data_eyt86 # start Validation Reply Form: One Alert A issue _vrf_PLAT029_eyt86 ; PROBLEM: Low completeness RESPONSE: The crystal diffracted very poorly at high angle. Multiple crystals of this compound were tested, but better data could not be collected. ; # end Validation Reply form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H55 Ca F9 Mn3 N6 O20 S3' _chemical_formula_weight 1748.26 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5027(13) _cell_length_b 19.1805(17) _cell_length_c 27.433(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.337(4) _cell_angle_gamma 90.00 _cell_volume 7102.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9309 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.63 _exptl_crystal_description blade _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3556 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8967 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _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_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 103876 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.03 _reflns_number_total 12137 _reflns_number_gt 7462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12137 _refine_ls_number_parameters 1023 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.901 _refine_ls_restrained_S_all 1.901 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.65606(7) 0.13977(5) 0.21352(3) 0.0185(2) Uani 1 1 d . . . Mn1 Mn 0.63414(5) 0.18886(3) 0.09785(2) 0.01380(18) Uani 1 1 d . A . Mn2 Mn 0.71477(5) 0.31214(3) 0.15659(2) 0.01385(18) Uani 1 1 d . A . Mn3 Mn 0.85628(5) 0.20594(3) 0.11651(2) 0.01500(18) Uani 1 1 d . . . C1 C 0.7735(3) 0.2823(3) 0.25675(17) 0.0187(12) Uani 1 1 d . . . C2 C 0.8371(3) 0.3042(3) 0.30022(16) 0.0329(13) Uani 1 1 d . A . H2A H 0.8007 0.2965 0.3302 0.049 Uiso 1 1 calc R . . H2B H 0.8538 0.3537 0.2974 0.049 Uiso 1 1 calc R . . H2C H 0.8981 0.2765 0.3012 0.049 Uiso 1 1 calc R . . C3 C 0.8390(4) 0.0620(2) 0.15621(16) 0.0205(12) Uani 1 1 d . . . C4 C 0.8982(3) -0.0034(2) 0.16502(18) 0.0321(14) Uani 1 1 d . A . H4A H 0.9306 -0.0012 0.1973 0.048 Uiso 1 1 calc R . . H4B H 0.9485 -0.0078 0.1400 0.048 Uiso 1 1 calc R . . H4C H 0.8540 -0.0439 0.1634 0.048 Uiso 1 1 calc R . . C5 C 0.5233(4) 0.1655(3) 0.31328(16) 0.0391(15) Uani 1 1 d . . . H5A H 0.4634 0.1862 0.3267 0.059 Uiso 1 1 calc R A . H5B H 0.5808 0.1943 0.3223 0.059 Uiso 1 1 calc R . . H5C H 0.5325 0.1184 0.3265 0.059 Uiso 1 1 calc R . . C6 C 0.4295(3) 0.1216(3) 0.24523(17) 0.0324(14) Uani 1 1 d . A . H6A H 0.4079 0.1376 0.2124 0.039 Uiso 1 1 calc R . . H6B H 0.3738 0.1284 0.2676 0.039 Uiso 1 1 calc R . . C7 C 0.4563(4) 0.0454(3) 0.24335(18) 0.0359(14) Uani 1 1 d . . . H7A H 0.4708 0.0276 0.2766 0.043 Uiso 1 1 calc R A . H7B H 0.4007 0.0182 0.2289 0.043 Uiso 1 1 calc R . . C8 C 0.5777(4) -0.0306(2) 0.21398(19) 0.0419(15) Uani 1 1 d . . . H8A H 0.5923 -0.0456 0.2475 0.063 Uiso 1 1 calc R A . H8B H 0.6383 -0.0327 0.1951 0.063 Uiso 1 1 calc R . . H8C H 0.5275 -0.0615 0.1992 0.063 Uiso 1 1 calc R . . C9 C 0.8211(5) 0.0926(3) 0.3578(2) 0.0345(14) Uani 1 1 d . . . C10 C 0.7938(4) 0.5660(3) 0.3540(2) 0.0398(15) Uani 1 1 d . . . C11 C 0.1571(8) 0.2567(3) 0.3751(2) 0.094(3) Uani 1 1 d . . . C12 C 0.6805(3) 0.3919(2) 0.02302(15) 0.0148(11) Uani 1 1 d . . . C13 C 0.7805(3) 0.4058(2) 0.03119(15) 0.0175(12) Uani 1 1 d . . . H13 H 0.7995 0.4471 0.0481 0.021 Uiso 1 1 calc R . . C14 C 0.8532(3) 0.3608(2) 0.01517(15) 0.0158(11) Uani 1 1 d . . . C15 C 0.8252(3) 0.3028(2) -0.01199(15) 0.0189(11) Uani 1 1 d . . . H15 H 0.8745 0.2728 -0.0244 0.023 Uiso 1 1 calc R . . C16 C 0.7245(3) 0.2882(2) -0.02135(15) 0.0151(11) Uani 1 1 d . . . C17 C 0.6543(3) 0.3343(2) -0.00499(15) 0.0164(11) Uani 1 1 d . . . H17 H 0.5864 0.3264 -0.0131 0.020 Uiso 1 1 calc R . . C18 C 0.6058(3) 0.4357(2) 0.04763(15) 0.0145(8) Uani 1 1 d . . . C19 C 0.5377(3) 0.4094(2) 0.08063(15) 0.0145(8) Uani 1 1 d . . . C20 C 0.4697(3) 0.4555(2) 0.10104(15) 0.0180(12) Uani 1 1 d . . . H20 H 0.4217 0.4380 0.1227 0.022 Uiso 1 1 calc R . . C21 C 0.4711(3) 0.5257(3) 0.09038(16) 0.0229(12) Uani 1 1 d . . . H21 H 0.4228 0.5556 0.1038 0.028 Uiso 1 1 calc R . . C22 C 0.5418(3) 0.5530(2) 0.06048(16) 0.0209(12) Uani 1 1 d . . . H22 H 0.5452 0.6018 0.0546 0.025 Uiso 1 1 calc R . . C23 C 0.6080(3) 0.5076(2) 0.03914(16) 0.0188(12) Uani 1 1 d . . . H23 H 0.6564 0.5259 0.0181 0.023 Uiso 1 1 calc R . . C24 C 0.9596(3) 0.3710(2) 0.03031(17) 0.0183(12) Uani 1 1 d . . . C25 C 0.9928(3) 0.3667(2) 0.07914(16) 0.0166(11) Uani 