# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Myoung Soo Lah' _publ_contact_author_address ; Department of Chemistry and Applied Chemistry Hanyang University, Ansan, Kyunggi-do, 426-791, Korea ; _publ_contact_author_email mslah@hanyang.ac.kr _publ_contact_author_phone '82 31 400 5496' _publ_contact_author_fax '82 31 407 3863' _publ_section_title ; Encapsulation of a guest molecule in a strained form: An extended 36-membered dodecanuclear manganese metallamacrocycle that accommodates a cyclooctane in the S4 symmetry conformation ; loop_ _publ_author_name 'Myoung Soo Lah.' 'Rohith P. John' 'Kyungjin Lee.' 'Dohyun Moon.' 'Jaejoon Park.' data_p5_04te _database_code_depnum_ccdc_archive 'CCDC 298633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C182 H238 Mn12 N24 O51' _chemical_formula_weight 4237.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 27.0406(3) _cell_length_b 27.0406(3) _cell_length_c 18.7658(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13721.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9167 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.80 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4394 _exptl_absorpt_coefficient_mu 0.592 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7563 _exptl_absorpt_correction_T_max 0.8908 _exptl_absorpt_process_details 'HKL2000 scale pack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.82657 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Bending Magnet (PAL)' _diffrn_radiation_monochromator 'Silicon double crystal monochromator' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54175 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7500 _reflns_number_gt 6793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Protenum2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Diamond 3.1a, ORTEP3' _computing_publication_material WinGX _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^)+(0.1059P)^2^+22.5871P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7500 _refine_ls_number_parameters 621 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1A Mn 0.56895(3) 0.02557(3) 0.27445(4) 0.0419(3) Uani 1 1 d . A . O1A O 0.52704(11) 0.06060(12) 0.21327(16) 0.0459(8) Uani 1 1 d . . . O2A O 0.67158(11) 0.08391(11) 0.13288(15) 0.0436(8) Uani 1 1 d . A . O3A O 0.62136(11) -0.00545(12) 0.32839(16) 0.0460(8) Uani 1 1 d . A . O4A O 0.57490(14) 0.09247(15) 0.34316(19) 0.0659(10) Uani 1 1 d . . . N1A N 0.62519(13) 0.04388(14) 0.21620(19) 0.0402(9) Uani 1 1 d . . . N2A N 0.67162(13) 0.02794(13) 0.24343(19) 0.0386(9) Uani 1 1 d . A . C1A C 0.53665(17) 0.08256(17) 0.1509(2) 0.0430(12) Uani 1 1 d . A . C2A C 0.58412(16) 0.08875(17) 0.1217(2) 0.0419(11) Uani 1 1 d . . . C3A C 0.58976(18) 0.1123(2) 0.0554(3) 0.0578(14) Uani 1 1 d . A . H3A H 0.6219 0.1156 0.0355 0.069 Uiso 1 1 calc R . . C4A C 0.5498(2) 0.1304(2) 0.0191(3) 0.0663(16) Uani 1 1 d . . . H4A H 0.5543 0.1466 -0.0254 0.080 Uiso 1 1 calc R A . C5A C 0.50265(19) 0.1248(2) 0.0476(3) 0.0602(15) Uani 1 1 d . A . H5A H 0.4748 0.1373 0.0225 0.072 Uiso 1 1 calc R . . C6A C 0.49605(18) 0.10124(18) 0.1125(3) 0.0511(13) Uani 1 1 d . . . H6A H 0.4636 0.0976 0.1312 0.061 Uiso 1 1 calc R A . C7A C 0.62895(16) 0.07170(17) 0.1584(2) 0.0394(11) Uani 1 1 d . A . C8A C 0.66519(17) 0.00238(17) 0.3012(2) 0.0395(11) Uani 1 1 d . . . C9A C 0.70895(16) -0.02128(16) 0.3356(2) 0.0390(11) Uani 1 1 d . A . H9A H 0.7386 -0.0166 0.3045 0.047 Uiso 1 1 calc R . . C10A C 0.6997(2) -0.07671(19) 0.3458(4) 0.0716(17) Uani 1 1 d . . . H10A H 0.6959 -0.0926 0.2986 0.086 Uiso 1 1 calc R A . H10B H 0.6684 -0.0815 0.3725 0.086 Uiso 1 1 calc R . . C11A C 0.7425(2) -0.1017(2) 0.3867(4) 0.085(2) Uani 1 1 d . A . H11A H 0.7335 -0.1365 0.3968 0.102 Uiso 1 1 calc R . . H11B H 0.7724 -0.1018 0.3562 0.102 Uiso 1 1 calc R . . C12A C 0.7539(2) -0.0763(3) 0.4543(3) 0.0763(19) Uani 1 1 d . . . H12A H 0.7261 -0.0811 0.4878 0.092 Uiso 1 1 calc R A . H12B H 0.7837 -0.0917 0.4758 0.092 Uiso 1 1 calc R . . C13A C 0.76283(18) -0.0229(2) 0.4451(3) 0.0589(15) Uani 1 1 d . A . H13A H 0.7929 -0.0179 0.4159 0.071 Uiso 1 1 calc R . . H13B H 0.7685 -0.0075 0.4922 0.071 Uiso 1 1 calc R . . C14A C 0.71896(18) 0.0021(2) 0.4089(2) 0.0512(13) Uani 1 1 d . . . H14A H 0.7260 0.0378 0.4030 0.061 Uiso 1 1 calc R A . H14B H 0.6892 -0.0013 0.4393 0.061 Uiso 1 1 calc R . . C15A C 0.5860(3) 0.0937(4) 0.4168(4) 0.102(3) Uani 0.865(12) 1 d P A 1 H15A H 0.5692 0.0663 0.4408 0.152 Uiso 0.865(12) 1 calc PR A 1 H15B H 0.5746 0.1252 0.4370 0.152 Uiso 0.865(12) 1 calc PR A 1 H15C H 0.6218 0.0907 0.4235 0.152 Uiso 0.865(12) 1 calc PR A 1 C25A C 0.5645(12) 0.1288(13) 0.3189(18) 0.035(10) Uiso 0.135(12) 1 d P A 2 H25A H 0.5613 0.1537 0.3565 0.053 Uiso 0.135(12) 1 calc PR A 2 H25B H 0.5328 0.1254 0.2939 0.053 Uiso 0.135(12) 1 calc PR A 2 H25C H 0.5901 0.1390 0.2851 0.053 Uiso 0.135(12) 1 calc PR A 2 Mn1B Mn 0.72971(2) 0.07771(3) 0.19600(4) 0.0392(3) Uani 1 1 d . . . O1B O 0.70754(11) 0.12860(11) 0.25434(18) 0.0472(8) Uani 1 1 d . A . O2B O 0.84441(11) 0.08204(11) 0.34361(15) 0.0386(7) Uani 1 1 d . A . O3B O 0.76288(11) 0.02534(11) 0.14454(15) 0.0419(8) Uani 1 1 d . A . O4B O 0.76213(12) 0.13202(13) 0.11710(18) 0.0562(9) Uani 1 1 d . A . N1B N 0.78813(13) 0.06951(13) 0.25511(19) 0.0373(9) Uani 1 1 d . A . N2B N 0.82196(13) 0.03282(13) 0.23032(18) 0.0369(9) Uani 1 1 d . . . C1B C 0.72383(17) 0.14257(17) 0.3187(3) 0.0442(12) Uani 1 1 d . . . C2B C 0.76937(17) 0.12740(15) 0.3485(2) 0.0407(11) Uani 1 1 d . A . C3B C 0.78428(19) 0.14709(17) 0.4148(2) 0.0473(12) Uani 1 1 d . . . H3B H 0.8152 0.1377 0.4346 0.057 Uiso 1 1 calc R A . C4B C 0.7540(2) 0.18021(19) 0.4514(3) 0.0621(15) Uani 1 1 d . A . H4B H 0.7642 0.1934 0.4960 0.075 Uiso 1 1 calc R . . C5B C 0.7085(2) 0.1938(2) 0.4219(3) 0.0613(15) Uani 1 1 d . . . H5B H 0.6877 0.2163 0.4467 0.074 Uiso 1 1 calc R A . C6B C 0.69364(19) 0.17497(18) 0.3572(3) 0.0534(13) Uani 1 1 d . A . H6B H 0.6623 0.1841 0.3384 0.064 Uiso 1 1 calc R . . C7B C 0.80293(17) 0.09209(16) 0.3150(2) 0.0367(11) Uani 1 1 d . . . C8B C 0.80452(17) 0.01188(17) 0.1735(2) 0.0405(11) Uani 1 1 d . A . C9B C 0.83281(17) -0.02959(18) 0.1406(2) 0.0490(13) Uani 1 1 d . . . H9B H 0.8585 -0.0407 0.1755 0.059 Uiso 1 1 calc R A . C10B C 0.85925(19) -0.0137(2) 0.0717(3) 0.0602(15) Uani 1 1 d . A . H10C H 0.8346 -0.0017 0.0367 0.072 Uiso 1 1 calc R . . H10D H 0.8825 0.0137 0.0822 0.072 Uiso 1 1 calc R . . C11B C 0.8873(2) -0.0570(3) 0.0408(3) 0.084(2) Uani 1 1 d . . . H11C H 0.9035 -0.0466 -0.0040 0.101 Uiso 1 1 calc R A . H11D H 0.9134 -0.0672 0.0746 0.101 Uiso 1 1 calc R . . C12B C 0.8539(2) -0.1004(3) 0.0259(3) 0.087(2) Uani 1 1 d . A . H12C H 0.8741 -0.1285 0.0087 0.105 Uiso 1 1 calc R . . H12D H 0.8304 -0.0913 -0.0125 0.105 Uiso 1 1 calc R . . C13B C 0.8244(3) -0.1168(2) 0.0921(4) 0.0818(19) Uani 1 1 d . . . H13C H 0.7998 -0.1422 0.0782 0.098 Uiso 1 1 calc R A . H13D H 0.8472 -0.1318 0.1273 0.098 Uiso 1 1 calc R . . C14B C 0.7985(2) -0.07357(19) 0.1251(3) 0.0593(14) Uani 1 1 d . A . H14C H 0.7829 -0.0843 0.1702 0.071 Uiso 1 1 calc R . . H14D H 0.7718 -0.0625 0.0927 0.071 Uiso 1 1 calc R . . C15B C 0.8134(2) 0.1327(3) 0.1024(4) 0.094(2) Uani 1 1 d . . . H15D H 0.8319 0.1306 0.1471 0.141 Uiso 1 1 calc R A . H15E H 0.8219 0.1635 0.0777 0.141 Uiso 1 1 calc R . . H15F H 0.8219 0.1044 0.0720 0.141 Uiso 1 1 calc R . . Mn1C Mn 0.89443(2) 0.04489(2) 0.28899(3) 0.0370(3) Uani 1 1 d . A . O1C O 0.90876(12) 0.09903(11) 0.23071(16) 0.0448(8) Uani 1 1 d . . . O2C O 1.00571(11) -0.01460(11) 0.16203(16) 0.0421(8) Uani 1 1 d . . . O3C O 0.89029(11) -0.01659(11) 0.34178(15) 0.0413(8) Uani 1 1 d . . . O4C O 0.95030(13) 0.07444(12) 0.36731(17) 0.0538(9) Uani 1 1 d . . . N1C N 0.94341(13) 0.00583(13) 0.23856(18) 0.0364(9) Uani 1 1 d . . . N2C N 0.95254(14) -0.04162(13) 0.26785(19) 0.0385(9) Uani 1 1 d . A . C1C C 0.93683(17) 0.10218(17) 0.1727(2) 0.0438(12) Uani 1 1 d . A . C2C C 0.96737(16) 0.06353(17) 0.1475(2) 0.0420(12) Uani 1 1 d . . . C3C C 0.9950(2) 0.0714(2) 0.0856(3) 0.0591(15) Uani 1 1 d . A . H3C H 1.0151 0.0453 0.0680 0.071 Uiso 1 1 calc R . . C4C C 0.9940(2) 0.1151(2) 0.0496(4) 0.087(2) Uani 1 1 d . . . H4C H 1.0132 0.1195 0.0077 0.104 Uiso 1 1 calc R A . C5C C 0.9646(3) 0.1530(2) 0.0753(3) 0.084(2) Uani 1 1 d . A . H5C H 0.9639 0.1837 0.0508 0.101 Uiso 1 1 calc R . . C6C C 0.9364(2) 0.1468(2) 0.1358(3) 0.0651(16) Uani 1 1 d . . . H6C H 0.9164 0.1733 0.1525 0.078 Uiso 1 1 calc R A . C7C C 0.97232(16) 0.01599(16) 0.1841(2) 0.0368(11) Uani 1 1 d . A . C8C C 0.92241(17) -0.04958(16) 0.3202(2) 0.0398(11) Uani 1 1 d . A . C9C C 0.92475(17) -0.09949(18) 0.3564(3) 0.0475(12) Uani 1 1 d . . . H9C H 0.9443 -0.1222 0.3251 0.057 Uiso 1 1 calc R A . C10C C 0.95149(19) -0.09616(18) 0.4286(3) 0.0522(13) Uani 1 1 d . A . H10E H 0.9855 -0.0836 0.4211 0.063 Uiso 1 1 calc R . . H10F H 0.9338 -0.0726 0.4598 0.063 Uiso 1 1 calc R . . C11C C 0.9538(2) -0.1465(2) 0.4647(3) 0.0745(17) Uani 1 1 d . . . H11E H 0.9745 -0.1691 0.4358 0.089 Uiso 1 1 calc R A . H11F H 0.9694 -0.1430 0.5121 0.089 Uiso 1 1 calc R . . C12C C 0.9035(3) -0.1680(2) 0.4730(3) 0.0815(19) Uani 1 1 d . A . H12E H 0.8842 -0.1473 0.5065 0.098 Uiso 1 1 calc R . . H12F H 0.9063 -0.2015 0.4939 0.098 Uiso 1 1 calc R . . C13C C 0.8760(2) -0.1713(2) 0.4029(3) 0.0723(17) Uani 1 1 d . . . H13E H 0.8418 -0.1830 0.4117 0.087 Uiso 1 1 calc R A . H13F H 0.8926 -0.1957 0.3716 0.087 Uiso 1 1 calc R . . C14C C 0.8743(2) -0.1214(2) 0.3655(3) 0.0687(16) Uani 1 1 d . A . H14E H 0.8587 -0.1255 0.3180 0.082 Uiso 1 1 calc R . . H14F H 0.8535 -0.0984 0.3935 0.082 Uiso 1 1 calc R . . C15C C 0.9781(2) 0.0455(2) 0.4149(3) 0.0756(17) Uani 1 1 d . A . H15G H 0.9563 0.0319 0.4516 0.113 Uiso 1 1 calc R . . H15H H 1.0036 0.0661 0.4374 0.113 Uiso 1 1 calc R . . H15I H 0.9940 0.0184 0.3888 0.113 Uiso 1 1 calc R . . O1M O 0.7500 -0.2500 0.2500 0.090(5) Uiso 0.50 4 d SPD . . C1M C 0.735(2) -0.3004(10) 0.237(3) 0.093(17) Uiso 0.13 1 d PD . . O1W O 0.7500 -0.2500 0.1292(15) 0.206(10) Uiso 0.50 2 d SP B 1 O21M O 0.7132(15) -0.258(2) -0.027(2) 0.125(15) Uiso 0.13 1 d PD . 