0.3359(2) 0.5316(5) 0.3169(5) 0.027(2) Uani 1 1 d . . . O23 O 0.2222(3) 0.5599(6) 0.2845(5) 0.031(2) Uani 1 1 d . . . O24 O 0.2729(2) 0.4273(5) 0.3356(4) 0.0233(18) Uani 1 1 d . . . O25 O 0.3081(2) 0.3810(5) 0.2564(5) 0.030(2) Uani 1 1 d . . . O26 O 0.3378(3) 0.4948(6) 0.1583(5) 0.037(2) Uani 1 1 d . . . O27 O 0.3859(3) 0.4958(8) 0.0942(6) 0.051(3) Uani 1 1 d . . . O28 O 0.4049(3) 0.4906(7) 0.2443(6) 0.046(3) Uani 1 1 d . . . O29 O 0.4569(2) 0.4839(6) 0.2032(5) 0.028(2) Uani 1 1 d . . . O30 O 0.3808(2) 0.3486(6) 0.1957(5) 0.033(2) Uani 1 1 d . . . O31 O 0.3879(3) 0.3128(7) 0.0881(6) 0.045(3) Uani 1 1 d . . . O32 O 0.4321(4) 0.3995(10) 0.0086(9) 0.081(5) Uani 1 1 d . . . O33 O 0.4598(3) 0.4928(9) 0.0558(6) 0.057(4) Uani 1 1 d . . . O34 O 0.4560(3) 0.3225(6) 0.1341(6) 0.039(2) Uani 1 1 d . . . O35 O 0.5068(2) 0.3815(6) 0.1406(5) 0.031(2) Uani 1 1 d . . . O36 O 0.4270(3) 0.1701(8) 0.0631(7) 0.064(4) Uani 1 1 d . . . O37 O 0.4239(3) 0.0879(9) -0.0243(8) 0.071(5) Uani 1 1 d . . . O38 O 0.4084(3) 0.2559(8) -0.0654(6) 0.057(4) Uani 1 1 d . . . O39 O 0.4853(3) 0.2730(12) -0.0046(7) 0.085(6) Uani 1 1 d . . . Mn1 Mn 0.37810(6) 0.17713(12) 0.74846(11) 0.0299(4) Uani 1 1 d . . . Mn2 Mn 0.32513(5) 0.15069(11) 0.62323(10) 0.0261(4) Uani 1 1 d . . . Mn3 Mn 0.32770(5) 0.31645(11) 0.54091(10) 0.0234(4) Uani 1 1 d . . . Mn4 Mn 0.31698(5) 0.45494(11) 0.40753(10) 0.0219(4) Uani 1 1 d . . . Mn5 Mn 0.24155(5) 0.52084(11) 0.38186(10) 0.0223(4) Uani 1 1 d . . . Mn6 Mn 0.35472(5) 0.44108(11) 0.24914(11) 0.0249(4) Uani 1 1 d . . . Mn7 Mn 0.42063(5) 0.41845(14) 0.13476(11) 0.0323(5) Uani 1 1 d . . . Mn8 Mn 0.5000 0.5000 0.12859(14) 0.0239(6) Uani 1 2 d S . . Mn9 Mn 0.43417(7) 0.28132(18) 0.03165(15) 0.0522(8) Uani 1 1 d . . . Mn10 Mn 0.43927(7) 0.1585(3) -0.1111(2) 0.0898(16) Uani 1 1 d . . . C134 C 0.5019(5) 0.2267(16) -0.0370(9) 0.070(7) Uani 1 1 d . . . C114 C 0.4485(4) 0.4964(10) -0.0626(6) 0.073(4) Uani 1 1 d GU . . C115 C 0.4662(5) 0.5643(11) -0.0704(10) 0.092(5) Uani 1 1 d GU . . H115 H 0.4767 0.5876 -0.0316 0.110 Uiso 1 1 calc R . . C116 C 0.4687(7) 0.5979(13) -0.1350(13) 0.193(5) Uani 1 1 d GU . . H116 H 0.4808 0.6442 -0.1403 0.231 Uiso 1 1 calc R . . C117 C 0.4534(8) 0.5636(18) -0.1918(9) 0.218(5) Uani 1 1 d GU . . H117 H 0.4550 0.5866 -0.2359 0.261 Uiso 1 1 calc R . . C118 C 0.4357(8) 0.4958(17) -0.1840(7) 0.209(5) Uani 1 1 d GU . . H118 H 0.4252 0.4724 -0.2228 0.250 Uiso 1 1 calc R . . C119 C 0.4333(5) 0.4622(11) -0.1194(9) 0.116(5) Uani 1 1 d GU . . H119 H 0.4212 0.4158 -0.1141 0.139 Uiso 1 1 calc R . . C29 C 0.4399(7) 0.2806(17) 0.7464(15) 0.087(9) Uani 1 1 d . . . C31 C 0.4913(7) 0.3453(16) 0.7078(12) 0.138(6) Uani 1 1 d GU . . H31 H 0.5048 0.3136 0.7367 0.165 Uiso 1 1 calc R . . C30 C 0.4556(7) 0.3384(12) 0.7075(11) 0.124(6) Uani 1 1 d GU . . C35 C 0.4359(5) 0.3848(15) 0.6651(14) 0.163(6) Uani 1 1 d GU . . H35 H 0.4116 0.3801 0.6649 0.196 Uiso 1 1 calc R . . C34 C 0.4519(7) 0.4380(13) 0.6231(14) 0.174(6) Uani 1 1 d GU . . H34 H 0.4384 0.4696 0.5941 0.208 Uiso 1 1 calc R . . C33 C 0.4875(7) 0.4448(15) 0.6234(16) 0.174(6) Uani 1 1 d GU . . H33 H 0.4984 0.4811 0.5946 0.209 Uiso 1 1 calc R . . C32 C 0.5073(5) 0.3984(19) 0.6657(17) 0.260(6) Uani 1 1 d GU . . H32 H 0.5316 0.4031 0.6659 0.312 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 C1 0.040(8) 0.044(9) 0.028(7) -0.006(6) 0.006(6) -0.019(7) C2 0.035(8) 0.048(9) 0.019(6) 0.000(6) 0.000(5) -0.012(7) C3 0.040(8) 0.058(10) 0.029(7) -0.013(7) 0.003(6) -0.013(8) C4 0.048(10) 0.060(11) 0.032(8) -0.015(7) 0.004(7) -0.002(8) C5 0.050(9) 0.055(10) 0.025(7) -0.004(7) -0.005(7) 0.000(8) C6 0.034(8) 0.050(10) 0.047(9) -0.002(8) -0.009(7) -0.006(7) C7 0.043(8) 0.033(7) 0.023(6) 0.004(5) -0.006(6) -0.008(6) C8 0.057(10) 0.036(8) 0.022(7) 0.005(6) 0.004(7) 0.011(7) C9 0.041(8) 0.026(7) 0.039(8) -0.002(6) 0.006(6) 0.003(6) C10 0.062(11) 0.038(9) 0.040(9) 0.007(7) -0.004(8) 0.007(8) C11 0.086(14) 0.039(9) 0.033(8) -0.013(7) -0.012(9) 0.011(9) C12 0.082(14) 0.039(9) 0.045(9) -0.017(8) -0.012(9) 0.024(9) C13 0.054(10) 0.044(10) 0.059(11) -0.012(8) -0.008(9) 0.018(8) C14 0.037(8) 0.038(8) 0.047(9) -0.012(7) -0.005(7) 0.011(7) C15 0.021(6) 0.043(8) 0.025(6) 0.009(6) -0.002(5) 0.002(6) C16 0.025(6) 0.032(7) 0.035(7) -0.001(6) -0.002(6) 0.003(5) C17 0.046(10) 0.039(9) 0.070(12) -0.011(8) -0.029(9) 0.000(8) C18 0.058(12) 0.050(11) 0.12(2) -0.027(12) -0.049(13) 0.007(10) C19 0.068(13) 0.032(9) 0.13(2) -0.031(12) -0.051(14) 0.012(9) C20 0.055(11) 0.051(11) 0.095(16) -0.028(12) -0.036(12) 0.021(9) C21 0.040(9) 0.049(10) 0.048(10) -0.017(8) -0.022(7) 0.007(8) C22 0.025(6) 0.032(7) 0.024(6) 0.001(6) -0.004(5) -0.002(6) C23 0.022(7) 0.077(13) 0.037(8) -0.002(8) 0.003(6) 0.014(8) C24 0.028(9) 0.16(2) 0.047(11) 0.046(14) 0.002(8) 0.002(12) C25 0.040(13) 0.32(5) 0.085(19) 0.10(3) 0.021(12) 0.05(2) C26 0.061(16) 0.36(7) 0.11(2) 0.10(4) 0.030(18) 0.09(3) C27 0.081(18) 0.21(4) 0.09(2) 0.05(2) 0.026(16) 0.10(2) C28 0.050(11) 0.105(18) 0.063(13) 0.005(12) 0.021(10) 0.042(12) C36 0.028(7) 0.019(6) 0.032(7) -0.005(5) 0.002(5) 0.005(5) C37 0.034(7) 0.025(6) 0.030(7) 0.002(6) -0.002(6) 0.004(6) C38 0.029(7) 0.044(9) 0.053(10) 0.007(8) -0.001(7) 0.002(7) C39 0.027(8) 0.061(12) 0.061(11) 0.012(9) -0.009(8) 0.001(8) C40 0.044(9) 0.050(10) 0.048(10) 0.002(8) -0.014(8) -0.002(8) C41 0.056(10) 0.044(9) 0.036(8) 0.009(7) -0.015(8) 0.003(8) C42 0.040(8) 0.030(7) 0.029(7) 0.007(6) -0.003(6) -0.003(6) C43 0.018(6) 0.033(7) 0.018(6) -0.005(5) -0.002(4) -0.002(5) C44 0.021(6) 0.034(7) 0.029(7) -0.010(6) -0.002(5) 0.005(5) C45 0.028(7) 0.029(7) 0.030(7) -0.009(6) 0.003(6) 0.001(6) C46 0.042(8) 0.025(7) 0.052(10) -0.003(6) 0.007(7) 0.011(6) C47 0.038(9) 0.040(9) 0.081(14) -0.007(9) 0.011(9) 0.009(8) C48 0.035(9) 0.053(11) 0.073(13) -0.024(10) 0.014(9) 0.008(8) C49 0.037(8) 0.034(8) 0.037(8) -0.003(6) 0.002(6) 0.002(6) C50 0.028(7) 0.030(7) 0.022(6) 0.000(5) 0.001(5) 0.003(6) C51 0.026(6) 0.034(7) 0.026(6) 0.006(5) 0.004(5) 0.008(6) C52 0.037(8) 0.036(8) 0.036(8) 0.009(6) 0.004(6) 0.002(6) C53 0.037(9) 0.058(11) 0.066(12) 0.033(9) 0.005(9) -0.006(8) C54 0.036(8) 0.068(12) 0.047(10) 0.013(9) 0.017(7) 0.010(8) C55 0.040(8) 0.057(10) 0.032(8) 0.007(7) 0.008(6) 0.022(8) C56 0.029(7) 0.037(8) 0.029(7) -0.002(6) 0.001(6) 0.004(6) C57 0.025(6) 0.026(7) 0.036(7) 0.002(6) 0.000(6) -0.002(5) C58 0.037(8) 0.041(9) 0.041(8) -0.002(7) -0.015(7) -0.011(7) C59 0.050(10) 0.041(9) 0.060(11) 0.003(8) -0.017(9) -0.015(8) C60 0.085(15) 0.061(13) 0.066(13) 0.003(10) -0.021(11) -0.048(12) C61 0.13(2) 0.11(2) 0.067(16) 0.003(15) -0.032(16) -0.07(2) C62 0.18(3) 0.14(3) 0.048(13) 0.000(15) -0.030(17) -0.10(3) C63 0.086(15) 0.058(12) 0.037(9) 0.000(8) -0.022(9) -0.034(11) C64 0.030(7) 0.023(7) 0.036(7) 0.001(6) 0.006(6) -0.008(6) C65 0.031(7) 0.028(7) 0.042(8) 0.002(6) -0.004(6) -0.014(6) C66 0.032(8) 0.032(8) 0.079(13) 0.008(8) -0.005(8) -0.008(7) C67 0.047(11) 0.048(12) 0.13(2) 0.042(13) -0.008(12) -0.014(9) C68 0.052(13) 0.10(2) 0.14(2) 0.069(19) 0.003(14) -0.031(14) C69 0.040(11) 0.080(17) 0.14(2) 0.014(16) 0.022(13) -0.017(11) C70 0.031(8) 0.050(10) 0.068(12) -0.002(9) 0.012(8) -0.006(7) C71 0.020(6) 0.023(6) 0.025(6) -0.003(5) -0.001(5) -0.005(5) C72 0.042(8) 0.029(7) 0.026(6) 0.007(6) -0.003(6) -0.004(6) C73 0.036(8) 0.031(8) 0.062(11) 0.001(7) -0.014(8) -0.002(7) C74 0.060(12) 0.032(9) 0.083(15) 0.009(9) -0.026(11) -0.001(8) C75 0.13(2) 0.038(10) 0.046(11) 0.012(8) -0.037(13) -0.009(12) C76 0.12(2) 0.035(10) 0.063(13) 0.012(9) 0.036(13) -0.001(11) C77 0.074(12) 0.029(8) 0.049(10) 0.004(7) 0.021(9) -0.002(8) C78 0.040(7) 0.020(6) 0.027(6) 0.004(5) 0.002(6) -0.007(5) C79 0.045(8) 0.026(7) 0.019(6) -0.002(5) -0.004(6) -0.001(6) C80 0.049(9) 0.020(6) 0.027(7) -0.007(5) -0.010(6) 0.006(6) C81 0.055(10) 0.037(8) 0.035(8) -0.013(7) -0.020(7) 0.004(7) C82 0.101(16) 0.042(9) 0.029(8) -0.003(7) -0.016(9) 0.004(10) C83 0.067(12) 0.042(9) 0.031(8) -0.004(7) 0.011(8) 0.004(8) C84 0.040(8) 0.039(8) 0.028(7) -0.006(6) 0.004(6) 0.001(7) C85 0.023(6) 0.021(6) 0.029(6) 0.000(5) 0.001(5) -0.002(5) C86 0.026(6) 0.026(6) 0.027(7) -0.002(5) -0.003(5) -0.007(5) C87 0.028(7) 0.023(6) 0.037(8) -0.007(5) 0.002(6) 0.000(5) C88 0.027(7) 0.029(7) 0.064(10) -0.003(7) -0.010(7) -0.002(6) C89 0.041(9) 0.038(8) 0.051(10) -0.010(7) -0.020(7) -0.004(7) C90 0.053(10) 0.046(9) 0.039(9) -0.011(8) -0.019(8) -0.005(8) C91 0.045(8) 0.025(7) 0.033(7) -0.002(5) -0.010(6) -0.004(6) C92 0.037(8) 0.048(9) 0.025(7) 0.012(6) -0.001(6) -0.006(7) C93 0.043(8) 0.033(7) 0.029(7) 0.005(6) -0.005(6) -0.006(7) C94 0.045(9) 0.053(10) 0.037(8) 0.001(8) 0.000(7) 0.008(8) C95 0.058(12) 0.056(12) 0.062(12) 0.009(10) -0.007(10) 0.016(10) C96 0.084(14) 0.030(8) 0.039(9) 0.007(7) -0.020(9) -0.006(9) C97 0.082(14) 0.036(9) 0.037(9) 0.006(7) -0.010(9) -0.012(9) C98 0.049(9) 0.032(8) 0.033(8) 0.001(6) 0.000(7) -0.009(7) C99 0.027(6) 0.026(6) 0.030(7) -0.001(6) -0.005(6) -0.004(5) C100 0.042(10) 0.082(14) 0.058(11) -0.042(11) 0.024(8) -0.021(10) C101 0.030(7) 0.051(10) 0.046(9) -0.023(8) 0.009(7) -0.008(7) C102 0.049(12) 0.13(2) 0.095(18) -0.076(17) 0.011(12) -0.024(14) C103 0.051(14) 0.19(3) 0.20(4) -0.15(3) -0.013(19) 0.005(18) C104 0.059(15) 0.16(3) 0.16(3) -0.12(3) 0.005(17) 0.017(17) C105 0.042(11) 0.087(17) 0.104(19) -0.046(15) -0.004(12) 0.000(11) C106 0.023(7) 0.054(10) 0.039(8) -0.014(7) 0.002(6) 0.002(7) C107 0.035(8) 0.037(8) 0.025(7) -0.010(6) 0.002(6) -0.007(6) C108 0.053(10) 0.053(10) 0.032(8) -0.012(7) 0.004(7) -0.022(8) C109 0.059(11) 0.057(11) 0.045(10) 0.000(8) -0.015(8) -0.029(9) C110 0.042(10) 0.049(11) 0.069(13) -0.011(9) -0.004(9) -0.016(8) C111 0.041(9) 0.047(10) 0.053(10) 0.008(8) 0.003(8) 0.006(8) C112 0.045(9) 0.036(8) 0.027(7) -0.007(6) -0.005(6) 0.000(7) C113 0.023(7) 0.070(11) 0.015(6) 0.005(6) -0.001(5) 0.000(7) C120 0.045(9) 0.037(8) 0.029(7) -0.009(6) 0.009(6) 0.001(7) C121 0.046(10) 0.033(8) 0.062(11) -0.013(8) 0.021(8) 0.002(7) C122 0.057(12) 0.040(10) 0.096(17) 0.005(10) 0.010(11) 0.022(9) C123 0.070(15) 0.041(12) 0.17(3) 0.032(15) 0.018(16) 0.027(11) C124 0.09(2) 0.067(17) 0.22(4) 0.04(2) 0.06(2) 0.050(16) C125 0.10(2) 0.025(10) 0.19(3) 0.005(14) 0.06(2) 0.004(12) C126 0.065(12) 0.028(8) 0.070(12) -0.007(8) 0.035(10) 0.003(8) C127 0.024(8) 0.058(11) 0.104(17) -0.054(12) 0.000(9) 0.005(8) C128 0.026(8) 0.054(11) 0.075(13) -0.029(10) -0.013(8) 0.010(7) C129 0.069(14) 0.057(13) 0.11(2) -0.045(14) -0.058(14) 0.030(11) C130 0.12(2) 0.030(9) 0.12(2) -0.014(12) -0.083(18) 0.012(12) C131 0.096(17) 0.037(10) 0.087(16) -0.009(10) -0.036(14) 0.016(11) C132 0.071(14) 0.041(10) 0.080(14) -0.005(10) 0.000(11) 0.010(10) C133 0.049(11) 0.042(10) 0.082(14) -0.020(10) -0.013(10) 0.003(8) O40 0.029(6) 0.114(12) 0.041(7) -0.007(7) -0.005(5) -0.019(7) C135 0.037(9) 0.125(19) 0.036(9) 0.007(11) 0.007(8) -0.027(11) C136 0.039(10) 0.13(2) 0.057(12) -0.007(13) 0.004(9) -0.038(13) C137 0.046(11) 0.12(2) 0.052(12) 0.018(12) 0.004(9) -0.032(12) C138 0.037(10) 0.13(2) 0.082(16) 0.057(16) -0.001(11) -0.022(13) C139 0.042(11) 0.098(19) 0.104(19) 0.026(16) -0.001(12) -0.020(12) C140 0.044(10) 0.090(16) 0.057(12) 0.004(11) 0.012(9) -0.023(11) O1 0.043(6) 0.039(6) 0.027(5) -0.003(4) -0.001(4) -0.007(5) O2 0.142(14) 0.061(8) 0.025(6) -0.003(6) -0.002(8) 0.063(9) O3 0.039(5) 0.030(5) 0.026(5) 0.004(4) 0.011(4) 0.005(4) O4 0.042(6) 0.037(5) 0.032(5) 0.002(5) -0.013(5) 0.008(5) O5 0.039(6) 0.044(6) 0.031(5) -0.011(5) -0.004(4) 0.017(5) O6 0.035(6) 0.042(6) 0.035(5) 0.016(4) 0.004(4) 0.002(5) O7 0.030(5) 0.029(5) 0.025(5) 0.004(4) 0.001(4) 0.001(4) O8 0.027(5) 0.034(5) 0.027(5) 0.003(4) 0.001(4) 0.001(4) O9 0.17(2) 0.093(14) 0.053(10) -0.009(9) -0.001(13) -0.048(15) O10 0.090(14) 0.130(18) 0.117(17) -0.019(15) 0.021(13) -0.017(13) O11 0.035(5) 0.025(5) 0.044(6) -0.003(4) -0.004(4) 0.002(4) O12 0.024(4) 0.020(4) 0.028(5) 0.005(3) 0.000(4) 0.000(3) O13 0.027(4) 0.021(4) 0.020(4) 0.005(3) 0.001(3) 0.002(4) O14 0.032(5) 0.027(5) 0.020(4) 0.009(4) 0.003(4) -0.002(4) O15 0.028(5) 0.026(5) 0.034(5) 0.006(4) 0.005(4) 0.006(4) O16 0.028(5) 0.027(5) 0.020(4) 0.003(4) 0.003(4) 0.000(4) O17 0.047(6) 0.025(5) 0.040(6) -0.004(4) 0.005(5) -0.007(5) O18 0.032(5) 0.025(5) 0.034(5) -0.001(4) -0.005(4) -0.003(4) O19 0.024(4) 0.024(5) 0.025(4) 0.001(4) 0.005(4) -0.001(4) O20 0.027(5) 0.025(5) 0.023(4) 0.000(4) 0.005(4) 0.001(4) O21 0.030(5) 0.029(5) 0.029(5) -0.008(4) 0.012(4) -0.008(4) O22 0.025(5) 0.021(4) 0.036(5) 0.003(4) 0.003(4) -0.001(4) O23 0.035(5) 0.040(6) 0.019(4) -0.002(4) -0.008(4) -0.002(4) O24 0.024(4) 0.022(4) 0.024(4) -0.003(3) -0.001(4) 0.000(4) O25 0.026(5) 0.030(5) 0.032(5) -0.006(4) 0.005(4) -0.003(4) O26 0.028(5) 0.049(6) 0.032(5) 0.009(5) 0.006(4) 0.000(5) O27 0.029(6) 0.086(9) 0.039(6) 0.020(6) 0.007(5) 0.002(6) O28 0.026(5) 0.055(7) 0.056(7) -0.009(6) 0.006(5) -0.012(5) O29 0.024(5) 0.038(5) 0.023(4) -0.003(4) 0.002(4) -0.005(4) O30 0.028(5) 0.039(5) 0.032(5) -0.009(4) 0.001(4) 0.001(4) O31 0.040(6) 0.059(7) 0.036(6) -0.012(5) 0.012(5) -0.010(5) O32 0.052(9) 0.089(12) 0.102(13) 0.015(10) -0.018(8) -0.038(8) O33 0.044(7) 0.095(10) 0.031(6) -0.018(6) -0.023(5) 0.016(7) O34 0.030(5) 0.043(6) 0.043(6) -0.018(5) -0.001(5) -0.002(5) O35 0.030(5) 0.033(5) 0.030(5) -0.005(4) -0.005(4) -0.001(4) O36 0.053(8) 0.073(9) 0.067(9) -0.042(7) 0.013(7) -0.017(7) O37 0.038(7) 0.101(11) 0.075(10) -0.058(9) -0.001(7) -0.003(7) O38 0.029(6) 0.088(10) 0.053(7) -0.042(7) 0.009(5) -0.016(6) O39 0.031(7) 0.171(18) 0.054(8) -0.054(10) 0.014(6) -0.029(9) Mn1 0.0394(11) 0.0281(10) 0.0222(9) -0.0008(8) -0.0047(9) 0.0031(9) Mn2 0.0280(10) 0.0249(9) 0.0253(10) 0.0038(8) -0.0013(8) 0.0007(8) Mn3 0.0265(10) 0.0210(9) 0.0227(9) 0.0010(7) 0.0011(8) 0.0010(8) Mn4 0.0212(9) 0.0219(9) 0.0225(9) 0.0006(7) 0.0012(7) 0.0014(7) Mn5 0.0217(9) 0.0216(9) 0.0235(9) -0.0013(7) 0.0011(8) 0.0010(7) Mn6 0.0204(9) 0.0293(10) 0.0252(9) -0.0006(8) 0.0031(8) -0.0004(8) Mn7 0.0238(10) 0.0494(13) 0.0237(10) -0.0133(9) 0.0014(8) -0.0038(10) Mn8 0.0192(12) 0.0330(15) 0.0193(13) 0.000 0.000 -0.0031(11) Mn9 0.0334(13) 0.0731(19) 0.0501(16) -0.0392(14) 0.0148(12) -0.0229(13) Mn10 0.0249(13) 0.140(3) 0.105(3) -0.100(3) -0.0045(15) 0.0060(17) C134 0.035(9) 0.14(2) 0.036(9) -0.012(12) 0.015(8) -0.032(12) C114 0.080(10) 0.106(12) 0.033(6) 0.003(7) -0.002(6) 0.036(9) C115 0.083(11) 0.108(12) 0.084(6) 0.025(7) 0.003(7) 0.027(9) C116 0.233(11) 0.209(12) 0.136(7) 0.116(8) 0.009(8) 0.018(9) C117 0.325(11) 0.261(12) 0.067(7) 0.093(8) 0.014(8) 0.111(10) C118 0.326(11) 0.260(12) 0.040(6) 0.000(8) -0.033(7) 0.104(10) C119 0.155(11) 0.157(12) 0.035(6) -0.003(7) -0.028(7) 0.049(9) C29 0.078(17) 0.10(2) 0.080(17) -0.041(16) -0.028(15) 0.048(16) C31 0.150(14) 0.142(13) 0.121(12) 0.018(10) 0.050(12) 0.035(12) C30 0.149(14) 0.144(13) 0.077(12) 0.002(10) 0.023(12) 0.032(12) C35 0.149(14) 0.151(13) 0.190(13) 0.108(10) 0.048(12) 0.029(12) C34 0.149(14) 0.107(13) 0.266(13) 0.091(10) 0.094(13) 0.024(12) C33 0.148(14) 0.184(13) 0.189(13) 0.089(10) 0.051(13) 0.019(12) C32 0.158(14) 0.351(13) 0.272(13) 0.196(10) 0.050(13) 0.039(12) _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 C1 O38 1.247(18) 1_556 ? C1 O1 1.263(18) . ? C1 C2 1.48(2) . ? C2 C3 1.39(2) . ? C2 C7 1.407(19) . ? C3 C4 1.39(2) . ? C3 H3 0.9500 . ? C4 C5 1.40(2) . ? C4 H4 0.9500 . ? C5 C6 1.40(2) . ? C5 H5 0.9500 . ? C6 C7 1.37(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O2 1.233(19) . ? C8 O3 1.279(17) . ? C8 C9 1.50(2) . ? C9 C14 1.37(2) . ? C9 C10 1.38(2) . ? C10 C11 1.38(2) . ? C10 H10 0.9500 . ? C11 C12 1.36(2) . ? C11 H11 0.9500 . ? C12 C13 1.39(2) . ? C12 H12 0.9500 . ? C13 C14 1.39(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O4 1.241(16) . ? C15 O5 1.272(17) . ? C15 C16 1.50(2) . ? C16 C21 1.37(2) . ? C16 C17 1.39(2) . ? C17 C18 1.40(3) . ? C17 H17 0.9500 . ? C18 C19 1.37(3) . ? C18 H18 0.9500 . ? C19 C20 1.35(3) . ? C19 H19 0.9500 . ? C20 C21 1.39(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O8 1.243(16) . ? C22 O7 1.290(16) . ? C22 C23 1.507(19) . ? C23 C24 1.37(3) . ? C23 C28 1.38(3) . ? C24 C25 1.38(3) . ? C24 H24 0.9500 . ? C25 C26 1.34(5) . ? C25 H25 0.9500 . ? C26 C27 1.43(5) . ? C26 H26 0.9500 . ? C27 C28 1.39(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C36 O12 1.261(16) . ? C36 O20 1.283(16) 4_546 ? C36 C37 1.473(19) . ? C37 C42 1.380(19) . ? C37 C38 1.40(2) . ? C38 C39 1.37(2) . ? C38 H38 0.9500 . ? C39 C40 1.35(3) . ? C39 H39 0.9500 . ? C40 C41 1.39(2) . ? C40 H40 0.9500 . ? C41 C42 1.37(2) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O14 1.264(15) . ? C43 O13 1.274(14) . ? C43 C44 1.480(18) . ? C44 C49 1.39(2) . ? C44 C45 1.40(2) . ? C45 C46 1.389(19) . ? C45 H45 0.9500 . ? C46 C47 1.40(2) . ? C46 H46 0.9500 . ? C47 C48 1.38(3) . ? C47 H47 0.9500 . ? C48 C49 1.38(2) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 O15 1.260(16) . ? C50 O16 1.277(16) . ? C50 C51 1.480(18) . ? C51 C56 1.39(2) . ? C51 C52 1.40(2) . ? C52 C53 1.38(2) . ? C52 H52 0.9500 . ? C53 C54 1.38(3) . ? C53 H53 0.9500 . ? C54 C55 1.38(2) . ? C54 H54 0.9500 . ? C55 C56 1.384(19) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 O17 1.237(16) . ? C57 O18 1.277(17) . ? C57 C58 1.493(19) . ? C58 C63 1.37(2) . ? C58 C59 1.39(2) . ? C59 C60 1.37(2) . ? C59 H59 0.9500 . ? C60 C61 1.38(3) . ? C60 H60 0.9500 . ? C61 C62 1.38(3) . ? C61 H61 0.9500 . ? C62 C63 1.39(3) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 O11 1.239(17) 4_556 ? C64 O19 1.267(16) . ? C64 C65 1.486(18) . ? C65 C70 1.39(2) . ? C65 C66 1.40(2) . ? C66 C67 1.38(2) . ? C66 H66 0.9500 . ? C67 C68 1.38(3) . ? C67 H67 0.9500 . ? C68 C69 1.37(4) . ? C68 H68 0.9500 . ? C69 C70 1.39(3) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 O22 1.259(15) . ? C71 O21 1.266(15) . ? C71 C72 1.502(18) . ? C72 C77 1.38(2) . ? C72 C73 1.40(2) . ? C73 C74 1.36(2) . ? C73 H73 0.9500 . ? C74 C75 1.36(3) . ? C74 H74 0.9500 . ? C75 C76 1.41(3) . ? C75 H75 0.9500 . ? C76 C77 1.37(2) . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? C78 O23 1.251(16) . ? C78 O6 1.284(17) 4_556 ? C78 C79 1.489(18) . ? C79 C84 1.38(2) . ? C79 C80 1.39(2) . ? C80 C81 1.381(19) . ? C80 H80 0.9500 . ? C81 C82 1.39(3) . ? C81 H81 0.9500 . ? C82 C83 1.39(3) . ? C82 H82 0.9500 . ? C83 C84 1.38(2) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 O24 1.252(15) . ? C85 O25 1.253(15) . ? C85 C86 1.512(17) . ? C86 C91 1.377(19) . ? C86 C87 1.392(18) . ? C87 C88 1.40(2) . ? C87 H87 0.9500 . ? C88 C89 1.36(2) . ? C88 H88 0.9500 . ? C89 C90 1.40(2) . ? C89 H89 0.9500 . ? C90 C91 1.39(2) . ? C90 H90 0.9500 . ? C91 H91 0.9500 . ? C92 O27 1.265(19) . ? C92 O26 1.264(16) . ? C92 C93 1.483(19) . ? C93 C98 1.38(2) . ? C93 C94 1.39(2) . ? C94 C95 1.40(2) . ? C94 H94 0.9500 . ? C95 C96 1.38(3) . ? C95 H95 0.9500 . ? C96 C97 1.35(3) . ? C96 H96 0.9500 . ? C97 C98 1.38(2) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 O28 1.231(16) . ? C99 O29 1.258(16) . ? C99 C100 1.47(2) . ? C100 C101 1.39(2) . ? C100 C105 1.41(3) . ? C101 C102 1.34(3) . ? C101 H101 0.9500 . ? C102 C103 1.43(3) . ? C102 H102 0.9500 . ? C103 C104 1.39(3) . ? C103 H103 0.9500 . ? C104 C105 1.38(3) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 O31 1.260(18) . ? C106 O30 1.283(17) . ? C106 C107 1.47(2) . ? C107 C112 1.38(2) . ? C107 C108 1.39(2) . ? C108 C109 1.37(2) . ? C108 H108 0.9500 . ? C109 C110 1.41(3) . ? C109 H109 0.9500 . ? C110 C111 1.39(2) . ? C110 H110 0.9500 . ? C111 C112 1.39(2) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? C113 O32 1.23(2) . ? C113 O33 1.251(18) . ? C113 C114 1.446(18) . ? C120 O35 1.242(18) . ? C120 O34 1.283(18) . ? C120 C121 1.50(2) . ? C121 C126 1.37(2) . ? C121 C122 1.39(3) . ? C122 C123 1.37(3) . ? C122 H122 0.9500 . ? C123 C124 1.36(4) . ? C123 H123 0.9500 . ? C124 C125 1.35(4) . ? C124 H124 0.9500 . ? C125 C126 1.43(3) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 O37 1.24(2) . ? C127 O36 1.25(2) . ? C127 C128 1.51(3) . ? C128 C129 1.38(3) . ? C128 C133 1.40(3) . ? C129 C130 1.38(4) . ? C129 H129 0.9500 . ? C130 C131 1.39(4) . ? C130 H130 0.9500 . ? C131 C132 1.38(3) . ? C131 H131 0.9500 . ? C132 C133 1.39(3) . ? C132 H132 0.9500 . ? C133 H133 0.9500 . ? O40 C134 1.28(2) . ? O40 Mn10 2.080(11) . ? C135 C140 1.36(3) . ? C135 C136 1.38(3) . ? C135 C134 1.51(3) . ? C136 C137 1.40(3) . ? C136 H136 0.9500 . ? C137 C138 1.35(4) . ? C137 H137 0.9500 . ? C138 C139 1.38(4) . ? C138 H138 0.9500 . ? C139 C140 1.38(3) . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? O1 Mn1 2.190(10) . ? O1 Mn10 2.292(11) 1_556 ? O2 Mn1 2.085(12) . ? O3 Mn2 2.232(10) . ? O3 Mn3 2.298(9) . ? O4 Mn1 2.077(10) . ? O5 Mn10 2.062(10) 1_556 ? O6 C78 1.284(17) 4_546 ? O6 Mn2 2.143(10) . ? O6 Mn1 2.271(11) . ? O7 Mn2 2.130(9) . ? O7 Mn1 2.216(9) . ? O8 Mn3 2.143(10) . ? O9 C29 1.10(3) . ? O9 Mn1 2.069(19) . ? O10 C29 1.36(3) . ? O10 Mn10 2.44(2) 1_556 ? O11 C64 1.239(17) 4_546 ? O11 Mn2 2.103(10) . ? O12 Mn3 2.177(9) . ? O12 Mn2 2.284(9) . ? O13 Mn3 2.217(8) . ? O13 Mn4 2.261(8) . ? O14 Mn6 2.209(9) . ? O14 Mn4 2.437(9) . ? O15 Mn3 2.127(9) . ? O16 Mn4 2.229(9) . ? O16 Mn5 2.247(9) . ? O17 Mn3 2.067(10) . ? O18 Mn4 2.105(9) . ? O19 Mn5 2.082(9) . ? O20 C36 1.283(16) 4_556 ? O20 Mn5 2.210(9) . ? O20 Mn2 2.257(9) 4_556 ? O21 Mn5 2.173(9) . ? O21 Mn4 2.465(10) . ? O22 Mn6 2.196(9) . ? O22 Mn4 2.338(9) . ? O23 Mn5 2.147(9) . ? O24 Mn5 2.239(9) . ? O24 Mn4 2.262(9) . ? O25 Mn6 2.103(9) . ? O26 Mn6 2.106(10) . ? O27 Mn7 2.076(12) . ? O28 Mn6 2.139(10) . ? O29 Mn8 2.230(9) . ? O29 Mn7 2.255(9) . ? O30 Mn6 2.184(10) . ? O30 Mn7 2.306(10) . ? O31 Mn9 2.176(11) . ? O31 Mn7 2.432(11) . ? O32 Mn9 2.137(17) . ? O32 Mn7 2.510(18) . ? O33 Mn8 2.110(10) . ? O33 Mn7 2.526(15) . ? O34 Mn7 2.182(11) . ? O34 Mn9 2.279(10) . ? O35 Mn8 2.124(10) . ? O36 Mn9 2.076(16) . ? O37 Mn10 2.179(18) . ? O38 C1 1.247(18) 1_554 ? O38 Mn9 2.178(12) . ? O38 Mn10 2.277(13) . ? O39 C134 1.22(3) . ? O39 Mn9 2.111(13) . ? Mn1 Mn2 3.217(3) . ? Mn2 O20 2.257(9) 4_546 ? Mn4 Mn5 3.191(3) . ? Mn7 Mn9 3.186(3) . ? Mn8 O33 2.110(10) 2_665 ? Mn8 O35 2.124(10) 2_665 ? Mn8 O29 2.230(9) 2_665 ? Mn10 O5 2.062(10) 1_554 ? Mn10 O1 2.292(11) 1_554 ? Mn10 O10 2.44(2) 1_554 ? C114 C115 1.3900 . ? C114 C119 1.3900 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 C117 1.3900 . ? C116 H116 0.9500 . ? C117 C118 1.3900 . ? C117 H117 0.9500 . ? C118 C119 1.3900 . ? C118 H118 0.9500 . ? C119 H119 0.9500 . ? C29 C30 1.41(4) . ? C31 C30 1.3900 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C30 C35 1.3900 . ? C35 C34 1.3900 . ? C35 H35 0.9500 . ? C34 C33 1.3900 . ? C34 H34 0.9500 . ? C33 C32 1.3900 . ? C33 H33 0.9500 . ? C32 H32 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O38 C1 O1 118.4(15) 1_556 . ? O38 C1 C2 121.4(14) 1_556 . ? O1 C1 C2 120.1(13) . . ? C3 C2 C7 119.7(15) . . ? C3 C2 C1 120.8(13) . . ? C7 C2 C1 119.5(14) . . ? C2 C3 C4 120.2(15) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 119.5(16) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 120.5(16) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 119.8(15) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 120.4(14) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? O2 C8 O3 123.3(14) . . ? O2 C8 C9 117.8(14) . . ? O3 C8 C9 118.9(13) . . ? C14 C9 C10 120.2(14) . . ? C14 C9 C8 120.9(14) . . ? C10 C9 C8 118.8(14) . . ? C11 C10 C9 119.6(16) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 120.9(16) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 119.5(16) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.2(17) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C9 C14 C13 119.5(16) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.3 . . ? O4 C15 O5 124.2(14) . . ? O4 C15 C16 117.9(12) . . ? O5 C15 C16 117.8(12) . . ? C21 C16 C17 119.9(14) . . ? C21 C16 C15 121.4(13) . . ? C17 C16 C15 118.7(13) . . ? C16 C17 C18 119.0(16) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 119.7(17) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 121.1(18) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.9(17) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 120.4(15) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? O8 C22 O7 124.8(12) . . ? O8 C22 C23 118.4(13) . . ? O7 C22 C23 116.8(13) . . ? C24 C23 C28 122.1(17) . . ? C24 C23 C22 118.4(16) . . ? C28 C23 C22 119.4(16) . . ? C23 C24 C25 119(2) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 121(3) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 120(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119(3) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.8 . . ? C23 C28 C27 119(2) . . ? C23 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? O12 C36 O20 118.5(12) . 4_546 ? O12 C36 C37 120.2(12) . . ? O20 C36 C37 121.3(12) 4_546 . ? C42 C37 C38 119.0(14) . . ? C42 C37 C36 120.0(13) . . ? C38 C37 C36 121.0(13) . . ? C39 C38 C37 119.8(16) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 120.7(16) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 120.5(16) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 119.4(16) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C37 120.4(15) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? O14 C43 O13 118.5(11) . . ? O14 C43 C44 120.2(11) . . ? O13 C43 C44 121.3(12) . . ? C49 C44 C45 119.7(13) . . ? C49 C44 C43 119.3(13) . . ? C45 C44 C43 120.9(12) . . ? C46 C45 C44 120.2(13) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 120.0(15) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 118.8(15) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C47 C48 C49 121.8(16) . . ? C47 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C48 C49 C44 119.3(16) . . ? C48 C49 H49 120.3 . . ? C44 C49 H49 120.3 . . ? O15 C50 O16 122.5(12) . . ? O15 C50 C51 118.1(12) . . ? O16 C50 C51 119.5(12) . . ? C56 C51 C52 118.4(13) . . ? C56 C51 C50 120.6(13) . . ? C52 C51 C50 120.7(13) . . ? C53 C52 C51 121.2(15) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 119.1(15) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.4 . . ? C55 C54 C53 120.7(15) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 120.1(16) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.3(14) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? O17 C57 O18 125.7(13) . . ? O17 C57 C58 118.1(13) . . ? O18 C57 C58 116.2(12) . . ? C63 C58 C59 119.9(16) . . ? C63 C58 C57 118.2(15) . . ? C59 C58 C57 121.8(15) . . ? C60 C59 C58 120.3(19) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 121(2) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.6 . . ? C62 C61 C60 118(2) . . ? C62 C61 H61 121.0 . . ? C60 C61 H61 121.0 . . ? C61 C62 C63 122(2) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.1 . . ? C58 C63 C62 119(2) . . ? C58 C63 H63 120.4 . . ? C62 C63 H63 120.4 . . ? O11 C64 O19 125.7(12) 4_556 . ? O11 C64 C65 116.6(13) 4_556 . ? O19 C64 C65 117.7(12) . . ? C70 C65 C66 119.0(14) . . ? C70 C65 C64 119.7(14) . . ? C66 C65 C64 121.2(14) . . ? C67 C66 C65 119.9(17) . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C68 C67 C66 120(2) . . ? C68 C67 H67 120.1 . . ? C66 C67 H67 120.1 . . ? C69 C68 C67 121.1(19) . . ? C69 C68 H68 119.5 . . ? C67 C68 H68 119.4 . . ? C68 C69 C70 119(2) . . ? C68 C69 H69 120.3 . . ? C70 C69 H69 120.3 . . ? C65 C70 C69 120.5(19) . . ? C65 C70 H70 119.7 . . ? C69 C70 H70 119.7 . . ? O22 C71 O21 119.5(12) . . ? O22 C71 C72 121.5(12) . . ? O21 C71 C72 118.8(12) . . ? C77 C72 C73 120.2(15) . . ? C77 C72 C71 120.1(14) . . ? C73 C72 C71 119.7(13) . . ? C74 C73 C72 120.9(18) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C75 C74 C73 119.1(19) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.5 . . ? C74 C75 C76 121.2(17) . . ? C74 C75 H75 119.4 . . ? C76 C75 H75 119.4 . . ? C77 C76 C75 119(2) . . ? C77 C76 H76 120.4 . . ? C75 C76 H76 120.4 . . ? C76 C77 C72 119.5(18) . . ? C76 C77 H77 120.2 . . ? C72 C77 H77 120.3 . . ? O23 C78 O6 122.9(13) . 4_556 ? O23 C78 C79 119.4(13) . . ? O6 C78 C79 117.7(13) 4_556 . ? C84 C79 C80 119.5(13) . . ? C84 C79 C78 120.4(13) . . ? C80 C79 C78 120.1(13) . . ? C81 C80 C79 120.4(15) . . ? C81 C80 H80 119.8 . . ? C79 C80 H80 119.8 . . ? C80 C81 C82 120.1(15) . . ? C80 C81 H81 119.9 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 119.2(15) . . ? C83 C82 H82 120.4 . . ? C81 C82 H82 120.4 . . ? C84 C83 C82 120.5(17) . . ? C84 C83 H83 119.8 . . ? C82 C83 H83 119.7 . . ? C83 C84 C79 120.4(15) . . ? C83 C84 H84 119.8 . . ? C79 C84 H84 119.8 . . ? O24 C85 O25 124.2(12) . . ? O24 C85 C86 119.5(11) . . ? O25 C85 C86 116.3(12) . . ? C91 C86 C87 120.3(13) . . ? C91 C86 C85 118.8(12) . . ? C87 C86 C85 120.9(12) . . ? C86 C87 C88 119.6(14) . . ? C86 C87 H87 120.2 . . ? C88 C87 H87 120.2 . . ? C89 C88 C87 120.5(15) . . ? C89 C88 H88 119.8 . . ? C87 C88 H88 119.7 . . ? C88 C89 C90 119.9(14) . . ? C88 C89 H89 120.0 . . ? C90 C89 H89 120.0 . . ? C91 C90 C89 119.8(15) . . ? C91 C90 H90 120.1 . . ? C89 C90 H90 120.1 . . ? C86 C91 C90 119.8(15) . . ? C86 C91 H91 120.1 . . ? C90 C91 H91 120.1 . . ? O27 C92 O26 124.9(14) . . ? O27 C92 C93 116.0(13) . . ? O26 C92 C93 119.1(14) . . ? C98 C93 C94 118.5(15) . . ? C98 C93 C92 121.0(15) . . ? C94 C93 C92 120.5(14) . . ? C93 C94 C95 121.9(17) . . ? C93 C94 H94 119.0 . . ? C95 C94 H94 119.1 . . ? C96 C95 C94 116.7(18) . . ? C96 C95 H95 121.7 . . ? C94 C95 H95 121.7 . . ? C97 C96 C95 122.4(17) . . ? C97 C96 H96 118.8 . . ? C95 C96 H96 118.8 . . ? C96 C97 C98 120.6(18) . . ? C96 C97 H97 119.7 . . ? C98 C97 H97 119.7 . . ? C97 C98 C93 119.9(17) . . ? C97 C98 H98 120.0 . . ? C93 C98 H98 120.0 . . ? O28 C99 O29 121.6(13) . . ? O28 C99 C100 117.9(13) . . ? O29 C99 C100 120.4(12) . . ? C101 C100 C105 119.8(17) . . ? C101 C100 C99 123.4(15) . . ? C105 C100 C99 116.6(16) . . ? C102 C101 C100 120.9(17) . . ? C102 C101 H101 119.6 . . ? C100 C101 H101 119.6 . . ? C101 C102 C103 121(2) . . ? C101 C102 H102 119.4 . . ? C103 C102 H102 119.4 . . ? C104 C103 C102 117(2) . . ? C104 C103 H103 121.6 . . ? C102 C103 H103 121.5 . . ? C105 C104 C103 122(2) . . ? C105 C104 H104 118.9 . . ? C103 C104 H104 118.9 . . ? C104 C105 C100 119(2) . . ? C104 C105 H105 120.7 . . ? C100 C105 H105 120.7 . . ? O31 C106 O30 119.7(15) . . ? O31 C106 C107 120.0(14) . . ? O30 C106 C107 120.4(14) . . ? C112 C107 C108 118.6(14) . . ? C112 C107 C106 121.6(13) . . ? C108 C107 C106 119.8(13) . . ? C109 C108 C107 121.5(16) . . ? C109 C108 H108 119.2 . . ? C107 C108 H108 119.3 . . ? C108 C109 C110 119.6(16) . . ? C108 C109 H109 120.2 . . ? C110 C109 H109 120.2 . . ? C111 C110 C109 119.4(16) . . ? C111 C110 H110 120.3 . . ? C109 C110 H110 120.3 . . ? C112 C111 C110 119.4(16) . . ? C112 C111 H111 120.3 . . ? C110 C111 H111 120.3 . . ? C107 C112 C111 121.5(14) . . ? C107 C112 H112 119.2 . . ? C111 C112 H112 119.3 . . ? O32 C113 O33 122.1(16) . . ? O32 C113 C114 117.6(15) . . ? O33 C113 C114 120.0(16) . . ? O35 C120 O34 124.8(15) . . ? O35 C120 C121 117.4(14) . . ? O34 C120 C121 117.8(14) . . ? C126 C121 C122 120.6(18) . . ? C126 C121 C120 119.9(17) . . ? C122 C121 C120 119.5(16) . . ? C123 C122 C121 120(2) . . ? C123 C122 H122 120.1 . . ? C121 C122 H122 120.1 . . ? C124 C123 C122 121(3) . . ? C124 C123 H123 119.5 . . ? C122 C123 H123 119.6 . . ? C125 C124 C123 120(2) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.9 . . ? C124 C125 C126 120(2) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C121 C126 C125 118(2) . . ? C121 C126 H126 121.2 . . ? C125 C126 H126 121.2 . . ? O37 C127 O36 127(2) . . ? O37 C127 C128 117.1(16) . . ? O36 C127 C128 116.0(19) . . ? C129 C128 C133 118(2) . . ? C129 C128 C127 123(2) . . ? C133 C128 C127 119.4(17) . . ? C128 C129 C130 122(2) . . ? C128 C129 H129 118.8 . . ? C130 C129 H129 118.8 . . ? C129 C130 C131 119(2) . . ? C129 C130 H130 120.6 . . ? C131 C130 H130 120.5 . . ? C132 C131 C130 120(2) . . ? C132 C131 H131 119.7 . . ? C130 C131 H131 119.9 . . ? C131 C132 C133 120(2) . . ? C131 C132 H132 120.0 . . ? C133 C132 H132 119.9 . . ? C132 C133 C128 120.3(19) . . ? C132 C133 H133 119.9 . . ? C128 C133 H133 119.8 . . ? C134 O40 Mn10 130.2(14) . . ? C140 C135 C136 117.9(19) . . ? C140 C135 C134 122(2) . . ? C136 C135 C134 120(2) . . ? C135 C136 C137 121(2) . . ? C135 C136 H136 119.4 . . ? C137 C136 H136 119.4 . . ? C138 C137 C136 118(2) . . ? C138 C137 H137 120.8 . . ? C136 C137 H137 120.7 . . ? C137 C138 C139 122(2) . . ? C137 C138 H138 119.2 . . ? C139 C138 H138 119.2 . . ? C140 C139 C138 118(3) . . ? C140 C139 H139 120.8 . . ? C138 C139 H139 120.9 . . ? C135 C140 C139 123(2) . . ? C135 C140 H140 118.7 . . ? C139 C140 H140 118.7 . . ? C1 O1 Mn1 135.2(10) . . ? C1 O1 Mn10 91.7(9) . 