1 1 d . A . C26 C 1.0927(3) 0.3802(2) 0.08938(17) 0.0238(12) Uani 1 1 d . . . H26 H 1.1168 0.3778 0.1221 0.029 Uiso 1 1 calc R . . C27 C 1.1571(3) 0.3969(2) 0.05279(19) 0.0301(13) Uani 1 1 d . . . H27 H 1.2242 0.4076 0.0609 0.036 Uiso 1 1 calc R . . C28 C 1.1253(4) 0.3983(2) 0.00486(19) 0.0316(13) Uani 1 1 d . . . H28 H 1.1700 0.4086 -0.0204 0.038 Uiso 1 1 calc R . . C29 C 1.0266(3) 0.3845(2) -0.00575(17) 0.0243(12) Uani 1 1 d . . . H29 H 1.0042 0.3843 -0.0388 0.029 Uiso 1 1 calc R . . C30 C 0.6909(3) 0.2226(2) -0.04610(15) 0.0153(11) Uani 1 1 d . . . C31 C 0.7100(3) 0.1554(2) -0.02744(15) 0.0146(11) Uani 1 1 d . A . C32 C 0.6750(3) 0.0989(2) -0.05351(16) 0.0212(12) Uani 1 1 d . . . H32 H 0.6894 0.0533 -0.0418 0.025 Uiso 1 1 calc R . . C33 C 0.6191(3) 0.1064(3) -0.09664(16) 0.0229(12) Uani 1 1 d . . . H33 H 0.5962 0.0666 -0.1141 0.028 Uiso 1 1 calc R . . C34 C 0.5979(3) 0.1712(3) -0.11332(17) 0.0270(13) Uani 1 1 d . . . H34 H 0.5584 0.1771 -0.1421 0.032 Uiso 1 1 calc R . . C35 C 0.6338(3) 0.2288(2) -0.08835(16) 0.0229(12) Uani 1 1 d . . . H35 H 0.6189 0.2741 -0.1006 0.027 Uiso 1 1 calc R . . C36 C 0.5368(3) 0.3319(2) 0.09645(15) 0.0148(8) Uani 1 1 d . A . C37 C 0.9217(3) 0.3500(2) 0.12130(15) 0.0148(8) Uani 1 1 d . . . C38 C 0.7654(3) 0.1435(2) 0.02245(15) 0.0155(11) Uani 1 1 d . . . C39 C 0.4804(3) 0.2878(2) 0.05891(15) 0.0143(11) Uani 1 1 d . A . C40 C 0.4706(3) 0.1830(2) 0.01739(16) 0.0202(12) Uani 1 1 d . A . H40 H 0.4946 0.1371 0.0124 0.024 Uiso 1 1 calc R . . C41 C 0.3925(3) 0.2068(3) -0.01147(16) 0.0238(12) Uani 1 1 d . . . H41 H 0.3647 0.1782 -0.0366 0.029 Uiso 1 1 calc R . . C42 C 0.3559(3) 0.2719(2) -0.00328(16) 0.0208(12) Uani 1 1 d . . . H42 H 0.3007 0.2888 -0.0218 0.025 Uiso 1 1 calc R . . C43 C 0.4000(3) 0.3125(2) 0.03203(15) 0.0179(11) Uani 1 1 d . . . H43 H 0.3751 0.3580 0.0381 0.021 Uiso 1 1 calc R . . C44 C 0.4923(3) 0.3237(2) 0.14677(16) 0.0143(11) Uani 1 1 d . A . C45 C 0.3956(3) 0.3081(2) 0.15567(17) 0.0195(11) Uani 1 1 d . . . H45 H 0.3493 0.3020 0.1294 0.023 Uiso 1 1 calc R . . C46 C 0.3657(3) 0.3011(2) 0.20336(18) 0.0244(12) Uani 1 1 d . . . H46 H 0.2991 0.2894 0.2102 0.029 Uiso 1 1 calc R . . C47 C 0.4339(3) 0.3114(2) 0.24063(16) 0.0219(12) Uani 1 1 d . . . H47 H 0.4149 0.3084 0.2737 0.026 Uiso 1 1 calc R . . C48 C 0.5307(3) 0.3263(2) 0.22918(17) 0.0208(12) Uani 1 1 d . A . H48 H 0.5777 0.3329 0.2551 0.025 Uiso 1 1 calc R . . C49 C 0.8694(3) 0.4174(2) 0.13753(15) 0.0167(11) Uani 1 1 d . A . C50 C 0.7228(3) 0.4717(2) 0.15839(15) 0.0195(11) Uani 1 1 d . A . H50 H 0.6542 0.4684 0.1650 0.023 Uiso 1 1 calc R . . C51 C 0.7665(4) 0.5357(2) 0.15989(17) 0.0289(13) Uani 1 1 d . . . H51 H 0.7291 0.5763 0.1670 0.035 Uiso 1 1 calc R . . C52 C 0.8664(4) 0.5404(2) 0.15087(18) 0.0327(14) Uani 1 1 d . A . H52 H 0.8994 0.5841 0.1526 0.039 Uiso 1 1 calc R . . C53 C 0.9174(3) 0.4808(2) 0.13931(16) 0.0255(13) Uani 1 1 d . . . H53 H 0.9860 0.4834 0.1325 0.031 Uiso 1 1 calc R A . C54 C 0.9805(3) 0.3162(2) 0.16413(15) 0.0156(11) Uani 1 1 d . A . C55 C 1.0343(3) 0.3506(2) 0.19976(16) 0.0167(11) Uani 1 1 d . . . H55 H 1.0357 0.4001 0.2005 0.020 Uiso 1 1 calc R A . C56 C 1.0865(3) 0.3123(3) 0.23459(17) 0.0272(12) Uani 1 1 d . A . H56 H 1.1248 0.3353 0.2592 0.033 Uiso 1 1 calc R . . C57 C 1.0826(3) 0.2408(3) 0.23322(16) 0.0286(13) Uani 1 1 d . . . H57 H 1.1189 0.2137 0.2564 0.034 Uiso 1 1 calc R A . C58 C 1.0244(3) 0.2091(2) 0.19727(16) 0.0247(12) Uani 1 1 d . A . H58 H 1.0204 0.1597 0.1965 0.030 Uiso 1 1 calc R . . C59 C 1.0295(3) 0.1808(2) 0.04801(17) 0.0233(12) Uani 1 1 d . . . H59 H 1.0669 0.2033 0.0732 0.028 Uiso 1 1 calc R A . C60 C 1.0792(3) 0.1542(2) 0.00963(17) 0.0251(13) Uani 1 1 d . A . H60 H 1.1491 0.1582 0.0079 0.030 Uiso 1 1 calc R . . C61 C 1.0240(4) 0.1209(2) -0.02689(17) 0.0281(13) Uani 1 1 d . . . H61 H 1.0561 0.1010 -0.0540 0.034 Uiso 1 1 calc R A . C62 C 0.9230(3) 0.1171(2) -0.02356(17) 0.0236(12) Uani 1 1 d . A . H62 H 0.8845 0.0950 -0.0485 0.028 Uiso 1 1 calc R . . C63 C 0.8782(3) 0.1454(2) 0.01598(17) 0.0174(11) Uani 1 1 d . A . C64 C 0.7293(3) 0.0753(2) 0.04440(15) 0.0173(8) Uani 1 1 d . A . C65 C 0.7727(3) 0.0100(2) 0.03875(15) 0.0173(8) Uani 1 1 d . . . H65 H 0.8320 0.0049 0.0211 0.021 Uiso 1 1 calc R A . C66 C 0.7281(3) -0.0470(2) 0.05922(16) 0.0220(12) Uani 1 1 d . A . H66 H 0.7564 -0.0920 0.0558 0.026 Uiso 1 1 calc R . . C67 C 0.6432(3) -0.0387(2) 0.08432(16) 0.0202(12) Uani 1 1 d . . . H67 H 0.6113 -0.0780 0.0981 0.024 Uiso 1 1 calc R A . C68 C 0.6042(3) 0.0266(2) 0.08965(16) 