2 O22M O 0.749(2) -0.2305(15) -0.0426(19) 0.127(16) Uiso 0.13 1 d PD . 2 C2M C 0.7500 -0.2500 0.0297(17) 0.165(12) Uiso 0.50 2 d SPD . 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 Mn1A 0.0379(4) 0.0459(5) 0.0418(5) 0.0119(3) -0.0044(3) -0.0039(3) O1A 0.0367(18) 0.054(2) 0.047(2) 0.0175(16) -0.0042(15) -0.0025(15) O2A 0.043(2) 0.0515(19) 0.0358(17) 0.0093(15) -0.0012(15) 0.0020(15) O3A 0.0378(19) 0.057(2) 0.0436(18) 0.0172(16) -0.0033(15) -0.0068(15) O4A 0.074(3) 0.071(3) 0.052(2) -0.009(2) 0.0019(19) -0.020(2) N1A 0.038(2) 0.043(2) 0.039(2) 0.0106(19) -0.0048(18) -0.0005(18) N2A 0.035(2) 0.045(2) 0.036(2) 0.0047(19) -0.0067(17) 0.0023(17) C1A 0.049(3) 0.043(3) 0.038(3) 0.008(2) -0.014(2) -0.001(2) C2A 0.040(3) 0.047(3) 0.039(3) 0.013(2) -0.001(2) 0.000(2) C3A 0.039(3) 0.083(4) 0.051(3) 0.021(3) -0.007(2) 0.005(3) C4A 0.058(4) 0.098(4) 0.043(3) 0.033(3) 0.001(3) 0.005(3) C5A 0.047(3) 0.073(4) 0.061(4) 0.015(3) -0.016(3) 0.005(3) C6A 0.045(3) 0.056(3) 0.053(3) 0.014(3) -0.004(2) -0.003(2) C7A 0.034(3) 0.045(3) 0.038(3) 0.000(2) -0.001(2) -0.003(2) C8A 0.042(3) 0.041(3) 0.036(3) 0.002(2) -0.007(2) -0.005(2) C9A 0.039(3) 0.044(3) 0.033(2) 0.004(2) -0.007(2) -0.002(2) C10A 0.067(4) 0.045(3) 0.103(5) 0.013(3) -0.032(3) 0.001(3) C11A 0.067(4) 0.044(3) 0.143(7) 0.013(4) -0.022(4) 0.005(3) C12A 0.044(3) 0.102(5) 0.083(4) 0.042(4) -0.014(3) -0.001(3) C13A 0.046(3) 0.098(5) 0.033(3) 0.000(3) -0.008(2) 0.005(3) C14A 0.051(3) 0.067(3) 0.036(3) 0.003(2) -0.003(2) 0.004(3) C15A 0.111(7) 0.128(7) 0.065(6) 0.014(5) -0.004(5) -0.039(6) Mn1B 0.0374(4) 0.0435(4) 0.0367(4) 0.0036(3) -0.0023(3) 0.0005(3) O1B 0.0467(19) 0.0415(18) 0.053(2) 0.0001(16) -0.0056(16) 0.0049(15) O2B 0.0400(19) 0.0468(18) 0.0289(16) 0.0011(13) -0.0042(14) 0.0014(14) O3B 0.0392(19) 0.0536(19) 0.0331(16) -0.0011(14) -0.0073(14) 0.0019(15) O4B 0.052(2) 0.063(2) 0.053(2) 0.0154(17) -0.0007(17) -0.0108(17) N1B 0.044(2) 0.034(2) 0.034(2) 0.0036(17) 0.0032(18) 0.0037(17) N2B 0.037(2) 0.042(2) 0.032(2) -0.0008(18) 0.0011(17) 0.0038(18) C1B 0.045(3) 0.039(3) 0.048(3) 0.006(2) 0.004(3) -0.001(2) C2B 0.051(3) 0.030(2) 0.041(3) 0.006(2) 0.006(2) -0.004(2) C3B 0.061(3) 0.038(3) 0.042(3) 0.002(2) 0.001(2) 0.008(2) C4B 0.086(4) 0.057(3) 0.044(3) -0.010(3) 0.004(3) 0.004(3) C5B 0.064(4) 0.055(3) 0.065(4) -0.004(3) 0.007(3) 0.018(3) C6B 0.049(3) 0.051(3) 0.060(3) -0.004(3) 0.004(3) 0.011(2) C7B 0.047(3) 0.035(3) 0.028(2) 0.005(2) 0.006(2) -0.001(2) C8B 0.040(3) 0.048(3) 0.033(3) -0.003(2) -0.001(2) -0.001(2) C9B 0.045(3) 0.064(3) 0.038(3) -0.008(2) -0.009(2) 0.011(2) C10B 0.043(3) 0.094(4) 0.044(3) -0.021(3) 0.003(2) 0.001(3) C11B 0.060(4) 0.137(6) 0.056(4) -0.042(4) 0.006(3) 0.021(4) C12B 0.077(4) 0.118(6) 0.067(4) -0.043(4) -0.009(4) 0.030(4) C13B 0.087(4) 0.075(4) 0.083(4) -0.021(4) -0.011(4) 0.015(3) C14B 0.070(4) 0.056(3) 0.052(3) -0.012(3) -0.004(3) 0.010(3) C15B 0.061(4) 0.120(6) 0.101(5) 0.060(5) -0.004(4) -0.017(4) Mn1C 0.0387(4) 0.0388(4) 0.0334(4) 0.0028(3) -0.0016(3) -0.0011(3) O1C 0.052(2) 0.0385(18) 0.0440(19) 0.0045(14) 0.0062(16) 0.0003(15) O2C 0.0443(18) 0.0433(18) 0.0387(18) -0.0019(14) -0.0081(15) 0.0078(16) O3C 0.0449(18) 0.0452(19) 0.0338(17) 0.0033(14) -0.0053(14) -0.0034(16) O4C 0.062(2) 0.053(2) 0.046(2) -0.0019(16) -0.0136(17) -0.0085(17) N1C 0.041(2) 0.035(2) 0.034(2) 0.0057(17) -0.0050(18) -0.0047(17) N2C 0.047(2) 0.034(2) 0.035(2) 0.0027(17) -0.0121(19) -0.0028(17) C1C 0.046(3) 0.051(3) 0.034(3) 0.003(2) 0.003(2) -0.002(2) C2C 0.035(3) 0.051(3) 0.040(3) 0.007(2) -0.002(2) 0.007(2) C3C 0.061(3) 0.064(4) 0.052(3) 0.017(3) 0.015(3) 0.027(3) C4C 0.091(5) 0.090(5) 0.080(4) 0.042(4) 0.044(4) 0.040(4) C5C 0.103(5) 0.074(4) 0.076(4) 0.042(3) 0.037(4) 0.031(4) C6C 0.076(4) 0.055(3) 0.064(4) 0.023(3) 0.020(3) 0.016(3) C7C 0.038(3) 0.041(3) 0.031(3) -0.003(2) -0.013(2) -0.003(2) C8C 0.043(3) 0.039(3) 0.038(3) 0.003(2) -0.011(2) -0.006(2) C9C 0.048(3) 0.047(3) 0.048(3) 0.007(2) -0.013(2) -0.003(2) C10C 0.060(3) 0.049(3) 0.048(3) 0.003(2) -0.005(2) 0.001(2) C11C 0.098(5) 0.056(3) 0.069(4) 0.021(3) -0.016(3) -0.005(3) C12C 0.111(5) 0.067(4) 0.067(4) 0.017(3) 0.017(4) 0.001(4) C13C 0.086(4) 0.049(3) 0.082(4) 0.012(3) 0.004(3) -0.013(3) C14C 0.069(4) 0.056(3) 0.080(4) 0.004(3) -0.006(3) -0.014(3) C15C 0.070(4) 0.080(4) 0.077(4) -0.010(3) -0.037(3) -0.002(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 Mn1A O1A 1.871(3) . ? Mn1A O3A 1.933(3) . ? Mn1A N1A 1.937(4) . ? Mn1A O2C 1.967(3) 8_646 ? Mn1A O4A 2.227(4) . ? Mn1A N2C 2.253(4) 8_646 ? O1A C1A 1.337(5) . ? O2A C7A 1.291(5) . ? O2A Mn1B 1.975(3) . ? O3A C8A 1.308(5) . ? O4A C25A 1.12(3) . ? O4A C15A 1.415(8) . ? N1A C7A 1.323(6) . ? N1A N2A 1.422(5) . ? N2A C8A 1.297(6) . ? N2A Mn1B 2.252(4) . ? C1A C2A 1.406(7) . ? C1A C6A 1.408(7) . ? C2A C3A 1.405(7) . ? C2A C7A 1.469(6) . ? C3A C4A 1.368(7) . ? C4A C5A 1.392(7) . ? C5A C6A 1.385(7) . ? C8A C9A 1.492(6) . ? C9A C10A 1.532(7) . ? C9A C14A 1.538(6) . ? C10A C11A 1.544(8) . ? C11A C12A 1.476(9) . ? C12A C13A 1.474(8) . ? C13A C14A 1.525(7) . ? Mn1B O1B 1.858(3) . ? Mn1B O3B 1.935(3) . ? Mn1B N1B 1.943(4) . ? Mn1B O4B 2.262(3) . ? O1B C1B 1.339(6) . ? O2B C7B 1.273(5) . ? O2B Mn1C 1.972(3) . ? O3B C8B 1.302(5) . ? O4B C15B 1.413(7) . ? N1B C7B 1.339(6) . ? N1B N2B 1.427(5) . ? N2B C8B 1.296(6) . ? N2B Mn1C 2.271(4) . ? C1B C6B 1.399(7) . ? C1B C2B 1.414(7) . ? C2B C3B 1.411(7) . ? C2B C7B 1.460(6) . ? C3B C4B 1.395(7) . ? C4B C5B 1.398(8) . ? C5B C6B 1.378(7) . ? C8B C9B 1.491(7) . ? C9B C14B 1.537(7) . ? C9B C10B 1.539(7) . ? C10B C11B 1.510(8) . ? C11B C12B 1.508(9) . ? C12B C13B 1.542(9) . ? C13B C14B 1.498(8) . ? Mn1C O1C 1.868(3) . ? Mn1C O3C 1.939(3) . ? Mn1C N1C 1.940(4) . ? Mn1C O4C 2.254(3) . ? O1C C1C 1.330(5) . ? O2C C7C 1.293(5) . ? O2C Mn1A 1.967(3) 7_666 ? O3C C8C 1.309(5) . ? O4C C15C 1.405(6) . ? N1C C7C 1.315(6) . ? N1C N2C 1.417(5) . ? N2C C8C 1.295(6) . ? N2C Mn1A 2.253(4) 7_666 ? C1C C6C 1.392(7) . ? C1C C2C 1.414(7) . ? C2C C3C 1.398(7) . ? C2C C7C 1.464(6) . ? C3C C4C 1.362(8) . ? C4C C5C 1.382(8) . ? C5C C6C 1.379(8) . ? C8C C9C 1.512(7) . ? C9C C14C 1.498(7) . ? C9C C10C 1.537(7) . ? C10C C11C 1.522(7) . ? C11C C12C 1.488(9) . ? C12C C13C 1.514(9) . ? C13C C14C 1.522(8) . ? O1M C1M 1.44(2) 8_646 ? O1M C1M 1.44(2) . ? O1M C1M 1.44(2) 7_666 ? O1M C1M 1.44(2) 2_645 ? O21M O22M 1.12(6) 2_645 ? O21M O22M 1.24(6) . ? O21M C2M 1.469(19) . ? O22M O22M 1.05(8) 2_645 ? O22M O21M 1.12(6) 2_645 ? O22M C2M 1.454(19) . ? C2M O22M 1.454(19) 2_645 ? C2M O21M 1.469(19) 2_645 ? 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 O1A Mn1A O3A 170.13(13) . . ? O1A Mn1A N1A 89.99(14) . . ? O3A Mn1A N1A 80.26(14) . . ? O1A Mn1A O2C 93.30(13) . 8_646 ? O3A Mn1A O2C 96.43(12) . 8_646 ? N1A Mn1A O2C 176.62(14) . 8_646 ? O1A Mn1A O4A 89.30(15) . . ? O3A Mn1A O4A 89.79(15) . . ? N1A Mn1A O4A 93.57(15) . . ? O2C Mn1A O4A 85.69(13) 8_646 . ? O1A Mn1A N2C 91.66(13) . 8_646 ? O3A Mn1A N2C 92.56(13) . 8_646 ? N1A Mn1A N2C 106.43(15) . 8_646 ? O2C Mn1A N2C 74.28(13) 8_646 8_646 ? O4A Mn1A N2C 159.97(13) . 