1_556 ? Mn1 O1 Mn10 108.1(5) . 1_556 ? C8 O2 Mn1 140.7(11) . . ? C8 O3 Mn2 119.3(9) . . ? C8 O3 Mn3 128.7(10) . . ? Mn2 O3 Mn3 94.9(3) . . ? C15 O4 Mn1 151.6(10) . . ? C15 O5 Mn10 123.8(9) . 1_556 ? C78 O6 Mn2 115.7(9) 4_546 . ? C78 O6 Mn1 146.5(10) 4_546 . ? Mn2 O6 Mn1 93.5(4) . . ? C22 O7 Mn2 119.5(8) . . ? C22 O7 Mn1 135.1(9) . . ? Mn2 O7 Mn1 95.5(4) . . ? C22 O8 Mn3 138.4(9) . . ? C29 O9 Mn1 143(3) . . ? C29 O10 Mn10 132(2) . 1_556 ? C64 O11 Mn2 133.1(10) 4_546 . ? C36 O12 Mn3 131.8(8) . . ? C36 O12 Mn2 91.7(8) . . ? Mn3 O12 Mn2 96.8(3) . . ? C43 O13 Mn3 137.9(8) . . ? C43 O13 Mn4 97.1(7) . . ? Mn3 O13 Mn4 106.4(4) . . ? C43 O14 Mn6 137.8(8) . . ? C43 O14 Mn4 89.2(7) . . ? Mn6 O14 Mn4 94.4(3) . . ? C50 O15 Mn3 140.2(9) . . ? C50 O16 Mn4 121.5(8) . . ? C50 O16 Mn5 131.1(9) . . ? Mn4 O16 Mn5 90.9(3) . . ? C57 O17 Mn3 140.8(10) . . ? C57 O18 Mn4 127.5(9) . . ? C64 O19 Mn5 130.8(8) . . ? C36 O20 Mn5 148.5(8) 4_556 . ? C36 O20 Mn2 92.3(8) 4_556 4_556 ? Mn5 O20 Mn2 101.6(4) . 4_556 ? C71 O21 Mn5 133.0(8) . . ? C71 O21 Mn4 90.2(8) . . ? Mn5 O21 Mn4 86.7(3) . . ? C71 O22 Mn6 142.7(8) . . ? C71 O22 Mn4 96.3(8) . . ? Mn6 O22 Mn4 97.6(3) . . ? C78 O23 Mn5 143.0(9) . . ? C85 O24 Mn5 141.8(8) . . ? C85 O24 Mn4 120.1(8) . . ? Mn5 O24 Mn4 90.3(3) . . ? C85 O25 Mn6 135.6(9) . . ? C92 O26 Mn6 129.5(10) . . ? C92 O27 Mn7 135.8(10) . . ? C99 O28 Mn6 172.2(11) . . ? C99 O29 Mn8 150.3(9) . . ? C99 O29 Mn7 98.9(8) . . ? Mn8 O29 Mn7 98.7(4) . . ? C106 O30 Mn6 135.5(9) . . ? C106 O30 Mn7 95.2(9) . . ? Mn6 O30 Mn7 98.8(4) . . ? C106 O31 Mn9 141.7(12) . . ? C106 O31 Mn7 89.9(9) . . ? Mn9 O31 Mn7 87.3(4) . . ? C113 O32 Mn9 147.9(13) . . ? C113 O32 Mn7 92.3(12) . . ? Mn9 O32 Mn7 86.1(6) . . ? C113 O33 Mn8 147.7(12) . . ? C113 O33 Mn7 91.0(10) . . ? Mn8 O33 Mn7 94.0(5) . . ? C120 O34 Mn7 126.4(10) . . ? C120 O34 Mn9 122.8(9) . . ? Mn7 O34 Mn9 91.1(4) . . ? C120 O35 Mn8 137.5(10) . . ? C127 O36 Mn9 138.9(16) . . ? C127 O37 Mn10 128.0(15) . . ? C1 O38 Mn9 147.5(11) 1_554 . ? C1 O38 Mn10 92.9(10) 1_554 . ? Mn9 O38 Mn10 104.5(6) . . ? C134 O39 Mn9 135.8(14) . . ? O9 Mn1 O4 104.7(8) . . ? O9 Mn1 O2 82.8(9) . . ? O4 Mn1 O2 172.4(6) . . ? O9 Mn1 O1 88.6(6) . . ? O4 Mn1 O1 87.4(4) . . ? O2 Mn1 O1 91.7(4) . . ? O9 Mn1 O7 85.0(6) . . ? O4 Mn1 O7 93.0(4) . . ? O2 Mn1 O7 88.7(4) . . ? O1 Mn1 O7 173.5(4) . . ? O9 Mn1 O6 158.5(7) . . ? O4 Mn1 O6 90.5(4) . . ? O2 Mn1 O6 82.6(6) . . ? O1 Mn1 O6 107.6(4) . . ? O7 Mn1 O6 78.9(4) . . ? O9 Mn1 Mn2 117.9(6) . . ? O4 Mn1 Mn2 106.1(3) . . ? O2 Mn1 Mn2 70.6(4) . . ? O1 Mn1 Mn2 144.6(3) . . ? O7 Mn1 Mn2 41.2(2) . . ? O6 Mn1 Mn2 41.7(2) . . ? O11 Mn2 O7 86.6(4) . . ? O11 Mn2 O6 95.3(4) . . ? O7 Mn2 O6 83.8(4) . . ? O11 Mn2 O3 162.1(4) . . ? O7 Mn2 O3 86.7(4) . . ? O6 Mn2 O3 100.4(4) . . ? O11 Mn2 O20 87.9(4) . 4_546 ? O7 Mn2 O20 160.7(3) . 4_546 ? O6 Mn2 O20 115.2(4) . 4_546 ? O3 Mn2 O20 93.0(4) . 4_546 ? O11 Mn2 O12 89.1(4) . . ? O7 Mn2 O12 103.8(3) . . ? O6 Mn2 O12 171.5(4) . . ? O3 Mn2 O12 76.5(3) . . ? O20 Mn2 O12 57.5(3) 4_546 . ? O11 Mn2 Mn1 106.2(3) . . ? O7 Mn2 Mn1 43.3(2) . . ? O6 Mn2 Mn1 44.8(3) . . ? O3 Mn2 Mn1 79.8(3) . . ? O20 Mn2 Mn1 155.4(2) 4_546 . ? O12 Mn2 Mn1 140.4(2) . . ? O17 Mn3 O15 92.6(4) . . ? O17 Mn3 O8 92.4(4) . . ? O15 Mn3 O8 174.1(4) . . ? O17 Mn3 O12 175.0(4) . . ? O15 Mn3 O12 87.8(4) . . ? O8 Mn3 O12 87.5(4) . . ? O17 Mn3 O13 94.5(4) . . ? O15 Mn3 O13 84.5(3) . . ? O8 Mn3 O13 92.0(3) . . ? O12 Mn3 O13 90.5(3) . . ? O17 Mn3 O3 97.7(4) . . ? O15 Mn3 O3 93.5(4) . . ? O8 Mn3 O3 88.9(4) . . ? O12 Mn3 O3 77.2(3) . . ? O13 Mn3 O3 167.7(4) . . ? O18 Mn4 O16 94.7(4) . . ? O18 Mn4 O13 93.0(3) . . ? O16 Mn4 O13 104.7(3) . . ? O18 Mn4 O24 164.8(4) . . ? O16 Mn4 O24 74.1(3) . . ? O13 Mn4 O24 99.6(3) . . ? O18 Mn4 O22 95.3(4) . . ? O16 Mn4 O22 128.5(3) . . ? O13 Mn4 O22 124.9(3) . . ? O24 Mn4 O22 84.3(3) . . ? O18 Mn4 O14 89.9(4) . . ? O16 Mn4 O14 159.6(3) . . ? O13 Mn4 O14 55.2(3) . . ? O24 Mn4 O14 104.1(3) . . ? O22 Mn4 O14 70.5(3) . . ? O18 Mn4 O21 94.5(3) . . ? O16 Mn4 O21 75.0(3) . . ? O13 Mn4 O21 172.5(3) . . ? O24 Mn4 O21 73.0(3) . . ? O22 Mn4 O21 53.9(3) . . ? O14 Mn4 O21 124.4(3) . . ? O18 Mn4 Mn5 120.3(3) . . ? O16 Mn4 Mn5 44.8(2) . . ? O13 Mn4 Mn5 132.2(2) . . ? O24 Mn4 Mn5 44.6(2) . . ? O22 Mn4 Mn5 87.7(2) . . ? O14 Mn4 Mn5 144.7(2) . . ? O21 Mn4 Mn5 42.8(2) . . ? O19 Mn5 O23 92.9(4) . . ? O19 Mn5 O21 172.1(4) . . ? O23 Mn5 O21 94.9(4) . . ? O19 Mn5 O20 98.2(3) . . ? O23 Mn5 O20 87.7(4) . . ? O21 Mn5 O20 82.0(3) . . ? O19 Mn5 O24 100.3(3) . . ? O23 Mn5 O24 94.3(4) . . ? O21 Mn5 O24 79.3(3) . . ? O20 Mn5 O24 161.3(3) . . ? O19 Mn5 O16 91.5(3) . . ? O23 Mn5 O16 168.3(4) . . ? O21 Mn5 O16 80.8(4) . . ? O20 Mn5 O16 102.4(3) . . ? O24 Mn5 O16 74.2(3) . . ? O19 Mn5 Mn4 124.1(3) . . ? O23 Mn5 Mn4 125.2(3) . . ? O21 Mn5 Mn4 50.5(3) . . ? O20 Mn5 Mn4 119.9(3) . . ? O24 Mn5 Mn4 45.1(2) . . ? O16 Mn5 Mn4 44.3(2) . . ? O25 Mn6 O26 90.9(4) . . ? O25 Mn6 O28 173.7(4) . . ? O26 Mn6 O28 93.6(4) . . ? O25 Mn6 O30 93.0(4) . . ? O26 Mn6 O30 94.9(4) . . ? O28 Mn6 O30 82.1(4) . . ? O25 Mn6 O22 92.4(3) . . ? O26 Mn6 O22 94.0(4) . . ? O28 Mn6 O22 91.8(4) . . ? O30 Mn6 O22 169.6(4) . . ? O25 Mn6 O14 86.9(4) . . ? O26 Mn6 O14 171.1(4) . . ? O28 Mn6 O14 89.4(4) . . ? O30 Mn6 O14 93.9(4) . . ? O22 Mn6 O14 77.5(3) . . ? O27 Mn7 O34 156.7(5) . . ? O27 Mn7 O29 107.0(5) . . ? O34 Mn7 O29 90.6(4) . . ? O27 Mn7 O30 96.4(4) . . ? O34 Mn7 O30 90.5(4) . . ? O29 Mn7 O30 113.1(3) . . ? O27 Mn7 O31 91.4(5) . . ? O34 Mn7 O31 74.3(4) . . ? O29 Mn7 O31 159.9(4) . . ? O30 Mn7 O31 55.2(3) . . ? O27 Mn7 O32 80.4(5) . . ? O34 Mn7 O32 77.2(5) . . ? O29 Mn7 O32 122.1(4) . . ? O30 Mn7 O32 123.2(4) . . ? O31 Mn7 O32 68.1(4) . . ? O27 Mn7 O33 79.6(4) . . ? O34 Mn7 O33 91.3(4) . . ? O29 Mn7 O33 73.4(3) . . ? O30 Mn7 O33 173.3(3) . . ? O31 Mn7 O33 119.1(4) . . ? O32 Mn7 O33 51.0(4) . . ? O27 Mn7 Mn9 111.7(4) . . ? O34 Mn7 Mn9 45.7(3) . . ? O29 Mn7 Mn9 131.1(3) . . ? O30 Mn7 Mn9 91.5(3) . . ? O31 Mn7 Mn9 43.0(3) . . ? O32 Mn7 Mn9 42.0(4) . . ? O33 Mn7 Mn9 85.1(3) . . ? O33 Mn8 O33 95.9(7) . 2_665 ? O33 Mn8 O35 96.1(5) . . ? O33 Mn8 O35 92.3(5) 2_665 . ? O33 Mn8 O35 92.3(5) . 2_665 ? O33 Mn8 O35 96.1(5) 2_665 2_665 ? O35 Mn8 O35 167.4(5) . 2_665 ? O33 Mn8 O29 82.6(4) . . ? O33 Mn8 O29 176.0(5) 2_665 . ? O35 Mn8 O29 84.1(4) . . ? O35 Mn8 O29 87.7(4) 2_665 . ? O33 Mn8 O29 176.0(5) . 2_665 ? O33 Mn8 O29 82.6(4) 2_665 2_665 ? O35 Mn8 O29 87.7(4) . 2_665 ? O35 Mn8 O29 84.1(4) 2_665 2_665 ? O29 Mn8 O29 99.1(5) . 2_665 ? O36 Mn9 O39 99.0(7) . . ? O36 Mn9 O32 168.9(6) . . ? O39 Mn9 O32 91.9(7) . . ? O36 Mn9 O31 89.1(5) . . ? O39 Mn9 O31 164.1(5) . . ? O32 Mn9 O31 79.9(6) . . ? O36 Mn9 O38 89.8(6) . . ? O39 Mn9 O38 97.4(5) . . ? O32 Mn9 O38 90.2(6) . . ? O31 Mn9 O38 96.2(4) . . ? O36 Mn9 O34 95.5(5) . . ? O39 Mn9 O34 87.9(4) . . ? O32 Mn9 O34 83.4(5) . . ? O31 Mn9 O34 77.7(4) . . ? O38 Mn9 O34 171.8(5) . . ? O36 Mn9 Mn7 120.9(4) . . ? O39 Mn9 Mn7 114.7(4) . . ? O32 Mn9 Mn7 51.8(5) . . ? O31 Mn9 Mn7 49.7(3) . . ? O38 Mn9 Mn7 128.6(4) . . ? O34 Mn9 Mn7 43.2(3) . . ? O5 Mn10 O40 95.8(5) 1_554 . ? O5 Mn10 O37 91.1(5) 1_554 . ? O40 Mn10 O37 94.5(5) . . ? O5 Mn10 O38 159.0(4) 1_554 . ? O40 Mn10 O38 105.0(5) . . ? O37 Mn10 O38 89.3(5) . . ? O5 Mn10 O1 102.7(4) 1_554 1_554 ? O40 Mn10 O1 160.2(6) . 1_554 ? O37 Mn10 O1 92.0(4) . 1_554 ? O38 Mn10 O1 56.3(4) . 1_554 ? O5 Mn10 O10 93.6(6) 1_554 1_554 ? O40 Mn10 O10 83.2(7) . 1_554 ? O37 Mn10 O10 175.0(6) . 1_554 ? O38 Mn10 O10 86.9(7) . 1_554 ? O1 Mn10 O10 88.7(6) 1_554 1_554 ? O39 C134 O40 125.8(17) . . ? O39 C134 C135 118.6(19) . . ? O40 C134 C135 116(2) . . ? C115 C114 C119 120.0 . . ? C115 C114 C113 119.6(13) . . ? C119 C114 C113 120.3(13) . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 C117 120.0 . . ? C115 C116 H116 120.0 . . ? C117 C116 H116 120.0 . . ? C116 C117 C118 120.0 . . ? C116 C117 H117 120.0 . . ? C118 C117 H117 120.0 . . ? C119 C118 C117 120.0 . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C118 C119 C114 120.0 . . ? C118 C119 H119 120.0 . . ? C114 C119 H119 120.0 . . ? O9 C29 O10 117(4) . . ? O9 C29 C30 122(3) . . ? O10 C29 C30 120(3) . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C35 C30 C31 120.0 . . ? C35 C30 C29 120(2) . . ? C31 C30 C29 120(2) . . ? C34 C35 C30 120.0 . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.964 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 949071' ####################################################################### # # 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_comp _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124 H143 Mn6 O34' _chemical_formula_weight 2507.02 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4356(3) _cell_length_b 12.0816(2) _cell_length_c 21.5601(5) _cell_angle_alpha 85.3518(12) _cell_angle_beta 89.0215(12) _cell_angle_gamma 82.4410(14) _cell_volume 2943.28(14) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36242 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'claret ' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1309 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17266 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9663 _reflns_number_gt 8556 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0224P)^2^+6.5232P] 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 9663 _refine_ls_number_parameters 749 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.6624(2) 0.2035(2) 0.45914(14) 0.0169(6) Uani 1 1 d . A . C2 C 0.7194(2) 0.1776(2) 0.39816(14) 0.0176(6) Uani 1 1 d . . . C3 C 0.7385(3) 0.2654(3) 0.35450(14) 0.0219(7) Uani 1 1 d . . . H3 H 0.7173 0.3407 0.3642 0.026 Uiso 1 1 calc R . . C4 C 0.7883(3) 0.2431(3) 0.29702(15) 0.0280(7) Uani 1 1 d . . . H4 H 0.7990 0.3029 0.2670 0.034 Uiso 1 1 calc R . . C5 C 0.8223(3) 0.1335(3) 0.28359(16) 0.0304(8) Uani 1 1 d . . . H5 H 0.8578 0.1182 0.2445 0.037 Uiso 1 1 calc R . . C6 C 0.8047(3) 0.0459(3) 0.32687(16) 0.0279(7) Uani 1 1 d . . . H6 H 0.8288 -0.0292 0.3174 0.034 Uiso 1 1 calc R . . C7 C 0.7521(3) 0.0674(3) 0.38408(14) 0.0205(7) Uani 1 1 d . . . H7 H 0.7386 0.0072 0.4133 0.025 Uiso 1 1 calc R . . C8 C 0.3292(3) 0.2313(2) 0.50605(13) 0.0162(6) Uani 1 1 d . . . C9 C 0.2142(3) 0.2767(2) 0.47477(13) 0.0176(6) Uani 1 1 d . . . C10 C 0.1732(3) 0.3907(2) 0.47031(16) 0.0237(7) Uani 1 1 d . . . H10 H 0.2169 0.4415 0.4884 0.028 Uiso 1 1 calc R . . C11 C 0.0686(3) 0.4303(3) 0.43950(18) 0.0320(8) Uani 1 1 d . . . H11 H 0.0417 0.5083 0.4361 0.038 Uiso 1 1 calc R . . C12 C 0.0028(3) 0.3574(3) 0.41354(16) 0.0306(8) Uani 1 1 d . . . H12 H -0.0688 0.3851 0.3926 0.037 Uiso 1 1 calc R . . C13 C 0.0428(3) 0.2431(3) 0.41861(16) 0.0272(7) Uani 1 1 d . . . H13 H -0.0015 0.1923 0.4011 0.033 Uiso 1 1 calc R . . C14 C 0.1474(3) 0.2035(3) 0.44918(15) 0.0233(7) Uani 1 1 d . . . H14 H 0.1739 0.1254 0.4528 0.028 Uiso 1 1 calc R . . C15 C 0.5254(2) 0.0297(2) 0.64423(13) 0.0156(6) Uani 1 1 d . . . C16 C 0.5240(2) -0.0298(2) 0.70824(13) 0.0154(6) Uani 1 1 d . . . C17 C 0.5410(3) 0.0251(2) 0.76080(14) 0.0186(6) Uani 1 1 d . . . H17 H 0.5489 0.1027 0.7567 0.022 Uiso 1 1 calc R . . C18 C 0.5465(3) -0.0327(3) 0.81954(15) 0.0249(7) Uani 1 1 d . . . H18 H 0.5601 0.0051 0.8552 0.030 Uiso 1 1 calc R . . C19 C 0.5321(3) -0.1451(3) 0.82598(14) 0.0226(7) Uani 1 1 d . . . H19 H 0.5360 -0.1845 0.8660 0.027 Uiso 1 1 calc R . . C20 C 0.5120(3) -0.1997(3) 0.77387(15) 0.0247(7) Uani 1 1 d . . . H20 H 0.5003 -0.2764 0.7784 0.030 Uiso 1 1 calc R . . C21 C 0.5088(3) -0.1430(2) 0.71478(14) 0.0194(6) Uani 1 1 d . . . H21 H 0.4964 -0.1812 0.6791 0.023 Uiso 1 1 calc R . . C22 C 0.5418(3) 0.5059(2) 0.58167(15) 0.0256(7) Uani 1 1 d . A . H22A H 0.4591 0.5317 0.5694 0.031 Uiso 1 1 calc R . . H22B H 0.5926 0.5076 0.5440 0.031 Uiso 1 1 calc R . . C23 C 0.5817(3) 0.5778(2) 0.62919(11) 0.0451(11) Uani 1 1 d . . . H23A H 0.6684 0.5763 0.6278 0.054 Uiso 0.688(6) 1 calc PR A 1 H23B H 0.5441 0.6563 0.6219 0.054 Uiso 0.688(6) 1 calc PR A 1 H23C H 0.6448 0.6196 0.6113 0.054 Uiso 0.688(6) 1 d PR A 2 H23D H 0.5148 0.6325 0.6415 0.054 Uiso 0.688(6) 1 d PR A 2 C25 C 0.5484(3) 0.4014(2) 0.67954(11) 0.0404(10) Uani 1 1 d R . . H25A H 0.6196 0.3581 0.6993 0.048 Uiso 0.688(6) 1 calc PR A 1 H25B H 0.4778 0.3710 0.6975 0.048 Uiso 0.688(6) 1 calc PR A 1 H25C H 0.6448 0.6196 0.6113 0.048 Uiso 0.688(6) 1 d PR A 2 H25D H 0.5148 0.6325 0.6415 0.048 Uiso 0.688(6) 1 d PR A 2 C26 C 0.8370(3) 0.2851(3) 0.58731(15) 0.0233(7) Uani 1 1 d . . . H26A H 0.8340 0.3421 0.6180 0.028 Uiso 1 1 calc R . . H26B H 0.8216 0.3236 0.5454 0.028 Uiso 1 1 calc R . . C27 C 0.9561(3) 0.2128(3) 0.58882(18) 0.0332(8) Uani 1 1 d . . . H27A H 0.9911 0.2057 0.6309 0.040 Uiso 1 1 calc R . . H27B H 1.0117 0.2436 0.5584 0.040 Uiso 1 1 calc R . . C28 C 0.9248(3) 0.1008(3) 0.57091(18) 0.0348(8) Uani 1 1 d . . . H28A H 0.9145 0.1010 0.5254 0.042 Uiso 1 1 calc R . . H28B H 0.9857 0.0382 0.5850 0.042 Uiso 1 1 calc R . . C29 C 0.8091(3) 0.0935(3) 0.60562(15) 0.0235(7) Uani 1 1 d . . . H29A H 0.7606 0.0450 0.5852 0.028 Uiso 1 1 calc R . . H29B H 0.8233 0.0631 0.6493 0.028 Uiso 1 1 calc R . . C30 C 0.1614(3) 0.2490(2) 0.03996(13) 0.0170(6) Uani 1 1 d . . . C31 C 0.2887(3) 0.2530(2) 0.02554(13) 0.0163(6) Uani 1 1 d . . . C32 C 0.3587(3) 0.1560(2) 0.00924(14) 0.0204(7) Uani 1 1 d . . . H32 H 0.3245 0.0890 0.0067 0.025 Uiso 1 1 calc R . . C33 C 0.4776(3) 0.1570(3) -0.00329(15) 0.0244(7) Uani 1 1 d . . . H33 H 0.5246 0.0913 -0.0154 0.029 Uiso 1 1 calc R . . C34 C 0.5283(3) 0.2548(3) 0.00188(15) 0.0270(7) Uani 1 1 d . . . H34 H 0.6103 0.2556 -0.0058 0.032 Uiso 1 1 calc R . . C35 C 0.4587(3) 0.3502(3) 0.01822(15) 0.0262(7) Uani 1 1 d . . . H35 H 0.4933 0.4167 0.0217 0.031 Uiso 1 1 calc R . . C36 C 0.3382(3) 0.3507(3) 0.02979(14) 0.0213(7) Uani 1 1 d . . . H36 H 0.2908 0.4171 0.0404 0.026 Uiso 1 1 calc R . . C37 C -0.1970(3) 0.4604(2) 0.10206(14) 0.0184(6) Uani 1 1 d . . . C38 C -0.3102(3) 0.5224(2) 0.12458(13) 0.0165(6) Uani 1 1 d . . . C39 C -0.4080(3) 0.4667(3) 0.13606(14) 0.0212(7) Uani 1 1 d . . . H39 H -0.4017 0.3883 0.1323 0.025 Uiso 1 1 calc R . . C40 C -0.5150(3) 0.5248(3) 0.15297(15) 0.0250(7) Uani 1 1 d . . . H40 H -0.5824 0.4868 0.1592 0.030 Uiso 1 1 calc R . . C41 C -0.5236(3) 0.6385(3) 0.16077(14) 0.0237(7) Uani 1 1 d . . . H41 H -0.5966 0.6782 0.1728 0.028 Uiso 1 1 calc R . . C42 C -0.4258(3) 0.6934(3) 0.15090(14) 0.0242(7) Uani 1 1 d . . . H42 H -0.4313 0.7709 0.1572 0.029 Uiso 1 1 calc R . . C43 C -0.3193(3) 0.6367(2) 0.13188(14) 0.0209(7) Uani 1 1 d . . . H43 H -0.2530 0.6756 0.1239 0.025 Uiso 1 1 calc R . . C44 C 0.1316(3) 0.6914(2) 0.05389(15) 0.0200(7) Uani 1 1 d . . . C45 C 0.1586(3) 0.7184(2) 0.11826(15) 0.0198(7) Uani 1 1 d . . . C46 C 0.1450(3) 0.6420(3) 0.16845(16) 0.0308(8) Uani 1 1 d . . . H46 H 0.1221 0.5713 0.1615 0.037 Uiso 1 1 calc R . . C47 C 0.1644(3) 0.6673(4) 0.22887(17) 0.0401(9) Uani 1 1 d . . . H47 H 0.1544 0.6144 0.2630 0.048 Uiso 1 1 calc R . . C48 C 0.1984(3) 0.7699(3) 0.23886(18) 0.0375(9) Uani 1 1 d . . . H48 H 0.2115 0.7878 0.2801 0.045 Uiso 1 1 calc R . . C49 C 0.2134(3) 0.8464(3) 0.18946(18) 0.0316(8) Uani 1 1 d . . . H49 H 0.2368 0.9169 0.1967 0.038 Uiso 1 1 calc R . . C50 C 0.1944(3) 0.8208(3) 0.12900(16) 0.0255(7) Uani 1 1 d . . . H50 H 0.2059 0.8733 0.0950 0.031 Uiso 1 1 calc R . . C51 C -0.0753(3) -0.0179(2) 0.07959(16) 0.0248(7) Uani 1 1 d . . . H51A H 0.0119 -0.0320 0.0811 0.030 Uiso 1 1 calc R . . H51B H -0.1008 -0.0131 0.0357 0.030 Uiso 1 1 calc R . . C52 C -0.1301(3) -0.1089(3) 0.11844(17) 0.0306(8) Uani 1 1 d . . . H52A H -0.0798 -0.1390 0.1544 0.037 Uiso 1 1 calc R . . H52B H -0.1424 -0.1712 0.0931 0.037 Uiso 1 1 calc R . . C53 C -0.2486(3) -0.0478(3) 0.14000(17) 0.0292(8) Uani 1 1 d . . . H53A H -0.3154 -0.0748 0.1197 0.035 Uiso 1 1 calc R . . H53B H -0.2579 -0.0597 0.1857 0.035 Uiso 1 1 calc R . . C54 C -0.2433(3) 0.0759(3) 0.12024(16) 0.0246(7) Uani 1 1 d . . . H54A H -0.2900 0.0996 0.0821 0.030 Uiso 1 1 calc R . . H54B H -0.2741 0.1235 0.1537 0.030 Uiso 1 1 calc R . . C55 C 0.1096(3) 0.1418(3) 0.19867(15) 0.0269(7) Uani 1 1 d . . . H55A H 0.1732 0.1230 0.1681 0.032 Uiso 1 1 calc R . . H55B H 0.0709 0.0743 0.2100 0.032 Uiso 1 1 calc R . . C56 C 0.1582(3) 0.1836(3) 0.25533(18) 0.0382(9) Uani 1 1 d . . . H56A H 0.2389 0.1462 0.2646 0.046 Uiso 1 1 calc R . . H56B H 0.1069 0.1724 0.2922 0.046 Uiso 1 1 calc R . . C57 C 0.1580(4) 0.3078(3) 0.2355(2) 0.0477(11) Uani 1 1 d . . . H57A H 0.1564 0.3525 0.2721 0.057 Uiso 1 1 calc R . . H57B H 0.2278 0.3206 0.2095 0.057 Uiso 1 1 calc R . . C58 C 0.0455(3) 0.3364(3) 0.19859(16) 0.0280(7) Uani 1 1 d . . . H58A H -0.0209 0.3636 0.2258 0.034 Uiso 1 1 calc R . . H58B H 0.0546 0.3951 0.1648 0.034 Uiso 1 1 calc R . . C59 C 0.8678(4) 0.5875(3) 0.2723(2) 0.0480(10) Uani 1 1 d . . . H59A H 0.8624 0.5651 0.2293 0.058 Uiso 1 1 calc R . . H59B H 0.9502 0.5669 0.2865 0.058 Uiso 1 1 calc R . . C60 C 0.8316(4) 0.7128(3) 0.27382(18) 0.0413(9) Uani 1 1 d . . . H60A H 0.7837 0.7434 0.2371 0.050 Uiso 1 1 calc R . . H60B H 0.9016 0.7528 0.2751 0.050 Uiso 1 1 calc R . . C61 C 0.7586(3) 0.7225(3) 0.33410(19) 0.0365(9) Uani 1 1 d . . . H61A H 0.7909 0.7720 0.3620 0.044 Uiso 1 1 calc R . . H61B H 0.6751 0.7515 0.3251 0.044 Uiso 1 1 calc R . . C62 C 0.7709(4) 0.6032(3) 0.36224(19) 0.0423(9) Uani 1 1 d . . . H62A H 0.8379 0.5888 0.3915 0.051 Uiso 1 1 calc R . . H62B H 0.6980 0.5884 0.3851 0.051 Uiso 1 1 calc R . . O1 O 0.65327(18) 0.30079(16) 0.47620(9) 0.0184(4) Uani 1 1 d . A . O2 O 0.62420(17) 0.12461(15) 0.49405(9) 0.0158(4) Uani 1 1 d . A . O3 O 0.39240(17) 0.30103(16) 0.52375(10) 0.0193(5) Uani 1 1 d . A . O4 O 0.35460(18) 0.12686(16) 0.51306(10) 0.0205(5) Uani 1 1 d . A . O5 O 0.52525(18) 0.13562(16) 0.64160(9) 0.0183(4) Uani 1 1 d . A . O6 O 0.52889(18) -0.02792(16) 0.59858(9) 0.0179(4) Uani 1 1 d . A . O7 O 0.55296(19) 0.39497(16) 0.61304(9) 0.0208(5) Uani 1 1 d . A . O8 O 0.75094(17) 0.20857(16) 0.60300(10) 0.0183(4) Uani 1 1 d . A . O10 O 0.09219(17) 0.34094(16) 0.04573(9) 0.0181(4) Uani 1 1 d . . . O9 O 0.12255(18) 0.15626(16) 0.04849(10) 0.0198(5) Uani 1 1 d . . . O11 O -0.18864(19) 0.35422(17) 0.10921(11) 0.0251(5) Uani 1 1 d . . . O12 O -0.11953(18) 0.51537(17) 0.07869(10) 0.0211(5) Uani 1 1 d . . . O13 O 0.11390(18) 0.59324(17) 0.04623(10) 0.0214(5) Uani 1 1 d . . . O14 O -0.1274(2) 0.22910(18) -0.01156(10) 0.0263(5) Uani 1 1 d . . . O15 O -0.11943(17) 0.08313(16) 0.10880(10) 0.0190(4) Uani 1 1 d . . . O16 O 0.02441(18) 0.23344(16) 0.17316(10) 0.0211(5) Uani 1 1 d . . . O17 O 0.7911(3) 0.5337(2) 0.31172(14) 0.0492(7) Uani 1 1 d . . . Mn1 Mn 0.55926(4) 0.24390(3) 0.56549(2) 0.01405(11) Uani 1 1 d . . . Mn2 Mn 0.5000 0.0000 0.5000 0.01249(13) Uani 1 2 d S . . Mn3 Mn -0.05540(4) 0.24031(4) 0.07711(2) 0.01660(11) Uani 1 1 d . . . Mn4 Mn 0.0000 0.5000 0.0000 0.01367(14) Uani 1 2 d S . . C24 C 0.5428(5) 0.5261(4) 0.6899(2) 0.0249(10) Uani 0.688(6) 1 d PU A 1 H24A H 0.4615 0.5585 0.7004 0.030 Uiso 0.688(6) 1 calc PR A 1 H24B H 0.5962 0.5374 0.7238 0.030 Uiso 0.688(6) 1 calc PR A 1 C24A C 0.6308(11) 0.5077(9) 0.6790(5) 0.0285(14) Uani 0.312(6) 1 d PU A 2 H24C H 0.6220 0.5450 0.7183 0.034 Uiso 0.312(6) 1 calc PR A 2 H24D H 0.7153 0.4818 0.6716 0.034 Uiso 0.312(6) 1 calc PR A 2 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 C1 0.0126(14) 0.0181(15) 0.0199(15) 0.0034(12) -0.0056(12) -0.0043(12) C2 0.0112(14) 0.0227(16) 0.0198(16) -0.0005(12) -0.0031(12) -0.0055(12) C3 0.0198(16) 0.0239(16) 0.0236(17) -0.0001(13) -0.0030(13) -0.0092(13) C4 0.0262(17) 0.0360(19) 0.0230(17) 0.0051(14) 0.0042(14) -0.0144(15) C5 0.0222(17) 0.049(2) 0.0227(17) -0.0070(15) 0.0088(14) -0.0136(16) C6 0.0239(17) 0.0301(18) 0.0310(19) -0.0077(15) 0.0000(15) -0.0050(14) C7 0.0182(15) 0.0223(16) 0.0218(16) -0.0016(13) 0.0001(13) -0.0056(13) C8 0.0166(15) 0.0151(15) 0.0165(15) -0.0006(11) 0.0049(12) -0.0020(12) C9 0.0168(15) 0.0199(15) 0.0159(15) 0.0004(12) 0.0007(12) -0.0029(12) C10 0.0215(16) 0.0140(15) 0.0364(19) 0.0010(13) -0.0056(14) -0.0059(13) C11 0.0234(17) 0.0186(17) 0.053(2) 0.0031(15) -0.0106(16) -0.0014(14) C12 0.0241(17) 0.0329(19) 0.035(2) 0.0021(15) -0.0104(15) -0.0051(15) C13 0.0237(17) 0.0267(18) 0.0338(19) -0.0087(14) -0.0059(15) -0.0079(14) C14 0.0222(16) 0.0171(15) 0.0308(18) -0.0039(13) 0.0015(14) -0.0026(13) C15 0.0115(14) 0.0178(15) 0.0173(15) 0.0001(12) -0.0012(12) -0.0025(11) C16 0.0116(14) 0.0183(15) 0.0160(15) 0.0015(12) 0.0010(11) -0.0023(11) C17 0.0177(15) 0.0174(15) 0.0204(16) -0.0020(12) -0.0018(12) -0.0010(12) C18 0.0269(17) 0.0311(18) 0.0167(16) -0.0053(13) -0.0015(13) -0.0021(14) C19 0.0207(16) 0.0271(17) 0.0175(16) 0.0071(13) 0.0015(13) 0.0004(13) C20 0.0251(17) 0.0188(16) 0.0298(18) 0.0042(13) 0.0006(14) -0.0053(13) C21 0.0189(15) 0.0196(15) 0.0202(16) -0.0004(12) -0.0032(13) -0.0043(12) C22 0.044(2) 0.0114(15) 0.0214(16) 0.0014(12) -0.0032(15) -0.0051(14) C23 0.084(3) 0.0242(19) 0.032(2) -0.0065(16) 0.003(2) -0.023(2) C25 0.083(3) 0.0218(18) 0.0188(18) -0.0040(14) -0.0086(19) -0.0143(19) C26 0.0201(16) 0.0265(17) 0.0259(17) -0.0006(13) -0.0005(13) -0.0133(13) C27 0.0205(17) 0.044(2) 0.037(2) -0.0066(17) -0.0009(15) -0.0095(16) C28 0.0234(18) 0.036(2) 0.045(2) -0.0144(17) 0.0021(16) 0.0012(15) C29 0.0242(17) 0.0183(16) 0.0268(17) -0.0013(13) -0.0076(14) 0.0015(13) C30 0.0236(16) 0.0147(15) 0.0121(14) 0.0004(11) -0.0019(12) -0.0013(12) C31 0.0173(15) 0.0182(15) 0.0131(14) 0.0048(11) -0.0024(12) -0.0045(12) C32 0.0231(16) 0.0168(15) 0.0213(16) 0.0004(12) -0.0014(13) -0.0034(12) C33 0.0178(16) 0.0280(17) 0.0255(17) 0.0026(14) 0.0020(13) 0.0005(13) C34 0.0175(16) 0.0343(19) 0.0284(18) 0.0089(14) -0.0014(14) -0.0068(14) C35 0.0270(17) 0.0245(17) 0.0279(18) 0.0108(14) -0.0092(14) -0.0136(14) C36 0.0260(17) 0.0165(15) 0.0211(16) 0.0043(12) -0.0052(13) -0.0043(13) C37 0.0186(15) 0.0202(16) 0.0162(15) -0.0015(12) -0.0016(12) -0.0018(13) C38 0.0179(15) 0.0159(14) 0.0148(14) -0.0005(11) 0.0005(12) -0.0001(12) C39 0.0213(16) 0.0177(15) 0.0235(16) 0.0004(12) 0.0014(13) 0.0001(13) C40 0.0193(16) 0.0296(18) 0.0263(17) -0.0002(14) 0.0043(13) -0.0065(14) C41 0.0206(16) 0.0270(17) 0.0201(16) 0.0003(13) 0.0029(13) 0.0072(13) C42 0.0326(18) 0.0178(16) 0.0211(16) -0.0033(13) 0.0046(14) 0.0012(14) C43 0.0230(16) 0.0190(15) 0.0210(16) -0.0017(12) 0.0007(13) -0.0042(13) C44 0.0135(14) 0.0206(16) 0.0262(17) -0.0019(13) 0.0007(13) -0.0031(12) C45 0.0132(14) 0.0195(15) 0.0272(17) -0.0085(13) -0.0003(13) 0.0001(12) C46 0.0345(19) 0.0322(19) 0.0292(19) -0.0054(15) 0.0007(15) -0.0151(16) C47 0.045(2) 0.056(3) 0.0239(19) -0.0060(17) 0.0038(17) -0.0208(19) C48 0.0295(19) 0.053(2) 0.031(2) -0.0220(18) -0.0016(16) 0.0023(17) C49 0.0223(17) 0.0243(18) 0.049(2) -0.0199(16) -0.0118(16) 0.0052(14) C50 0.0197(16) 0.0203(16) 0.0360(19) -0.0052(14) -0.0104(14) 0.0018(13) C51 0.0250(17) 0.0166(15) 0.0327(18) -0.0044(13) 0.0082(14) -0.0023(13) C52 0.0347(19) 0.0156(16) 0.042(2) 0.0001(14) 0.0110(16) -0.0085(14) C53 0.0267(18) 0.0270(18) 0.035(2) 0.0007(15) 0.0054(15) -0.0107(14) C54 0.0139(15) 0.0243(17) 0.0345(19) 0.0041(14) 0.0011(14) -0.0025(13) C55 0.0247(17) 0.0246(17) 0.0286(18) 0.0021(14) 0.0019(14) 0.0043(14) C56 0.033(2) 0.041(2) 0.038(2) 0.0019(17) -0.0120(17) 0.0039(17) C57 0.037(2) 0.044(2) 0.066(3) -0.013(2) -0.020(2) -0.0088(18) C58 0.0342(19) 0.0212(17) 0.0303(19) -0.0069(14) -0.0002(15) -0.0064(14) C59 0.052(3) 0.044(2) 0.047(3) -0.0083(19) 0.008(2) -0.003(2) C60 0.051(2) 0.040(2) 0.033(2) 0.0085(17) -0.0008(18) -0.0137(19) C61 0.0248(18) 0.033(2) 0.051(2) -0.0070(17) 0.0066(17) -0.0011(15) C62 0.047(2) 0.041(2) 0.039(2) -0.0063(18) 0.0119(19) -0.0033(18) O1 0.0207(11) 0.0150(10) 0.0201(11) -0.0010(8) -0.0001(9) -0.0056(8) O2 0.0182(10) 0.0136(10) 0.0164(10) 0.0000(8) -0.0001(8) -0.0059(8) O3 0.0164(10) 0.0153(10) 0.0253(12) 0.0017(9) -0.0043(9) -0.0007(8) O4 0.0182(11) 0.0146(11) 0.0276(12) -0.0001(9) 0.0024(9) 0.0009(9) O5 0.0208(11) 0.0143(10) 0.0201(11) 0.0009(8) 0.0017(9) -0.0044(8) O6 0.0224(11) 0.0180(10) 0.0137(10) 0.0003(8) -0.0026(9) -0.0048(9) O7 0.0343(12) 0.0109(10) 0.0171(11) -0.0008(8) -0.0035(9) -0.0014(9) O8 0.0161(10) 0.0148(10) 0.0246(11) -0.0013(8) 0.0012(9) -0.0046(8) O10 0.0186(11) 0.0125(10) 0.0224(11) 0.0007(8) 0.0002(9) -0.0001(8) O9 0.0192(11) 0.0142(11) 0.0267(12) -0.0039(9) 0.0029(9) -0.0042(8) O11 0.0214(11) 0.0171(11) 0.0349(13) 0.0002(9) 0.0058(10) 0.0026(9) O12 0.0187(11) 0.0231(11) 0.0221(11) -0.0046(9) 0.0054(9) -0.0039(9) O13 0.0219(11) 0.0173(11) 0.0268(12) -0.0065(9) -0.0047(9) -0.0056(9) O14 0.0295(12) 0.0224(12) 0.0275(12) 0.0019(10) -0.0068(10) -0.0072(10) O15 0.0176(10) 0.0126(10) 0.0271(12) -0.0027(8) 0.0026(9) -0.0025(8) O16 0.0227(11) 0.0147(10) 0.0257(12) -0.0026(9) -0.0027(9) -0.0003(9) O17 0.0581(19) 0.0345(15) 0.0564(19) -0.0053(13) 0.0031(15) -0.0098(14) Mn1 0.0157(2) 0.0111(2) 0.0157(2) -0.00081(17) -0.00133(18) -0.00279(17) Mn2 0.0140(3) 0.0102(3) 0.0135(3) -0.0004(2) -0.0016(2) -0.0025(2) Mn3 0.0162(2) 0.0115(2) 0.0220(2) -0.00045(17) 0.00122(18) -0.00235(17) Mn4 0.0149(3) 0.0100(3) 0.0165(3) -0.0015(2) 0.0003(2) -0.0029(2) C24 0.037(3) 0.017(2) 0.021(2) -0.0078(17) 0.001(2) 0.000(2) C24A 0.040(3) 0.021(3) 0.024(3) -0.007(2) 0.000(3) 0.000(3) _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 C1 O1 1.250(4) . ? C1 O2 1.284(3) . ? C1 C2 1.495(4) . ? C1 Mn1 2.612(3) . ? C2 C7 1.392(4) . ? C2 C3 1.396(4) . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 C7 1.392(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O4 1.255(3) . ? C8 O3 1.265(4) . ? C8 C9 1.505(4) . ? C9 C10 1.392(4) . ? C9 C14 1.394(4) . ? C10 C11 1.388(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 C13 1.393(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O6 1.248(3) . ? C15 O5 1.276(3) . ? C15 C16 1.504(4) . ? C16 C17 1.388(4) . ? C16 C21 1.397(4) . ? C17 C18 1.394(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 C21 1.396(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O7 1.443(3) . ? C22 C23 1.508(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24A 1.390(11) . ? C23 C24 1.490(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 H23C 0.9900 . ? C23 H23D 0.9900 . ? C23 H25C 0.9900 . ? C23 H25D 0.9900 . ? C25 O7 1.442(3) . ? C25 C24 1.535(5) . ? C25 C24A 1.690(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O8 1.454(4) . ? C26 C27 1.517(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.526(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.519(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O8 1.457(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O9 1.257(4) . ? C30 O10 1.290(3) . ? C30 C31 1.490(4) . ? C30 Mn3 2.605(3) . ? C31 C36 1.385(4) . ? C31 C32 1.395(4) . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 C34 1.396(5) . ? C33 H33 0.9500 . ? C34 C35 1.379(5) . ? C34 H34 0.9500 . ? C35 C36 1.395(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 O12 1.251(4) . ? C37 O11 1.271(4) . ? C37 C38 1.502(4) . ? C38 C39 1.389(4) . ? C38 C43 1.392(4) . ? C39 C40 1.386(4) . ? C39 H39 0.9500 . ? C40 C41 1.388(5) . ? C40 H40 0.9500 . ? C41 C42 1.379(5) . ? C41 H41 0.9500 . ? C42 C43 1.389(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 O13 1.254(4) . ? C44 O14 1.267(4) 2_565 ? C44 C45 1.497(4) . ? C45 C46 1.385(5) . ? C45 C50 1.390(4) . ? C46 C47 1.390(5) . ? C46 H46 0.9500 . ? C47 C48 1.381(5) . ? C47 H47 0.9500 . ? C48 C49 1.377(5) . ? C48 H48 0.9500 . ? C49 C50 1.391(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 O15 1.447(4) . ? C51 C52 1.523(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.539(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.529(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O15 1.447(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O16 1.453(4) . ? C55 C56 1.501(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.526(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.510(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O16 1.449(4) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 O17 1.396(5) . ? C59 C60 1.519(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.537(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.507(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O17 1.426(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? O1 Mn1 2.290(2) . ? O2 Mn2 2.1968(19) . ? O2 Mn1 2.245(2) . ? O3 Mn1 2.131(2) . ? O4 Mn2 2.1393(19) . ? O5 Mn1 2.078(2) . ? O6 Mn2 2.1491(19) . ? O7 Mn1 2.157(2) . ? O8 Mn1 2.324(2) . ? O10 Mn4 2.2298(19) . ? O10 Mn3 2.270(2) . ? O9 Mn3 2.251(2) . ? O11 Mn3 2.064(2) . ? O12 Mn4 2.165(2) . ? O13 Mn4 2.138(2) . ? O14 C44 1.267(4) 2_565 ? O14 Mn3 2.116(2) . ? O15 Mn3 2.179(2) . ? O16 Mn3 2.268(2) . ? Mn2 O4 2.1393(19) 2_656 ? Mn2 O6 2.1491(19) 2_656 ? Mn2 O2 2.1968(19) 2_656 ? Mn4 O13 2.138(2) 2_565 ? Mn4 O12 2.165(2) 2_565 ? Mn4 O10 2.2298(19) 2_565 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 120.4(3) . . ? O1 C1 C2 120.3(3) . . ? O2 C1 C2 119.3(3) . . ? O1 C1 Mn1 61.23(16) . . ? O2 C1 Mn1 59.23(15) . . ? C2 C1 Mn1 178.3(2) . . ? C7 C2 C3 119.7(3) . . ? C7 C2 C1 120.9(3) . . ? C3 C2 C1 119.4(3) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 119.6(3) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O4 C8 O3 124.9(3) . . ? O4 C8 C9 117.4(3) . . ? O3 C8 C9 117.7(2) . . ? C10 C9 C14 119.0(3) . . ? C10 C9 C8 121.4(3) . . ? C14 C9 C8 119.6(3) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 119.2(3) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 120.9(3) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? O6 C15 O5 125.6(3) . . ? O6 C15 C16 118.0(3) . . ? O5 C15 C16 116.4(2) . . ? C17 C16 C21 119.5(3) . . ? C17 C16 C15 121.0(3) . . ? C21 C16 C15 119.5(3) . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 119.7(3) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? O7 C22 C23 104.2(2) . . ? O7 C22 H22A 110.9 . . ? C23 C22 H22A 110.9 . . ? O7 C22 H22B 110.9 . . ? C23 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? C24A C23 C24 41.7(5) . . ? C24A C23 C22 108.3(5) . . ? C24 C23 C22 104.2(3) . . ? C24A C23 H23A 71.0 . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24A C23 H23B 137.3 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? C24A C23 H23C 106.9 . . ? C24 C23 H23C 140.5 . . ? C22 C23 H23C 109.9 . . ? H23A C23 H23C 37.7 . . ? H23B C23 H23C 74.9 . . ? C24A C23 H23D 113.2 . . ? C24 C23 H23D 76.9 . . ? C22 C23 H23D 110.0 . . ? H23A C23 H23D 134.5 . . ? H23B C23 H23D 36.0 . . ? H23C C23 H23D 108.4 . . ? C24A C23 H25C 106.9 . . ? C24 C23 H25C 140.5 . . ? C22 C23 H25C 109.9 . . ? H23A C23 H25C 37.7 . . ? H23B C23 H25C 74.9 . . ? H23C C23 H25C 0.0 . . ? H23D C23 H25C 108.4 . . ? C24A C23 H25D 113.2 . . ? C24 C23 H25D 76.9 . . ? C22 C23 H25D 110.0 . . ? H23A C23 H25D 134.5 . . ? H23B C23 H25D 36.0 . . ? H23C C23 H25D 108.4 . . ? H23D C23 H25D 0.0 . . ? H25C C23 H25D 108.4 . . ? O7 C25 C24 105.8(2) . . ? O7 C25 C24A 94.9(4) . . ? C24 C25 C24A 36.8(4) . . ? O7 C25 H25A 110.6 . . ? C24 C25 H25A 110.6 . . ? C24A C25 H25A 82.6 . . ? O7 C25 H25B 110.6 . . ? C24 C25 H25B 110.6 . . ? C24A C25 H25B 145.1 . . ? H25A C25 H25B 108.7 . . ? O8 C26 C27 105.6(3) . . ? O8 C26 H26A 110.6 . . ? C27 C26 H26A 110.6 . . ? O8 C26 H26B 110.6 . . ? C27 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C26 C27 C28 102.3(3) . . ? C26 C27 H27A 111.3 . . ? C28 C27 H27A 111.3 . . ? C26 C27 H27B 111.3 . . ? C28 C27 H27B 111.3 . . ? H27A C27 H27B 109.2 . . ? C29 C28 C27 101.7(3) . . ? C29 C28 H28A 111.4 . . ? C27 C28 H28A 111.4 . . ? C29 C28 H28B 111.4 . . ? C27 C28 H28B 111.4 . . ? H28A C28 H28B 109.3 . . ? O8 C29 C28 104.6(3) . . ? O8 C29 H29A 110.8 . . ? C28 C29 H29A 110.8 . . ? O8 C29 H29B 110.8 . . ? C28 C29 H29B 110.8 . . ? H29A C29 H29B 108.9 . . ? O9 C30 O10 120.3(3) . . ? O9 C30 C31 120.1(3) . . ? O10 C30 C31 119.6(3) . . ? O9 C30 Mn3 59.78(15) . . ? O10 C30 Mn3 60.63(15) . . ? C31 C30 Mn3 174.2(2) . . ? C36 C31 C32 120.1(3) . . ? C36 C31 C30 120.7(3) . . ? C32 C31 C30 119.2(3) . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 119.8(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 119.6(3) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 121.1(3) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C31 C36 C35 119.1(3) . . ? C31 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? O12 C37 O11 125.5(3) . . ? O12 C37 C38 118.8(3) . . ? O11 C37 C38 115.7(3) . . ? C39 C38 C43 119.5(3) . . ? C39 C38 C37 120.0(3) . . ? C43 C38 C37 120.5(3) . . ? C40 C39 C38 120.4(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 120.0(3) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 119.7(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.7(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C38 119.7(3) . . ? C42 C43 H43 120.1 . . ? C38 C43 H43 120.1 . . ? O13 C44 O14 125.3(3) . 2_565 ? O13 C44 C45 117.9(3) . . ? O14 C44 C45 116.7(3) 2_565 . ? C46 C45 C50 118.9(3) . . ? C46 C45 C44 120.0(3) . . ? C50 C45 C44 121.1(3) . . ? C45 C46 C47 121.0(3) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 119.4(4) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C49 C48 C47 120.4(3) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C50 120.1(3) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C45 C50 C49 120.2(3) . . ? C45 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? O15 C51 C52 103.5(2) . . ? O15 C51 H51A 111.1 . . ? C52 C51 H51A 111.1 . . ? O15 C51 H51B 111.1 . . ? C52 C51 H51B 111.1 . . ? H51A C51 H51B 109.0 . . ? C51 C52 C53 103.5(3) . . ? C51 C52 H52A 111.1 . . ? C53 C52 H52A 111.1 . . ? C51 C52 H52B 111.1 . . ? C53 C52 H52B 111.1 . . ? H52A C52 H52B 109.0 . . ? C54 C53 C52 104.9(3) . . ? C54 C53 H53A 110.8 . . ? C52 C53 H53A 110.8 . . ? C54 C53 H53B 110.8 . . ? C52 C53 H53B 110.8 . . ? H53A C53 H53B 108.9 . . ? O15 C54 C53 104.6(2) . . ? O15 C54 H54A 110.8 . . ? C53 C54 H54A 110.8 . . ? O15 C54 H54B 110.8 . . ? C53 C54 H54B 110.8 . . ? H54A C54 H54B 108.9 . . ? O16 C55 C56 105.3(3) . . ? O16 C55 H55A 110.7 . . ? C56 C55 H55A 110.7 . . ? O16 C55 H55B 110.7 . . ? C56 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? C55 C56 C57 101.9(3) . . ? C55 C56 H56A 111.4 . . ? C57 C56 H56A 111.4 . . ? C55 C56 H56B 111.4 . . ? C57 C56 H56B 111.4 . . ? H56A C56 H56B 109.3 . . ? C58 C57 C56 102.7(3) . . ? C58 C57 H57A 111.2 . . ? C56 C57 H57A 111.2 . . ? C58 C57 H57B 111.2 . . ? C56 C57 H57B 111.2 . . ? H57A C57 H57B 109.1 . . ? O16 C58 C57 105.9(3) . . ? O16 C58 H58A 110.6 . . ? C57 C58 H58A 110.6 . . ? O16 C58 H58B 110.6 . . ? C57 C58 H58B 110.6 . . ? H58A C58 H58B 108.7 . . ? O17 C59 C60 107.4(3) . . ? O17 C59 H59A 110.2 . . ? C60 C59 H59A 110.2 . . ? O17 C59 H59B 110.2 . . ? C60 C59 H59B 110.2 . . ? H59A C59 H59B 108.5 . . ? C59 C60 C61 103.5(3) . . ? C59 C60 H60A 111.1 . . ? C61 C60 H60A 111.1 . . ? C59 C60 H60B 111.1 . . ? C61 C60 H60B 111.1 . . ? H60A C60 H60B 109.0 . . ? C62 C61 C60 102.8(3) . . ? C62 C61 H61A 111.2 . . ? C60 C61 H61A 111.2 . . ? C62 C61 H61B 111.2 . . ? C60 C61 H61B 111.2 . . ? H61A C61 H61B 109.1 . . ? O17 C62 C61 106.4(3) . . ? O17 C62 H62A 110.4 . . ? C61 C62 H62A 110.4 . . ? O17 C62 H62B 110.4 . . ? C61 C62 H62B 110.4 . . ? H62A C62 H62B 108.6 . . ? C1 O1 Mn1 90.17(17) . . ? C1 O2 Mn2 144.50(18) . . ? C1 O2 Mn1 91.34(17) . . ? Mn2 O2 Mn1 104.70(8) . . ? C8 O3 Mn1 120.09(17) . . ? C8 O4 Mn2 139.91(19) . . ? C15 O5 Mn1 128.62(19) . . ? C15 O6 Mn2 137.38(18) . . ? C25 O7 C22 110.3(2) . . ? C25 O7 Mn1 125.74(15) . . ? C22 O7 Mn1 123.75(17) . . ? C26 O8 C29 109.6(2) . . ? C26 O8 Mn1 121.66(17) . . ? C29 O8 Mn1 117.74(17) . . ? C30 O10 Mn4 147.83(19) . . ? C30 O10 Mn3 89.70(17) . . ? Mn4 O10 Mn3 104.46(8) . . ? C30 O9 Mn3 91.37(17) . . ? C37 O11 Mn3 127.3(2) . . ? C37 O12 Mn4 135.11(19) . . ? C44 O13 Mn4 142.15(19) . . ? C44 O14 Mn3 122.2(2) 2_565 . ? C51 O15 C54 105.1(2) . . ? C51 O15 Mn3 119.50(18) . . ? C54 O15 Mn3 122.04(17) . . ? C58 O16 C55 109.4(2) . . ? C58 O16 Mn3 119.56(18) . . ? C55 O16 Mn3 123.72(18) . . ? C59 O17 C62 104.2(3) . . ? O5 Mn1 O3 105.79(8) . . ? O5 Mn1 O7 98.13(8) . . ? O3 Mn1 O7 91.22(8) . . ? O5 Mn1 O2 102.15(7) . . ? O3 Mn1 O2 96.47(8) . . ? O7 Mn1 O2 155.40(8) . . ? O5 Mn1 O1 156.30(8) . . ? O3 Mn1 O1 90.37(8) . . ? O7 Mn1 O1 98.75(8) . . ? O2 Mn1 O1 58.02(7) . . ? O5 Mn1 O8 82.97(8) . . ? O3 Mn1 O8 170.50(8) . . ? O7 Mn1 O8 83.77(8) . . ? O2 Mn1 O8 85.03(7) . . ? O1 Mn1 O8 82.45(7) . . ? O5 Mn1 C1 130.61(8) . . ? O3 Mn1 C1 93.40(8) . . ? O7 Mn1 C1 127.04(9) . . ? O2 Mn1 C1 29.43(8) . . ? O1 Mn1 C1 28.60(8) . . ? O8 Mn1 C1 83.28(8) . . ? O4 Mn2 O4 180.00(11) 2_656 . ? O4 Mn2 O6 88.38(8) 2_656 . ? O4 Mn2 O6 91.62(8) . . ? O4 Mn2 O6 91.62(8) 2_656 2_656 ? O4 Mn2 O6 88.38(8) . 2_656 ? O6 Mn2 O6 180.00(2) . 2_656 ? O4 Mn2 O2 88.73(8) 2_656 . ? O4 Mn2 O2 91.27(8) . . ? O6 Mn2 O2 89.94(7) . . ? O6 Mn2 O2 90.06(7) 2_656 . ? O4 Mn2 O2 91.27(8) 2_656 2_656 ? O4 Mn2 O2 88.73(8) . 2_656 ? O6 Mn2 O2 90.06(7) . 2_656 ? O6 Mn2 O2 89.94(7) 2_656 2_656 ? O2 Mn2 O2 180.00(9) . 2_656 ? O11 Mn3 O14 97.33(9) . . ? O11 Mn3 O15 100.68(8) . . ? O14 Mn3 O15 89.08(8) . . ? O11 Mn3 O9 162.78(8) . . ? O14 Mn3 O9 92.15(8) . . ? O15 Mn3 O9 93.79(7) . . ? O11 Mn3 O16 86.41(8) . . ? O14 Mn3 O16 174.30(8) . . ? O15 Mn3 O16 85.99(8) . . ? O9 Mn3 O16 85.33(8) . . ? O11 Mn3 O10 105.78(8) . . ? O14 Mn3 O10 97.77(8) . . ? O15 Mn3 O10 151.49(7) . . ? O9 Mn3 O10 58.48(7) . . ? O16 Mn3 O10 85.28(8) . . ? O11 Mn3 C30 134.86(9) . . ? O14 Mn3 C30 96.85(9) . . ? O15 Mn3 C30 122.19(8) . . ? O9 Mn3 C30 28.85(8) . . ? O16 Mn3 C30 83.40(8) . . ? O10 Mn3 C30 29.68(8) . . ? O13 Mn4 O13 180.00(10) . 2_565 ? O13 Mn4 O12 88.35(8) . . ? O13 Mn4 O12 91.65(8) 2_565 . ? O13 Mn4 O12 91.65(8) . 2_565 ? O13 Mn4 O12 88.35(8) 2_565 2_565 ? O12 Mn4 O12 180.00(7) . 2_565 ? O13 Mn4 O10 89.91(7) . 2_565 ? O13 Mn4 O10 90.09(7) 2_565 2_565 ? O12 Mn4 O10 90.05(8) . 2_565 ? O12 Mn4 O10 89.95(8) 2_565 2_565 ? O13 Mn4 O10 90.09(7) . . ? O13 Mn4 O10 89.91(7) 2_565 . ? O12 Mn4 O10 89.95(8) . . ? O12 Mn4 O10 90.05(8) 2_565 . ? O10 Mn4 O10 180.00(12) 2_565 . ? C23 C24 C25 104.1(3) . . ? C23 C24 H24A 110.9 . . ? C25 C24 H24A 110.9 . . ? C23 C24 H24B 110.9 . . ? C25 C24 H24B 110.9 . . ? H24A C24 H24B 109.0 . . ? C23 C24A C25 101.1(7) . . ? C23 C24A H24C 111.6 . . ? C25 C24A H24C 111.6 . . ? C23 C24A H24D 111.6 . . ? C25 C24A H24D 111.6 . . ? H24C C24A H24D 109.4 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.690 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 949072' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H140 Mn6 O28' _chemical_formula_weight 1831.52 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4470(13) _cell_length_b 18.7120(16) _cell_length_c 21.509(2) _cell_angle_alpha 91.782(6) _cell_angle_beta 90.506(6) _cell_angle_gamma 108.686(4) _cell_volume 4742.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9705 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 24.713 _exptl_crystal_description block _exptl_crystal_colour 'claret ' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; Twinned crystal with partially superimposed reciprocal lattices. The transformation matrix of indices of the twin components for crystals was determined roughly as: | -1.000 0.000 0.000| | 0.000 -1.000 0.000| | 0.072 0.087 1.000| which comply with conditions: rotation twin axis [0 0 1] rotation angle 23\% or reflection twin plane (1 1 24). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12491 _diffrn_reflns_av_R_equivalents 0.1011 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 23.26 _reflns_number_total 12491 _reflns_number_gt 8611 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1041P)^2^+120.2606P] 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 12491 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2292 _refine_ls_R_factor_gt 0.1761 _refine_ls_wR_factor_ref 0.4142 _refine_ls_wR_factor_gt 0.3905 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5145(17) 0.2674(12) 0.0888(11) 0.031(5) Uani 1 1 d . . . C2 C 0.465(2) 0.2472(13) 0.0202(12) 0.046(7) Uani 1 1 d . . . C3 C 0.451(3) 0.3146(14) -0.0096(14) 0.070(9) Uani 1 1 d . . . H3A H 0.4225 0.3009 -0.0523 0.105 Uiso 1 1 calc R . . H3B H 0.5251 0.3545 -0.0102 0.105 Uiso 1 1 calc R . . H3C H 0.3979 0.3328 0.0141 0.105 Uiso 1 1 calc R . . C4 C 0.357(3) 0.1806(16) 0.0235(12) 0.060(8) Uani 1 1 d . . . H4A H 0.3014 0.1952 0.0482 0.090 Uiso 1 1 calc R . . H4B H 0.3741 0.1386 0.0430 0.090 Uiso 1 1 calc R . . H4C H 0.3264 0.1647 -0.0186 0.090 Uiso 1 1 calc R . . C5 C 0.5548(19) 0.2183(16) -0.0132(12) 0.056(8) Uani 1 1 d . . . H5A H 0.5346 0.2087 -0.0575 0.084 Uiso 1 1 calc R . . H5B H 0.5565 0.1715 0.0054 0.084 Uiso 1 1 calc R . . H5C H 0.6298 0.2567 -0.0084 0.084 Uiso 1 1 calc R . . C6 C 0.826(2) 0.3624(14) 0.2004(12) 0.047(7) Uani 1 1 d . . . C7 C 0.9042(18) 0.3229(12) 0.1688(12) 0.039(6) Uani 1 1 d . . . C8 C 0.8440(19) 0.2783(12) 0.1073(10) 0.036(6) Uani 1 1 d . . . H8A H 0.8303 0.3140 0.0782 0.055 Uiso 1 1 calc R . . H8B H 0.7716 0.2410 0.1177 0.055 Uiso 1 1 calc R . . H8C H 0.8931 0.2525 0.0879 0.055 Uiso 1 1 calc R . . C9 C 0.919(2) 0.2635(15) 0.2151(14) 0.059(8) Uani 1 1 d . . . H9A H 0.9763 0.2422 0.1994 0.088 Uiso 1 1 calc R . . H9B H 0.8466 0.2231 0.2189 0.088 Uiso 1 1 calc R . . H9C H 0.9436 0.2882 0.2560 0.088 Uiso 1 1 calc R . . C10 C 1.0132(19) 0.3807(16) 0.1525(16) 0.066(9) Uani 1 1 d . . . H10A H 1.0550 0.3578 0.1240 0.099 Uiso 1 1 calc R . . H10B H 1.0590 0.3998 0.1904 0.099 Uiso 1 1 calc R . . H10C H 0.9973 0.4226 0.1323 0.099 Uiso 1 1 calc R . . C11 C 0.650(2) 0.4761(16) 0.3295(12) 0.045(6) Uani 1 1 d . . . C12 C 0.597(2) 0.4844(14) 0.3945(12) 0.046(6) Uani 1 1 d . . . C13 C 0.681(3) 0.5465(13) 0.4336(14) 0.065(9) Uani 1 1 d . . . H13A H 0.7076 0.5923 0.4096 0.097 Uiso 1 1 calc R . . H13B H 0.7458 0.5304 0.4452 0.097 Uiso 1 1 calc R . . H13C H 0.6441 0.5569 0.4712 0.097 Uiso 1 1 calc R . . C14 C 0.490(3) 0.5071(16) 0.3824(15) 0.069(9) Uani 1 1 d . . . H14A H 0.4576 0.5152 0.4223 0.104 Uiso 1 1 calc R . . H14B H 0.4346 0.4668 0.3580 0.104 Uiso 1 1 calc R . . H14C H 0.5109 0.5538 0.3594 0.104 Uiso 1 1 calc R . . C15 C 0.573(3) 0.4109(13) 0.4294(13) 0.066(9) Uani 1 1 d . . . H15A H 0.5684 0.4215 0.4740 0.098 Uiso 1 1 calc R . . H15B H 0.6345 0.3896 0.4223 0.098 Uiso 1 1 calc R . . H15C H 0.5011 0.3748 0.4143 0.098 Uiso 1 1 calc R . . C16 C 0.4747(18) 0.5216(12) 0.2060(11) 0.035(5) Uani 1 1 d . . . H16A H 0.5567 0.5501 0.2052 0.042 Uiso 1 1 calc R . . H16B H 0.4495 0.5208 0.2496 0.042 Uiso 1 1 calc R . . C17 C 0.410(3) 0.5587(16) 0.1664(19) 0.086(12) Uani 1 1 d . . . H17A H 0.3864 0.5967 0.1909 0.103 Uiso 1 1 calc R . . H17B H 0.4549 0.5832 0.1307 0.103 Uiso 1 1 calc R . . C18 C 0.314(2) 0.4959(15) 0.1463(15) 0.057(7) Uani 1 1 d . . . H18A H 0.2831 0.5057 0.1060 0.068 Uiso 1 1 calc R . . H18B H 0.2531 0.4861 0.1774 0.068 Uiso 1 1 calc R . . C19 C 0.359(2) 0.4292(13) 0.1398(11) 0.045(7) Uani 1 1 d . . . H19A H 0.2997 0.3818 0.1509 0.054 Uiso 1 1 calc R . . H19B H 0.3820 0.4234 0.0965 0.054 Uiso 1 1 calc R . . C20 C 0.4088(16) 0.2197(11) 0.2511(9) 0.020(4) Uani 1 1 d U . . C21 C 0.2904(17) 0.2280(11) 0.2685(10) 0.027(5) Uani 1 1 d U . . C22 C 0.239(2) 0.1732(15) 0.3164(17) 0.072(10) Uani 1 1 d . . . H22A H 0.1819 0.1894 0.3387 0.108 Uiso 1 1 calc R . . H22B H 0.2979 0.1705 0.3458 0.108 Uiso 1 1 calc R . . H22C H 0.2025 0.1233 0.2964 0.108 Uiso 1 1 calc R . . C23 C 0.223(2) 0.2039(13) 0.2083(13) 0.048(7) Uani 1 1 d . . . H23A H 0.2237 0.1533 0.1952 0.073 Uiso 1 1 calc R . . H23B H 0.2579 0.2397 0.1761 0.073 Uiso 1 1 calc R . . H23C H 0.1451 0.2030 0.2145 0.073 Uiso 1 1 calc R . . C24 C 0.299(2) 0.3068(13) 0.2901(14) 0.052(7) Uani 1 1 d . . . H24A H 0.3246 0.3412 0.2559 0.078 Uiso 1 1 calc R . . H24B H 0.3537 0.3228 0.3250 0.078 Uiso 1 1 calc R . . H24C H 0.2246 0.3079 0.3037 0.078 Uiso 1 1 calc R . . C25 C 0.602(2) 0.0617(13) 0.1741(10) 0.035(6) Uani 1 1 d . . . C26 C 0.648(2) 0.0102(13) 0.1300(10) 0.040(6) Uani 1 1 d . . . C27 C 0.635(3) -0.0643(15) 0.1588(14) 0.063(8) Uani 1 1 d . . . H27A H 0.6591 -0.0968 0.1294 0.095 Uiso 1 1 calc R . . H27B H 0.5547 -0.0887 0.1686 0.095 Uiso 1 1 calc R . . H27C H 0.6810 -0.0560 0.1970 0.095 Uiso 1 1 calc R . . C28 C 0.573(2) -0.0007(14) 0.0675(12) 0.049(7) Uani 1 1 d . . . H28A H 0.5975 0.0457 0.0441 0.073 Uiso 1 1 calc R . . H28B H 0.4928 -0.0118 0.0783 0.073 Uiso 1 1 calc R . . H28C H 0.5816 -0.0427 0.0421 0.073 Uiso 1 1 calc R . . C29 C 0.771(2) 0.0467(15) 0.1190(13) 0.051(7) Uani 1 1 d . . . H29A H 0.8116 0.0628 0.1590 0.076 Uiso 1 1 calc R . . H29B H 0.7819 0.0908 0.0934 0.076 Uiso 1 1 calc R . . H29C H 0.8015 0.0106 0.0974 0.076 Uiso 1 1 calc R . . C30 C 0.705(3) 0.2928(15) 0.3412(16) 0.075(10) Uani 1 1 d . . . H30A H 0.6476 0.3186 0.3379 0.090 Uiso 1 1 calc R . . H30B H 0.7797 0.3278 0.3290 0.090 Uiso 1 1 calc R . . C31 C 0.712(3) 0.2659(16) 0.4082(14) 0.069(9) Uani 1 1 d . . . H31A H 0.7718 0.3034 0.4336 0.083 Uiso 1 1 calc R . . H31B H 0.6384 0.2550 0.4293 0.083 Uiso 1 1 calc R . . C32 C 0.742(3) 0.1937(15) 0.3945(14) 0.063(8) Uani 1 1 d . . . H32A H 0.8246 0.2060 0.3872 0.075 Uiso 1 1 calc R . . H32B H 0.7218 0.1594 0.4297 0.075 Uiso 1 1 calc R . . C33 C 0.678(2) 0.1592(14) 0.3394(14) 0.061(9) Uani 1 1 d . . . H33A H 0.6002 0.1275 0.3501 0.073 Uiso 1 1 calc R . . H33B H 0.7152 0.1277 0.3161 0.073 Uiso 1 1 calc R . . C34 C 0.308(2) 0.0248(11) 0.3735(10) 0.032(6) Uani 1 1 d . . . C35 C 0.3096(19) 0.0367(11) 0.4461(11) 0.033(5) Uani 1 1 d . . . C36 C 0.4052(19) 0.1069(13) 0.4673(11) 0.041(6) Uani 1 1 d U . . H36A H 0.4000 0.1502 0.4443 0.062 Uiso 1 1 calc R . . H36B H 0.4782 0.0994 0.4592 0.062 Uiso 1 1 calc R . . H36C H 0.3990 0.1166 0.5119 0.062 Uiso 1 1 calc R . . C37 C 0.329(2) -0.0338(13) 0.4727(13) 0.055(8) Uani 1 1 d . . . H37A H 0.2706 -0.0793 0.4562 0.083 Uiso 1 1 calc R . . H37B H 0.3255 -0.0315 0.5182 0.083 Uiso 1 1 calc R . . H37C H 0.4041 -0.0356 0.4606 0.083 Uiso 1 1 calc R . . C38 C 0.1947(19) 0.0387(14) 0.4616(13) 0.048(7) Uani 1 1 d . . . H38A H 0.1904 0.0469 0.5066 0.072 Uiso 1 1 calc R . . H38B H 0.1380 -0.0093 0.4484 0.072 Uiso 1 1 calc R . . H38C H 0.1798 0.0800 