0.0227(12) Uani 1 1 d . A . H68 H 0.5448 0.0321 0.1071 0.027 Uiso 1 1 calc R . . F4 F 0.8891(2) 0.57240(16) 0.36780(11) 0.0534(9) Uani 1 1 d . . . F5 F 0.7847(2) 0.59284(17) 0.30948(11) 0.0536(9) Uani 1 1 d . . . F6 F 0.7761(2) 0.49727(16) 0.35023(12) 0.0597(10) Uani 1 1 d . . . F7 F 0.1478(3) 0.2701(2) 0.42294(13) 0.1099(16) Uani 1 1 d . . . F8 F 0.0840(3) 0.2137(2) 0.36064(16) 0.0910(14) Uani 1 1 d . . . F9 F 0.1051(3) 0.3191(2) 0.35582(13) 0.1063(14) Uani 1 1 d . . . F1A F 0.7457(5) 0.1230(4) 0.3766(2) 0.054(2) Uani 0.649(5) 1 d P A 1 F2A F 0.8825(5) 0.1402(3) 0.3410(2) 0.069(2) Uani 0.649(5) 1 d P A 1 F3A F 0.8702(6) 0.0585(4) 0.3932(2) 0.061(2) Uani 0.649(5) 1 d P A 1 F1B F 0.7851(9) 0.1599(7) 0.3629(4) 0.045(3) Uani 0.351(5) 1 d P A 2 F2B F 0.9133(7) 0.0996(7) 0.3734(5) 0.048(3) Uani 0.351(5) 1 d P A 2 F3B F 0.7735(9) 0.0556(5) 0.3897(3) 0.051(3) Uani 0.351(5) 1 d P A 2 N1 N 0.6478(3) 0.08307(18) 0.07081(12) 0.0169(9) Uani 1 1 d . . . N2 N 0.5137(2) 0.22248(18) 0.05219(12) 0.0138(9) Uani 1 1 d . . . N3 N 0.5617(3) 0.33193(17) 0.18326(13) 0.0142(9) Uani 1 1 d . . . N4 N 0.7726(3) 0.41261(18) 0.14788(12) 0.0140(9) Uani 1 1 d . . . N5 N 0.9736(2) 0.24618(19) 0.16349(12) 0.0155(9) Uani 1 1 d . A . N6 N 0.9311(3) 0.17705(17) 0.05234(13) 0.0167(9) Uani 1 1 d . A . O1 O 0.73222(19) 0.21344(13) 0.15171(9) 0.0135(7) Uani 1 1 d . A . O2 O 0.54955(19) 0.16800(13) 0.14753(9) 0.0145(7) Uani 1 1 d . A . O3 O 0.63434(19) 0.30433(14) 0.09982(9) 0.0135(7) Uani 1 1 d . . . O4 O 0.84617(18) 0.30237(14) 0.10722(9) 0.0140(7) Uani 1 1 d . A . O5 O 0.74263(19) 0.19608(14) 0.05653(9) 0.0144(7) Uani 1 1 d . A . O6 O 0.7160(2) 0.23295(16) 0.25933(10) 0.0241(8) Uani 1 1 d . A . O7 O 0.7843(2) 0.32029(15) 0.21790(10) 0.0188(7) Uani 1 1 d . A . O8 O 0.7524(2) 0.06459(15) 0.16951(11) 0.0251(8) Uani 1 1 d . A . O9 O 0.8856(2) 0.11195(15) 0.13479(10) 0.0172(7) Uani 1 1 d . A . O10 O 0.5412(2) 0.03921(15) 0.21419(11) 0.0271(8) Uani 1 1 d . A . O11 O 0.5134(2) 0.16201(15) 0.26192(10) 0.0244(8) Uani 1 1 d . A . O12 O 0.7191(3) 0.07470(17) 0.28027(12) 0.0491(11) Uani 1 1 d . A . O13 O 0.8667(3) 0.0037(2) 0.29284(15) 0.0792(15) Uani 1 1 d . . . O15 O 0.7436(2) 0.67888(15) 0.39581(11) 0.0363(9) Uani 1 1 d . . . O16 O 0.6165(2) 0.59221(16) 0.37680(11) 0.0313(9) Uani 1 1 d . . . O17 O 0.7364(2) 0.57100(16) 0.44201(11) 0.0359(9) Uani 1 1 d . . . O18 O 0.2934(4) 0.1853(2) 0.38690(14) 0.1059(18) Uani 1 1 d . . . O19 O 0.2632(2) 0.2320(2) 0.30687(12) 0.0631(13) Uani 1 1 d . . . O20 O 0.3240(4) 0.3060(3) 0.37074(17) 0.1168(19) Uani 1 1 d . . . O14A O 0.7300(4) -0.0197(3) 0.33369(19) 0.055(2) Uani 0.649(5) 1 d P A 1 O14B O 0.8738(8) 0.1099(5) 0.2694(3) 0.053(4) Uani 0.351(5) 1 d P A 2 S2 S 0.71416(9) 0.60708(7) 0.39737(5) 0.0251(3) Uani 1 1 d . . . S3 S 0.26879(12) 0.25087(9) 0.35581(6) 0.0565(5) Uani 1 1 d . . . S1A S 0.7838(3) 0.0319(2) 0.30933(11) 0.0246(8) Uani 0.649(5) 1 d P A 1 S1B S 0.8114(5) 0.0641(4) 0.2966(3) 0.0358(17) Uani 0.351(5) 1 d P 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 Ca1 0.0169(6) 0.0167(6) 0.0216(6) 0.0024(5) -0.0063(4) -0.0008(4) Mn1 0.0111(4) 0.0123(4) 0.0177(4) -0.0004(3) -0.0054(3) -0.0009(3) Mn2 0.0123(4) 0.0122(4) 0.0167(4) -0.0007(3) -0.0061(3) -0.0015(3) Mn3 0.0121(4) 0.0131(4) 0.0195(4) -0.0009(3) -0.0057(3) 0.0004(3) C1 0.018(3) 0.018(3) 0.020(3) -0.004(3) 0.001(2) 0.003(2) C2 0.034(3) 0.042(3) 0.023(3) 0.003(3) -0.011(2) -0.010(3) C3 0.023(3) 0.016(3) 0.021(3) -0.005(2) -0.008(3) 0.001(3) C4 0.024(3) 0.021(3) 0.051(4) 0.007(3) 0.000(3) 0.003(3) C5 0.038(4) 0.053(4) 0.026(4) 0.004(3) -0.003(3) -0.003(3) C6 0.025(3) 0.043(4) 0.029(3) -0.003(3) -0.004(3) -0.011(3) C7 0.031(3) 0.039(4) 0.038(4) 0.008(3) 0.004(3) -0.016(3) C8 0.050(4) 0.020(3) 0.056(4) 0.006(3) -0.016(3) -0.007(3) C9 0.026(4) 0.035(4) 0.041(4) 0.000(3) -0.016(3) 0.017(4) C10 0.026(4) 0.032(4) 0.060(5) 0.001(3) -0.006(3) -0.007(3) C11 0.229(11) 0.039(5) 0.015(4) -0.001(4) 0.033(5) 0.010(6) C12 0.015(3) 0.011(3) 0.018(3) 0.010(2) -0.010(2) -0.003(2) C13 0.022(3) 0.013(3) 0.018(3) 0.002(2) -0.004(2) -0.004(2) C14 0.013(3) 0.022(3) 0.013(3) 0.005(2) -0.002(2) -0.005(2) C15 0.020(3) 0.025(3) 0.012(3) 0.009(2) 0.002(2) 0.008(2) C16 0.012(3) 0.015(3) 0.018(3) 0.004(2) -0.004(2) -0.006(2) C17 0.015(3) 0.014(3) 0.019(3) 0.007(2) -0.009(2) -0.001(2) C18 0.014(2) 0.013(2) 0.016(2) 0.0007(16) -0.0114(15) -0.0001(16) C19 0.014(2) 0.013(2) 0.016(2) 0.0007(16) -0.0114(15) -0.0001(16) C20 0.010(3) 0.020(3) 0.024(3) 0.003(2) -0.008(2) -0.001(2) C21 0.018(3) 0.027(3) 