8_646 ? C1A O1A Mn1A 130.1(3) . . ? C7A O2A Mn1B 117.8(3) . . ? C8A O3A Mn1A 112.9(3) . . ? C25A O4A C15A 115.4(18) . . ? C25A O4A Mn1A 117.3(17) . . ? C15A O4A Mn1A 126.9(5) . . ? C7A N1A N2A 113.5(4) . . ? C7A N1A Mn1A 131.9(3) . . ? N2A N1A Mn1A 114.4(3) . . ? C8A N2A N1A 110.1(4) . . ? C8A N2A Mn1B 137.9(3) . . ? N1A N2A Mn1B 107.0(2) . . ? O1A C1A C2A 124.8(4) . . ? O1A C1A C6A 117.2(4) . . ? C2A C1A C6A 118.0(4) . . ? C3A C2A C1A 119.9(4) . . ? C3A C2A C7A 117.9(4) . . ? C1A C2A C7A 122.2(4) . . ? C4A C3A C2A 121.2(5) . . ? C3A C4A C5A 119.5(5) . . ? C6A C5A C4A 120.4(5) . . ? C5A C6A C1A 121.0(5) . . ? O2A C7A N1A 121.2(4) . . ? O2A C7A C2A 118.8(4) . . ? N1A C7A C2A 120.0(4) . . ? N2A C8A O3A 122.3(4) . . ? N2A C8A C9A 118.9(4) . . ? O3A C8A C9A 118.7(4) . . ? C8A C9A C10A 110.1(4) . . ? C8A C9A C14A 110.5(4) . . ? C10A C9A C14A 108.6(4) . . ? C9A C10A C11A 111.5(4) . . ? C12A C11A C10A 112.4(5) . . ? C13A C12A C11A 112.8(5) . . ? C12A C13A C14A 111.1(4) . . ? C13A C14A C9A 110.6(4) . . ? O1B Mn1B O3B 170.38(13) . . ? O1B Mn1B N1B 90.60(14) . . ? O3B Mn1B N1B 79.89(14) . . ? O1B Mn1B O2A 91.94(13) . . ? O3B Mn1B O2A 97.58(13) . . ? N1B Mn1B O2A 177.45(14) . . ? O1B Mn1B N2A 89.12(14) . . ? O3B Mn1B N2A 94.78(13) . . ? N1B Mn1B N2A 105.86(14) . . ? O2A Mn1B N2A 74.50(12) . . ? O1B Mn1B O4B 91.71(14) . . ? O3B Mn1B O4B 88.21(13) . . ? N1B Mn1B O4B 97.62(13) . . ? O2A Mn1B O4B 82.00(12) . . ? N2A Mn1B O4B 156.50(12) . . ? C1B O1B Mn1B 129.3(3) . . ? C7B O2B Mn1C 119.6(3) . . ? C8B O3B Mn1B 113.4(3) . . ? C15B O4B Mn1B 121.1(3) . . ? C7B N1B N2B 113.5(3) . . ? C7B N1B Mn1B 132.0(3) . . ? N2B N1B Mn1B 114.5(3) . . ? C8B N2B N1B 109.8(3) . . ? C8B N2B Mn1C 140.8(3) . . ? N1B N2B Mn1C 107.2(2) . . ? O1B C1B C6B 116.8(4) . . ? O1B C1B C2B 124.2(4) . . ? C6B C1B C2B 119.0(5) . . ? C3B C2B C1B 119.3(4) . . ? C3B C2B C7B 116.7(4) . . ? C1B C2B C7B 124.0(4) . . ? C4B C3B C2B 120.6(5) . . ? C3B C4B C5B 119.4(5) . . ? C6B C5B C4B 120.6(5) . . ? C5B C6B C1B 121.1(5) . . ? O2B C7B N1B 121.3(4) . . ? O2B C7B C2B 120.3(4) . . ? N1B C7B C2B 118.3(4) . . ? N2B C8B O3B 122.4(4) . . ? N2B C8B C9B 118.8(4) . . ? O3B C8B C9B 118.8(4) . . ? C8B C9B C14B 110.5(4) . . ? C8B C9B C10B 112.1(4) . . ? C14B C9B C10B 109.7(4) . . ? C11B C10B C9B 109.8(5) . . ? C12B C11B C10B 111.9(5) . . ? C11B C12B C13B 112.6(5) . . ? C14B C13B C12B 110.5(5) . . ? C13B C14B C9B 113.6(5) . . ? O1C Mn1C O3C 169.52(14) . . ? O1C Mn1C N1C 89.97(14) . . ? O3C Mn1C N1C 79.74(14) . . ? O1C Mn1C O2B 92.72(13) . . ? O3C Mn1C O2B 97.56(13) . . ? N1C Mn1C O2B 177.27(13) . . ? O1C Mn1C O4C 87.99(13) . . ? O3C Mn1C O4C 90.54(12) . . ? N1C Mn1C O4C 93.07(14) . . ? O2B Mn1C O4C 86.57(12) . . ? O1C Mn1C N2B 90.44(13) . . ? O3C Mn1C N2B 94.28(12) . . ? N1C Mn1C N2B 105.92(14) . . ? O2B Mn1C N2B 74.54(12) . . ? O4C Mn1C N2B 160.95(13) . . ? C1C O1C Mn1C 130.4(3) . . ? C7C O2C Mn1A 118.3(3) . 7_666 ? C8C O3C Mn1C 112.8(3) . . ? C15C O4C Mn1C 125.2(3) . . ? C7C N1C N2C 112.7(4) . . ? C7C N1C Mn1C 132.1(3) . . ? N2C N1C Mn1C 115.0(3) . . ? C8C N2C N1C 109.6(4) . . ? C8C N2C Mn1A 139.9(3) . 7_666 ? N1C N2C Mn1A 108.2(3) . 7_666 ? O1C C1C C6C 117.2(4) . . ? O1C C1C C2C 124.1(4) . . ? C6C C1C C2C 118.7(4) . . ? C3C C2C C1C 118.6(4) . . ? C3C C2C C7C 118.3(4) . . ? C1C C2C C7C 123.1(4) . . ? C4C C3C C2C 122.2(5) . . ? C3C C4C C5C 118.8(5) . . ? C6C C5C C4C 121.1(5) . . ? C5C C6C C1C 120.6(5) . . ? O2C C7C N1C 122.1(4) . . ? O2C C7C C2C 118.4(4) . . ? N1C C7C C2C 119.6(4) . . ? N2C C8C O3C 122.6(4) . . ? N2C C8C C9C 117.6(4) . . ? O3C C8C C9C 119.8(4) . . ? C14C C9C C8C 111.5(4) . . ? C14C C9C C10C 110.6(4) . . ? C8C C9C C10C 111.3(4) . . ? C11C C10C C9C 111.0(4) . . ? C12C C11C C10C 111.0(5) . . ? C11C C12C C13C 112.4(5) . . ? C12C C13C C14C 111.3(5) . . ? C9C C14C C13C 112.0(5) . . ? C1M O1M C1M 91.5(8) 8_646 . ? C1M O1M C1M 161(5) 8_646 7_666 ? C1M O1M C1M 91.5(8) . 7_666 ? C1M O1M C1M 91.5(8) 8_646 2_645 ? C1M O1M C1M 161(5) . 2_645 ? C1M O1M C1M 91.5(8) 7_666 2_645 ? O22M O21M O22M 53(5) 2_645 . ? O22M O21M C2M 66.9(19) 2_645 . ? O22M O21M C2M 64.2(18) . . ? O22M O22M O21M 70(5) 2_645 2_645 ? O22M O22M O21M 57(5) 2_645 . ? O21M O22M O21M 119(3) 2_645 . ? O22M O22M C2M 68.7(17) 2_645 . ? O21M O22M C2M 68.2(19) 2_645 . ? O21M O22M C2M 65.4(18) . . ? O22M C2M O22M 43(3) 2_645 . ? O22M C2M O21M 45(3) 2_645 . ? O22M C2M O21M 50(3) . . ? O22M C2M O21M 50(3) 2_645 2_645 ? O22M C2M O21M 45(3) . 2_645 ? O21M C2M O21M 88(4) . 2_645 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.693 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.075 #===END data_l5_71te _database_code_depnum_ccdc_archive 'CCDC 298634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C186 H240 Mn12 N24 O48' _chemical_formula_weight 4239.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 27.189(3) _cell_length_b 27.189(3) _cell_length_c 18.904(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13974(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7306 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.34 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Brown' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_T_max 0.8451 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67612 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.39 _reflns_number_total 16082 _reflns_number_gt 12169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Diamond 3.1a' _computing_publication_material WinGX _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^)+(0.0622P)^2^+57.6840P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16082 _refine_ls_number_parameters 628 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Mn1A Mn 0.56844(2) 0.02626(2) 0.27449(3) 0.02313(14) Uani 1 1 d . . . O1A O 0.52710(11) 0.06105(11) 0.21341(16) 0.0295(6) Uani 1 1 d . . . O2A O 0.67122(10) 0.08352(12) 0.13354(15) 0.0291(7) Uani 1 1 d . . . O3A O 0.62042(10) -0.00424(12) 0.32918(14) 0.0268(6) Uani 1 1 d . . . O4A O 0.57405(16) 0.09318(15) 0.3425(2) 0.0472(10) Uani 1 1 d . . . H4OA H 0.569(3) 0.118(3) 0.324(4) 0.071 Uiso 1 1 d . . . N1A N 0.62490(11) 0.04371(13) 0.21664(17) 0.0215(7) Uani 1 1 d . . . N2A N 0.67082(12) 0.02801(13) 0.24443(17) 0.0229(7) Uani 1 1 d . . . C1A C 0.53693(16) 0.08221(15) 0.1502(2) 0.0257(8) Uani 1 1 d . . . C2A C 0.58453(16) 0.08763(17) 0.1218(2) 0.0282(9) Uani 1 1 d . . . C3A C 0.58959(19) 0.1098(2) 0.0548(2) 0.0409(12) Uani 1 1 d . . . H3A H 0.6215 0.1125 0.0346 0.049 Uiso 1 1 calc R . . C4A C 0.54971(19) 0.1278(2) 0.0174(3) 0.0473(14) Uani 1 1 d . . . H4A H 0.5542 0.1429 -0.0274 0.057 Uiso 1 1 calc R . . C5A C 0.50291(18) 0.12337(19) 0.0466(3) 0.0389(11) Uani 1 1 d . . . H5A H 0.4752 0.1355 0.0215 0.047 Uiso 1 1 calc R . . C6A C 0.49655(18) 0.10150(18) 0.1117(3) 0.0362(11) Uani 1 1 d . . . H6A H 0.4644 0.0993 0.1312 0.043 Uiso 1 1 calc R . . C7A C 0.62892(15) 0.07085(15) 0.1583(2) 0.0237(8) Uani 1 1 d . . . C8A C 0.66402(15) 0.00244(16) 0.3022(2) 0.0252(8) Uani 1 1 d . . . C9A C 0.70755(15) -0.01963(15) 0.33882(19) 0.0227(8) Uani 1 1 d . . . H9A H 0.7370 -0.0165 0.3074 0.027 Uiso 1 1 calc R . . C10A C 0.69751(18) -0.07478(17) 0.3522(3) 0.0391(11) Uani 1 1 d . . . H10A H 0.6670 -0.0784 0.3803 0.047 Uiso 1 1 calc R . . H10B H 0.6925 -0.0917 0.3063 0.047 Uiso 1 1 calc R . . C11A C 0.7406(2) -0.0993(2) 0.3920(4) 0.0525(15) Uani 1 1 d . . . H11A H 0.7318 -0.1337 0.4034 0.063 Uiso 1 1 calc R . . H11B H 0.7700 -0.0998 0.3612 0.063 Uiso 1 1 calc R . . C12A C 0.7521(2) -0.0717(2) 0.4595(3) 0.0535(16) Uani 1 1 d . . . H12A H 0.7241 -0.0752 0.4927 0.064 Uiso 1 1 calc R . . H12B H 0.7814 -0.0866 0.4821 0.064 Uiso 1 1 calc R . . C13A C 0.76182(18) -0.0176(2) 0.4468(2) 0.0434(13) Uani 1 1 d . . . H13A H 0.7918 -0.0137 0.4176 0.052 Uiso 1 1 calc R . . H13B H 0.7675 -0.0009 0.4926 0.052 Uiso 1 1 calc R . . C14A C 0.71850(16) 0.00602(19) 0.4093(2) 0.0318(10) Uani 1 1 d . . . H14A H 0.7258 0.0412 0.4005 0.038 Uiso 1 1 calc R . . H14B H 0.6891 0.0042 0.4401 0.038 Uiso 1 1 calc R . . C15A C 0.5820(4) 0.0967(3) 0.4156(4) 0.102(3) Uani 1 1 d . . . H15A H 0.5613 0.0726 0.4402 0.153 Uiso 1 1 calc R . . H15B H 0.5735 0.1299 0.4318 0.153 Uiso 1 1 calc R . . H15C H 0.6167 0.0901 0.4260 0.153 Uiso 1 1 calc R . . Mn1B Mn 0.72924(2) 0.07665(2) 0.19651(3) 0.02412(15) Uani 1 1 d . . . O1B O 0.70786(11) 0.12837(11) 0.25370(17) 0.0316(7) Uani 1 1 d . . . O2B O 0.84439(10) 0.08065(11) 0.34275(14) 0.0237(6) Uani 1 1 d . . . O3B O 0.76168(11) 0.02419(12) 0.14531(15) 0.0296(7) Uani 1 1 d . . . O4B O 0.76219(13) 0.13066(14) 0.11757(18) 0.0425(8) Uani 1 1 d . . . N1B N 0.78794(11) 0.06864(13) 0.25487(17) 0.0224(7) Uani 1 1 d . . . N2B N 0.82125(12) 0.03214(13) 0.23039(17) 0.0233(7) Uani 1 1 d . . . C1B C 0.72463(16) 0.14195(16) 0.3184(2) 0.0280(9) Uani 1 1 d . . . C2B C 0.76968(15) 0.12671(15) 0.3482(2) 0.0239(8) Uani 1 1 d . . . C3B C 0.78448(18) 0.14657(16) 0.4137(2) 0.0312(9) Uani 1 1 d . . . H3B H 0.8152 0.1371 0.4334 0.037 Uiso 1 1 calc R . . C4B C 0.7550(2) 0.17963(19) 0.4498(3) 0.0434(12) Uani 1 1 d . . . H4B H 0.7657 0.1929 0.4937 0.052 Uiso 1 1 calc R . . C5B C 0.7093(2) 0.1936(2) 0.4218(3) 0.0461(13) Uani 1 1 d . . . H5B H 0.6888 0.2157 0.4470 0.055 Uiso 1 1 calc R . . C6B C 0.69443(18) 0.17504(18) 0.3573(3) 0.0380(11) Uani 1 1 d . . . H6B H 0.6634 0.1845 0.3386 0.046 Uiso 1 1 calc R . . C7B C 0.80218(15) 