0.4400 0.072 Uiso 1 1 calc R . . C39 C 0.148(2) -0.0322(14) 0.1756(12) 0.045(7) Uani 1 1 d . . . C40 C 0.101(2) -0.0429(16) 0.1079(10) 0.048(7) Uani 1 1 d . . . C41 C -0.004(3) -0.1072(15) 0.0957(12) 0.066(9) Uani 1 1 d . . . H41A H -0.0652 -0.1002 0.1211 0.099 Uiso 1 1 calc R . . H41B H 0.0089 -0.1543 0.1065 0.099 Uiso 1 1 calc R . . H41C H -0.0256 -0.1096 0.0516 0.099 Uiso 1 1 calc R . . C42 C 0.198(3) -0.0558(16) 0.0673(12) 0.058(7) Uani 1 1 d . . . H42A H 0.1888 -0.1098 0.0643 0.087 Uiso 1 1 calc R . . H42B H 0.2720 -0.0284 0.0867 0.087 Uiso 1 1 calc R . . H42C H 0.1939 -0.0372 0.0255 0.087 Uiso 1 1 calc R . . C43 C 0.090(3) 0.0330(17) 0.0894(16) 0.076(9) Uani 1 1 d U . . H43A H 0.0713 0.0308 0.0449 0.114 Uiso 1 1 calc R . . H43B H 0.1625 0.0731 0.0979 0.114 Uiso 1 1 calc R . . H43C H 0.0304 0.0436 0.1135 0.114 Uiso 1 1 calc R . . C44 C 0.3128(19) -0.1426(13) 0.2981(10) 0.035(6) Uani 1 1 d . . . C45 C 0.4020(19) -0.1744(11) 0.3274(11) 0.036(6) Uani 1 1 d . . . C46 C 0.5161(19) -0.1106(14) 0.3321(12) 0.046(6) Uani 1 1 d . . . H46A H 0.5100 -0.0708 0.3612 0.069 Uiso 1 1 calc R . . H46B H 0.5362 -0.0897 0.2910 0.069 Uiso 1 1 calc R . . H46C H 0.5750 -0.1307 0.3472 0.069 Uiso 1 1 calc R . . C47 C 0.366(2) -0.2093(11) 0.3890(12) 0.046(7) Uani 1 1 d . . . H47A H 0.2969 -0.2526 0.3831 0.069 Uiso 1 1 calc R . . H47B H 0.3518 -0.1719 0.4177 0.069 Uiso 1 1 calc R . . H47C H 0.4267 -0.2262 0.4063 0.069 Uiso 1 1 calc R . . C48 C 0.418(2) -0.2346(16) 0.2806(15) 0.064(8) Uani 1 1 d . . . H48A H 0.4770 -0.2541 0.2966 0.096 Uiso 1 1 calc R . . H48B H 0.4413 -0.2116 0.2405 0.096 Uiso 1 1 calc R . . H48C H 0.3466 -0.2761 0.2752 0.096 Uiso 1 1 calc R . . C49 C -0.0368(19) 0.0164(13) 0.2676(10) 0.037(6) Uani 1 1 d . . . H49A H -0.0805 -0.0121 0.2310 0.045 Uiso 1 1 calc R . . H49B H 0.0389 0.0476 0.2538 0.045 Uiso 1 1 calc R . . C50 C -0.098(2) 0.0654(14) 0.2977(11) 0.042(6) Uani 1 1 d . . . H50A H -0.1456 0.0806 0.2670 0.050 Uiso 1 1 calc R . . H50B H -0.0443 0.1112 0.3181 0.050 Uiso 1 1 calc R . . C51 C -0.170(2) 0.0146(13) 0.3450(11) 0.041(6) Uani 1 1 d . . . H51A H -0.1916 0.0441 0.3790 0.049 Uiso 1 1 calc R . . H51B H -0.2401 -0.0212 0.3255 0.049 Uiso 1 1 calc R . . C52 C -0.0926(18) -0.0247(13) 0.3675(12) 0.040(6) Uani 1 1 d . . . H52A H -0.0424 0.0057 0.4013 0.048 Uiso 1 1 calc R . . H52B H -0.1363 -0.0743 0.3839 0.048 Uiso 1 1 calc R . . C53 C 0.0040(19) -0.2126(14) 0.4169(10) 0.038(6) Uani 1 1 d . . . C54 C -0.0506(17) -0.2211(14) 0.4824(11) 0.041(6) Uani 1 1 d . . . C55 C 0.0007(19) -0.1519(12) 0.5230(10) 0.037(6) Uani 1 1 d . . . H55A H -0.0200 -0.1097 0.5065 0.056 Uiso 1 1 calc R . . H55B H 0.0835 -0.1392 0.5238 0.056 Uiso 1 1 calc R . . H55C H -0.0277 -0.1613 0.5653 0.056 Uiso 1 1 calc R . . C56 C -0.039(3) -0.2941(14) 0.5135(13) 0.060(8) Uani 1 1 d . . . H56A H 0.0416 -0.2865 0.5229 0.090 Uiso 1 1 calc R . . H56B H -0.0686 -0.3379 0.4848 0.090 Uiso 1 1 calc R . . H56C H -0.0814 -0.3030 0.5521 0.090 Uiso 1 1 calc R . . C57 C -0.174(2) -0.2315(16) 0.4708(14) 0.058(7) Uani 1 1 d . . . H57A H -0.2113 -0.2314 0.5106 0.087 Uiso 1 1 calc R . . H57B H -0.2095 -0.2797 0.4482 0.087 Uiso 1 1 calc R . . H57C H -0.1810 -0.1902 0.4459 0.087 Uiso 1 1 calc R . . C58 C 0.148(5) -0.2463(17) 0.1635(14) 0.15(3) Uani 1 1 d . . . H58A H 0.2105 -0.1985 0.1726 0.180 Uiso 1 1 calc R . . H58B H 0.0757 -0.2351 0.1652 0.180 Uiso 1 1 calc R . . C59 C 0.161(4) -0.273(2) 0.1034(16) 0.118(18) Uani 1 1 d . . . H59A H 0.2228 -0.2363 0.0815 0.142 Uiso 1 1 calc R . . H59B H 0.0899 -0.2846 0.0785 0.142 Uiso 1 1 calc R . . C60 C 0.190(4) -0.3448(19) 0.1139(14) 0.085(12) Uani 1 1 d . . . H60A H 0.1450 -0.3861 0.0851 0.102 Uiso 1 1 calc R . . H60B H 0.2716 -0.3362 0.1066 0.102 Uiso 1 1 calc R . . C61 C 0.162(2) -0.3651(13) 0.1806(13) 0.048(7) Uani 1 1 d . . . H61A H 0.0911 -0.4082 0.1829 0.057 Uiso 1 1 calc R . . H61B H 0.2244 -0.3782 0.2012 0.057 Uiso 1 1 calc R . . C62 C -0.1102(19) -0.2795(11) 0.2615(9) 0.025(5) Uani 1 1 d . . . C63 C -0.225(2) -0.2694(13) 0.2452(12) 0.041(6) Uani 1 1 d U . . C64 C -0.228(3) -0.1897(14) 0.2492(14) 0.069(10) Uani 1 1 d . . . H64A H -0.2023 -0.1677 0.2909 0.104 Uiso 1 1 calc R . . H64B H -0.3052 -0.1895 0.2413 0.104 Uiso 1 1 calc R . . H64C H -0.1772 -0.1598 0.2181 0.104 Uiso 1 1 calc R . . C65 C -0.322(2) -0.3186(16) 0.2901(14) 0.062(9) Uani 1 1 d . . . H65A H -0.3122 -0.3680 0.2955 0.094 Uiso 1 1 calc R . . H65B H -0.3968 -0.3255 0.2714 0.094 Uiso 1 1 calc R . . H65C H -0.3157 -0.2921 0.3307 0.094 Uiso 1 1 calc R . . C66 C -0.257(2) -0.2991(16) 0.1757(12) 0.052(7) Uani 1 1 d . . . H66A H -0.1940 -0.2736 0.1487 0.079 Uiso 1 1 calc R . . H66B H -0.3254 -0.2886 0.1625 0.079 Uiso 1 1 calc R . . H66C H -0.2700 -0.3537 0.1729 0.079 Uiso 1 1 calc R . . C67 C 0.098(2) -0.4261(16) 0.3327(12) 0.043(7) Uani 1 1 d . . . C68 C 0.118(2) -0.4887(13) 0.3785(11) 0.042(6) Uani 1 1 d . . . C69 C 0.198(4) -0.454(2) 0.427(2) 0.113(14) Uani 1 1 d U . . H69A H 0.2280 -0.4920 0.4446 0.169 Uiso 1 1 calc R . . H69B H 0.1616 -0.4333 0.4597 0.169 Uiso 1 1 calc R . . H69C H 0.2611 -0.4135 0.4101 0.169 Uiso 1 1 calc R . . C70 C 0.159(4) -0.542(2) 0.3401(17) 0.116(17) Uani 1 1 d . . . H70A H 0.2108 -0.5134 0.3085 0.174 Uiso 1 1 calc R . . H70B H 0.0948 -0.5798 0.3195 0.174 Uiso 1 1 calc R . . H70C H 0.2000 -0.5662 0.3668 0.174 Uiso 1 1 calc R . . C71 C 0.004(3) -0.5334(19) 0.4087(16) 0.087(12) Uani 1 1 d . . . H71A H -0.0289 -0.5819 0.3861 0.130 Uiso 1 1 calc R . . H71B H -0.0485 -0.5042 0.4069 0.130 Uiso 1 1 calc R . . H71C H 0.0185 -0.5423 0.4522 0.130 Uiso 1 1 calc R . . C72 C -0.2134(19) -0.4791(11) 0.1327(9) 0.029(5) Uani 1 1 d . . . C73 C -0.2422(19) -0.4790(14) 0.0627(12) 0.043(6) Uani 1 1 d . . . C74 C -0.159(2) -0.4118(15) 0.0308(12) 0.059(8) Uani 1 1 d . . . H74A H -0.1743 -0.4165 -0.0141 0.088 Uiso 1 1 calc R . . H74B H -0.0809 -0.4115 0.0389 0.088 Uiso 1 1 calc R . . H74C H -0.1675 -0.3647 0.0474 0.088 Uiso 1 1 calc R . . C75 C -0.3615(18) -0.4839(14) 0.0509(10) 0.043(6) Uani 1 1 d . . . H75A H -0.4115 -0.5250 0.0745 0.065 Uiso 1 1 calc R . . H75B H -0.3795 -0.4938 0.0064 0.065 Uiso 1 1 calc R . . H75C H -0.3725 -0.4361 0.0640 0.065 Uiso 1 1 calc R . . C76 C -0.220(2) -0.5527(12) 0.0367(11) 0.045(7) Uani 1 1 d . . . H76A H -0.2607 -0.5955 0.0618 0.068 Uiso 1 1 calc R . . H76B H -0.1386 -0.5455 0.0388 0.068 Uiso 1 1 calc R . . H76C H -0.2471 -0.5628 -0.0066 0.068 Uiso 1 1 calc R . . O1 O 0.5244(13) 0.3333(9) 0.1112(7) 0.037(4) Uani 1 1 d . . . O2 O 0.5346(15) 0.2164(9) 0.1193(7) 0.047(4) Uani 1 1 d . . . O3 O 0.7183(12) 0.3309(8) 0.1982(7) 0.034(4) Uani 1 1 d U . . O4 O 0.5882(14) 0.4304(9) 0.2915(7) 0.041(4) Uani 1 1 d . . . O5 O 0.4546(13) 0.4466(8) 0.1821(7) 0.039(4) Uani 1 1 d . . . O6 O 0.7130(11) 0.4908(8) 0.1700(7) 0.030(3) Uani 1 1 d . . . O7 O 0.4862(12) 0.2812(8) 0.2432(7) 0.033(4) Uani 1 1 d . . . O8 O 0.4179(11) 0.1585(8) 0.2470(7) 0.030(3) Uani 1 1 d . . . O9 O 0.6610(12) 0.1248(9) 0.1867(7) 0.037(4) Uani 1 1 d . . . O10 O 0.5002(17) 0.0307(10) 0.1935(9) 0.061(5) Uani 1 1 d . . . O11 O 0.6740(14) 0.2244(9) 0.3025(7) 0.041(4) Uani 1 1 d . . . O12 O 0.4062(14) 0.0501(9) 0.3472(7) 0.041(4) Uani 1 1 d . . . O13 O 0.2193(13) -0.0084(9) 0.3445(7) 0.039(4) Uani 1 1 d . . . O14 O 0.2414(14) 0.0201(9) 0.1897(7) 0.041(4) Uani 1 1 d . . . O15 O 0.0912(15) -0.0799(10) 0.2113(8) 0.050(4) Uani 1 1 d . . . O16 O 0.3494(12) -0.0880(10) 0.2629(7) 0.040(4) Uani 1 1 d . . . O17 O 0.2129(11) -0.1705(9) 0.3096(7) 0.040(4) Uani 1 1 d . . . O18 O -0.0260(12) -0.0348(8) 0.3147(7) 0.034(4) Uani 1 1 d . . . O19 O 0.0237(14) -0.1478(9) 0.3940(7) 0.042(4) Uani 1 1 d . . . O20 O 0.0245(14) -0.2676(9) 0.3919(7) 0.043(4) Uani 1 1 d . . . O21 O 0.1491(14) -0.2973(8) 0.2086(7) 0.043(4) Uani 1 1 d . . . O22 O -0.0253(13) -0.2160(9) 0.2686(7) 0.038(4) Uani 1 1 d . . . O23 O -0.1014(12) -0.3417(7) 0.2669(6) 0.028(3) Uani 1 1 d . . . O24 O 0.1618(14) -0.3634(8) 0.3361(8) 0.046(4) Uani 1 1 d . . . O25 O 0.0125(17) -0.4516(13) 0.3018(11) 0.076(6) Uani 1 1 d . . . O26 O -0.1165(17) -0.4421(10) 0.1532(8) 0.056(5) Uani 1 1 d . . . O27 O -0.2522(15) -0.4894(9) 0.3228(7) 0.042(4) Uani 1 1 d . . . O28 O -0.1266(15) -0.5779(9) 0.2271(8) 0.048(4) Uani 1 1 d . . . Mn1 Mn 0.5862(3) 0.3892(2) 0.19886(16) 0.0331(9) Uani 1 1 d . . . Mn2 Mn 0.6009(3) 0.2154(2) 0.20850(17) 0.0351(9) Uani 1 1 d . . . Mn3 Mn 0.3687(3) 0.0296(2) 0.25113(16) 0.0335(8) Uani 1 1 d . . . Mn4 Mn 0.0909(3) -0.10469(19) 0.30781(16) 0.0290(8) Uani 1 1 d . . . Mn5 Mn 0.0862(3) -0.2847(2) 0.30465(17) 0.0368(9) Uani 1 1 d . . . Mn6 Mn -0.1381(3) -0.4670(2) 0.25085(16) 0.0338(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(12) 0.035(14) 0.035(14) -0.002(11) -0.006(10) 0.012(10) C2 0.054(16) 0.029(13) 0.040(15) -0.004(11) -0.025(13) -0.007(12) C3 0.12(3) 0.040(16) 0.059(19) 0.001(14) -0.031(18) 0.034(17) C4 0.09(2) 0.067(19) 0.031(15) -0.001(13) 0.009(14) 0.032(17) C5 0.031(13) 0.080(19) 0.042(16) -0.020(14) 0.021(12) -0.001(13) C6 0.067(18) 0.032(14) 0.043(16) -0.004(12) -0.003(14) 0.019(13) C7 0.025(12) 0.036(13) 0.060(17) 0.003(12) -0.003(11) 0.015(10) C8 0.043(14) 0.038(13) 0.029(13) 0.004(10) 0.018(11) 0.013(11) C9 0.062(18) 0.055(17) 0.08(2) 0.015(15) 0.013(16) 0.043(15) C10 0.015(12) 0.065(19) 0.11(3) 0.007(18) -0.011(14) 0.004(12) C11 0.051(18) 0.054(17) 0.038(16) 0.006(13) -0.012(14) 0.027(15) C12 0.041(14) 0.053(16) 0.039(15) -0.001(12) -0.002(12) 0.005(12) C13 0.10(2) 0.025(14) 0.07(2) 0.001(13) 0.010(17) 0.009(15) C14 0.08(2) 0.049(17) 0.08(2) -0.030(16) 0.007(17) 0.023(15) C15 0.11(3) 0.025(14) 0.050(18) 0.005(12) 0.032(17) 0.004(15) C16 0.028(12) 0.047(14) 0.032(14) 0.013(11) 0.000(10) 0.014(11) C17 0.08(2) 0.045(18) 0.14(4) 0.000(19) -0.03(2) 0.034(17) C18 0.045(16) 0.057(17) 0.07(2) 0.006(15) 0.001(15) 0.024(14) C19 0.066(17) 0.040(14) 0.025(13) 0.013(11) -0.025(12) 0.013(13) C20 0.021(5) 0.020(5) 0.020(6) 0.004(4) -0.002(4) 0.008(4) C21 0.027(6) 0.027(6) 0.027(6) 0.001(4) 0.004(4) 0.007(4) C22 0.034(14) 0.040(16) 0.13(3) -0.007(17) 0.011(17) -0.010(12) C23 0.055(16) 0.031(13) 0.062(19) 0.009(12) 0.004(14) 0.018(12) C24 0.054(16) 0.033(14) 0.07(2) -0.003(13) 0.005(14) 0.014(12) C25 0.035(13) 0.037(14) 0.027(13) -0.001(11) -0.025(11) 0.006(12) C26 0.044(14) 0.048(15) 0.017(12) 0.006(10) -0.004(10) -0.003(12) C27 0.08(2) 0.048(16) 0.07(2) 0.000(14) -0.019(17) 0.037(16) C28 0.053(16) 0.048(15) 0.056(17) -0.005(13) -0.003(13) 0.031(13) C29 0.045(15) 0.066(18) 0.049(17) 0.005(13) 0.012(13) 0.027(14) C30 0.11(3) 0.038(16) 0.08(2) -0.011(16) 0.00(2) 0.027(17) C31 0.09(2) 0.06(2) 0.051(19) -0.022(15) -0.027(17) 0.022(17) C32 0.068(19) 0.053(17) 0.06(2) 0.015(15) 0.000(17) 0.015(15) C33 0.068(18) 0.034(15) 0.07(2) 0.043(14) -0.015(16) -0.005(13) C34 0.058(16) 0.023(12) 0.023(13) 0.021(10) 0.015(12) 0.020(11) C35 0.046(14) 0.012(10) 0.044(14) 0.001(9) 0.005(11) 0.011(10) C36 0.042(7) 0.041(7) 0.039(7) -0.001(4) 0.002(4) 0.012(4) C37 0.075(19) 0.034(14) 0.053(18) 0.017(12) 0.038(15) 0.009(13) C38 0.033(13) 0.053(16) 0.058(18) 0.017(13) 0.010(12) 0.013(12) C39 0.057(17) 0.042(16) 0.047(17) -0.021(13) -0.014(14) 0.031(14) C40 0.071(18) 0.08(2) 0.008(12) 0.005(12) -0.002(12) 0.047(16) C41 0.11(3) 0.054(17) 0.032(16) -0.002(13) -0.032(16) 0.029(18) C42 0.08(2) 0.062(18) 0.031(15) 0.017(13) 0.008(14) 0.026(16) C43 0.077(10) 0.075(10) 0.075(10) 0.006(4) 0.000(4) 0.023(5) C44 0.038(14) 0.045(14) 0.020(13) 0.006(11) -0.002(11) 0.009(12) C45 0.042(14) 0.021(12) 0.041(15) -0.011(10) -0.017(11) 0.007(10) C46 0.040(14) 0.053(16) 0.054(17) 0.002(13) -0.002(12) 0.028(13) C47 0.067(17) 0.014(11) 0.071(19) 0.012(11) 0.023(14) 0.030(12) C48 0.047(16) 0.066(19) 0.08(2) -0.014(16) -0.002(15) 0.024(15) C49 0.031(12) 0.055(15) 0.024(13) 0.004(11) -0.014(10) 0.013(11) C50 0.055(15) 0.056(15) 0.028(13) 0.013(11) 0.007(12) 0.036(13) C51 0.044(14) 0.038(14) 0.043(15) -0.008(11) 0.000(12) 0.019(11) C52 0.028(12) 0.035(13) 0.066(18) 0.019(12) 0.013(12) 0.020(11) C53 0.033(13) 0.054(16) 0.021(12) -0.027(12) -0.018(10) 0.011(12) C54 0.021(11) 0.071(17) 0.033(14) 0.023(12) 0.017(10) 0.016(11) C55 0.048(14) 0.044(14) 0.016(12) -0.014(10) 0.016(10) 0.011(11) C56 0.08(2) 0.041(15) 0.06(2) 0.015(13) 0.044(17) 0.030(14) C57 0.043(15) 0.070(19) 0.058(19) -0.006(15) 0.006(14) 0.016(14) C58 0.41(8) 0.037(18) 0.033(19) -0.001(14) -0.03(3) 0.11(3) C59 0.26(5) 0.09(3) 0.07(2) 0.013(19) 0.06(3) 0.13(3) C60 0.16(4) 0.10(3) 0.040(18) 0.032(17) 0.04(2) 0.10(3) C61 0.038(14) 0.031(13) 0.07(2) -0.001(12) 0.023(13) 0.012(11) C62 0.055(15) 0.014(11) 0.011(11) 0.006(8) -0.005(10) 0.017(11) C63 0.040(7) 0.043(7) 0.042(7) 0.004(4) -0.003(4) 0.015(4) C64 0.10(2) 0.037(15) 0.07(2) -0.001(13) -0.065(19) 0.017(15) C65 0.074(19) 0.074(19) 0.06(2) 0.036(16) 0.043(16) 0.053(17) C66 0.054(16) 0.075(19) 0.037(16) -0.020(14) -0.001(13) 0.035(15) C67 0.050(16) 0.062(19) 0.039(15) 0.006(13) -0.003(13) 0.050(16) C68 0.059(16) 0.036(13) 0.037(15) 0.003(11) -0.023(13) 0.025(12) C69 0.113(14) 0.112(14) 0.113(14) 0.005(4) 0.001(4) 0.036(6) C70 0.20(5) 0.13(4) 0.07(3) -0.02(2) -0.01(3) 0.13(4) C71 0.07(2) 0.10(3) 0.09(3) 0.08(2) 0.009(19) 0.021(19) C72 0.035(13) 0.022(11) 0.014(11) -0.007(9) 0.000(10) -0.013(10) C73 0.027(12) 0.051(15) 0.050(16) 0.002(12) 0.014(11) 0.012(11) C74 0.070(19) 0.062(18) 0.037(16) 0.005(13) 0.009(14) 0.011(15) C75 0.029(12) 0.071(18) 0.017(12) 0.003(11) 0.003(10) 0.000(12) C76 0.080(19) 0.035(13) 0.038(15) 0.004(11) 0.013(13) 0.039(14) O1 0.038(9) 0.038(9) 0.033(9) 0.010(7) -0.003(7) 0.009(7) O2 0.074(12) 0.048(10) 0.030(9) -0.004(8) -0.015(9) 0.033(9) O3 0.030(5) 0.035(5) 0.037(5) 0.005(4) 0.003(4) 0.009(4) O4 0.058(11) 0.048(10) 0.029(9) 0.000(8) 0.003(8) 0.033(9) O5 0.047(9) 0.035(9) 0.040(10) -0.001(7) 0.007(8) 0.019(8) O6 0.020(7) 0.038(8) 0.032(9) -0.005(7) 0.010(7) 0.011(7) O7 0.036(8) 0.036(9) 0.033(9) 0.003(7) 0.002(7) 0.021(7) O8 0.032(8) 0.034(8) 0.034(9) 0.020(7) 0.021(7) 0.023(7) O9 0.032(9) 0.038(10) 0.041(10) -0.014(7) 0.002(7) 0.013(8) O10 0.080(14) 0.051(11) 0.051(12) 0.010(9) 0.042(11) 0.016(10) O11 0.062(10) 0.057(10) 0.014(8) -0.004(7) 0.019(7) 0.032(9) O12 0.055(11) 0.053(10) 0.028(9) 0.008(8) -0.005(8) 0.035(9) O13 0.037(9) 0.060(11) 0.030(9) -0.020(8) -0.024(8) 0.033(8) O14 0.056(11) 0.048(10) 0.027(9) 0.008(7) -0.011(8) 0.027(9) O15 0.052(11) 0.048(10) 0.039(11) 0.013(9) 0.004(9) 0.000(9) O16 0.024(8) 0.070(12) 0.032(10) -0.011(9) -0.004(7) 0.028(8) O17 0.011(7) 0.059(10) 0.037(10) 0.001(8) 0.004(7) -0.007(7) O18 0.029(8) 0.023(8) 0.050(10) -0.007(7) 0.000(7) 0.011(7) O19 0.054(10) 0.043(10) 0.030(9) 0.019(8) 0.001(8) 0.015(8) O20 0.059(11) 0.044(10) 0.029(9) 0.002(8) 0.023(8) 0.018(8) O21 0.060(11) 0.035(9) 0.040(10) -0.005(8) 0.021(8) 0.025(8) O22 0.048(10) 0.039(10) 0.030(9) 0.011(7) -0.002(7) 0.016(8) O23 0.035(8) 0.024(8) 0.025(8) -0.009(6) -0.013(6) 0.009(7) O24 0.045(10) 0.013(8) 0.074(13) 0.003(8) -0.005(9) 0.002(8) O25 0.049(12) 0.102(17) 0.085(16) 0.024(13) 0.001(12) 0.036(12) O26 0.085(14) 0.057(12) 0.036(11) -0.007(9) -0.008(10) 0.039(11) O27 0.048(11) 0.049(10) 0.025(9) -0.002(7) 0.002(8) 0.012(9) O28 0.060(11) 0.037(10) 0.046(11) -0.002(8) -0.004(9) 0.016(9) Mn1 0.0348(19) 0.0346(19) 0.031(2) 0.0045(15) 0.0022(16) 0.0127(16) Mn2 0.035(2) 0.0340(19) 0.037(2) -0.0024(16) 0.0033(16) 0.0127(16) Mn3 0.0362(19) 0.0345(19) 0.032(2) 0.0005(15) 0.0044(16) 0.0143(15) Mn4 0.0305(18) 0.0350(19) 0.0267(19) 0.0030(15) -0.0019(15) 0.0174(15) Mn5 0.041(2) 0.038(2) 0.034(2) -0.0008(16) 0.0004(16) 0.0158(17) Mn6 0.0337(19) 0.039(2) 0.030(2) 0.0039(15) 0.0024(16) 0.0139(15) _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 C1 O2 1.26(3) . ? C1 O1 1.28(3) . ? C1 C2 1.58(3) . ? C2 C3 1.49(3) . ? C2 C4 1.51(3) . ? C2 C5 1.56(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O28 1.21(3) 1_665 ? C6 O3 1.28(3) . ? C6 C7 1.55(3) . ? C7 C10 1.49(3) . ? C7 C9 1.57(3) . ? C7 C8 1.59(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O27 1.19(3) 1_665 ? C11 O4 1.23(3) . ? C11 C12 1.58(4) . ? C12 C13 1.52(4) . ? C12 C15 1.53(3) . ? C12 C14 1.54(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O5 1.42(3) . ? C16 C17 1.50(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.43(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.53(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O5 1.44(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O8 1.19(2) . ? C20 O7 1.26(2) . ? C20 C21 1.58(3) . ? C20 Mn2 2.594(19) . ? C21 C22 1.48(4) . ? C21 C24 1.50(3) . ? C21 C23 1.51(3) . ? 