0.023(3) -0.003(3) -0.011(2) 0.010(3) C22 0.022(3) 0.014(3) 0.026(3) 0.003(2) -0.012(3) -0.002(3) C23 0.012(3) 0.023(3) 0.022(3) 0.008(2) -0.008(2) -0.008(2) C24 0.013(3) 0.015(3) 0.027(3) 0.004(2) 0.001(3) 0.001(2) C25 0.013(3) 0.009(3) 0.028(3) 0.000(2) -0.003(2) -0.004(2) C26 0.017(3) 0.029(3) 0.025(3) -0.001(2) -0.006(3) -0.005(2) C27 0.010(3) 0.038(3) 0.042(4) 0.001(3) -0.005(3) -0.004(3) C28 0.021(3) 0.038(3) 0.036(4) 0.005(3) 0.004(3) -0.005(3) C29 0.020(3) 0.029(3) 0.024(3) 0.004(2) -0.001(3) -0.006(2) C30 0.009(3) 0.023(3) 0.013(3) 0.000(2) 0.000(2) 0.001(2) C31 0.012(3) 0.017(3) 0.015(3) -0.007(2) -0.004(2) 0.001(2) C32 0.015(3) 0.022(3) 0.027(3) 0.000(3) -0.004(2) 0.001(2) C33 0.022(3) 0.026(3) 0.021(3) -0.007(3) -0.007(2) -0.002(2) C34 0.026(3) 0.034(4) 0.020(3) 0.001(3) -0.012(2) 0.000(3) C35 0.028(3) 0.023(3) 0.017(3) 0.003(2) -0.006(2) 0.001(2) C36 0.0060(19) 0.0133(19) 0.025(2) -0.0029(16) -0.0074(16) -0.0011(15) C37 0.0060(19) 0.0133(19) 0.025(2) -0.0029(16) -0.0074(16) -0.0011(15) C38 0.010(3) 0.019(3) 0.017(3) -0.004(2) -0.005(2) 0.001(2) C39 0.012(3) 0.012(3) 0.019(3) 0.003(2) -0.001(2) 0.000(2) C40 0.017(3) 0.018(3) 0.025(3) -0.001(3) -0.007(2) -0.003(2) C41 0.021(3) 0.031(3) 0.019(3) -0.001(2) -0.010(2) -0.006(3) C42 0.016(3) 0.017(3) 0.029(3) 0.003(2) -0.009(2) 0.002(2) C43 0.013(3) 0.014(3) 0.026(3) 0.002(2) -0.006(2) -0.001(2) C44 0.017(3) 0.009(3) 0.017(3) 0.001(2) -0.002(2) -0.001(2) C45 0.019(3) 0.014(3) 0.026(3) 0.000(2) -0.003(2) 0.000(2) C46 0.015(3) 0.020(3) 0.039(4) 0.002(3) 0.003(3) 0.000(2) C47 0.029(3) 0.020(3) 0.017(3) 0.004(2) 0.006(3) 0.007(3) C48 0.020(3) 0.015(3) 0.027(3) 0.001(2) -0.004(2) 0.003(2) C49 0.012(3) 0.016(3) 0.021(3) 0.002(2) -0.008(2) -0.003(2) C50 0.018(3) 0.016(3) 0.024(3) 0.000(2) -0.003(2) 0.003(3) C51 0.028(3) 0.012(3) 0.047(4) -0.003(3) 0.002(3) 0.004(3) C52 0.022(3) 0.015(3) 0.061(4) -0.002(3) 0.001(3) -0.002(3) C53 0.017(3) 0.017(3) 0.042(4) -0.002(3) -0.001(2) -0.003(3) C54 0.007(3) 0.019(3) 0.021(3) 0.001(2) 0.001(2) 0.003(2) C55 0.011(3) 0.012(3) 0.027(3) -0.006(2) -0.004(2) -0.005(2) C56 0.016(3) 0.032(4) 0.034(3) -0.005(3) -0.011(2) -0.007(3) C57 0.025(3) 0.031(4) 0.029(3) -0.001(3) -0.014(3) 0.001(3) C58 0.023(3) 0.017(3) 0.033(3) 0.000(3) -0.009(3) 0.003(2) C59 0.017(3) 0.027(3) 0.026(3) 0.002(3) -0.009(2) 0.000(2) C60 0.010(3) 0.042(3) 0.024(3) -0.001(3) 0.004(3) 0.006(2) C61 0.027(3) 0.036(3) 0.022(3) -0.005(3) 0.003(3) 0.012(3) C62 0.015(3) 0.028(3) 0.028(3) -0.006(3) -0.003(2) 0.003(2) C63 0.020(3) 0.010(3) 0.023(3) 0.001(2) -0.001(3) 0.002(2) C64 0.013(2) 0.019(2) 0.019(2) -0.0051(18) -0.0091(16) -0.0023(16) C65 0.013(2) 0.019(2) 0.019(2) -0.0051(18) -0.0091(16) -0.0023(16) C66 0.022(3) 0.010(3) 0.034(3) -0.009(2) -0.007(3) 0.002(2) C67 0.020(3) 0.009(3) 0.031(3) 0.001(2) -0.003(3) -0.004(2) C68 0.019(3) 0.019(3) 0.030(3) 0.001(3) -0.002(2) -0.006(3) F4 0.0163(18) 0.066(2) 0.078(2) -0.0092(18) 0.0014(16) 0.0056(16) F5 0.046(2) 0.077(3) 0.038(2) 0.0017(18) 0.0086(16) -0.0111(18) F6 0.046(2) 0.039(2) 0.095(3) -0.0215(19) 0.0248(19) -0.0053(17) F7 0.172(4) 0.109(3) 0.049(3) 0.002(2) 0.015(3) 0.080(3) F8 0.050(2) 0.063(3) 0.162(4) -0.004(3) 0.044(2) -0.003(2) F9 0.169(4) 0.074(3) 0.076(3) -0.001(2) -0.004(3) 0.032(3) F1A 0.034(5) 0.068(7) 0.058(5) -0.034(4) -0.014(3) 0.020(4) F2A 0.055(4) 0.052(4) 0.098(5) -0.013(4) -0.021(4) -0.021(4) F3A 0.079(7) 0.064(5) 0.039(4) -0.017(3) -0.034(4) 0.044(4) F1B 0.040(9) 0.055(9) 0.042(7) -0.002(6) -0.002(6) 0.021(6) F2B 0.028(7) 0.059(9) 0.055(9) -0.021(7) -0.015(6) 0.009(6) F3B 0.055(9) 0.058(8) 0.039(6) 0.022(5) 0.004(6) 0.013(6) N1 0.015(2) 0.017(2) 0.019(2) -0.0033(19) -0.0088(19) 0.0003(19) N2 0.010(2) 0.013(2) 0.018(2) -0.0017(19) -0.0046(17) -0.0016(18) N3 0.020(2) 0.012(2) 0.011(2) 0.0013(17) -0.0013(19) 0.0005(17) N4 0.012(2) 0.015(2) 0.015(2) -0.0002(18) -0.0040(17) -0.0014(19) N5 0.013(2) 0.011(2) 0.023(2) -0.0007(19) -0.0102(18) 0.0056(18) N6 0.010(2) 0.015(2) 0.025(2) -0.0019(19) -0.0054(19) 0.0016(18) O1 0.0118(17) 0.0140(17) 0.0143(17) 0.0009(14) -0.0080(13) 0.0016(14) O2 0.0162(17) 0.0144(18) 0.0128(17) 0.0028(13) -0.0031(14) 0.0020(14) O3 0.0080(16) 0.0150(17) 0.0171(17) -0.0015(14) -0.0060(13) 0.0022(14) O4 0.0104(17) 0.0089(17) 0.0222(18) 0.0002(14) -0.0078(13) -0.0005(14) O5 0.0151(17) 0.0139(18) 0.0139(17) -0.0060(15) -0.0037(13) 0.0000(14) O6 0.030(2) 0.020(2) 0.0223(19) 0.0006(15) -0.0072(16) -0.0095(17) O7 0.0209(19) 0.0195(19) 0.0156(19) -0.0019(16) -0.0058(14) -0.0049(15) O8 