0.09129(15) 0.3141(2) 0.0239(8) Uani 1 1 d . . . C8B C 0.80374(14) 0.01076(16) 0.1743(2) 0.0236(8) Uani 1 1 d . . . C9B C 0.83142(15) -0.03052(17) 0.1408(2) 0.0279(9) Uani 1 1 d . . . H9B H 0.8566 -0.0422 0.1755 0.033 Uiso 1 1 calc R . . C10B C 0.85848(18) -0.0142(2) 0.0734(3) 0.0424(12) Uani 1 1 d . . . H10C H 0.8814 0.0129 0.0848 0.051 Uiso 1 1 calc R . . H10D H 0.8344 -0.0020 0.0383 0.051 Uiso 1 1 calc R . . C11B C 0.8873(2) -0.0577(3) 0.0420(3) 0.0633(18) Uani 1 1 d . . . H11C H 0.9039 -0.0471 -0.0021 0.076 Uiso 1 1 calc R . . H11D H 0.9129 -0.0683 0.0759 0.076 Uiso 1 1 calc R . . C12B C 0.8537(3) -0.1005(3) 0.0259(3) 0.068(2) Uani 1 1 d . . . H12C H 0.8736 -0.1283 0.0081 0.082 Uiso 1 1 calc R . . H12D H 0.8304 -0.0908 -0.0119 0.082 Uiso 1 1 calc R . . C13B C 0.8243(2) -0.1174(2) 0.0910(3) 0.0566(16) Uani 1 1 d . . . H13C H 0.8005 -0.1432 0.0768 0.068 Uiso 1 1 calc R . . H13D H 0.8470 -0.1318 0.1264 0.068 Uiso 1 1 calc R . . C14B C 0.79700(18) -0.07423(18) 0.1236(3) 0.0381(11) Uani 1 1 d . . . H14C H 0.7806 -0.0852 0.1676 0.046 Uiso 1 1 calc R . . H14D H 0.7711 -0.0631 0.0904 0.046 Uiso 1 1 calc R . . C15B C 0.8124(2) 0.1304(4) 0.1006(4) 0.095(3) Uani 1 1 d . . . H15D H 0.8318 0.1278 0.1441 0.142 Uiso 1 1 calc R . . H15E H 0.8209 0.1610 0.0761 0.142 Uiso 1 1 calc R . . H15F H 0.8196 0.1023 0.0699 0.142 Uiso 1 1 calc R . . Mn1C Mn 0.89400(2) 0.04381(2) 0.28806(3) 0.02229(14) Uani 1 1 d . . . O1C O 0.90730(11) 0.09799(11) 0.23015(16) 0.0306(7) Uani 1 1 d . . . O2C O 1.00670(11) -0.01394(10) 0.16288(15) 0.0257(6) Uani 1 1 d . . . O3C O 0.89043(10) -0.01720(10) 0.34129(14) 0.0240(6) Uani 1 1 d . . . O4C O 0.94839(15) 0.07379(14) 0.3659(2) 0.0438(9) Uani 1 1 d . . . H4OC H 0.968(3) 0.093(3) 0.358(4) 0.066 Uiso 1 1 d . . . N1C N 0.94365(12) 0.00521(12) 0.23824(17) 0.0228(7) Uani 1 1 d . . . N2C N 0.95300(13) -0.04194(13) 0.26715(17) 0.0253(7) Uani 1 1 d . . . C1C C 0.93603(17) 0.10069(18) 0.1727(2) 0.0337(10) Uani 1 1 d . . . C2C C 0.96659(15) 0.06303(18) 0.1474(2) 0.0306(10) Uani 1 1 d . . . C3C C 0.9947(2) 0.0710(2) 0.0853(3) 0.0500(15) Uani 1 1 d . . . H3C H 1.0151 0.0454 0.0678 0.060 Uiso 1 1 calc R . . C4C C 0.9928(3) 0.1153(3) 0.0499(4) 0.076(2) Uani 1 1 d . . . H4C H 1.0128 0.1207 0.0094 0.091 Uiso 1 1 calc R . . C5C C 0.9613(3) 0.1520(3) 0.0744(4) 0.074(2) Uani 1 1 d . . . H5C H 0.9587 0.1819 0.0486 0.088 Uiso 1 1 calc R . . C6C C 0.9339(2) 0.1460(2) 0.1347(3) 0.0548(16) Uani 1 1 d . . . H6C H 0.9135 0.1720 0.1511 0.066 Uiso 1 1 calc R . . C7C C 0.97268(15) 0.01578(16) 0.1837(2) 0.0248(8) Uani 1 1 d . . . C8C C 0.92220(14) -0.04940(15) 0.3202(2) 0.0219(8) Uani 1 1 d . . . C9C C 0.92499(16) -0.09914(15) 0.3570(2) 0.0257(8) Uani 1 1 d . . . H9C H 0.9436 -0.1223 0.3259 0.031 Uiso 1 1 calc R . . C10C C 0.95210(18) -0.09535(18) 0.4283(2) 0.0336(10) Uani 1 1 d . . . H10E H 0.9857 -0.0824 0.4205 0.040 Uiso 1 1 calc R . . H10F H 0.9344 -0.0722 0.4597 0.040 Uiso 1 1 calc R . . C11C C 0.9551(2) -0.1460(2) 0.4638(3) 0.0507(14) Uani 1 1 d . . . H11E H 0.9717 -0.1428 0.5102 0.061 Uiso 1 1 calc R . . H11F H 0.9749 -0.1684 0.4339 0.061 Uiso 1 1 calc R . . C12C C 0.9033(2) -0.1677(2) 0.4743(3) 0.0554(16) Uani 1 1 d . . . H12E H 0.9061 -0.2013 0.4940 0.066 Uiso 1 1 calc R . . H12F H 0.8849 -0.1474 0.5088 0.066 Uiso 1 1 calc R . . C13C C 0.8754(2) -0.1696(2) 0.4063(3) 0.0538(15) Uani 1 1 d . . . H13E H 0.8416 -0.1812 0.4159 0.065 Uiso 1 1 calc R . . H13F H 0.8913 -0.1938 0.3745 0.065 Uiso 1 1 calc R . . C14C C 0.87279(18) -0.11996(18) 0.3686(3) 0.0383(11) Uani 1 1 d . . . H14E H 0.8533 -0.0966 0.3973 0.046 Uiso 1 1 calc R . . H14F H 0.8562 -0.1240 0.3223 0.046 Uiso 1 1 calc R . . C15C C 0.9795(2) 0.0464(3) 0.4113(3) 0.0619(17) Uani 1 1 d . . . H15G H 0.9598 0.0313 0.4489 0.093 Uiso 1 1 calc R . . H15H H 1.0040 0.0684 0.4324 0.093 Uiso 1 1 calc R . . H15I H 0.9961 0.0207 0.3842 0.093 Uiso 1 1 calc R . . C1H C 0.7221(15) -0.2063(12) 0.266(2) 0.064(8) Uiso 0.25 1 d PD . . C2H C 0.7766(16) -0.2044(11) 0.243(3) 0.084(17) Uiso 0.25 1 d PD . . C3H C 0.8023(8) -0.2518(17) 0.269(2) 0.073(9) Uiso 0.25 1 d PD . . C4H C 0.7772(13) -0.2971(10) 0.2356(17) 0.052(7) Uiso 0.25 1 d PD . . C5H C 0.7232(14) -0.2992(11) 0.2593(19) 0.058(11) Uiso 0.25 1 d PD . . C6H C 0.6959(9) -0.2521(17) 0.236(2) 0.074(9) Uiso 0.25 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1A 0.0202(3) 0.0281(3) 0.0211(3) 0.0025(2) 0.0013(2) 0.0008(2) O1A 0.0265(15) 0.0318(16) 0.0303(15) 0.0084(13) 0.0006(12) 0.0027(12) O2A 0.0205(14) 0.0445(18) 0.0222(14) 0.0078(13) 0.0019(11) 0.0013(13) O3A 0.0163(13) 0.0436(18) 0.0204(13) 0.0067(12) 0.0008(10) -0.0011(12) O4A 0.058(2) 0.047(2) 0.0360(19) -0.0109(16) 0.0055(17) -0.0157(19) N1A 0.0124(14) 0.0325(18) 0.0197(15) 0.0005(13) 0.0011(12) 0.0015(13) N2A 0.0219(17) 0.0269(18) 0.0200(15) -0.0002(13) -0.0019(13) 0.0045(14) C1A 0.031(2) 0.0197(19) 0.0262(19) -0.0024(15) -0.0023(16) -0.0030(16) C2A 0.027(2) 0.033(2) 0.0247(19) 0.0026(17) 0.0021(16) 0.0023(18) C3A 0.036(3) 0.057(3) 0.029(2) 0.009(2) 0.006(2) 0.015(2) C4A 0.039(3) 0.069(4) 0.034(3) 0.021(2) -0.003(2) 0.009(3) C5A 0.035(3) 0.040(3) 0.042(3) 0.013(2) -0.011(2) 0.007(2) C6A 0.032(2) 0.038(3) 0.038(2) 0.011(2) -0.0085(19) 0.000(2) C7A 0.026(2) 0.0218(19) 0.0232(19) 0.0007(15) 0.0007(16) 0.0040(16) C8A 0.027(2) 0.029(2) 0.0195(18) -0.0034(16) -0.0024(15) 0.0011(17) C9A 0.024(2) 0.027(2) 0.0176(17) 0.0042(15) -0.0002(15) 0.0062(16) C10A 0.031(2) 0.030(2) 0.057(3) 0.006(2) -0.021(2) -0.0018(19) C11A 0.038(3) 0.036(3) 0.084(4) 0.022(3) -0.012(3) 0.007(2) C12A 0.034(3) 0.082(4) 0.045(3) 0.036(3) -0.003(2) 0.008(3) C13A 0.031(2) 0.076(4) 0.024(2) 0.005(2) -0.0043(18) -0.002(2) C14A 0.025(2) 0.049(3) 0.0219(19) 0.0024(18) -0.0045(16) -0.0089(19) C15A 0.171(10) 0.099(6) 0.037(3) -0.024(4) 0.010(5) -0.027(6) Mn1B 0.0181(3) 0.0319(3) 0.0224(3) 0.0033(2) 0.0014(2) 0.0045(2) O1B 0.0289(16) 0.0306(16) 0.0353(16) -0.0012(13) -0.0034(13) 0.0095(13) O2B 0.0201(14) 0.0325(16) 0.0184(12) -0.0001(11) -0.0029(10) 0.0066(12) O3B 0.0241(15) 0.0452(19) 0.0194(13) -0.0053(12) -0.0009(11) 0.0053(13) O4B 0.0367(19) 0.050(2) 0.0406(19) 0.0158(16) 0.0049(15) -0.0110(16) N1B 0.0132(15) 0.0327(19) 0.0212(15) 0.0025(13) 0.0022(12) 0.0069(13) N2B 0.0241(17) 0.0274(18) 0.0185(15) -0.0021(13) 0.0051(13) 0.0016(14) C1B 0.026(2) 0.029(2) 0.030(2) 0.0045(17) 0.0074(17) -0.0005(17) C2B 0.025(2) 0.0221(19) 0.0242(19) 0.0042(15) 0.0066(15) 0.0053(16) C3B 0.037(2) 0.027(2) 0.029(2) 0.0012(17) -0.0011(18) 0.0017(19) C4B 0.052(3) 0.038(3) 0.040(3) -0.014(2) 0.004(2) 0.008(2) C5B 0.050(3) 0.044(3) 0.045(3) -0.003(2) 0.009(2) 0.022(2) C6B 0.030(2) 0.036(3) 0.048(3) 0.000(2) 0.007(2) 0.013(2) C7B 0.029(2) 0.025(2) 0.0181(17) 0.0044(15) 0.0069(15) -0.0024(16) C8B 0.0186(18) 0.031(2) 0.0208(18) 0.0035(16) 0.0040(14) 0.0013(16) C9B 0.022(2) 0.037(2) 0.0252(19) -0.0078(17) -0.0003(16) 0.0051(17) C10B 0.025(2) 0.070(4) 0.032(2) -0.011(2) 0.0085(19) 0.000(2) C11B 0.054(4) 0.095(5) 0.041(3) -0.022(3) 0.016(3) 0.006(3) C12B 0.069(4) 0.087(5) 0.048(3) -0.035(3) -0.005(3) 0.028(4) C13B 0.046(3) 0.060(4) 0.064(4) -0.028(3) -0.006(3) 0.015(3) C14B 0.035(3) 0.037(3) 0.042(3) -0.012(2) -0.004(2) 0.005(2) C15B 0.037(3) 0.150(8) 0.098(6) 0.084(6) 0.009(4) -0.001(4) Mn1C 0.0216(3) 0.0260(3) 0.0193(3) 0.0028(2) 0.0000(2) 0.0014(2) O1C 0.0330(16) 0.0272(16) 0.0315(15) 0.0084(12) 0.0065(13) -0.0017(13) O2C 0.0271(15) 0.0250(15) 0.0250(14) 0.0028(11) 0.0057(12) 0.0039(12) O3C 0.0285(15) 0.0221(14) 0.0213(13) 0.0038(11) 0.0021(11) 0.0006(11) O4C 0.047(2) 0.042(2) 0.043(2) 0.0043(16) -0.0121(17) -0.0082(16) N1C 0.0241(17) 0.0254(17) 0.0189(15) 0.0061(13) -0.0034(13) -0.0019(13) N2C 0.0294(18) 0.0275(18) 0.0191(15) 0.0036(13) -0.0017(13) -0.0059(14) C1C 0.029(2) 0.041(3) 0.031(2) 0.0085(19) 0.0017(18) 0.0008(19) C2C 0.0145(18) 0.048(3) 0.029(2) 0.0094(19) -0.0004(16) 0.0075(18) C3C 0.051(3) 0.058(3) 0.040(3) 0.025(3) 0.016(2) 0.026(3) C4C 0.085(5) 0.077(5) 0.066(4) 0.051(4) 0.040(4) 0.042(4) C5C 0.082(5) 0.066(4) 0.073(4) 0.051(4) 0.043(4) 0.047(4) C6C 0.057(4) 0.056(4) 0.052(3) 0.028(3) 0.020(3) 0.027(3) C7C 0.022(2) 0.032(2) 0.0201(18) 0.0050(16) -0.0040(15) -0.0041(16) C8C 0.0223(19) 0.024(2) 0.0195(17) 0.0014(15) -0.0016(14) 0.0021(15) C9C 0.030(2) 0.024(2) 0.0233(19) 0.0040(16) -0.0016(16) -0.0050(17) C10C 0.039(3) 0.037(3) 0.025(2) 0.0058(18) -0.0075(18) 0.001(2) C11C 0.080(4) 0.036(3) 0.036(3) 0.015(2) -0.008(3) 0.008(3) C12C 0.072(4) 0.042(3) 0.052(3) 0.025(3) 0.019(3) 0.005(3) C13C 0.052(3) 0.043(3) 0.067(4) 0.018(3) 0.004(3) -0.014(3) C14C 0.034(3) 0.035(3) 0.045(3) 0.006(2) 0.000(2) -0.007(2) C15C 0.044(3) 0.084(5) 0.057(4) -0.013(3) -0.028(3) 0.007(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 Mn1A O1A 1.868(3) . ? Mn1A O3A 1.937(3) . ? Mn1A N1A 1.944(3) . ? Mn1A O2C 1.970(3) 8_646 ? Mn1A O4A 2.233(4) . ? Mn1A