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 O9 1.20(2) . ? C25 O10 1.29(3) . ? C25 C26 1.57(3) . ? C26 C29 1.49(3) . ? C26 C27 1.50(3) . ? C26 C28 1.60(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O11 1.45(3) . ? C30 C31 1.55(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.54(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.44(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O11 1.49(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O13 1.23(3) . ? C34 O12 1.30(3) . ? C34 C35 1.57(3) . ? C35 C38 1.48(3) . ? C35 C36 1.52(3) . ? C35 C37 1.54(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O15 1.24(3) . ? C39 O14 1.28(3) . ? C39 C40 1.55(3) . ? C40 C41 1.48(4) . ? C40 C43 1.53(4) . ? C40 C42 1.57(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 O17 1.22(3) . ? C44 O16 1.26(3) . ? C44 C45 1.56(3) . ? C45 C47 1.50(3) . ? C45 C46 1.53(3) . ? C45 C48 1.55(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 O18 1.45(3) . ? C49 C50 1.50(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.51(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.48(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O18 1.46(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 O20 1.24(3) . ? C53 O19 1.27(3) . ? C53 C54 1.56(3) . ? C54 C55 1.50(3) . ? C54 C57 1.50(3) . ? C54 C56 1.59(3) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 O21 1.38(3) . ? C58 C59 1.40(4) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.51(4) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.51(4) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 O21 1.44(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O23 1.21(2) . ? C62 O22 1.32(3) . ? C62 C63 1.54(3) . ? C62 Mn5 2.64(2) . ? C63 C64 1.50(3) . ? C63 C66 1.58(3) . ? C63 C65 1.61(3) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 O24 1.19(3) . ? C67 O25 1.21(3) . ? C67 C68 1.63(3) . ? C68 C69 1.43(5) . ? C68 C70 1.49(4) . ? C68 C71 1.55(4) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 O6 1.23(2) 1_445 ? C72 O26 1.25(3) . ? C72 C73 1.55(3) . ? C73 C75 1.48(3) . ? C73 C74 1.54(3) . ? C73 C76 1.58(3) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? O1 Mn1 2.140(16) . ? O2 Mn2 2.084(16) . ? O3 Mn2 2.207(15) . ? O3 Mn1 2.245(15) . ? O4 Mn1 2.112(16) . ? O5 Mn1 2.260(16) . ? O6 C72 1.23(2) 1_665 ? O6 Mn1 2.159(14) . ? O6 Mn6 2.450(15) 1_665 ? O7 Mn1 2.253(15) . ? O7 Mn2 2.281(14) . ? O8 Mn3 2.295(14) . ? O8 Mn2 2.355(13) . ? O9 Mn2 2.102(15) . ? O10 Mn3 2.057(17) . ? O11 Mn2 2.188(16) . ? O12 Mn3 2.110(16) . ? O13 Mn4 2.113(16) . ? O14 Mn3 2.015(16) . ? O15 Mn4 2.142(18) . ? O16 Mn3 2.159(18) . ? O17 Mn5 2.212(15) . ? O17 Mn4 2.241(16) . ? O18 Mn4 2.250(14) . ? O19 Mn4 2.116(16) . ? O20 Mn5 2.088(15) . ? O21 Mn5 2.249(15) . ? O22 Mn4 2.255(16) . ? O22 Mn5 2.316(15) . ? O23 Mn6 2.254(14) . ? O23 Mn5 2.359(14) . ? O24 Mn5 2.110(16) . ? O25 Mn6 2.10(2) . ? O26 Mn6 2.165(18) . ? O27 C11 1.19(3) 1_445 ? O27 Mn6 2.070(16) . ? O28 C6 1.21(3) 1_445 ? O28 Mn6 2.172(16) . ? Mn6 O6 2.450(15) 1_445 ? 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 C1 O1 124(2) . . ? O2 C1 C2 118.3(19) . . ? O1 C1 C2 117.4(19) . . ? C3 C2 C4 115(2) . . ? C3 C2 C5 112(2) . . ? C4 C2 C5 107(2) . . ? C3 C2 C1 111(2) . . ? C4 C2 C1 107(2) . . ? C5 C2 C1 103.7(19) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O28 C6 O3 124(2) 1_665 . ? O28 C6 C7 116(2) 1_665 . ? O3 C6 C7 120(2) . . ? C10 C7 C6 109(2) . . ? C10 C7 C9 114(2) . . ? C6 C7 C9 107(2) . . ? C10 C7 C8 109(2) . . ? C6 C7 C8 109.6(18) . . ? C9 C7 C8 107.8(19) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O27 C11 O4 126(3) 1_665 . ? O27 C11 C12 118(2) 1_665 . ? O4 C11 C12 116(2) . . ? C13 C12 C15 108(2) . . ? C13 C12 C14 109(2) . . ? C15 C12 C14 113(2) . . ? C13 C12 C11 110(2) . . ? C15 C12 C11 110(2) . . ? C14 C12 C11 108(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 C17 109(2) . . ? O5 C16 H16A 110.0 . . ? C17 C16 H16A 110.0 . . ? O5 C16 H16B 110.0 . . ? C17 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C18 C17 C16 102(2) . . ? C18 C17 H17A 111.4 . . ? C16 C17 H17A 111.4 . . ? C18 C17 H17B 111.4 . . ? C16 C17 H17B 111.4 . . ? H17A C17 H17B 109.2 . . ? C17 C18 C19 105(2) . . ? C17 C18 H18A 110.7 . . ? C19 C18 H18A 110.7 . . ? C17 C18 H18B 110.7 . . ? C19 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? O5 C19 C18 105.4(19) . . ? O5 C19 H19A 110.7 . . ? C18 C19 H19A 110.7 . . ? O5 C19 H19B 110.7 . . ? C18 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? O8 C20 O7 126.2(18) . . ? O8 C20 C21 119.1(17) . . ? O7 C20 C21 114.6(16) . . ? O8 C20 Mn2 65.1(10) . . ? O7 C20 Mn2 61.6(10) . . ? C21 C20 Mn2 172.0(14) . . ? C22 C21 C24 111(2) . . ? C22 C21 C23 109(2) . . ? C24 C21 C23 112.8(19) . . ? C22 C21 C20 108.5(19) . . ? C24 C21 C20 112.8(18) . . ? C23 C21 C20 102.2(17) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O9 C25 O10 126(2) . . ? O9 C25 C26 119(2) . . ? O10 C25 C26 115.4(19) . . ? C29 C26 C27 107(2) . . ? C29 C26 C25 110.8(19) . . ? C27 C26 C25 111(2) . . ? C29 C26 C28 112(2) . . ? C27 C26 C28 111(2) . . ? C25 C26 C28 104.3(19) . . ? 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 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O11 C30 C31 105(2) . . ? O11 C30 H30A 110.8 . . ? C31 C30 H30A 110.8 . . ? O11 C30 H30B 110.8 . . ? C31 C30 H30B 110.8 . . ? H30A C30 H30B 108.9 . . ? C32 C31 C30 100(2) . . ? C32 C31 H31A 111.7 . . ? C30 C31 H31A 111.7 . . ? C32 C31 H31B 111.7 . . ? C30 C31 H31B 111.7 . . ? H31A C31 H31B 109.4 . . ? C33 C32 C31 106(2) . . ? C33 C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? C33 C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.8 . . ? C32 C33 O11 104(2) . . ? C32 C33 H33A 111.0 . . ? O11 C33 H33A 111.0 . . ? C32 C33 H33B 110.9 . . ? O11 C33 H33B 110.9 . . ? H33A C33 H33B 109.0 . . ? O13 C34 O12 123(2) . . ? O13 C34 C35 121(2) . . ? O12 C34 C35 115(2) . . ? C38 C35 C36 114.2(19) . . ? C38 C35 C37 110.4(19) . . ? C36 C35 C37 110(2) . . ? C38 C35 C34 105(2) . . ? C36 C35 C34 110.9(18) . . ? C37 C35 C34 105.7(17) . . ? 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 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O15 C39 O14 126(2) . . ? O15 C39 C40 114(2) . . ? O14 C39 C40 120(3) . . ? C41 C40 C43 113(2) . . ? C41 C40 C39 116(2) . . ? C43 C40 C39 107(2) . . ? C41 C40 C42 109(2) . . ? C43 C40 C42 106(2) . . ? C39 C40 C42 105(2) . . ? 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 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O17 C44 O16 123(2) . . ? O17 C44 C45 120(2) . . ? O16 C44 C45 117(2) . . ? C47 C45 C46 112(2) . . ? C47 C45 C48 110(2) . . ? C46 C45 C48 106(2) . . ? C47 C45 C44 113(2) . . ? C46 C45 C44 108.3(18) . . ? C48 C45 C44 107(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O18 C49 C50 106.0(18) . . ? O18 C49 H49A 110.5 . . ? C50 C49 H49A 110.5 . . ? O18 C49 H49B 110.5 . . ? C50 C49 H49B 110.5 . . ? H49A C49 H49B 108.7 . . ? C49 C50 C51 103.0(18) . . ? C49 C50 H50A 111.2 . . ? C51 C50 H50A 111.2 . . ? C49 C50 H50B 111.2 . . ? C51 C50 H50B 111.2 . . ? H50A C50 H50B 109.1 . . ? C52 C51 C50 101.3(19) . . ? C52 C51 H51A 111.5 . . ? C50 C51 H51A 111.5 . . ? C52 C51 H51B 111.5 . . ? C50 C51 H51B 111.5 . . ? H51A C51 H51B 109.3 . . ? O18 C52 C51 107.0(19) . . ? O18 C52 H52A 110.3 . . ? C51 C52 H52A 110.3 . . ? O18 C52 H52B 110.3 . . ? C51 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? O20 C53 O19 126(2) . . ? O20 C53 C54 119(2) . . ? O19 C53 C54 115(2) . . ? C55 C54 C57 109(2) . . ? C55 C54 C53 111.4(18) . . ? C57 C54 C53 105(2) . . ? C55 C54 C56 111(2) . . ? C57 C54 C56 109(2) . . ? C53 C54 C56 110(2) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O21 C58 C59 112(2) . . ? O21 C58 H58A 109.1 . . ? C59 C58 H58A 109.1 . . ? O21 C58 H58B 109.1 . . ? C59 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? C58 C59 C60 104(3) . . ? C58 C59 H59A 110.9 . . ? C60 C59 H59A 110.9 . . ? C58 C59 H59B 110.9 . . ? C60 C59 H59B 110.9 . . ? H59A C59 H59B 108.9 . . ? C61 C60 C59 107(2) . . ? C61 C60 H60A 110.4 . . ? C59 C60 H60A 110.4 . . ? C61 C60 H60B 110.4 . . ? C59 C60 H60B 110.4 . . ? H60A C60 H60B 108.6 . . ? O21 C61 C60 104(2) . . ? O21 C61 H61A 111.0 . . ? C60 C61 H61A 111.0 . . ? O21 C61 H61B 111.0 . . ? C60 C61 H61B 111.0 . . ? H61A C61 H61B 109.0 . . ? O23 C62 O22 124(2) . . ? O23 C62 C63 121.3(19) . . ? O22 C62 C63 114.6(17) . . ? O23 C62 Mn5 63.3(11) . . ? O22 C62 Mn5 61.3(10) . . ? C63 C62 Mn5 171.5(15) . . ? C64 C63 C62 116(2) . . ? C64 C63 C66 107(2) . . ? C62 C63 C66 107.5(19) . . ? C64 C63 C65 107(2) . . ? C62 C63 C65 110.2(19) . . ? C66 C63 C65 109(2) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O24 C67 O25 129(2) . . ? O24 C67 C68 119(2) . . ? O25 C67 C68 111(2) . . ? C69 C68 C70 110(3) . . ? C69 C68 C71 108(3) . . ? C70 C68 C71 109(3) . . ? C69 C68 C67 111(3) . . ? C70 C68 C67 108(2) . . ? C71 C68 C67 110(2) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O6 C72 O26 118.5(19) 1_445 . ? O6 C72 C73 121.1(19) 1_445 . ? O26 C72 C73 120.0(19) . . ? C75 C73 C74 112(2) . . ? C75 C73 C72 112.7(19) . . ? C74 C73 C72 112(2) . . ? C75 C73 C76 110(2) . . ? C74 C73 C76 107(2) . . ? C72 C73 C76 102.2(19) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C1 O1 Mn1 132.7(14) . . ? C1 O2 Mn2 132.8(15) . . ? C6 O3 Mn2 135.8(15) . . ? C6 O3 Mn1 126.7(14) . . ? Mn2 O3 Mn1 96.8(6) . . ? C11 O4 Mn1 141.1(18) . . ? C16 O5 C19 107.2(16) . . ? C16 O5 Mn1 119.2(13) . . ? C19 O5 Mn1 132.2(13) . . ? C72 O6 Mn1 147.8(13) 1_665 . ? C72 O6 Mn6 86.8(12) 1_665 1_665 ? Mn1 O6 Mn6 108.9(6) . 1_665 ? C20 O7 Mn1 159.7(14) . . ? C20 O7 Mn2 89.4(11) . . ? Mn1 O7 Mn2 94.5(5) . . ? C20 O8 Mn3 159.0(13) . . ? C20 O8 Mn2 87.7(12) . . ? Mn3 O8 Mn2 113.3(5) . . ? C25 O9 Mn2 124.4(15) . . ? C25 O10 Mn3 151.3(17) . . ? C30 O11 C33 110(2) . . ? C30 O11 Mn2 123.9(16) . . ? C33 O11 Mn2 124.8(15) . . ? C34 O12 Mn3 104.3(14) . . ? C34 O13 Mn4 154.8(14) . . ? C39 O14 Mn3 133.8(15) . . ? C39 O15 Mn4 138.4(16) . . ? C44 O16 Mn3 144.6(15) . . ? C44 O17 Mn5 136.6(16) . . ? C44 O17 Mn4 122.5(16) . . ? Mn5 O17 Mn4 97.5(5) . . ? C49 O18 C52 107.4(15) . . ? C49 O18 Mn4 124.0(13) . . ? C52 O18 Mn4 128.2(13) . . ? C53 O19 Mn4 131.8(15) . . ? C53 O20 Mn5 132.4(16) . . ? C58 O21 C61 111(2) . . ? C58 O21 Mn5 120.7(18) . . ? C61 O21 Mn5 126.3(14) . . ? C62 O22 Mn4 162.2(14) . . ? C62 O22 Mn5 88.8(11) . . ? Mn4 O22 Mn5 94.2(6) . . ? C62 O23 Mn6 158.7(13) . . ? C62 O23 Mn5 89.3(12) . . ? Mn6 O23 Mn5 110.4(6) . . ? C67 O24 Mn5 112.2(15) . . ? C67 O25 Mn6 165(2) . . ? C72 O26 Mn6 99.8(15) . . ? C11 O27 Mn6 137.3(17) 1_445 . ? C6 O28 Mn6 144.1(18) 1_445 . ? O4 Mn1 O1 160.6(6) . . ? O4 Mn1 O6 93.4(6) . . ? O1 Mn1 O6 101.5(6) . . ? O4 Mn1 O3 104.5(6) . . ? O1 Mn1 O3 88.2(6) . . ? O6 Mn1 O3 89.2(5) . . ? O4 Mn1 O7 80.8(6) . . ? O1 Mn1 O7 87.0(6) . . ? O6 Mn1 O7 166.9(6) . . ? O3 Mn1 O7 81.0(5) . . ? O4 Mn1 O5 84.8(6) . . ? O1 Mn1 O5 83.4(6) . . ? O6 Mn1 O5 88.0(5) . . ? O3 Mn1 O5 170.5(6) . . ? O7 Mn1 O5 103.0(5) . . ? O2 Mn2 O9 93.9(6) . . ? O2 Mn2 O11 175.3(6) . . ? O9 Mn2 O11 90.0(6) . . ? O2 Mn2 O3 90.3(6) . . ? O9 Mn2 O3 117.8(6) . . ? O11 Mn2 O3 85.5(6) . . ? O2 Mn2 O7 88.1(6) . . ? O9 Mn2 O7 160.8(6) . . ? O11 Mn2 O7 89.2(5) . . ? O3 Mn2 O7 81.2(5) . . ? O2 Mn2 O8 91.1(6) . . ? O9 Mn2 O8 104.7(5) . . ? O11 Mn2 O8 90.5(6) . . ? O3 Mn2 O8 137.2(5) . . ? O7 Mn2 O8 56.1(5) . . ? O2 Mn2 C20 87.6(7) . . ? O9 Mn2 C20 131.9(6) . . ? O11 Mn2 C20 91.8(6) . . ? O3 Mn2 C20 110.2(6) . . ? O7 Mn2 C20 29.0(5) . . ? O8 Mn2 C20 27.2(5) . . ? O14 Mn3 O10 102.0(8) . . ? O14 Mn3 O12 140.0(7) . . ? O10 Mn3 O12 117.5(8) . . ? O14 Mn3 O16 100.4(6) . . ? O10 Mn3 O16 86.0(6) . . ? O12 Mn3 O16 89.1(6) . . ? O14 Mn3 O8 89.0(6) . . ? O10 Mn3 O8 90.1(6) . . ? O12 Mn3 O8 85.0(6) . . ? O16 Mn3 O8 170.5(5) . . ? O13 Mn4 O19 96.9(7) . . ? O13 Mn4 O15 101.5(6) . . ? O19 Mn4 O15 157.9(7) . . ? O13 Mn4 O17 89.9(5) . . ? O19 Mn4 O17 91.1(6) . . ? O15 Mn4 O17 101.1(7) . . ? O13 Mn4 O18 86.6(5) . . ? O19 Mn4 O18 85.6(6) . . ? O15 Mn4 O18 83.3(7) . . ? O17 Mn4 O18 174.8(6) . . ? O13 Mn4 O22 171.2(6) . . ? O19 Mn4 O22 83.9(6) . . ? O15 Mn4 O22 79.9(6) . . ? O17 Mn4 O22 81.3(5) . . ? O18 Mn4 O22 102.2(5) . . ? O20 Mn5 O24 94.1(7) . . ? O20 Mn5 O17 91.4(6) . . ? O24 Mn5 O17 109.3(6) . . ? O20 Mn5 O21 176.5(6) . . ? O24 Mn5 O21 89.4(7) . . ? O17 Mn5 O21 87.0(6) . . ? O20 Mn5 O22 84.9(6) . . ? O24 Mn5 O22 170.1(6) . . ? O17 Mn5 O22 80.6(6) . . ? O21 Mn5 O22 91.7(6) . . ? O20 Mn5 O23 89.9(6) . . ? O24 Mn5 O23 113.1(6) . . ? O17 Mn5 O23 137.4(6) . . ? O21 Mn5 O23 89.1(6) . . ? O22 Mn5 O23 57.1(5) . . ? O20 Mn5 C62 85.0(7) . . ? O24 Mn5 C62 140.2(6) . . ? O17 Mn5 C62 110.5(6) . . ? O21 Mn5 C62 92.6(6) . . ? O22 Mn5 C62 29.9(5) . . ? O23 Mn5 C62 27.4(5) . . ? O27 Mn6 O25 99.5(8) . . ? O27 Mn6 O26 144.7(7) . . ? O25 Mn6 O26 115.2(8) . . ? O27 Mn6 O28 102.4(7) . . ? O25 Mn6 O28 84.6(8) . . ? O26 Mn6 O28 87.8(6) . . ? O27 Mn6 O23 91.0(6) . . ? O25 Mn6 O23 85.5(7) . . ? O26 Mn6 O23 85.6(6) . . ? O28 Mn6 O23 164.5(6) . . ? O27 Mn6 O6 93.6(6) . 1_445 ? O25 Mn6 O6 161.5(7) . 1_445 ? O26 Mn6 O6 54.6(6) . 1_445 ? O28 Mn6 O6 79.9(6) . 1_445 ? O23 Mn6 O6 107.3(5) . 