0.019(2) 0.021(2) 0.035(2) 0.0011(16) 0.0001(17) 0.0000(16) O9 0.0151(18) 0.0101(18) 0.026(2) 0.0030(15) -0.0064(15) 0.0009(15) O10 0.026(2) 0.022(2) 0.033(2) 0.0049(16) -0.0029(17) -0.0049(16) O11 0.025(2) 0.034(2) 0.014(2) 0.0025(15) -0.0058(15) -0.0038(17) O12 0.065(3) 0.033(2) 0.048(2) -0.0001(19) -0.038(2) 0.023(2) O13 0.080(3) 0.084(4) 0.071(3) -0.040(3) -0.037(3) 0.059(3) O15 0.038(2) 0.017(2) 0.053(2) 0.0071(17) -0.0107(18) -0.0013(17) O16 0.0122(19) 0.041(2) 0.040(2) 0.0007(17) -0.0094(16) 0.0038(16) O17 0.041(2) 0.036(2) 0.031(2) 0.0112(18) -0.0140(17) -0.0047(18) O18 0.215(6) 0.045(3) 0.055(3) 0.000(2) -0.047(3) 0.039(3) O19 0.028(2) 0.136(4) 0.025(2) -0.004(2) -0.0088(18) -0.018(2) O20 0.147(5) 0.088(4) 0.113(4) -0.024(3) -0.051(4) -0.064(4) O14A 0.081(5) 0.040(4) 0.046(4) 0.010(3) 0.011(3) -0.031(4) O14B 0.066(8) 0.058(8) 0.037(7) -0.009(6) 0.024(6) -0.026(7) S2 0.0188(8) 0.0252(8) 0.0310(8) 0.0033(7) -0.0052(6) 0.0030(6) S3 0.0578(12) 0.0698(13) 0.0410(11) -0.0223(10) -0.0158(9) -0.0183(10) S1A 0.0258(18) 0.026(2) 0.0218(17) 0.0011(15) -0.0053(13) 0.0047(16) S1B 0.035(4) 0.033(4) 0.039(4) -0.003(3) -0.006(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O8 2.303(3) . ? Ca1 O6 2.320(3) . ? Ca1 O2 2.349(3) . ? Ca1 O12 2.358(3) . ? Ca1 O11 2.403(3) . ? Ca1 O1 2.452(3) . ? Ca1 O10 2.475(3) . ? Ca1 C6 3.218(5) . ? Ca1 Mn1 3.3165(11) . ? Ca1 S1B 3.387(7) . ? Ca1 Mn2 3.7491(11) . ? Mn1 O2 1.842(3) . ? Mn1 O5 1.878(3) . ? Mn1 O1 2.017(3) . ? Mn1 N2 2.129(3) . ? Mn1 N1 2.170(3) . ? Mn1 O3 2.215(3) . ? Mn1 Mn2 3.0480(9) . ? Mn1 Mn3 3.0486(9) . ? Mn2 O3 1.884(3) . ? Mn2 O1 1.913(3) . ? Mn2 O7 1.913(3) . ? Mn2 N4 2.095(3) . ? Mn2 N3 2.241(3) . ? Mn2 O4 2.265(3) . ? Mn2 Mn3 3.0179(9) . ? Mn3 O4 1.872(3) . ? Mn3 O9 1.910(3) . ? Mn3 O1 1.958(3) . ? Mn3 N6 2.124(3) . ? Mn3 N5 2.161(3) . ? Mn3 O5 2.232(3) . ? C1 O6 1.228(5) . ? C1 O7 1.302(5) . ? C1 C2 1.513(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O8 1.234(5) . ? C3 O9 1.294(5) . ? C3 C4 1.504(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O11 1.414(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O11 1.438(5) . ? C6 C7 1.506(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O10 1.418(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O10 1.427(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 F1A 1.291(8) . ? C9 F3B 1.307(10) . ? C9 F2B 1.313(11) . ? C9 F2A 1.324(8) . ? C9 F3A 1.336(8) . ? C9 F1B 1.388(13) . ? C9 S1B 1.767(8) . ? C9 S1A 1.829(6) . ? C10 F5 1.329(6) . ? C10 F4 1.337(5) . ? C10 F6 1.344(5) . ? C10 S2 1.802(6) . ? C11 F8 1.338(9) . ? C11 F7 1.347(6) . ? C11 F9 1.478(8) . ? C11 S3 1.614(9) . ? C12 C17 1.387(6) . ? C12 C13 1.390(6) . ? C12 C18 1.488(6) . ? C13 C14 1.386(6) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 C24 1.499(6) . ? C15 C16 1.407(6) . ? C15 H15 0.9500 . ? C16 C17 1.379(6) . ? C16 C30 1.495(6) . ? C17 H17 0.9500 . ? C18 C23 1.399(6) . ? C18 C19 1.399(6) . ? C19 C20 1.401(6) . ? C19 C36 1.548(6) . ? C20 C21 1.379(6) . ? C20 H20 0.9500 . ? C21 C22 1.377(6) . ? C21 H21 0.9500 . ? C22 C23 1.387(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.380(6) . ? C24 C25 1.405(6) . ? C25 C26 1.395(6) . ? C25 C37 1.553(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9500 . ? C27 C28 1.374(6) . ? C27 H27 0.9500 . ? C28 C29 1.384(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C35 1.382(6) . ? C30 C31 1.408(6) . ? C31 C32 1.376(6) . ? C31 C38 1.561(6) . ? C32 C33 1.397(6) . ? C32 H32 0.9500 . ? C33 C34 1.353(6) . ? C33 H33 0.9500 . ? C34 C35 1.382(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 O3 1.420(5) . ? C36 C39 1.524(6) . ? C36 C44 1.527(6) . ? C37 O4 1.416(5) . ? C37 C49 1.545(6) . ? C37 C54 1.545(6) . ? C38 O5 1.414(5) . ? C38 C64 1.525(6) . ? C38 C63 1.538(6) . ? C39 N2 1.345(5) . ? C39 C43 1.383(5) . ? C40 N2 1.341(5) . ? C40 C41 1.381(6) . ? C40 H40 0.9500 . ? C41 C42 1.363(6) . ? C41 H41 0.9500 . ? C42 C43 1.369(6) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 N3 1.364(5) . ? C44 C45 1.368(5) . ? C45 C46 1.385(6) . ? C45 H45 0.9500 . ? C46 C47 1.375(6) . ? C46 H46 0.9500 . ? C47 C48 1.381(6) . ? C47 H47 0.9500 . ? C48 N3 1.341(5) . ? C48 H48 0.9500 . ? C49 N4 1.348(5) . ? C49 C53 1.378(6) . ? C50 N4 1.352(5) . ? C50 C51 1.364(6) . ? C50 H50 0.9500 . ? C51 C52 1.379(6) . ? C51 H51 0.9500 . ? C52 C53 1.376(6) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 N5 1.346(5) . ? C54 C55 1.373(6) . ? C55 C56 1.385(6) . ? C55 H55 0.9500 . ? C56 C57 1.372(6) . ? C56 H56 0.9500 . ? C57 C58 1.386(6) . ? C57 H57 0.9500 . ? C58 N5 1.344(5) . ? C58 H58 0.9500 . ? C59 N6 1.339(5) . ? C59 C60 1.361(6) . ? C59 H59 0.9500 . ? C60 C61 1.390(6) . ? C60 H60 0.9500 . ? C61 C62 1.371(6) . ? C61 H61 0.9500 . ? C62 C63 1.367(6) . ? C62 H62 0.9500 . ? C63 N6 1.357(5) . ? C64 N1 1.340(5) . ? C64 C65 1.394(6) . ? C65 C66 1.375(6) . ? C65 H65 0.9500 . ? C66 C67 1.359(6) . ? C66 H66 0.9500 . ? C67 C68 1.368(6) . ? C67 H67 0.9500 . ? C68 N1 1.342(5) . ? C68 H68 0.9500 . ? O12 S1B 1.330(7) . ? O12 S1A 1.429(4) . ? O13 S1A 1.332(5) . ? O13 S1B 1.384(7) . ? O15 S2 1.434(3) . ? O16 S2 1.450(3) . ? O17 S2 1.433(3) . ? O18 S3 1.552(4) . ? O19 S3 1.391(3) . ? O20 S3 1.352(4) . ? O14A S1A 1.406(6) . ? O14B S1B 1.438(13) . ? 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 O8 Ca1 O6 124.90(11) . . ? O8 Ca1 O2 94.79(10) . . ? O6 Ca1 O2 116.07(10) . . ? O8 Ca1 O12 82.98(11) . . ? O6 Ca1 O12 82.66(11) . . ? O2 Ca1 O12 157.47(12) . . ? O8 Ca1 O11 150.55(11) . . ? O6 Ca1 O11 80.68(10) . . ? O2 Ca1 O11 84.29(10) . . ? O12 Ca1 O11 86.81(12) . . ? O8 Ca1 O1 75.35(10) . . ? O6 Ca1 O1 77.52(10) . . ? O2 Ca1 O1 66.00(9) . . ? O12 Ca1 O1 133.84(12) . . ? O11 Ca1 O1 129.37(10) . . ? O8 Ca1 O10 82.98(11) . . ? O6 Ca1 O10 143.81(11) . . ? O2 Ca1 O10 79.22(10) . . ? O12 Ca1 O10 78.26(12) . . ? O11 Ca1 O10 67.89(10) . . ? O1 Ca1 O10 136.65(10) . . ? O8 Ca1 C6 128.76(12) . . ? O6 Ca1 C6 104.99(12) . . ? O2 Ca1 C6 70.40(11) . . ? O12 Ca1 C6 93.48(13) . . ? O11 Ca1 C6 24.59(10) . . ? O1 Ca1 C6 131.75(11) . . ? O10 Ca1 C6 46.69(11) . . ? O8 Ca1 Mn1 73.45(8) . . ? O6 Ca1 Mn1 108.77(8) . . ? O2 Ca1 Mn1 32.63(6) . . ? O12 Ca1 Mn1 156.30(9) . . ? O11 Ca1 Mn1 115.04(8) . . ? O1 Ca1 Mn1 37.26(6) . . ? O10 Ca1 Mn1 100.74(7) . . ? C6 Ca1 Mn1 103.02(9) . . ? O8 Ca1 S1B 74.69(13) . . ? O6 Ca1 S1B 76.29(14) . . ? O2 Ca1 S1B 167.32(13) . . ? O12 Ca1 S1B 17.15(18) . . ? O11 Ca1 S1B 101.31(14) . . ? O1 Ca1 S1B 116.69(16) . . ? O10 Ca1 S1B 92.26(16) . . ? C6 Ca1 S1B 110.43(17) . . ? Mn1 Ca1 S1B 143.65(13) . . ? O8 Ca1 Mn2 101.90(8) . . ? O6 Ca1 Mn2 58.11(7) . . ? O2 Ca1 Mn2 66.87(7) . . ? O12 Ca1 Mn2 135.58(9) . . ? O11 Ca1 Mn2 104.69(7) . . ? O1 Ca1 Mn2 26.81(6) . . ? O10 Ca1 Mn2 145.98(8) . . ? C6 Ca1 Mn2 114.81(9) . . ? Mn1 Ca1 Mn2 50.660(19) . . ? S1B Ca1 Mn2 121.63(15) . . ? O2 Mn1 O5 165.51(12) . . ? O2 Mn1 O1 85.23(11) . . ? O5 Mn1 O1 85.23(11) . . ? O2 Mn1 N2 91.30(12) . . ? O5 Mn1 N2 102.60(12) . . ? O1 Mn1 N2 147.09(12) . . ? O2 Mn1 N1 96.25(13) . . ? O5 Mn1 N1 77.81(13) . . ? O1 Mn1 N1 114.17(12) . . ? N2 Mn1 N1 98.74(13) . . ? O2 Mn1 O3 101.51(11) . . ? O5 Mn1 O3 86.59(11) . . ? O1 Mn1 O3 75.41(10) . . ? N2 Mn1 O3 73.26(12) . . ? N1 Mn1 O3 160.58(12) . . ? O2 Mn1 Mn2 89.85(8) . . ? O5 Mn1 Mn2 89.31(8) . . ? O1 Mn1 Mn2 37.92(7) . . ? N2 Mn1 Mn2 109.54(10) . . ? N1 Mn1 Mn2 150.93(9) . . ? O3 Mn1 Mn2 37.95(7) . . ? O2 Mn1 Mn3 121.58(8) . . ? O5 Mn1 Mn3 46.79(8) . . ? O1 Mn1 Mn3 39.22(7) . . ? N2 Mn1 Mn3 143.23(9) . . ? N1 Mn1 Mn3 93.82(9) . . ? O3 Mn1 Mn3 83.57(7) . . ? Mn2 Mn1 Mn3 59.34(2) . . ? O2 Mn1 Ca1 43.42(8) . . ? O5 Mn1 Ca1 123.03(8) . . ? O1 Mn1 Ca1 47.40(8) . . ? N2 Mn1 Ca1 134.32(9) . . ? N1 Mn1 Ca1 93.16(9) . . ? O3 Mn1 Ca1 105.10(7) . . ? Mn2 Mn1 Ca1 72.04(2) . . ? Mn3 Mn1 Ca1 78.72(2) . . ? O3 Mn2 O1 86.16(11) . . ? O3 Mn2 O7 174.18(12) . . ? O1 Mn2 O7 94.81(12) . . ? O3 Mn2 N4 100.83(12) . . ? O1 Mn2 N4 148.82(13) . . ? O7 Mn2 N4 81.29(13) . . ? O3 Mn2 N3 76.41(12) . . ? O1 Mn2 N3 107.85(12) . . ? O7 Mn2 N3 97.85(13) . . ? N4 Mn2 N3 103.33(13) . . ? O3 Mn2 O4 86.77(10) . . ? O1 Mn2 O4 77.10(10) . . ? O7 Mn2 O4 99.05(11) . . ? N4 Mn2 O4 73.06(12) . . ? N3 Mn2 O4 161.92(11) . . ? O3 Mn2 Mn3 90.16(8) . . ? O1 Mn2 Mn3 39.32(8) . . ? O7 Mn2 Mn3 94.22(9) . . ? N4 Mn2 Mn3 109.78(10) . . ? N3 Mn2 Mn3 146.09(9) . . ? O4 Mn2 Mn3 38.26(7) . . ? O3 Mn2 Mn1 46.32(8) . . ? O1 Mn2 Mn1 40.38(8) . . ? O7 Mn2 Mn1 133.63(9) . . ? N4 Mn2 Mn1 141.51(9) . . ? N3 Mn2 Mn1 89.04(9) . . ? O4 Mn2 Mn1 83.96(7) . . ? Mn3 Mn2 Mn1 60.34(2) . . ? O3 Mn2 Ca1 98.68(8) . . ? O1 Mn2 Ca1 35.31(8) . . ? O7 Mn2 Ca1 79.05(9) . . ? N4 Mn2 Ca1 160.33(9) . . ? N3 Mn2 Ca1 78.92(9) . . ? O4 Mn2 Ca1 110.63(7) . . ? Mn3 Mn2 Ca1 72.44(2) . . ? Mn1 Mn2 Ca1 57.30(2) . . ? O4 Mn3 O9 169.23(12) . . ? O4 Mn3 O1 86.21(11) . . ? O9 Mn3 O1 96.57(12) . . ? O4 Mn3 N6 100.35(12) . . ? O9 Mn3 N6 82.63(12) . . ? O1 Mn3 N6 148.98(13) . . ? O4 Mn3 N5 77.19(12) . . ? O9 Mn3 N5 92.06(13) . . ? O1 Mn3 N5 107.66(12) . . ? N6 Mn3 N5 103.35(13) . . ? O4 Mn3 O5 86.37(11) . . ? O9 Mn3 O5 