N2C 2.260(4) 8_646 ? O1A C1A 1.352(5) . ? O2A C7A 1.289(5) . ? O2A Mn1B 1.985(3) . ? O3A C8A 1.303(5) . ? O4A C15A 1.403(8) . ? N1A C7A 1.332(5) . ? N1A N2A 1.420(4) . ? N2A C8A 1.307(5) . ? N2A Mn1B 2.257(3) . ? C1A C2A 1.409(6) . ? C1A C6A 1.418(6) . ? C2A C3A 1.410(6) . ? C2A C7A 1.462(6) . ? C3A C4A 1.383(7) . ? C4A C5A 1.392(7) . ? C5A C6A 1.378(7) . ? C8A C9A 1.497(5) . ? C9A C14A 1.533(6) . ? C9A C10A 1.545(6) . ? C10A C11A 1.543(6) . ? C11A C12A 1.514(9) . ? C12A C13A 1.514(8) . ? C13A C14A 1.517(6) . ? Mn1B O1B 1.867(3) . ? Mn1B O3B 1.936(3) . ? Mn1B N1B 1.952(3) . ? Mn1B O4B 2.277(3) . ? O1B C1B 1.357(5) . ? O2B C7B 1.301(5) . ? O2B Mn1C 1.973(3) . ? O3B C8B 1.319(5) . ? O4B C15B 1.402(7) . ? N1B C7B 1.336(5) . ? N1B N2B 1.421(5) . ? N2B C8B 1.299(5) . ? N2B Mn1C 2.281(3) . ? C1B C2B 1.410(6) . ? C1B C6B 1.423(6) . ? C2B C3B 1.409(6) . ? C2B C7B 1.457(6) . ? C3B C4B 1.385(6) . ? C4B C5B 1.402(8) . ? C5B C6B 1.379(8) . ? C8B C9B 1.493(6) . ? C9B C10B 1.536(6) . ? C9B C14B 1.547(6) . ? C10B C11B 1.538(8) . ? C11B C12B 1.509(10) . ? C12B C13B 1.536(10) . ? C13B C14B 1.521(7) . ? Mn1C O1C 1.871(3) . ? Mn1C O3C 1.942(3) . ? Mn1C N1C 1.952(4) . ? Mn1C O4C 2.239(4) . ? O1C C1C 1.340(5) . ? O2C C7C 1.290(5) . ? O2C Mn1A 1.970(3) 7_666 ? O3C C8C 1.293(5) . ? O4C C15C 1.416(7) . ? N1C C7C 1.330(5) . ? N1C N2C 1.417(5) . ? N2C C8C 1.322(5) . ? N2C Mn1A 2.260(4) 7_666 ? C1C C2C 1.403(7) . ? C1C C6C 1.428(7) . ? C2C C3C 1.417(6) . ? C2C C7C 1.466(6) . ? C3C C4C 1.377(8) . ? C4C C5C 1.396(9) . ? C5C C6C 1.372(8) . ? C8C C9C 1.523(5) . ? C9C C10C 1.540(6) . ? C9C C14C 1.543(6) . ? C10C C11C 1.533(6) . ? C11C C12C 1.541(9) . ? C12C C13C 1.494(9) . ? C13C C14C 1.528(7) . ? C1H C4H 0.58(4) 2_645 ? C1H C2H 0.69(3) 8_646 ? C1H C6H 0.76(3) 7_666 ? C1H C5H 0.88(4) 7_666 ? C1H C3H 1.06(6) 8_646 ? C1H C3H 1.32(5) 2_645 ? C1H C5H 1.50(5) 2_645 ? C1H C6H 1.538(10) . ? C1H C2H 1.545(10) . ? C1H C4H 2.00(4) 7_666 ? C2H C5H 0.33(6) 2_645 ? C2H C1H 0.69(3) 7_666 ? C2H C3H 0.73(4) 8_646 ? C2H C4H 0.86(5) 8_646 ? C2H C6H 0.91(4) 7_666 ? C2H C6H 1.40(4) 2_645 ? C2H C4H 1.47(5) 2_645 ? C2H C3H 1.546(10) . ? C3H C6H 0.62(4) 2_645 ? C3H C2H 0.73(4) 7_666 ? C3H C4H 0.80(3) 8_646 ? C3H C5H 0.87(4) 8_646 ? C3H C1H 1.06(6) 7_666 ? C3H C1H 1.32(5) 2_645 ? C3H C4H 1.543(10) . ? C3H C5H 1.56(5) 2_645 ? C3H C6H 1.97(4) 8_646 ? C4H C1H 0.58(4) 2_645 ? C4H C3H 0.80(3) 7_666 ? C4H C5H 0.82(3) 8_646 ? C4H C2H 0.86(5) 7_666 ? C4H C6H 0.88(4) 8_646 ? C4H C2H 1.47(5) 2_645 ? C4H C6H 1.53(4) 2_645 ? C4H C5H 1.536(10) . ? C4H C1H 2.00(4) 8_646 ? C5H C2H 0.33(6) 2_645 ? C5H C6H 0.80(3) 8_646 ? C5H C4H 0.82(3) 7_666 ? C5H C3H 0.87(4) 7_666 ? C5H C1H 0.88(4) 8_646 ? C5H C1H 1.50(5) 2_645 ? C5H C6H 1.543(10) . ? C5H C3H 1.56(5) 2_645 ? C6H C3H 0.62(4) 2_645 ? C6H C1H 0.76(3) 8_646 ? C6H C5H 0.80(3) 7_666 ? C6H C4H 0.88(4) 7_666 ? C6H C2H 0.91(4) 8_646 ? C6H C2H 1.40(4) 2_645 ? C6H C4H 1.53(4) 2_645 ? C6H C3H 1.97(4) 7_666 ? 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 O1A Mn1A O3A 170.12(13) . . ? O1A Mn1A N1A 90.22(13) . . ? O3A Mn1A N1A 80.12(12) . . ? O1A Mn1A O2C 93.19(13) . 8_646 ? O3A Mn1A O2C 96.46(12) . 8_646 ? N1A Mn1A O2C 176.58(13) . 8_646 ? O1A Mn1A O4A 89.10(15) . . ? O3A Mn1A O4A 89.52(15) . . ? N1A Mn1A O4A 94.06(14) . . ? O2C Mn1A O4A 85.73(13) 8_646 . ? O1A Mn1A N2C 92.25(13) . 8_646 ? O3A Mn1A N2C 92.36(13) . 8_646 ? N1A Mn1A N2C 105.72(13) . 8_646 ? O2C Mn1A N2C 74.43(12) 8_646 8_646 ? O4A Mn1A N2C 160.16(13) . 8_646 ? C1A O1A Mn1A 130.0(3) . . ? C7A O2A Mn1B 117.8(3) . . ? C8A O3A Mn1A 113.2(2) . . ? C15A O4A Mn1A 129.3(5) . . ? C7A N1A N2A 113.6(3) . . ? C7A N1A Mn1A 131.8(3) . . ? N2A N1A Mn1A 114.4(2) . . ? C8A N2A N1A 110.1(3) . . ? C8A N2A Mn1B 138.3(3) . . ? N1A N2A Mn1B 107.1(2) . . ? O1A C1A C2A 124.2(4) . . ? O1A C1A C6A 117.2(4) . . ? C2A C1A C6A 118.5(4) . . ? C1A C2A C3A 118.5(4) . . ? C1A C2A C7A 123.1(4) . . ? C3A C2A C7A 118.4(4) . . ? C4A C3A C2A 122.2(5) . . ? C3A C4A C5A 118.9(5) . . ? C6A C5A C4A 120.4(4) . . ? C5A C6A C1A 121.4(5) . . ? O2A C7A N1A 121.5(4) . . ? O2A C7A C2A 118.8(4) . . ? N1A C7A C2A 119.7(4) . . ? O3A C8A N2A 122.0(4) . . ? O3A C8A C9A 118.8(3) . . ? N2A C8A C9A 119.2(4) . . ? C8A C9A C14A 111.9(3) . . ? C8A C9A C10A 109.0(3) . . ? C14A C9A C10A 109.5(4) . . ? C11A C10A C9A 111.4(4) . . ? C12A C11A C10A 110.8(5) . . ? C13A C12A C11A 112.6(4) . . ? C12A C13A C14A 110.5(4) . . ? C13A C14A C9A 111.4(4) . . ? O1B Mn1B O3B 170.52(13) . . ? O1B Mn1B N1B 90.65(14) . . ? O3B Mn1B N1B 80.09(13) . . ? O1B Mn1B O2A 91.66(13) . . ? O3B Mn1B O2A 97.56(13) . . ? N1B Mn1B O2A 177.43(13) . . ? O1B Mn1B N2A 89.41(13) . . ? O3B Mn1B N2A 95.14(13) . . ? N1B Mn1B N2A 106.44(13) . . ? O2A Mn1B N2A 74.72(12) . . ? O1B Mn1B O4B 90.93(14) . . ? O3B Mn1B O4B 88.19(14) . . ? N1B Mn1B O4B 96.93(13) . . ? O2A Mn1B O4B 81.89(12) . . ? N2A Mn1B O4B 156.61(12) . . ? C1B O1B Mn1B 128.5(3) . . ? C7B O2B Mn1C 119.9(2) . . ? C8B O3B Mn1B 113.0(2) . . ? C15B O4B Mn1B 122.0(4) . . ? C7B N1B N2B 114.2(3) . . ? C7B N1B Mn1B 131.3(3) . . ? N2B N1B Mn1B 114.5(2) . . ? C8B N2B N1B 110.1(3) . . ? C8B N2B Mn1C 140.4(3) . . ? N1B N2B Mn1C 107.5(2) . . ? O1B C1B C2B 124.9(4) . . ? O1B C1B C6B 116.4(4) . . ? C2B C1B C6B 118.7(4) . . ? C3B C2B C1B 119.1(4) . . ? C3B C2B C7B 117.9(4) . . ? C1B C2B C7B 123.0(4) . . ? C4B C3B C2B 121.1(4) . . ? C3B C4B C5B 120.1(5) . . ? C6B C5B C4B 119.7(4) . . ? C5B C6B C1B 121.2(5) . . ? O2B C7B N1B 120.1(4) . . ? O2B C7B C2B 119.9(4) . . ? N1B C7B C2B 120.0(4) . . ? N2B C8B O3B 122.2(4) . . ? N2B C8B C9B 119.9(4) . . ? O3B C8B C9B 117.9(4) . . ? C8B C9B C10B 112.1(4) . . ? C8B C9B C14B 111.2(4) . . ? C10B C9B C14B 109.7(4) . . ? C9B C10B C11B 110.1(5) . . ? C12B C11B C10B 111.2(5) . . ? C11B C12B C13B 112.6(5) . . ? C14B C13B C12B 110.2(5) . . ? C13B C14B C9B 112.5(4) . . ? O1C Mn1C O3C 170.15(13) . . ? O1C Mn1C N1C 90.42(14) . . ? O3C Mn1C N1C 79.95(13) . . ? O1C Mn1C O2B 92.23(13) . . ? O3C Mn1C O2B 97.35(12) . . ? N1C Mn1C O2B 177.04(13) . . ? O1C Mn1C O4C 88.29(14) . . ? O3C Mn1C O4C 90.20(13) . . ? N1C Mn1C O4C 93.21(15) . . ? O2B Mn1C O4C 85.55(13) . . ? O1C Mn1C N2B 89.86(13) . . ? O3C Mn1C N2B 94.90(12) . . ? N1C Mn1C N2B 107.12(13) . . ? O2B Mn1C N2B 74.23(11) . . ? O4C Mn1C N2B 159.60(14) . . ? C1C O1C Mn1C 129.1(3) . . ? C7C O2C Mn1A 118.8(2) . 7_666 ? C8C O3C Mn1C 112.7(2) . . ? C15C O4C Mn1C 127.0(4) . . ? C7C N1C N2C 112.8(3) . . ? C7C N1C Mn1C 131.9(3) . . ? N2C N1C Mn1C 115.1(2) . . ? C8C N2C N1C 108.5(3) . . ? C8C N2C Mn1A 140.7(3) . 7_666 ? N1C N2C Mn1A 108.2(2) . 7_666 ? O1C C1C C2C 125.6(4) . . ? O1C C1C C6C 115.6(4) . . ? C2C C1C C6C 118.8(4) . . ? C1C C2C C3C 119.3(4) . . ? C1C C2C C7C 123.2(4) . . ? C3C C2C C7C 117.5(4) . . ? C4C C3C C2C 121.1(5) . . ? C3C C4C C5C 119.1(5) . . ? C6C C5C C4C 121.6(5) . . ? C5C C6C C1C 120.0(5) . . ? O2C C7C N1C 121.8(4) . . ? O2C C7C C2C 119.2(4) . . ? N1C C7C C2C 119.0(4) . . ? O3C C8C N2C 123.6(4) . . ? O3C C8C C9C 119.6(3) . . ? N2C C8C C9C 116.8(4) . . ? C8C C9C C10C 111.4(3) . . ? C8C C9C C14C 110.1(4) . . ? C10C C9C C14C 109.9(4) . . ? C11C C10C C9C 110.4(4) . . ? C10C C11C C12C 110.6(5) . . ? C13C C12C C11C 111.4(4) . . ? C12C C13C C14C 113.3(5) . . ? C13C C14C C9C 110.3(4) . . ? C4H C1H C2H 85(8) 2_645 8_646 ? C4H C1H C6H 82(7) 2_645 7_666 ? C2H C1H C6H 153(7) 8_646 7_666 ? C4H C1H C5H 65(5) 2_645 7_666 ? C2H C1H C5H 20(6) 8_646 7_666 ? C6H C1H C5H 141(8) 7_666 7_666 ? C4H C1H C3H 48(4) 2_645 8_646 ? C2H C1H C3H 123(9) 8_646 8_646 ? C6H C1H C3H 35(3) 7_666 8_646 ? C5H C1H C3H 107(6) 7_666 8_646 ? C4H C1H C3H 101(5) 2_645 2_645 ? C2H C1H C3H 22(6) 8_646 2_645 ? C6H C1H C3H 142(4) 7_666 2_645 ? C5H C1H C3H 40(3) 7_666 2_645 ? C3H C1H C3H 127(4) 8_646 2_645 ? C4H C1H C5H 83(5) 2_645 2_645 ? C2H C1H C5H 138(5) 8_646 2_645 ? C6H C1H C5H 16(2) 7_666 2_645 ? C5H C1H C5H 132(4) 7_666 2_645 ? C3H C1H C5H 34(3) 8_646 2_645 ? C3H C1H C5H 126(3) 2_645 2_645 ? C4H C1H C6H 78(4) 2_645 . ? C2H C1H C6H 17(4) 8_646 . ? C6H C1H C6H 136(4) 7_666 . ? C5H C1H C6H 23(3) 7_666 . ? C3H C1H C6H 108(3) 8_646 . ? C3H C1H C6H 23.6(17) 2_645 . ? C5H C1H C6H 121(2) 2_645 . ? C4H C1H C2H 72(4) 2_645 . ? C2H C1H C2H 129(5) 8_646 . ? C6H C1H C2H 24(4) 7_666 . ? C5H C1H C2H 120(4) 7_666 . ? C3H C1H C2H 25(3) 8_646 . ? C3H C1H C2H 122(2) 2_645 . ? C5H C1H C2H 12(2) 2_645 . ? C6H C1H C2H 112(2) . . ? C4H C1H C4H 99(5) 2_645 7_666 ? C2H C1H C4H 33(4) 8_646 7_666 ? C6H C1H C4H 127(4) 7_666 7_666 ? C5H C1H C4H 47(2) 7_666 7_666 ? C3H C1H C4H 114(3) 8_646 7_666 ? C3H C1H C4H 15.4(14) 2_645 7_666 ? C5H C1H C4H 111(2) 2_645 7_666 ? C6H C1H C4H 24.9(15) . 7_666 ? C2H C1H C4H 106.3(14) . 