1_445 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.104 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.231 _database_code_depnum_ccdc_archive 'CCDC 959486' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H62 Mn6 N4 O22' _chemical_formula_weight 1736.86 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' Zn Zn 0.2839 1.4301 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.5001(2) _cell_length_b 18.4522(2) _cell_length_c 24.6381(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7956.02(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'claret ' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.787 _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17400 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9086 _reflns_number_gt 7767 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0267P)^2^+7.8842P] 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 9086 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.88191(11) 0.12612(10) 0.38376(7) 0.0233(4) Uani 1 1 d . . . C2 C 0.84380(11) 0.08627(11) 0.42920(8) 0.0262(4) Uani 1 1 d . . . C3 C 0.77067(13) 0.10650(12) 0.44532(9) 0.0341(5) Uani 1 1 d . . . H3 H 0.7451 0.1451 0.4274 0.041 Uiso 1 1 calc R . . C4 C 0.73509(15) 0.07000(14) 0.48787(11) 0.0485(6) Uani 1 1 d . . . H4 H 0.6854 0.0839 0.4993 0.058 Uiso 1 1 calc R . . C5 C 0.77244(16) 0.01327(14) 0.51354(11) 0.0499(7) Uani 1 1 d . . . H5 H 0.7482 -0.0115 0.5427 0.060 Uiso 1 1 calc R . . C6 C 0.84464(15) -0.00754(13) 0.49703(9) 0.0403(5) Uani 1 1 d . . . H6 H 0.8697 -0.0468 0.5145 0.048 Uiso 1 1 calc R . . C7 C 0.88052(13) 0.02893(11) 0.45485(8) 0.0302(4) Uani 1 1 d . . . H7 H 0.9302 0.0147 0.4435 0.036 Uiso 1 1 calc R . . C8 C 0.73162(11) 0.11844(12) 0.28097(8) 0.0287(4) Uani 1 1 d . . . C9 C 0.64821(12) 0.11465(14) 0.29473(9) 0.0380(5) Uani 1 1 d . . . C10 C 0.60690(14) 0.17698(18) 0.30395(12) 0.0571(8) Uani 1 1 d . . . H10 H 0.6304 0.2232 0.3006 0.068 Uiso 1 1 calc R . . C11 C 0.52910(18) 0.1712(2) 0.31851(15) 0.0785(11) Uani 1 1 d . . . H11 H 0.4998 0.2135 0.3255 0.094 Uiso 1 1 calc R . . C12 C 0.49631(17) 0.1043(3) 0.32251(15) 0.0824(12) Uani 1 1 d . . . H12 H 0.4440 0.1006 0.3324 0.099 Uiso 1 1 calc R . . C13 C 0.53654(17) 0.0428(2) 0.31268(14) 0.0724(10) Uani 1 1 d . . . H13 H 0.5123 -0.0032 0.3154 0.087 Uiso 1 1 calc R . . C14 C 0.61256(15) 0.04708(17) 0.29877(12) 0.0538(7) Uani 1 1 d . . . H14 H 0.6408 0.0041 0.2919 0.065 Uiso 1 1 calc R . . C15 C 0.95346(10) 0.28459(10) 0.18351(8) 0.0223(4) Uani 1 1 d . . . C16 C 0.95637(11) 0.34340(10) 0.14161(8) 0.0240(4) Uani 1 1 d . . . C17 C 0.90034(12) 0.39720(11) 0.14148(9) 0.0291(4) Uani 1 1 d . . . H17 H 0.8614 0.3969 0.1683 0.035 Uiso 1 1 calc R . . C18 C 0.90146(14) 0.45108(12) 0.10220(10) 0.0391(5) Uani 1 1 d . . . H18 H 0.8630 0.4874 0.1019 0.047 Uiso 1 1 calc R . . C19 C 0.95869(16) 0.45173(14) 0.06354(11) 0.0506(7) Uani 1 1 d . . . H19 H 0.9597 0.4888 0.0368 0.061 Uiso 1 1 calc R . . C20 C 1.01438(16) 0.39889(15) 0.06351(10) 0.0489(6) Uani 1 1 d . . . H20 H 1.0535 0.3997 0.0368 0.059 Uiso 1 1 calc R . . C21 C 1.01336(13) 0.34437(12) 0.10251(9) 0.0341(5) Uani 1 1 d . . . H21 H 1.0517 0.3079 0.1024 0.041 Uiso 1 1 calc R . . C22 C 1.16267(10) 0.11521(10) 0.35919(7) 0.0223(4) Uani 1 1 d . . . C23 C 1.21314(11) 0.14721(10) 0.40229(8) 0.0237(4) Uani 1 1 d . . . C24 C 1.18263(12) 0.18872(12) 0.44404(9) 0.0325(5) Uani 1 1 d . . . H24 H 1.1294 0.1986 0.4450 0.039 Uiso 1 1 calc R . . C25 C 1.23024(14) 0.21585(13) 0.48447(9) 0.0408(6) Uani 1 1 d . . . H25 H 1.2093 0.2435 0.5134 0.049 Uiso 1 1 calc R . . C26 C 1.30815(13) 0.20263(14) 0.48271(10) 0.0426(6) Uani 1 1 d . . . H26 H 1.3405 0.2209 0.5105 0.051 Uiso 1 1 calc R . . C27 C 1.33881(13) 0.16280(12) 0.44052(9) 0.0358(5) Uani 1 1 d . . . H27 H 1.3924 0.1546 0.4390 0.043 Uiso 1 1 calc R . . C28 C 1.29166(11) 0.13477(11) 0.40043(9) 0.0276(4) Uani 1 1 d . . . H28 H 1.3129 0.1070 0.3717 0.033 Uiso 1 1 calc R . . C29 C 0.98034(11) -0.04108(10) 0.32441(8) 0.0236(4) Uani 1 1 d . . . C30 C 0.99634(11) -0.09592(10) 0.36790(8) 0.0257(4) Uani 1 1 d . . . C31 C 0.94126(13) -0.14819(12) 0.38007(10) 0.0380(5) Uani 1 1 d . . . H31 H 0.8956 -0.1509 0.3593 0.046 Uiso 1 1 calc R . . C32 C 0.95342(15) -0.19644(14) 0.42278(11) 0.0493(7) Uani 1 1 d . . . H32 H 0.9157 -0.2316 0.4315 0.059 Uiso 1 1 calc R . . C33 C 1.02019(15) -0.19299(14) 0.45242(10) 0.0444(6) Uani 1 1 d . . . H33 H 1.0281 -0.2257 0.4817 0.053 Uiso 1 1 calc R . . C34 C 1.07529(14) -0.14268(13) 0.43997(9) 0.0380(5) Uani 1 1 d . . . H34 H 1.1215 -0.1413 0.4602 0.046 Uiso 1 1 calc R . . C35 C 1.06364(12) -0.09350(11) 0.39773(8) 0.0294(4) Uani 1 1 d . . . H35 H 1.1016 -0.0585 0.3894 0.035 Uiso 1 1 calc R . . C36 C 0.79211(12) 0.37045(11) 0.34295(9) 0.0305(4) Uani 1 1 d . . . C37 C 0.76099(16) 0.42874(13) 0.37611(10) 0.0450(6) Uani 1 1 d . . . H37A H 0.7347 0.4081 0.4076 0.068 Uiso 1 1 calc R . . H37B H 0.7247 0.4572 0.3545 0.068 Uiso 1 1 calc R . . H37C H 0.8026 0.4602 0.3885 0.068 Uiso 1 1 calc R . . C38 C 1.20008(12) -0.13877(11) 0.30314(9) 0.0296(4) Uani 1 1 d . . . C39 C 1.21192(15) -0.20822(12) 0.32970(10) 0.0424(6) Uani 1 1 d . . . H39A H 1.2629 -0.2093 0.3461 0.064 Uiso 1 1 calc R . . H39B H 1.2075 -0.2472 0.3029 0.064 Uiso 1 1 calc R . . H39C H 1.1733 -0.2149 0.3580 0.064 Uiso 1 1 calc R . . O1 O 0.92832(7) 0.12210(6) 0.25675(5) 0.0195(2) Uani 1 1 d . . . O2 O 0.99024(7) 0.24132(7) 0.31347(5) 0.0226(3) Uani 1 1 d . . . O3 O 0.84924(8) 0.17996(7) 0.36343(5) 0.0265(3) Uani 1 1 d . . . O4 O 0.94704(7) 0.10185(7) 0.36954(5) 0.0251(3) Uani 1 1 d . . . O5 O 0.75856(8) 0.17803(8) 0.26431(6) 0.0302(3) Uani 1 1 d . . . O6 O 0.89444(8) 0.28113(7) 0.21231(6) 0.0273(3) Uani 1 1 d . . . O7 O 1.09476(7) 0.14026(7) 0.35729(5) 0.0243(3) Uani 1 1 d . . . O8 O 1.18926(8) 0.06691(7) 0.32937(6) 0.0273(3) Uani 1 1 d . . . O9 O 1.03377(7) 0.00222(7) 0.31085(5) 0.0244(3) Uani 1 1 d . . . O10 O 1.23070(8) 0.06077(8) 0.21278(6) 0.0306(3) Uani 1 1 d . . . O11 O 1.08595(8) -0.03999(8) 0.19474(6) 0.0302(3) Uani 1 1 d . . . N1 N 0.81684(10) 0.32460(10) 0.31755(7) 0.0322(4) Uani 1 1 d . . . N2 N 1.19043(10) -0.08417(9) 0.28292(8) 0.0320(4) Uani 1 1 d . . . Mn1 Mn 0.867962(15) 0.220787(15) 0.282799(12) 0.02122(7) Uani 1 1 d . . . Mn2 Mn 1.010666(15) 0.121962(15) 0.306523(11) 0.01877(7) Uani 1 1 d . . . Mn3 Mn 1.137020(16) 0.022068(15) 0.257244(12) 0.02272(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0248(9) 0.0234(9) 0.0218(9) -0.0019(7) 0.0006(7) -0.0035(7) C2 0.0305(10) 0.0231(9) 0.0250(10) -0.0013(8) 0.0050(8) -0.0049(8) C3 0.0354(11) 0.0303(11) 0.0366(12) 0.0057(9) 0.0095(9) 0.0001(9) C4 0.0438(14) 0.0492(15) 0.0525(15) 0.0127(12) 0.0261(12) 0.0023(11) C5 0.0593(16) 0.0410(14) 0.0492(15) 0.0166(12) 0.0247(13) -0.0039(12) C6 0.0549(14) 0.0309(12) 0.0352(12) 0.0096(9) 0.0102(11) -0.0003(10) C7 0.0378(11) 0.0243(10) 0.0285(10) -0.0011(8) 0.0056(9) -0.0004(8) C8 0.0209(9) 0.0360(11) 0.0292(10) -0.0022(9) 0.0024(8) -0.0049(8) C9 0.0243(10) 0.0551(15) 0.0347(12) -0.0038(11) 0.0038(9) -0.0054(10) C10 0.0291(12) 0.074(2) 0.0682(19) -0.0287(16) 0.0025(12) 0.0043(13) C11 0.0394(16) 0.111(3) 0.085(2) -0.036(2) 0.0110(16) 0.0159(19) C12 0.0294(14) 0.141(4) 0.077(2) -0.011(2) 0.0183(15) -0.015(2) C13 0.0376(15) 0.103(3) 0.076(2) 0.015(2) 0.0133(15) -0.0218(17) C14 0.0322(12) 0.0691(18) 0.0602(17) 0.0158(15) 0.0023(12) -0.0175(13) C15 0.0231(9) 0.0197(9) 0.0242(9) 0.0001(7) -0.0010(7) 0.0014(7) C16 0.0271(9) 0.0223(9) 0.0226(9) 0.0025(7) -0.0022(7) -0.0013(7) C17 0.0294(10) 0.0257(10) 0.0321(11) 0.0036(8) -0.0055(8) 0.0006(8) C18 0.0431(13) 0.0299(11) 0.0442(13) 0.0109(10) -0.0117(11) 0.0033(10) C19 0.0642(17) 0.0446(14) 0.0429(14) 0.0261(12) -0.0049(13) -0.0026(13) C20 0.0553(16) 0.0569(16) 0.0343(13) 0.0194(12) 0.0116(11) 0.0017(13) C21 0.0368(11) 0.0358(11) 0.0297(11) 0.0073(9) 0.0047(9) 0.0027(9) C22 0.0225(9) 0.0212(9) 0.0232(9) 0.0041(7) 0.0002(7) -0.0018(7) C23 0.0258(9) 0.0208(9) 0.0244(9) 0.0038(7) -0.0033(7) -0.0048(7) C24 0.0289(10) 0.0352(11) 0.0333(11) -0.0032(9) 0.0010(9) -0.0071(9) C25 0.0427(13) 0.0484(14) 0.0314(12) -0.0107(10) -0.0006(10) -0.0137(11) C26 0.0385(12) 0.0502(14) 0.0390(13) 0.0019(11) -0.0135(10) -0.0197(11) C27 0.0282(10) 0.0366(12) 0.0426(13) 0.0053(10) -0.0093(9) -0.0083(9) C28 0.0274(10) 0.0230(9) 0.0324(11) 0.0064(8) -0.0027(8) -0.0028(8) C29 0.0288(10) 0.0189(9) 0.0231(9) -0.0006(7) -0.0011(8) 0.0011(7) C30 0.0320(10) 0.0189(9) 0.0261(10) 0.0013(7) 0.0043(8) 0.0042(8) C31 0.0359(12) 0.0303(11) 0.0477(14) 0.0129(10) 0.0023(10) 0.0010(9) C32 0.0466(14) 0.0386(13) 0.0628(17) 0.0235(12) 0.0167(13) 0.0067(11) C33 0.0583(16) 0.0409(13) 0.0341(12) 0.0170(10) 0.0131(11) 0.0194(12) C34 0.0470(13) 0.0403(12) 0.0266(11) 0.0018(9) -0.0015(10) 0.0153(11) C35 0.0360(11) 0.0266(10) 0.0256(10) -0.0015(8) 0.0012(9) 0.0063(8) C36 0.0314(10) 0.0269(10) 0.0331(11) 0.0060(9) 0.0027(9) 0.0052(8) C37 0.0572(16) 0.0354(12) 0.0425(13) -0.0036(11) 0.0046(12) 0.0157(11) C38 0.0280(10) 0.0281(11) 0.0327(11) -0.0041(9) 0.0025(8) 0.0046(8) C39 0.0500(14) 0.0301(12) 0.0471(14) 0.0114(10) 0.0129(11) 0.0116(10) O1 0.0174(6) 0.0181(6) 0.0230(6) 0.0004(5) 0.0007(5) -0.0006(5) O2 0.0200(6) 0.0195(6) 0.0282(7) -0.0011(5) 0.0004(5) -0.0008(5) O3 0.0282(7) 0.0266(7) 0.0247(7) 0.0033(6) 0.0063(6) 0.0028(6) O4 0.0240(7) 0.0282(7) 0.0232(7) 0.0025(5) 0.0026(5) 0.0001(5) O5 0.0222(7) 0.0290(7) 0.0395(8) 0.0024(6) -0.0018(6) 0.0002(6) O6 0.0236(6) 0.0289(7) 0.0294(7) 0.0073(6) 0.0049(6) 0.0033(6) O7 0.0225(6) 0.0255(7) 0.0249(7) -0.0018(5) -0.0024(5) 0.0014(5) O8 0.0262(7) 0.0267(7) 0.0289(7) -0.0041(6) -0.0040(6) 0.0026(6) O9 0.0255(6) 0.0195(6) 0.0284(7) 0.0014(5) 0.0007(6) -0.0002(5) O10 0.0288(7) 0.0284(7) 0.0345(8) -0.0025(6) 0.0065(6) 0.0029(6) O11 0.0278(7) 0.0274(7) 0.0353(8) -0.0080(6) -0.0057(6) 0.0044(6) N1 0.0324(9) 0.0278(9) 0.0365(10) 0.0030(8) 0.0045(8) 0.0056(8) N2 0.0317(9) 0.0260(9) 0.0382(10) -0.0001(8) -0.0019(8) 0.0069(7) Mn1 0.01888(13) 0.02068(14) 0.02410(15) 0.00239(11) 0.00307(11) 0.00167(11) Mn2 0.01762(13) 0.01860(13) 0.02009(14) 0.00012(11) 0.00034(10) 0.00026(10) Mn3 0.02172(14) 0.02016(14) 0.02627(15) -0.00206(11) -0.00154(11) 0.00343(11) _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 C1 O3 1.251(2) . ? C1 O4 1.274(2) . ? C1 C2 1.496(3) . ? C2 C7 1.390(3) . ? C2 C3 1.391(3) . ? C3 C4 1.393(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 C6 1.382(4) . ? C5 H5 0.9500 . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O10 1.261(2) 4_755 ? C8 O5 1.265(2) . ? C8 C9 1.500(3) . ? C9 C10 1.377(4) . ? C9 C14 1.398(4) . ? C10 C11 1.412(4) . ? C10 H10 0.9500 . ? C11 C12 1.365(5) . ? C11 H11 0.9500 . ? C12 C13 1.357(5) . ? C12 H12 0.9500 . ? C13 C14 1.376(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O6 1.255(2) . ? C15 O2 1.270(2) 4_755 ? C15 C16 1.499(3) . ? C16 C21 1.387(3) . ? C16 C17 1.395(3) . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 C19 1.382(4) . ? C18 H18 0.9500 . ? C19 C20 1.379(4) . ? C19 H19 0.9500 . ? C20 C21 1.391(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O8 1.245(2) . ? C22 O7 1.276(2) . ? C22 C23 1.502(3) . ? C23 C24 1.389(3) . ? C23 C28 1.394(3) . ? C24 C25 1.392(3) . ? C24 H24 0.9500 . ? C25 C26 1.386(3) . ? C25 H25 0.9500 . ? C26 C27 1.381(3) . ? C26 H26 0.9500 . ? C27 C28 1.387(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 O11 1.252(2) 4_755 ? C29 O9 1.275(2) . ? C29 C30 1.500(3) . ? C30 C35 1.389(3) . ? C30 C31 1.396(3) . ? C31 C32 1.395(3) . ? C31 H31 0.9500 . ? C32 C33 1.379(4) . ? C32 H32 0.9500 . ? C33 C34 1.373(4) . ? C33 H33 0.9500 . ? C34 C35 1.396(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 N1 1.138(3) . ? C36 C37 1.456(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 N2 1.137(3) . ? C38 C39 1.454(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O1 Mn2 1.8895(12) 4_755 ? O1 Mn2 1.8922(12) . ? O1 Mn3 2.1985(12) 4_755 ? O1 Mn1 2.2008(12) . ? O2 C15 1.270(2) 4_755 ? O2 Mn2 2.2377(13) . ? O2 Mn1 2.3008(13) . ? O3 Mn1 2.1499(13) . ? O4 Mn2 1.9463(13) . ? O5 Mn1 2.1202(14) . ? O6 Mn1 2.1143(13) . ? O7 Mn2 1.9608(13) . ? O8 Mn3 2.1629(14) . ? O9 Mn2 2.2487(13) . ? O9 Mn3 2.2679(13) . ? O10 C8 1.261(2) 4_755 ? O10 Mn3 2.0970(14) . ? O11 C29 1.252(2) 4_755 ? O11 Mn3 2.1169(14) . ? N1 Mn1 2.2810(18) . ? N2 Mn3 2.2620(17) . ? Mn1 Mn2 3.1470(4) . ? Mn2 O1 1.8895(12) 4_755 ? Mn2 Mn2 2.8101(5) 4_755 ? Mn2 Mn3 3.1243(4) . ? Mn3 O1 2.1985(12) 4_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 O4 125.32(17) . . ? O3 C1 C2 119.08(17) . . ? O4 C1 C2 115.59(17) . . ? C7 C2 C3 119.99(19) . . ? C7 C2 C1 120.54(18) . . ? C3 C2 C1 119.46(18) . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0(2) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O10 C8 O5 125.33(17) 4_755 . ? O10 C8 C9 116.22(19) 4_755 . ? O5 C8 C9 118.46(19) . . ? C10 C9 C14 119.9(2) . . ? C10 C9 C8 120.6(2) . . ? C14 C9 C8 119.5(2) . . ? C9 C10 C11 119.0(3) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 121.7(3) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C9 120.1(3) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? O6 C15 O2 124.98(17) . 4_755 ? O6 C15 C16 117.03(16) . . ? O2 C15 C16 117.98(16) 4_755 . ? C21 C16 C17 119.64(18) . . ? C21 C16 C15 120.82(18) . . ? C17 C16 C15 119.54(17) . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.4(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.1(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C16 C21 C20 119.9(2) . . ? C16 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? O8 C22 O7 125.85(17) . . ? O8 C22 C23 118.60(17) . . ? O7 C22 C23 115.54(16) . . ? C24 C23 C28 119.60(19) . . ? C24 C23 C22 120.95(17) . . ? C28 C23 C22 119.45(18) . . ? C23 C24 C25 119.9(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 120.2(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.0(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.2(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C23 120.1(2) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? O11 C29 O9 124.81(18) 4_755 . ? O11 C29 C30 116.92(17) 4_755 . ? O9 C29 C30 118.23(17) . . ? C35 C30 C31 119.60(19) . . ? C35 C30 C29 120.97(18) . . ? C31 C30 C29 119.37(19) . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 119.9(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 120.2(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C30 C35 C34 119.8(2) . . ? C30 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? N1 C36 C37 179.2(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 C39 179.2(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Mn2 O1 Mn2 95.99(5) 4_755 . ? Mn2 O1 Mn3 99.40(5) 4_755 4_755 ? Mn2 O1 Mn3 119.77(6) . 4_755 ? Mn2 O1 Mn1 120.86(6) 4_755 . ? Mn2 O1 Mn1 100.23(5) . . ? Mn3 O1 Mn1 119.39(5) 4_755 . ? C15 O2 Mn2 119.95(11) 4_755 . ? C15 O2 Mn1 147.57(12) 4_755 . ? Mn2 O2 Mn1 87.79(4) . . ? C1 O3 Mn1 125.36(12) . . ? C1 O4 Mn2 131.63(13) . . ? C8 O5 Mn1 126.18(13) . . ? C15 O6 Mn1 132.20(12) . . ? C22 O7 Mn2 131.30(12) . . ? C22 O8 Mn3 126.92(12) . . ? C29 O9 Mn2 119.77(12) . . ? C29 O9 Mn3 146.97(12) . . ? Mn2 O9 Mn3 87.53(5) . . ? C8 O10 Mn3 129.21(13) 4_755 . ? C29 O11 Mn3 132.36(13) 4_755 . ? C36 N1 Mn1 168.53(17) . . ? C38 N2 Mn3 162.21(17) . . ? O6 Mn1 O5 102.56(6) . . ? O6 Mn1 O3 167.68(6) . . ? O5 Mn1 O3 86.01(5) . . ? O6 Mn1 O1 95.22(5) . . ? O5 Mn1 O1 93.61(5) . . ? O3 Mn1 O1 93.02(5) . . ? O6 Mn1 N1 87.25(6) . . ? O5 Mn1 N1 92.23(6) . . ? O3 Mn1 N1 83.55(6) . . ? O1 Mn1 N1 173.01(6) . . ? O6 Mn1 O2 88.81(5) . . ? O5 Mn1 O2 166.33(5) . . ? O3 Mn1 O2 84.03(5) . . ? O1 Mn1 O2 77.62(5) . . ? N1 Mn1 O2 95.93(6) . . ? O6 Mn1 Mn2 106.49(4) . . ? O5 Mn1 Mn2 122.74(4) . . ? O3 Mn1 Mn2 75.30(4) . . ? O1 Mn1 Mn2 36.28(3) . . ? N1 Mn1 Mn2 136.73(5) . . ? O2 Mn1 Mn2 45.28(3) . . ? O1 Mn2 O1 84.01(5) 4_755 . ? O1 Mn2 O4 169.02(6) 4_755 . ? O1 Mn2 O4 94.68(5) . . ? O1 Mn2 O7 95.85(5) 4_755 . ? O1 Mn2 O7 170.01(5) . . ? O4 Mn2 O7 87.32(6) . . ? O1 Mn2 O2 98.74(5) 4_755 . ? O1 Mn2 O2 85.79(5) . . ? O4 Mn2 O2 92.03(5) . . ? O7 Mn2 O2 84.36(5) . . ? O1 Mn2 O9 86.50(5) 4_755 . ? O1 Mn2 O9 99.73(5) . . ? O4 Mn2 O9 82.97(5) . . ? O7 Mn2 O9 90.22(5) . . ? O2 Mn2 O9 172.80(5) . . ? O1 Mn2 Mn2 42.04(4) 4_755 4_755 ? O1 Mn2 Mn2 41.97(4) . 4_755 ? O4 Mn2 Mn2 135.61(4) . 4_755 ? O7 Mn2 Mn2 137.06(4) . 4_755 ? O2 Mn2 Mn2 93.13(3) . 4_755 ? O9 Mn2 Mn2 94.07(3) . 4_755 ? O1 Mn2 Mn3 43.97(4) 4_755 . ? O1 Mn2 Mn3 106.74(4) . . ? O4 Mn2 Mn3 127.04(4) . . ? O7 Mn2 Mn3 79.53(4) . . ? O2 Mn2 Mn3 136.34(3) . . ? O9 Mn2 Mn3 46.49(3) . . ? Mn2 Mn2 Mn3 73.073(10) 4_755 . ? O1 Mn2 Mn1 107.12(4) 4_755 . ? O1 Mn2 Mn1 43.49(4) . . ? O4 Mn2 Mn1 78.74(4) . . ? O7 Mn2 Mn1 127.90(4) . . ? O2 Mn2 Mn1 46.93(3) . . ? O9 Mn2 Mn1 136.13(4) . . ? Mn2 Mn2 Mn1 73.171(10) 4_755 . ? Mn3 Mn2 Mn1 146.235(12) . . ? O10 Mn3 O11 97.71(6) . . ? O10 Mn3 O8 88.19(6) . . ? O11 Mn3 O8 169.43(6) . . ? O10 Mn3 O1 92.22(5) . 4_755 ? O11 Mn3 O1 96.92(5) . 4_755 ? O8 Mn3 O1 91.58(5) . 4_755 ? O10 Mn3 N2 96.78(6) . . ? O11 Mn3 N2 84.78(6) . . ? O8 Mn3 N2 85.82(6) . . ? O1 Mn3 N2 170.53(6) 4_755 . ? O10 Mn3 O9 169.13(5) . . ? O11 Mn3 O9 90.00(5) . . ? O8 Mn3 O9 85.41(5) . . ? O1 Mn3 O9 79.20(5) 4_755 . ? N2 Mn3 O9 91.51(6) . . ? O10 Mn3 Mn2 123.74(4) . . ? O11 Mn3 Mn2 107.64(4) . . ? O8 Mn3 Mn2 75.77(4) . . ? O1 Mn3 Mn2 36.63(3) 4_755 . ? N2 Mn3 Mn2 134.03(5) . . ? O9 Mn3 Mn2 45.98(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.367 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 959487'