104.39(11) . . ? O1 Mn3 O5 77.78(10) . . ? N6 Mn3 O5 72.49(12) . . ? N5 Mn3 O5 162.13(12) . . ? O4 Mn3 Mn2 48.53(8) . . ? O9 Mn3 Mn2 132.10(9) . . ? O1 Mn3 Mn2 38.24(8) . . ? N6 Mn3 Mn2 142.72(9) . . ? N5 Mn3 Mn2 90.19(9) . . ? O5 Mn3 Mn2 84.00(7) . . ? O4 Mn3 Mn1 90.86(8) . . ? O9 Mn3 Mn1 98.04(9) . . ? O1 Mn3 Mn1 40.63(8) . . ? N6 Mn3 Mn1 108.56(10) . . ? N5 Mn3 Mn1 147.47(9) . . ? O5 Mn3 Mn1 37.84(7) . . ? Mn2 Mn3 Mn1 60.32(2) . . ? O6 C1 O7 124.2(4) . . ? O6 C1 C2 121.1(4) . . ? O7 C1 C2 114.7(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O8 C3 O9 125.3(4) . . ? O8 C3 C4 119.3(4) . . ? O9 C3 C4 115.4(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O11 C5 H5A 109.5 . . ? O11 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O11 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O11 C6 C7 110.2(4) . . ? O11 C6 Ca1 44.07(19) . . ? C7 C6 Ca1 82.3(3) . . ? O11 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 . . ? Ca1 C6 H6A 89.0 . . ? O11 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 . . ? Ca1 C6 H6B 153.3 . . ? H6A C6 H6B 108.1 . . ? O10 C7 C6 107.4(4) . . ? O10 C7 H7A 110.2 . . ? C6 C7 H7A 110.2 . . ? O10 C7 H7B 110.2 . . ? C6 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O10 C8 H8A 109.5 . . ? O10 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O10 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? F1A C9 F3B 64.8(7) . . ? F1A C9 F2B 125.1(6) . . ? F3B C9 F2B 108.3(9) . . ? F1A C9 F2A 109.5(6) . . ? F3B C9 F2A 158.4(7) . . ? F2B C9 F2A 56.4(7) . . ? F1A C9 F3A 108.3(7) . . ? F3B C9 F3A 59.3(6) . . ? F2B C9 F3A 50.5(6) . . ? F2A C9 F3A 106.8(7) . . ? F1A C9 F1B 42.2(5) . . ? F3B C9 F1B 105.1(8) . . ? F2B C9 F1B 101.7(9) . . ? F2A C9 F1B 67.5(6) . . ? F3A C9 F1B 123.5(7) . . ? F1A C9 S1B 118.5(5) . . ? F3B C9 S1B 116.2(7) . . ? F2B C9 S1B 112.9(7) . . ? F2A C9 S1B 85.1(5) . . ? F3A C9 S1B 124.4(5) . . ? F1B C9 S1B 111.4(6) . . ? F1A C9 S1A 111.8(5) . . ? F3B C9 S1A 90.6(6) . . ? F2B C9 S1A 123.0(6) . . ? F2A C9 S1A 110.5(5) . . ? F3A C9 S1A 109.9(5) . . ? F1B C9 S1A 125.0(6) . . ? S1B C9 S1A 25.8(2) . . ? F5 C10 F4 107.0(4) . . ? F5 C10 F6 107.2(5) . . ? F4 C10 F6 106.3(4) . . ? F5 C10 S2 113.2(4) . . ? F4 C10 S2 111.0(4) . . ? F6 C10 S2 111.8(4) . . ? F8 C11 F7 108.7(7) . . ? F8 C11 F9 93.0(7) . . ? F7 C11 F9 98.0(5) . . ? F8 C11 S3 123.2(5) . . ? F7 C11 S3 116.2(7) . . ? F9 C11 S3 112.3(5) . . ? C17 C12 C13 118.5(4) . . ? C17 C12 C18 122.3(4) . . ? C13 C12 C18 119.0(4) . . ? C14 C13 C12 121.4(4) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 C24 120.8(4) . . ? C15 C14 C24 120.0(4) . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.8(4) . . ? C17 C16 C30 118.9(4) . . ? C15 C16 C30 122.2(4) . . ? C16 C17 C12 121.5(4) . . ? C16 C17 H17 119.3 . . ? C12 C17 H17 119.3 . . ? C23 C18 C19 118.7(4) . . ? C23 C18 C12 117.6(4) . . ? C19 C18 C12 123.6(4) . . ? C18 C19 C20 118.5(4) . . ? C18 C19 C36 122.5(4) . . ? C20 C19 C36 119.0(4) . . ? C21 C20 C19 121.3(4) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 120.7(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 118.4(4) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C22 C23 C18 122.1(4) . . ? C22 C23 H23 118.9 . . ? C18 C23 H23 118.9 . . ? C29 C24 C25 119.6(4) . . ? C29 C24 C14 117.7(4) . . ? C25 C24 C14 122.6(4) . . ? C26 C25 C24 117.8(4) . . ? C26 C25 C37 120.0(4) . . ? C24 C25 C37 122.2(4) . . ? C27 C26 C25 121.3(4) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C28 C27 C26 120.8(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 118.4(4) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C24 C29 C28 122.0(4) . . ? C24 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C35 C30 C31 118.6(4) . . ? C35 C30 C16 117.7(4) . . ? C31 C30 C16 123.6(4) . . ? C32 C31 C30 118.3(4) . . ? C32 C31 C38 119.5(4) . . ? C30 C31 C38 122.2(4) . . ? C31 C32 C33 122.0(4) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C34 C33 C32 119.2(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.9(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C30 C35 C34 121.9(4) . . ? C30 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? O3 C36 C39 106.6(3) . . ? O3 C36 C44 106.7(3) . . ? C39 C36 C44 110.6(3) . . ? O3 C36 C19 111.3(3) . . ? C39 C36 C19 110.5(3) . . ? C44 C36 C19 111.0(3) . . ? O4 C37 C49 106.7(3) . . ? O4 C37 C54 106.9(3) . . ? C49 C37 C54 111.3(3) . . ? O4 C37 C25 112.6(3) . . ? C49 C37 C25 109.6(3) . . ? C54 C37 C25 109.7(3) . . ? O5 C38 C64 105.9(3) . . ? O5 C38 C63 106.9(3) . . ? C64 C38 C63 113.1(4) . . ? O5 