7_666 ? C5H C2H C1H 114(10) 2_645 7_666 ? C5H C2H C3H 103(10) 2_645 8_646 ? C1H C2H C3H 137(10) 7_666 8_646 ? C5H C2H C4H 73(10) 2_645 8_646 ? C1H C2H C4H 42(4) 7_666 8_646 ? C3H C2H C4H 153(6) 8_646 8_646 ? C5H C2H C6H 61(8) 2_645 7_666 ? C1H C2H C6H 149(7) 7_666 7_666 ? C3H C2H C6H 43(4) 8_646 7_666 ? C4H C2H C6H 120(8) 8_646 7_666 ? C5H C2H C6H 109(9) 2_645 2_645 ? C1H C2H C6H 14(4) 7_666 2_645 ? C3H C2H C6H 133(5) 8_646 2_645 ? C4H C2H C6H 37(3) 8_646 2_645 ? C6H C2H C6H 135(4) 7_666 2_645 ? C5H C2H C4H 96(8) 2_645 2_645 ? C1H C2H C4H 132(5) 7_666 2_645 ? C3H C2H C4H 18(4) 8_646 2_645 ? C4H C2H C4H 135(4) 8_646 2_645 ? C6H C2H C4H 34(4) 7_666 2_645 ? C6H C2H C4H 123(3) 2_645 2_645 ? C5H C2H C1H 76(8) 2_645 . ? C1H C2H C1H 134(4) 7_666 . ? C3H C2H C1H 37(6) 8_646 . ? C4H C2H C1H 118(4) 8_646 . ? C6H C2H C1H 20(3) 7_666 . ? C6H C2H C1H 120(2) 2_645 . ? C4H C2H C1H 21.9(15) 2_645 . ? C5H C2H C3H 86(9) 2_645 . ? C1H C2H C3H 35(6) 7_666 . ? C3H C2H C3H 136(3) 8_646 . ? C4H C2H C3H 21(2) 8_646 . ? C6H C2H C3H 117(4) 7_666 . ? C6H C2H C3H 23.7(17) 2_645 . ? C4H C2H C3H 120.1(19) 2_645 . ? C1H C2H C3H 108.4(13) . . ? C6H C3H C2H 84(7) 2_645 7_666 ? C6H C3H C4H 76(6) 2_645 8_646 ? C2H C3H C4H 146(7) 7_666 8_646 ? C6H C3H C5H 63(4) 2_645 8_646 ? C2H C3H C5H 22(5) 7_666 8_646 ? C4H C3H C5H 134(7) 8_646 8_646 ? C6H C3H C1H 45(4) 2_645 7_666 ? C2H C3H C1H 118(8) 7_666 7_666 ? C4H C3H C1H 32(3) 8_646 7_666 ? C5H C3H C1H 102(6) 8_646 7_666 ? C6H C3H C1H 98(4) 2_645 2_645 ? C2H C3H C1H 21(5) 7_666 2_645 ? C4H C3H C1H 139(3) 8_646 2_645 ? C5H C3H C1H 41(3) 8_646 2_645 ? C1H C3H C1H 121(3) 7_666 2_645 ? C6H C3H C4H 77(4) 2_645 . ? C2H C3H C4H 15(4) 7_666 . ? C4H C3H C4H 132(4) 8_646 . ? C5H C3H C4H 23(3) 8_646 . ? C1H C3H C4H 105(3) 7_666 . ? C1H C3H C4H 21.5(16) 2_645 . ? C6H C3H C2H 65(4) 2_645 . ? C2H C3H C2H 124(4) 7_666 . ? C4H C3H C2H 22(3) 8_646 . ? C5H C3H C2H 115(3) 8_646 . ? C1H C3H C2H 22(3) 7_666 . ? C1H C3H C2H 118.6(19) 2_645 . ? C4H C3H C2H 109.6(13) . . ? C6H C3H C5H 77(4) 2_645 2_645 ? C2H C3H C5H 133(4) 7_666 2_645 ? C4H C3H C5H 16.3(15) 8_646 2_645 ? C5H C3H C5H 126(4) 8_646 2_645 ? C1H C3H C5H 33(3) 7_666 2_645 ? C1H C3H C5H 123(3) 2_645 2_645 ? C4H C3H C5H 117.9(19) . 2_645 ? C2H C3H C5H 12(2) . 2_645 ? C6H C3H C6H 97(4) 2_645 8_646 ? C2H C3H C6H 32(3) 7_666 8_646 ? C4H C3H C6H 125(3) 8_646 8_646 ? C5H C3H C6H 48(2) 8_646 8_646 ? C1H C3H C6H 111(3) 7_666 8_646 ? C1H C3H C6H 13.6(15) 2_645 8_646 ? C4H C3H C6H 25.6(15) . 8_646 ? C2H C3H C6H 105.8(14) . 8_646 ? C5H C3H C6H 109(2) 2_645 8_646 ? C1H C4H C3H 99(6) 2_645 7_666 ? C1H C4H C5H 75(5) 2_645 8_646 ? C3H C4H C5H 148(3) 7_666 8_646 ? C1H C4H C2H 53(5) 2_645 7_666 ? C3H C4H C2H 137(5) 7_666 7_666 ? C5H C4H C2H 23(4) 8_646 7_666 ? C1H C4H C6H 58(5) 2_645 8_646 ? C3H C4H C6H 43(3) 7_666 8_646 ? C5H C4H C6H 129(6) 8_646 8_646 ? C2H C4H C6H 107(6) 7_666 8_646 ? C1H C4H C2H 87(4) 2_645 2_645 ? C3H C4H C2H 16(3) 7_666 2_645 ? C5H C4H C2H 134(3) 8_646 2_645 ? C2H C4H C2H 121(4) 7_666 2_645 ? C6H C4H C2H 35(4) 8_646 2_645 ? C1H C4H C6H 80(4) 2_645 2_645 ? C3H C4H C6H 129(3) 7_666 2_645 ? C5H C4H C6H 19.7(18) 8_646 2_645 ? C2H C4H C6H 31(4) 7_666 2_645 ? C6H C4H C6H 124(3) 8_646 2_645 ? C2H C4H C6H 117(3) 2_645 2_645 ? C1H C4H C5H 76(5) 2_645 . ? C3H C4H C5H 24(4) 7_666 . ? C5H C4H C5H 134(3) 8_646 . ? C2H C4H C5H 116(4) 7_666 . ? C6H C4H C5H 23(3) 8_646 . ? C2H C4H C5H 12(2) 2_645 . ? C6H C4H C5H 119.3(16) 2_645 . ? C1H C4H C3H 57(5) 2_645 . ? C3H C4H C3H 128(3) 7_666 . ? C5H C4H C3H 25(3) 8_646 . ? C2H C4H C3H 13(3) 7_666 . ? C6H C4H C3H 106(3) 8_646 . ? C2H C4H C3H 112(2) 2_645 . ? C6H C4H C3H 23.4(16) 2_645 . ? C5H C4H C3H 109.6(12) . . ? C1H C4H C1H 90(5) 2_645 8_646 ? C3H C4H C1H 26(2) 7_666 8_646 ? C5H C4H C1H 122(3) 8_646 8_646 ? C2H C4H C1H 114(3) 7_666 8_646 ? C6H C4H C1H 47(2) 8_646 8_646 ? C2H C4H C1H 14.8(17) 2_645 8_646 ? C6H C4H C1H 104(2) 2_645 8_646 ? C5H C4H C1H 24.6(16) . 8_646 ? C3H C4H C1H 102.9(13) . 8_646 ? C2H C5H C6H 97(8) 2_645 8_646 ? C2H C5H C4H 85(9) 2_645 7_666 ? C6H C5H C4H 140(4) 8_646 7_666 ? C2H C5H C3H 55(8) 2_645 7_666 ? C6H C5H C3H 44(3) 8_646 7_666 ? C4H C5H C3H 132(6) 7_666 7_666 ? C2H C5H C1H 46(8) 2_645 8_646 ? C6H C5H C1H 133(6) 8_646 8_646 ? C4H C5H C1H 40(3) 7_666 8_646 ? C3H C5H C1H 98(6) 7_666 8_646 ? C2H C5H C1H 92(8) 2_645 2_645 ? C6H C5H C1H 15.3(17) 8_646 2_645 ? C4H C5H C1H 126(3) 7_666 2_645 ? C3H C5H C1H 44(4) 7_666 2_645 ? C1H C5H C1H 120(4) 8_646 2_645 ? C2H C5H C4H 72(8) 2_645 . ? C6H C5H C4H 26(4) 8_646 . ? C4H C5H C4H 130(3) 7_666 . ? C3H C5H C4H 22(3) 7_666 . ? C1H C5H C4H 109(3) 8_646 . ? C1H C5H C4H 21.9(15) 2_645 . ? C2H C5H C6H 60(8) 2_645 . ? C6H C5H C6H 130(3) 8_646 . ? C4H C5H C6H 26(4) 7_666 . ? C3H C5H C6H 107(3) 7_666 . ? C1H C5H C6H 18(3) 8_646 . ? C1H C5H C6H 114.6(17) 2_645 . ? C4H C5H C6H 110.2(12) . . ? C2H C5H C3H 81(8) 2_645 2_645 ? C6H C5H C3H 125(3) 8_646 2_645 ? C4H C5H C3H 15.9(14) 7_666 2_645 ? C3H C5H C3H 120(4) 7_666 2_645 ? C1H C5H C3H 41(4) 8_646 2_645 ? C1H C5H C3H 110(3) 2_645 2_645 ? C4H C5H C3H 115.1(17) . 2_645 ? C6H C5H C3H 23.1(16) . 2_645 ? C3H C6H C1H 100(7) 2_645 8_646 ? C3H C6H C5H 74(5) 2_645 7_666 ? C1H C6H C5H 148(4) 8_646 7_666 ? C3H C6H C4H 62(5) 2_645 7_666 ? C1H C6H C4H 40(4) 8_646 7_666 ? C5H C6H C4H 131(7) 7_666 7_666 ? C3H C6H C2H 53(5) 2_645 8_646 ? C1H C6H C2H 136(6) 8_646 8_646 ? C5H C6H C2H 21(4) 7_666 8_646 ? C4H C6H C2H 110(7) 7_666 8_646 ? C3H C6H C2H 91(4) 2_645 2_645 ? C1H C6H C2H 13(4) 8_646 2_645 ? C5H C6H C2H 137(3) 7_666 2_645 ? C4H C6H C2H 36(3) 7_666 2_645 ? C2H C6H C2H 124(4) 8_646 2_645 ? C3H C6H C4H 80(4) 2_645 2_645 ? C1H C6H C4H 129(4) 8_646 2_645 ? C5H C6H C4H 20.2(18) 7_666 2_645 ? C4H C6H C4H 125(3) 7_666 2_645 ? C2H C6H C4H 29(4) 8_646 2_645 ? C2H C6H C4H 119(3) 2_645 2_645 ? C3H C6H C1H 58(4) 2_645 . ? C1H C6H C1H 126(4) 8_646 . ? C5H C6H C1H 25(3) 7_666 . ? C4H C6H C1H 108(3) 7_666 . ? C2H C6H C1H 13(3) 8_646 . ? C2H C6H C1H 114(2) 2_645 . ? C4H C6H C1H 21.7(15) 2_645 . ? C3H C6H C5H 80(4) 2_645 . ? C1H C6H C5H 21(5) 8_646 . ? C5H C6H C5H 135(3) 7_666 . ? C4H C6H C5H 24(3) 7_666 . ? C2H C6H C5H 118(4) 8_646 . ? C2H C6H C5H 12(3) 2_645 . ? C4H C6H C5H 120.0(17) 2_645 . ? C1H C6H C5H 110.4(13) . . ? C3H C6H C3H 96(5) 2_645 7_666 ? C1H C6H C3H 24(3) 8_646 7_666 ? C5H C6H C3H 124(3) 7_666 7_666 ? C4H C6H C3H 49(2) 7_666 7_666 ? C2H C6H C3H 116(3) 8_646 7_666 ? C2H C6H C3H 15.8(18) 2_645 7_666 ? C4H C6H C3H 105(2) 2_645 7_666 ? C1H C6H C3H 104.1(13) . 7_666 ? C5H C6H C3H 24.9(15) . 7_666 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.796 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.096 #===END data_l5_85te _database_code_depnum_ccdc_archive 'CCDC 298635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C188 H244 Mn12 N24 O48' _chemical_formula_weight 4267.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 27.073(2) _cell_length_b 27.073(2) _cell_length_c 18.909(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13860(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7906 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.23 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Brown' _exptl_crystal_size_max 1.25 _exptl_crystal_size_mid 0.88 _exptl_crystal_size_min 0.65 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5280 _exptl_absorpt_correction_T_max 0.7021 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73193 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.36 _reflns_number_total 16854 _reflns_number_gt 12152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Diamond 3.1a, ORTEP3' _computing_publication_material WinGX _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^)+(0.0973P)^2^+49.9077P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16854 _refine_ls_number_parameters 620 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.2515 _refine_ls_wR_factor_gt 0.2394 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.064 _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 Mn1A Mn 0.56789(2) 0.02590(3) 0.27191(3) 0.03004(17) Uani 1 1 d . . . O1A O 0.52700(12) 0.06055(12) 0.21056(17) 0.0350(7) Uani 1 1 d . . . O2A O 0.67134(11) 0.08310(14) 0.13356(16) 0.0372(8) Uani 1 1 d . . . O3A O 0.61951(11) -0.00424(14) 0.32700(16) 0.0366(7) Uani 1 1 d . . . O4A O 0.57306(17) 0.09310(17) 0.3387(2) 0.0569(11) Uani 1 1 d . . . H4OA H 0.570(3) 0.118(3) 0.316(5) 0.085 Uiso 1 1 d . . . N1A N 0.62454(13) 0.04335(15) 0.21486(18) 0.0295(8) Uani 1 1 d . . . N2A N 0.67046(13) 0.02818(15) 0.24379(18) 0.0319(8) Uani 1 1 d . . . C1A C 0.53716(17) 0.08194(16) 0.1479(2) 0.0322(9) Uani 1 1 d . . . C2A C 0.58500(17) 0.08771(19) 0.1199(2) 0.0352(10) Uani 1 1 d . . . C3A C 0.5902(2) 0.1099(2) 0.0540(3) 0.0472(13) Uani 1 1 d . . . H3A H 0.6224 0.1130 0.0345 0.057 Uiso 1 1 calc R . . C4A C 0.5509(2) 0.1274(2) 0.0161(3) 0.0492(13) Uani 1 1 d . . . H4A H 0.5555 0.1421 -0.0290 0.059 Uiso 1 1 calc R . . C5A C 0.5043(2) 0.1231(2) 0.0454(3) 0.0452(12) Uani 1 1 d . . . H5A H 0.4765 0.1356 0.0204 0.054 Uiso 1 1 calc R . . C6A C 0.49760(19) 0.1011(2) 0.1098(3) 0.0424(11) Uani 1 1 d . . . H6A H 0.4652 0.0988 0.1289 0.051 Uiso 1 1 calc R . . C7A C 0.62907(16) 0.07081(17) 0.1576(2) 0.0304(9) Uani 1 1 d . . . C8A C 0.66350(16) 0.00343(18) 0.3010(2) 0.0324(9) Uani 1 1 d . . . C9A C 0.70695(16) -0.01805(19) 0.3391(2) 0.0347(10) Uani 1 1 d . . . H9A H 0.7369 -0.0143 0.3086 0.042 Uiso 1 1 calc R . . C10A C 0.6990(3) -0.0727(3) 0.3539(5) 0.0693(19) Uani 1 1 d . . . H10A H 0.6968 -0.0909 0.3086 0.083 Uiso 1 1 calc R . . H10B H 0.6675 -0.0773 0.3797 0.083 Uiso 1 1 calc R . . C11A C 0.7423(3) -0.0939(3) 0.3986(5) 0.083(2) Uani 1 1 d . . . H11A H 0.7342 -0.1282 0.4125 0.100 Uiso 1 1 calc R . . H11B H 0.7724 -0.0950 0.3690 0.100 Uiso 1 1 calc R . . C12A C 0.7525(3) -0.0653(4) 0.4616(4) 0.080(2) Uani 1 1 d . . . H12A H 0.7824 -0.0787 0.4847 0.097 Uiso 1 1 calc R . . H12B H 0.7246 -0.0692 0.4950 0.097 Uiso 1 1 calc R . . C13A C 0.7599(2) -0.0129(3) 0.4477(3) 0.0581(16) Uani 1 1 d . . . H13A H 0.7901 -0.0084 0.4189 0.070 Uiso 1 1 calc R . . H13B H 0.7646 0.0048 0.4930 0.070 Uiso 1 1 calc R . . C14A C 0.71612(19) 0.0085(2) 0.4091(3) 0.0470(13) Uani 1 1 d . . . H14A H 0.7220 0.0440 0.3999 0.056 Uiso 1 1 calc R . . H14B H 0.6864 0.0056 0.4392 0.056 Uiso 1 1 calc R . . C15A C 0.5820(4) 0.0982(4) 0.4114(4) 0.114(4) Uani 1 1 d . . . H15A H 0.5626 0.0737 0.4375 0.171 Uiso 1 1 calc R . . H15B H 0.5726 0.1314 0.4267 0.171 Uiso 1 1 calc R . . H15C H 0.6173 0.0929 0.4209 0.171 Uiso 1 1 calc R . . Mn1B Mn 0.72901(2) 0.07688(3) 0.19638(3) 0.03207(18) Uani 1 1 d . . . O1B O 0.70727(12) 0.12807(13) 0.25376(18) 0.0377(7) Uani 1 1 d . . . O2B O 0.84352(10) 0.08154(12) 0.34236(14) 0.0286(6) Uani 1 1 d . . . O3B O 0.76210(12) 0.02502(14) 0.14528(16) 0.0377(8) Uani 1 1 d . . . O4B O 0.76150(14) 0.13155(15) 0.1176(2) 0.0489(9) Uani 1 1 d . . . N1B N 0.78783(12) 0.06887(15) 0.25445(18) 0.0285(7) Uani 1 1 d . . . N2B N 0.82159(13) 0.03344(15) 0.23009(18) 0.0305(8) Uani 1 1 d . . . C1B C 0.72402(17) 0.14182(19) 0.3173(2) 0.0345(10) Uani 1 1 d . . . C2B C 0.76878(16) 0.12693(17) 0.3475(2) 0.0302(9) Uani 1 1 d . . . C3B C 0.78303(19) 0.14673(18) 0.4127(2) 0.0373(10) Uani 1 1 d . . . H3B H 0.8135 0.1368 0.4330 0.045 Uiso 1 1 calc R . . C4B C 0.7542(2) 0.1799(2) 0.4477(3) 0.0467(12) Uani 1 1 d . . . H4B H 0.7650 0.1938 0.4911 0.056 Uiso 1 1 calc R . . C5B C 0.7086(2) 0.1931(2) 0.4190(3) 0.0485(13) Uani 1 1 d . . . H5B H 0.6875 0.2149 0.4441 0.058 Uiso 1 1 calc R . . C6B C 0.69452(19) 0.1747(2) 0.3552(3) 0.0449(12) Uani 1 1 d . . . H6B H 0.6636 0.1845 0.3359 0.054 Uiso 1 1 calc R . . C7B C 0.80138(16) 0.09133(16) 0.3133(2) 0.0284(9) Uani 1 1 d . . . C8B C 0.80464(17) 0.01249(18) 0.1732(2) 0.0322(9) Uani 1 1 d . . . C9B C 0.83326(19) -0.0273(2) 0.1386(2) 0.0407(11) Uani 1 1 d . . . H9B H 0.8592 -0.0388 0.1725 0.049 Uiso 1 1 calc R . . C10B C 0.8588(2) -0.0087(3) 0.0722(3) 0.0577(16) Uani 1 1 d . . . H10C H 0.8337 0.0028 0.0379 0.069 Uiso 1 1 calc R . . H10D H 0.8802 0.0197 0.0843 0.069 Uiso 1 1 calc R . . C11B C 0.8895(3) -0.0487(3) 0.0390(4) 0.077(2) Uani 1 1 d . . . H11C H 0.9052 -0.0358 -0.0045 0.092 Uiso 1 1 calc R . . H11D H 0.9160 -0.0585 0.0722 0.092 Uiso 1 1 calc R . . C12B C 0.8596(3) -0.0922(3) 0.0212(4) 0.087(3) Uani 1 1 d . . . H12C H 0.8817 -0.1188 0.0041 0.104 Uiso 1 1 calc R . . H12D H 0.8367 -0.0836 -0.0177 0.104 Uiso 1 1 calc R . . C13B C 0.8290(4) -0.1119(3) 0.0857(5) 0.092(3) Uani 1 1 d . . . H13C H 0.8061 -0.1381 0.0694 0.111 Uiso 1 1 calc R . . H13D H 0.8517 -0.1266 0.1209 0.111 Uiso 1 1 calc R . . C14B C 0.8002(3) -0.0717(2) 0.1196(3) 0.0579(15) Uani 1 1 d . . . H14C H 0.7844 -0.0845 0.1631 0.069 Uiso 1 1 calc R . . H14D H 0.7738 -0.0608 0.0870 0.069 Uiso 1 1 calc R . . C15B C 0.8121(3) 0.1333(4) 0.1014(5) 0.102(3) Uani 1 1 d . . . H15D H 0.8314 0.1293 0.1448 0.152 Uiso 1 1 calc R . . H15E H 0.8199 0.1653 0.0797 0.152 Uiso 1 1 calc R . . H15F H 0.8202 0.1067 0.0682 0.152 Uiso 1 1 calc R . . Mn1C Mn 0.89360(2) 0.04473(2) 0.28871(3) 0.02743(16) Uani 1 1 d . . . O1C O 0.90767(12) 0.09842(12) 0.23102(16) 0.0341(7) Uani 1 1 d . . . O2C O 1.00657(12) -0.01321(11) 0.16567(15) 0.0307(6) Uani 1 1 d . . . O3C O 0.88985(12) -0.01610(12) 0.34185(15) 0.0323(7) Uani 1 1 d . . . O4C O 0.94787(15) 0.07466(15) 0.3666(2) 0.0467(9) Uani 1 1 d . . . H4OC H 0.968(3) 0.095(3) 0.349(4) 0.070 Uiso 1 1 d . . . N1C N 0.94312(13) 0.00584(14) 0.24027(18) 0.0282(7) Uani 1 1 d . . . N2C N 0.95272(15) -0.04083(13) 0.26968(19) 0.0315(8) Uani 1 1 d . . . C1C C 0.93555(18) 0.10113(19) 0.1738(3) 0.0374(10) Uani 1 1 d . . . C2C C 0.96608(16) 0.06224(19) 0.1488(2) 0.0356(10) Uani 1 1 d . . . C3C C 0.9935(2) 0.0694(2) 0.0865(3) 0.0501(14) Uani 1 1 d . . . H3C H 1.0144 0.0437 0.0696 0.060 Uiso 1 1 calc R . . C4C C 0.9906(3) 0.1129(3) 0.0500(4) 0.081(3) Uani 1 1 d . . . H4C H 1.0094 0.1171 0.0080 0.097 Uiso 1 1 calc R . . C5C C 0.9603(3) 0.1512(3) 0.0740(4) 0.082(3) Uani 1 1 d . . . H5C H 0.9583 0.1813 0.0483 0.099 Uiso 1 1 calc R . . C6C C 0.9332(3) 0.1451(3) 0.1349(3) 0.0655(19) Uani 1 1 d . . . H6C H 0.9126 0.1712 0.1509 0.079 Uiso 1 1 calc R . . C7C C 0.97218(16) 0.01606(17) 0.1858(2) 0.0293(9) Uani 1 1 d . . . C8C C 0.92172(17) -0.04851(16) 0.3215(2) 0.0306(9) Uani 1 1 d . . . C9C C 0.92600(19) -0.09800(18) 0.3595(3) 0.0378(10) Uani 1 1 d . . . H9C H 0.9442 -0.1214 0.3280 0.045 Uiso 1 1 calc R . . C10C C 0.9540(2) -0.09362(19) 0.4282(3) 0.0436(12) Uani 1 1 d . . . H10E H 0.9366 -0.0704 0.4599 0.052 Uiso 1 1 calc R . . H10F H 0.9874 -0.0802 0.4188 0.052 Uiso 1 1 calc R . . C11C C 0.9585(3) -0.1437(2) 0.4642(3) 0.072(2) Uani 1 1 d . . . H11E H 0.9783 -0.1662 0.4342 0.086 Uiso 1 1 calc R . . H11F H 0.9760 -0.1398 0.5099 0.086 Uiso 1 1 calc R . . C12C C 0.9082(3) -0.1660(3) 0.4770(4) 0.087(3) Uani 1 1 d . . . H12E H 0.9121 -0.1997 0.4965 0.104 Uiso 1 1 calc R . . H12F H 0.8903 -0.1458 0.5124 0.104 Uiso 1 1 calc R . . C13C C 0.8784(3) -0.1684(3) 0.4103(5) 0.081(2) Uani 1 1 d . . . H13E H 0.8447 -0.1803 0.4216 0.097 Uiso 1 1 calc R . . H13F H 0.8937 -0.1926 0.3777 0.097 Uiso 1 1 calc R . . C14C C 0.8747(2) -0.1192(2) 0.3735(4) 0.0647(18) Uani 1 1 d . . . H14E H 0.8556 -0.0960 0.4033 0.078 Uiso 1 1 calc R . . H14F H 0.8569 -0.1233 0.3281 0.078 Uiso 1 1 calc R . . C15C C 0.9787(3) 0.0460(3) 0.4113(4) 0.0654(18) Uani 1 1 d . . . H15G H 0.9596 0.0343 0.4520 0.098 Uiso 1 1 calc R . . H15H H 1.0063 0.0664 0.4279 0.098 Uiso 1 1 calc R . . H15I H 0.9916 0.0176 0.3849 0.098 Uiso 1 1 calc R . . C1O C 0.7480(10) -0.1807(6) 0.2509(15) 0.139(9) Uiso 0.50 1 d PD A 1 C2O C 0.7854(12) -0.2131(11) 0.2039(12) 0.179(13) Uiso 0.50 1 d PD A 1 C12O C 0.7479(12) -0.2037(14) 0.2021(12) 0.25(2) Uiso 0.50 1 d PD B 2 C22O C 0.7963(8) -0.2003(8) 0.2502(17) 0.131(9) Uiso 0.50 1 d PD B 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 Mn1A 0.0240(3) 0.0410(4) 0.0251(3) 0.0020(3) -0.0007(2) -0.0020(3) O1A 0.0295(16) 0.0407(18) 0.0348(16) 0.0055(14) -0.0004(13) -0.0043(13) O2A 0.0254(15) 0.062(2) 0.0241(14) 0.0035(14) 0.0013(12) 0.0012(14) O3A 0.0209(14) 0.064(2) 0.0246(14) 0.0041(14) -0.0011(12) -0.0007(14) O4A 0.061(3) 0.066(3) 0.044(2) -0.0061(19) 0.0018(19) -0.028(2) N1A 0.0209(16) 0.043(2) 0.0243(16) -0.0008(15) -0.0012(13) -0.0027(15) N2A 0.0258(18) 0.049(2) 0.0212(16) -0.0009(15) 0.0002(14) 0.0046(16) C1A 0.035(2) 0.029(2) 0.033(2) -0.0004(17) -0.0018(18) -0.0060(18) C2A 0.029(2) 0.051(3) 0.025(2) 0.0021(19) 0.0000(17) 0.001(2) C3A 0.043(3) 0.071(4) 0.028(2) 0.003(2) 0.000(2) 0.008(3) C4A 0.042(3) 0.072(4) 0.034(3) 0.007(3) -0.003(2) 0.000(3) C5A 0.043(3) 0.046(3) 0.047(3) 0.003(2) -0.008(2) 0.006(2) C6A 0.034(2) 0.046(3) 0.047(3) 0.005(2) -0.006(2) -0.006(2) C7A 0.032(2) 0.037(2) 0.0218(19) -0.0011(17) 0.0000(16) 0.0025(18) C8A 0.027(2) 0.047(3) 0.0231(19) -0.0004(18) -0.0016(16) -0.0045(19) C9A 0.025(2) 0.056(3) 0.0230(19) 0.0042(19) 0.0015(16) 0.006(2) C10A 0.058(4) 0.056(4) 0.094(5) 0.005(4) -0.019(4) 0.002(3) C11A 0.056(4) 0.067(5) 0.127(8) 0.018(5) -0.006(4) 0.005(3) C12A 0.043(4) 0.124(7) 0.074(5) 0.028(5) -0.006(3) 0.000(4) C13A 0.040(3) 0.101(5) 0.033(3) 0.010(3) -0.002(2) -0.002(3) C14A 0.035(3) 0.077(4) 0.029(2) 0.002(2) -0.002(2) -0.006(3) C15A 0.154(10) 0.148(9) 0.040(4) -0.017(5) 0.011(5) -0.072(8) Mn1B 0.0227(3) 0.0487(4) 0.0248(3) 0.0000(3) 0.0008(2) 0.0040(3) O1B 0.0301(16) 0.0471(19) 0.0359(17) -0.0035(15) -0.0013(13) 0.0059(14) O2B 0.0231(14) 0.0427(17) 0.0199(13) -0.0007(12) -0.0010(11) 0.0085(12) O3B 0.0299(16) 0.058(2) 0.0249(15) -0.0047(14) -0.0012(12) 0.0029(15) O4B 0.041(2) 0.056(2) 0.049(2) 0.0050(18) 0.0031(17) -0.0081(17) N1B 0.0189(16) 0.046(2) 0.0208(15) -0.0013(15) 0.0006(13) 0.0036(15) N2B 0.0285(18) 0.040(2) 0.0228(16) -0.0025(15) 0.0012(14) 0.0034(15) C1B 0.028(2) 0.045(3) 0.030(2) 0.0003(19) 0.0038(17) -0.0045(19) C2B 0.030(2) 