C38 C31 111.6(3) . . ? C64 C38 C31 108.7(3) . . ? C63 C38 C31 110.5(3) . . ? N2 C39 C43 120.5(4) . . ? N2 C39 C36 116.5(4) . . ? C43 C39 C36 123.0(4) . . ? N2 C40 C41 122.4(4) . . ? N2 C40 H40 118.8 . . ? C41 C40 H40 118.8 . . ? C42 C41 C40 118.8(4) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C41 C42 C43 119.1(4) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C42 C43 C39 120.3(4) . . ? C42 C43 H43 119.8 . . ? C39 C43 H43 119.8 . . ? N3 C44 C45 122.5(4) . . ? N3 C44 C36 111.9(4) . . ? C45 C44 C36 125.6(4) . . ? C44 C45 C46 119.4(4) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C47 C46 C45 118.9(4) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C48 118.8(4) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? N3 C48 C47 123.2(4) . . ? N3 C48 H48 118.4 . . ? C47 C48 H48 118.4 . . ? N4 C49 C53 120.7(4) . . ? N4 C49 C37 117.1(4) . . ? C53 C49 C37 122.1(4) . . ? N4 C50 C51 122.9(4) . . ? N4 C50 H50 118.5 . . ? C51 C50 H50 118.5 . . ? C50 C51 C52 118.6(4) . . ? C50 C51 H51 120.7 . . ? C52 C51 H51 120.7 . . ? C53 C52 C51 119.0(4) . . ? C53 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? C52 C53 C49 120.3(4) . . ? C52 C53 H53 119.9 . . ? C49 C53 H53 119.9 . . ? N5 C54 C55 121.6(4) . . ? N5 C54 C37 112.0(4) . . ? C55 C54 C37 126.4(4) . . ? C54 C55 C56 119.2(4) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? C57 C56 C55 119.5(4) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 118.6(4) . . ? C56 C57 H57 120.7 . . ? C58 C57 H57 120.7 . . ? N5 C58 C57 122.0(4) . . ? N5 C58 H58 119.0 . . ? C57 C58 H58 119.0 . . ? N6 C59 C60 123.8(4) . . ? N6 C59 H59 118.1 . . ? C60 C59 H59 118.1 . . ? C59 C60 C61 117.7(4) . . ? C59 C60 H60 121.2 . . ? C61 C60 H60 121.2 . . ? C62 C61 C60 119.6(4) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C63 C62 C61 119.4(4) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? N6 C63 C62 121.7(4) . . ? N6 C63 C38 115.6(4) . . ? C62 C63 C38 122.7(4) . . ? N1 C64 C65 120.9(4) . . ? N1 C64 C38 113.1(4) . . ? C65 C64 C38 126.0(4) . . ? C66 C65 C64 118.6(4) . . ? C66 C65 H65 120.7 . . ? C64 C65 H65 120.7 . . ? C67 C66 C65 119.8(4) . . ? C67 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C66 C67 C68 119.5(4) . . ? C66 C67 H67 120.3 . . ? C68 C67 H67 120.3 . . ? N1 C68 C67 121.6(4) . . ? N1 C68 H68 119.2 . . ? C67 C68 H68 119.2 . . ? C64 N1 C68 119.5(4) . . ? C64 N1 Mn1 111.5(3) . . ? C68 N1 Mn1 125.6(3) . . ? C40 N2 C39 118.8(4) . . ? C40 N2 Mn1 124.1(3) . . ? C39 N2 Mn1 117.0(3) . . ? C48 N3 C44 117.1(4) . . ? C48 N3 Mn2 127.1(3) . . ? C44 N3 Mn2 111.3(3) . . ? C49 N4 C50 118.5(4) . . ? C49 N4 Mn2 116.9(3) . . ? C50 N4 Mn2 123.9(3) . . ? C58 N5 C54 119.0(4) . . ? C58 N5 Mn3 125.3(3) . . ? C54 N5 Mn3 114.4(3) . . ? C59 N6 C63 117.8(4) . . ? C59 N6 Mn3 123.5(3) . . ? C63 N6 Mn3 118.2(3) . . ? Mn2 O1 Mn3 102.44(12) . . ? Mn2 O1 Mn1 101.70(12) . . ? Mn3 O1 Mn1 100.15(12) . . ? Mn2 O1 Ca1 117.88(12) . . ? Mn3 O1 Ca1 132.54(12) . . ? Mn1 O1 Ca1 95.34(10) . . ? Mn1 O2 Ca1 103.95(12) . . ? C36 O3 Mn2 122.7(2) . . ? C36 O3 Mn1 111.7(2) . . ? Mn2 O3 Mn1 95.73(11) . . ? C37 O4 Mn3 123.4(2) . . ? C37 O4 Mn2 110.7(2) . . ? Mn3 O4 Mn2 93.21(11) . . ? C38 O5 Mn1 122.1(2) . . ? C38 O5 Mn3 113.1(2) . . ? Mn1 O5 Mn3 95.38(11) . . ? C1 O6 Ca1 140.9(3) . . ? C1 O7 Mn2 127.7(3) . . ? C3 O8 Ca1 137.0(3) . . ? C3 O9 Mn3 135.9(3) . . ? C7 O10 C8 111.4(3) . . ? C7 O10 Ca1 117.0(3) . . ? C8 O10 Ca1 121.0(3) . . ? C5 O11 C6 113.5(3) . . ? C5 O11 Ca1 120.0(3) . . ? C6 O11 Ca1 111.3(3) . . ? S1B O12 S1A 33.7(3) . . ? S1B O12 Ca1 131.3(5) . . ? S1A O12 Ca1 160.4(3) . . ? S1A O13 S1B 34.4(3) . . ? O17 S2 O15 115.9(2) . . ? O17 S2 O16 114.11(19) . . ? O15 S2 O16 115.28(19) . . ? O17 S2 C10 103.7(2) . . ? O15 S2 C10 103.3(2) . . ? O16 S2 C10 102.1(2) . . ? O20 S3 O19 120.8(3) . . ? O20 S3 O18 111.0(3) . . ? O19 S3 O18 109.0(3) . . ? O20 S3 C11 111.1(4) . . ? O19 S3 C11 107.7(3) . . ? O18 S3 C11 93.8(3) . . ? O13 S1A O14A 108.8(4) . . ? O13 S1A O12 123.5(4) . . ? O14A S1A O12 110.7(4) . . ? O13 S1A C9 106.6(3) . . ? O14A S1A C9 103.8(4) . . ? O12 S1A C9 101.2(3) . . ? O12 S1B O13 127.3(6) . . ? O12 S1B O14B 106.7(7) . . ? O13 S1B O14B 98.5(6) . . ? O12 S1B C9 108.7(5) . . ? O13 S1B C9 107.5(5) . . ? O14B S1B C9 105.9(6) . . ? O12 S1B Ca1 31.5(3) . . ? O13 S1B Ca1 129.4(4) . . ? O14B S1B Ca1 75.5(5) . . ? C9 S1B Ca1 122.5(3) . . ? _diffrn_measured_fraction_theta_max 0.781 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.471 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.106