0.033(2) 0.028(2) 0.0021(17) 0.0033(17) 0.0000(17) C3B 0.045(3) 0.037(2) 0.030(2) 0.0027(19) -0.002(2) 0.001(2) C4B 0.052(3) 0.048(3) 0.040(3) -0.005(2) 0.003(2) 0.011(2) C5B 0.049(3) 0.051(3) 0.046(3) -0.005(2) 0.003(2) 0.018(2) C6B 0.033(3) 0.051(3) 0.050(3) -0.004(2) -0.003(2) 0.011(2) C7B 0.031(2) 0.034(2) 0.0206(18) 0.0023(16) 0.0035(16) -0.0045(17) C8B 0.031(2) 0.044(3) 0.0213(18) -0.0011(18) -0.0001(16) 0.0025(19) C9B 0.042(3) 0.053(3) 0.027(2) -0.007(2) -0.0027(19) 0.016(2) C10B 0.040(3) 0.093(5) 0.040(3) -0.016(3) 0.003(2) 0.000(3) C11B 0.066(4) 0.115(7) 0.049(4) -0.019(4) 0.008(3) 0.005(4) C12B 0.102(6) 0.105(7) 0.054(4) -0.023(4) 0.002(4) 0.037(5) C13B 0.114(7) 0.077(5) 0.086(6) -0.017(5) -0.012(5) 0.026(5) C14B 0.069(4) 0.058(4) 0.047(3) -0.012(3) 0.002(3) 0.004(3) C15B 0.050(4) 0.160(9) 0.095(6) 0.055(6) 0.016(4) 0.005(5) Mn1C 0.0267(3) 0.0333(3) 0.0222(3) 0.0022(2) 0.0001(2) 0.0029(3) O1C 0.0354(17) 0.0352(17) 0.0316(16) 0.0034(13) 0.0033(13) 0.0037(13) O2C 0.0383(17) 0.0278(15) 0.0259(14) 0.0013(12) 0.0036(13) 0.0080(13) O3C 0.0376(17) 0.0354(17) 0.0240(14) 0.0030(12) -0.0001(12) 0.0000(13) O4C 0.051(2) 0.046(2) 0.043(2) 0.0021(17) -0.0044(17) -0.0030(17) N1C 0.0294(18) 0.0332(19) 0.0221(16) 0.0042(14) -0.0019(14) -0.0031(14) N2C 0.040(2) 0.0253(18) 0.0296(18) 0.0021(14) -0.0034(16) -0.0035(15) C1C 0.033(2) 0.042(3) 0.036(2) 0.005(2) 0.0013(19) 0.012(2) C2C 0.026(2) 0.051(3) 0.029(2) 0.008(2) 0.0029(17) 0.0109(19) C3C 0.061(3) 0.051(3) 0.038(3) 0.009(2) 0.010(2) 0.029(3) C4C 0.106(6) 0.085(5) 0.051(4) 0.033(4) 0.029(4) 0.050(5) C5C 0.101(6) 0.074(5) 0.072(5) 0.037(4) 0.033(4) 0.053(4) C6C 0.075(4) 0.067(4) 0.054(3) 0.021(3) 0.012(3) 0.039(4) C7C 0.032(2) 0.034(2) 0.0217(18) 0.0038(16) -0.0012(16) -0.0075(17) C8C 0.037(2) 0.029(2) 0.026(2) 0.0011(16) 0.0016(17) -0.0043(18) C9C 0.043(3) 0.032(2) 0.038(2) 0.0007(19) 0.002(2) -0.012(2) C10C 0.059(3) 0.039(3) 0.032(2) 0.007(2) -0.003(2) 0.003(2) C11C 0.123(7) 0.048(4) 0.044(3) 0.006(3) -0.003(4) 0.011(4) C12C 0.107(7) 0.087(6) 0.066(5) 0.029(4) 0.026(5) 0.025(5) C13C 0.078(5) 0.059(4) 0.106(6) 0.014(4) 0.004(5) -0.018(4) C14C 0.054(4) 0.054(4) 0.086(5) 0.011(3) 0.000(3) -0.014(3) C15C 0.058(4) 0.084(5) 0.055(4) -0.007(3) -0.007(3) 0.012(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 Mn1A O1A 1.858(3) . ? Mn1A O3A 1.925(3) . ? Mn1A N1A 1.934(4) . ? Mn1A O2C 1.964(3) 8_646 ? Mn1A O4A 2.219(4) . ? Mn1A N2C 2.254(4) 8_646 ? O1A C1A 1.347(5) . ? O2A C7A 1.275(5) . ? O2A Mn1B 1.969(3) . ? O3A C8A 1.305(5) . ? O4A C15A 1.403(8) . ? N1A C7A 1.320(6) . ? N1A N2A 1.419(5) . ? N2A C8A 1.287(6) . ? N2A Mn1B 2.248(4) . ? C1A C6A 1.391(7) . ? C1A C2A 1.408(6) . ? C2A C3A 1.391(7) . ? C2A C7A 1.463(6) . ? C3A C4A 1.366(7) . ? C4A C5A 1.384(8) . ? C5A C6A 1.368(8) . ? C8A C9A 1.497(6) . ? C9A C10A 1.521(8) . ? C9A C14A 1.525(7) . ? C10A C11A 1.554(10) . ? C11A C12A 1.447(12) . ? C12A C13A 1.457(11) . ? C13A C14A 1.508(8) . ? Mn1B O1B 1.856(3) . ? Mn1B O3B 1.926(3) . ? Mn1B N1B 1.946(3) . ? Mn1B O4B 2.277(4) . ? O1B C1B 1.336(6) . ? O2B C7B 1.294(5) . ? O2B Mn1C 1.965(3) . ? O3B C8B 1.311(5) . ? O4B C15B 1.404(8) . ? N1B C7B 1.320(5) . ? N1B N2B 1.403(5) . ? N2B C8B 1.300(6) . ? N2B Mn1C 2.263(4) . ? C1B C6B 1.394(7) . ? C1B C2B 1.400(6) . ? C2B C3B 1.398(6) . ? C2B C7B 1.458(6) . ? C3B C4B 1.361(7) . ? C4B C5B 1.394(8) . ? C5B C6B 1.362(8) . ? C8B C9B 1.479(6) . ? C9B C10B 1.520(8) . ? C9B C14B 1.542(8) . ? C10B C11B 1.503(10) . ? C11B C12B 1.468(12) . ? C12B C13B 1.568(13) . ? C13B C14B 1.482(10) . ? Mn1C O1C 1.857(3) . ? Mn1C O3C 1.932(3) . ? Mn1C N1C 1.935(4) . ? Mn1C O4C 2.232(4) . ? O1C C1C 1.321(6) . ? O2C C7C 1.280(5) . ? O2C Mn1A 1.964(3) 7_666 ? O3C C8C 1.290(6) . ? O4C C15C 1.420(8) . ? N1C C7C 1.326(5) . ? N1C N2C 1.405(5) . ? N2C C8C 1.307(6) . ? N2C Mn1A 2.254(4) 7_666 ? C1C C6C 1.401(8) . ? C1C C2C 1.420(7) . ? C2C C3C 1.406(7) . ? C2C C7C 1.442(6) . ? C3C C4C 1.367(8) . ? C4C C5C 1.398(9) . ? C5C C6C 1.375(9) . ? C8C C9C 1.524(6) . ? C9C C10C 1.508(7) . ? C9C C14C 1.526(8) . ? C10C C11C 1.523(8) . ? C11C C12C 1.510(12) . ? C12C C13C 1.499(12) . ? C13C C14C 1.506(10) . ? C1O C2O 1.569(11) 8_646 ? C1O C2O 1.607(17) . ? C2O C1O 1.569(11) 7_666 ? C12O C22O 1.574(14) 8_646 ? C12O C22O 1.595(18) . ? C22O C12O 1.574(14) 7_666 ? 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 O1A Mn1A O3A 169.98(14) . . ? O1A Mn1A N1A 90.05(15) . . ? O3A Mn1A N1A 80.18(14) . . ? O1A Mn1A O2C 93.48(14) . 8_646 ? O3A Mn1A O2C 96.26(13) . 8_646 ? N1A Mn1A O2C 176.42(14) . 8_646 ? O1A Mn1A O4A 88.79(17) . . ? O3A Mn1A O4A 89.64(17) . . ? N1A Mn1A O4A 93.85(16) . . ? O2C Mn1A O4A 85.64(14) 8_646 . ? O1A Mn1A N2C 91.86(14) . 8_646 ? O3A Mn1A N2C 92.99(15) . 8_646 ? N1A Mn1A N2C 106.13(15) . 8_646 ? O2C Mn1A N2C 74.37(13) 8_646 8_646 ? O4A Mn1A N2C 160.00(14) . 8_646 ? C1A O1A Mn1A 130.1(3) . . ? C7A O2A Mn1B 118.3(3) . . ? C8A O3A Mn1A 113.1(3) . . ? C15A O4A Mn1A 130.4(6) . . ? C7A N1A N2A 113.5(3) . . ? C7A N1A Mn1A 132.0(3) . . ? N2A N1A Mn1A 114.2(3) . . ? C8A N2A N1A 110.3(4) . . ? C8A N2A Mn1B 138.1(3) . . ? N1A N2A Mn1B 107.1(3) . . ? O1A C1A C6A 117.3(4) . . ? O1A C1A C2A 124.5(4) . . ? C6A C1A C2A 118.2(4) . . ? C3A C2A C1A 118.5(4) . . ? C3A C2A C7A 119.3(4) . . ? C1A C2A C7A 122.2(4) . . ? C4A C3A C2A 122.8(5) . . ? C3A C4A C5A 118.1(5) . . ? C6A C5A C4A 120.9(5) . . ? C5A C6A C1A 121.4(5) . . ? O2A C7A N1A 121.5(4) . . ? O2A C7A C2A 118.5(4) . . ? N1A C7A C2A 120.0(4) . . ? N2A C8A O3A 122.2(4) . . ? N2A C8A C9A 119.5(4) . . ? O3A C8A C9A 118.3(4) . . ? C8A C9A C10A 110.8(4) . . ? C8A C9A C14A 111.2(4) . . ? C10A C9A C14A 108.8(5) . . ? C9A C10A C11A 110.6(6) . . ? C12A C11A C10A 113.3(7) . . ? C11A C12A C13A 113.4(7) . . ? C12A C13A C14A 110.6(5) . . ? C13A C14A C9A 111.6(5) . . ? O1B Mn1B O3B 170.22(14) . . ? O1B Mn1B N1B 90.74(15) . . ? O3B Mn1B N1B 79.70(14) . . ? O1B Mn1B O2A 92.13(15) . . ? O3B Mn1B O2A 97.39(14) . . ? N1B Mn1B O2A 176.95(15) . . ? O1B Mn1B N2A 88.92(15) . . ? O3B Mn1B N2A 95.76(15) . . ? N1B Mn1B N2A 106.65(14) . . ? O2A Mn1B N2A 74.43(13) . . ? O1B Mn1B O4B 91.13(15) . . ? O3B Mn1B O4B 88.05(15) . . ? N1B Mn1B O4B 97.22(15) . . ? O2A Mn1B O4B 81.71(14) . . ? N2A Mn1B O4B 156.13(14) . . ? C1B O1B Mn1B 128.7(3) . . ? C7B O2B Mn1C 119.6(3) . . ? C8B O3B Mn1B 113.3(3) . . ? C15B O4B Mn1B 122.8(4) . . ? C7B N1B N2B 114.2(3) . . ? C7B N1B Mn1B 130.7(3) . . ? N2B N1B Mn1B 115.1(3) . . ? C8B N2B N1B 109.9(4) . . ? C8B N2B Mn1C 140.2(3) . . ? N1B N2B Mn1C 107.9(2) . . ? O1B C1B C6B 116.4(4) . . ? O1B C1B C2B 125.5(4) . . ? C6B C1B C2B 118.0(4) . . ? C3B C2B C1B 119.3(4) . . ? C3B C2B C7B 118.5(4) . . ? C1B C2B C7B 122.2(4) . . ? C4B C3B C2B 121.5(5) . . ? C3B C4B C5B 119.2(5) . . ? C6B C5B C4B 119.9(5) . . ? C5B C6B C1B 121.9(5) . . ? O2B C7B N1B 120.6(4) . . ? O2B C7B C2B 118.7(4) . . ? N1B C7B C2B 120.7(4) . . ? N2B C8B O3B 122.0(4) . . ? N2B C8B C9B 119.9(4) . . ? O3B C8B C9B 118.1(4) . . ? C8B C9B C10B 111.2(5) . . ? C8B C9B C14B 111.6(4) . . ? C10B C9B C14B 109.3(4) . . ? C11B C10B C9B 110.9(6) . . ? C12B C11B C10B 111.7(6) . . ? C11B C12B C13B 112.7(6) . . ? C14B C13B C12B 111.4(7) . . ? C13B C14B C9B 111.6(6) . . ? O1C Mn1C O3C 169.63(14) . . ? O1C Mn1C N1C 90.33(14) . . ? O3C Mn1C N1C 79.56(14) . . ? O1C Mn1C O2B 92.75(14) . . ? O3C Mn1C O2B 97.32(13) . . ? N1C Mn1C O2B 176.75(14) . . ? O1C Mn1C O4C 88.18(15) . . ? O3C Mn1C O4C 90.06(14) . . ? N1C Mn1C O4C 93.08(15) . . ? O2B Mn1C O4C 85.96(14) . . ? O1C Mn1C N2B 89.70(14) . . ? O3C Mn1C N2B 95.41(14) . . ? N1C Mn1C N2B 106.94(14) . . ? O2B Mn1C N2B 74.16(12) . . ? O4C Mn1C N2B 159.88(14) . . ? C1C O1C Mn1C 129.9(3) . . ? C7C O2C Mn1A 118.8(3) . 7_666 ? C8C O3C Mn1C 112.9(3) . . ? C15C O4C Mn1C 125.6(4) . . ? C7C N1C N2C 112.7(4) . . ? C7C N1C Mn1C 131.7(3) . . ? N2C N1C Mn1C 115.5(3) . . ? C8C N2C N1C 108.7(4) . . ? C8C N2C Mn1A 140.8(3) . 7_666 ? N1C N2C Mn1A 108.5(3) . 7_666 ? O1C C1C C6C 116.8(4) . . ? O1C C1C C2C 124.4(4) . . ? C6C C1C C2C 118.8(5) . . ? C3C C2C C1C 119.0(5) . . ? C3C C2C C7C 117.7(4) . . ? C1C C2C C7C 123.2(4) . . ? C4C C3C C2C 120.7(5) . . ? C3C C4C C5C 120.6(6) . . ? C6C C5C C4C 119.8(6) . . ? C5C C6C C1C 121.1(6) . . ? O2C C7C N1C 122.2(4) . . ? O2C C7C C2C 118.4(4) . . ? N1C C7C C2C 119.3(4) . . ? O3C C8C N2C 123.1(4) . . ? O3C C8C C9C 120.6(4) . . ? N2C C8C C9C 116.4(4) . . ? C10C C9C C8C 112.0(4) . . ? C10C C9C C14C 109.7(5) . . ? C8C C9C C14C 110.1(5) . . ? C9C C10C C11C 110.9(5) . . ? C12C C11C C10C 110.7(6) . . ? C13C C12C C11C 111.6(6) . . ? C12C C13C C14C 112.7(7) . . ? C13C C14C C9C 110.7(6) . . ? C2O C1O C2O 111(2) 8_646 . ? C1O C2O C1O 113.3(16) 7_666 . ? C22O C12O C22O 110.2(17) 8_646 . ? C12O C22O C12O 106(2) 7_666 . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.873 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.102 #===END