Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Boskovic, Colette' 'Breechin, Euan K.' 'Christou, George' 'Folting, Kirsten' 'Hendrickson, David' 'Strieb, William E.' _publ_contact_author_name 'Prof George Christou' _publ_contact_author_address ; Prof George Christou Department of Chemistry Indiana University Bloomington IN 47405-4001 USA ; data_MSC98192 _database_code_CSD 154915 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C105 H102 Cl18 Mn12 N6 O30' _chemical_formula_moiety 'C98 H88 Cl4 Mn12 N6 O30, 7(C H2 Cl2)' _chemical_formula_weight 3225.39 _cell_length_a 36.774(3) _cell_length_b 14.9295(12) _cell_length_c 27.037(2) _cell_angle_alpha 90 _cell_angle_beta 121.884(4) _cell_angle_gamma 90 _cell_volume 12604.3(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 255 _cell_measurement_theta_min 7.51 _cell_measurement_theta_max 13.37 _cell_measurement_temperature 105 _exptl_crystal_colour black _exptl_crystal_description 'triangular plate' _exptl_crystal_size_max .40 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 1.7 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6480 _exptl_absorpt_coefficient_mu 1.6119 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_T_max 0.724 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 105 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22434 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 3.02457 _diffrn_reflns_theta_max 25.1043 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.5 _diffrn_standards_interval_count 300 _reflns_number_total 11190 _reflns_number_gt 7908 _reflns_threshold_expression F^2^>2.0\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source MN Mn 0.295 0.729 'International Tables Vol. IV (1974) Table 2.2B' CL Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 7908 _refine_ls_number_parameters 772 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.000000003(5) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0379 _refine_ls_goodness_of_fit_ref 0.8413 _refine_ls_shift/su_max 0.155 _refine_diff_density_max 0.26 _refine_diff_density_min -0.26 _refine_special_details ; Hydrogens were included in fixed calculated positions with thermal parameters fixed at one plus the isotropic thermal parameter of the parent carbon atom. ; _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution DIRDIF _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly MN1 MN 0.250252(19) 0.14902(4) 0.98231(3) 0.0121(3) Uani 1 0 . MN2 MN 0.153814(19) 0.20492(4) 0.95397(3) 0.0125(3) Uani 1 0 . MN3 MN 0.294729(19) 0.21134(4) 1.10901(3) 0.0126(3) Uani 1 0 . MN4 MN 0.20966(2) 0.08799(4) 1.06420(3) 0.0127(3) Uani 1 0 . MN5 MN 0.20898(2) 0.29124(4) 1.09988(3) 0.0134(3) Uani 1 0 . MN6 MN 0.12151(2) 0.17933(4) 1.04326(3) 0.0155(3) Uani 1 0 . CL7 CL 0.26260(3) 0.15301(7) 1.16980(4) 0.0177(5) Uani 1 0 . CL8 CL 0.07789(3) 0.12028(8) 1.07853(5) 0.0212(5) Uani 1 0 . O9 O 0.20576(8) 0.23410(19) 0.96246(12) 0.0123(12) Uani 1 0 . O10 O 0.18052(9) 0.20263(19) 1.03894(12) 0.0137(13) Uani 1 0 . O11 O 0.25557(8) 0.12432(19) 1.05546(12) 0.0129(13) Uani 1 0 . O12 O 0.25298(9) 0.30517(19) 1.08584(12) 0.0137(13) Uani 1 0 . O13 O 0.20783(10) 0.0359(2) 0.93002(13) 0.0238(15) Uani 1 0 . C14 C 0.17809(13) 0.0179(3) 0.9373(2) 0.021(2) Uani 1 0 . O15 O 0.17076(10) 0.0513(2) 0.97241(13) 0.0218(14) Uani 1 0 . C16 C 0.14409(14) -0.0487(3) 0.89360(19) 0.022(2) Uani 1 0 . C17 C 0.10660(15) -0.0617(3) 0.8931(2) 0.026(2) Uani 1 0 . C18 C 0.07447(15) -0.1201(3) 0.8516(2) 0.027(2) Uani 1 0 . C19 C 0.08134(18) -0.1630(4) 0.8136(2) 0.038(3) Uani 1 0 . C20 C 0.11959(17) -0.1518(3) 0.8131(2) 0.033(3) Uani 1 0 . C21 C 0.14975(16) -0.0947(3) 0.8528(2) 0.028(2) Uani 1 0 . O22 O 0.20562(9) 0.4404(2) 0.99933(13) 0.0174(14) Uani 1 0 . C23 C 0.18350(13) 0.4593(3) 1.02162(18) 0.0178(19) Uani 1 0 . O24 O 0.17693(9) 0.4084(2) 1.05280(13) 0.0185(14) Uani 1 0 . C25 C 0.16303(14) 0.5498(3) 1.00738(19) 0.020(2) Uani 1 0 . C26 C 0.16600(15) 0.6070(3) 0.9688(2) 0.026(2) Uani 1 0 . C27 C 0.14390(17) 0.6870(3) 0.9523(2) 0.030(2) Uani 1 0 . C28 C 0.11855(16) 0.7106(3) 0.9738(2) 0.032(2) Uani 1 0 . C29 C 0.11683(16) 0.6568(3) 1.0139(2) 0.032(3) Uani 1 0 . C30 C 0.13897(16) 0.5771(3) 1.0306(2) 0.028(2) Uani 1 0 . O31 O 0.12868(9) 0.3308(2) 0.91776(13) 0.0171(14) Uani 1 0 . C32 C 0.13167(13) 0.3817(3) 0.88341(18) 0.0184(19) Uani 1 0 . O33 O 0.15792(9) 0.3734(2) 0.86614(12) 0.0172(13) Uani 1 0 . C34 C 0.10175(13) 0.4602(3) 0.85985(18) 0.0181(19) Uani 1 0 . C35 C 0.07681(14) 0.4795(3) 0.8830(2) 0.024(2) Uani 1 0 . C36 C 0.04952(15) 0.5518(3) 0.8631(2) 0.029(2) Uani 1 0 . C37 C 0.04688(15) 0.6058(3) 0.8193(2) 0.029(2) Uani 1 0 . C38 C 0.07126(16) 0.5864(3) 0.7955(2) 0.029(2) Uani 1 0 . C39 C 0.09891(14) 0.5133(3) 0.8160(2) 0.024(2) Uani 1 0 . O40 O 0.12606(9) 0.1629(2) 0.86960(12) 0.0169(13) Uani 1 0 . C41 C 0.13382(14) 0.1656(3) 0.82914(19) 0.017(2) Uani 1 0 . O42 O 0.16352(9) 0.2098(2) 0.83000(12) 0.0175(13) Uani 1 0 . C43 C 0.10605(14) 0.1107(3) 0.77599(19) 0.019(2) Uani 1 0 . C44 C 0.11970(15) 0.0920(3) 0.7376(2) 0.024(2) Uani 1 0 . C45 C 0.09505(16) 0.0392(3) 0.6893(2) 0.029(2) Uani 1 0 . C46 C 0.05616(16) 0.0068(3) 0.6778(2) 0.029(2) Uani 1 0 . C47 C 0.04194(15) 0.0258(3) 0.7152(2) 0.030(2) Uani 1 0 . C48 C 0.06700(15) 0.0773(3) 0.7643(2) 0.024(2) Uani 1 0 . O49 O 0.16510(9) 0.06172(19) 1.07688(13) 0.0170(14) Uani 1 0 . C50 C 0.15608(14) -0.0240(3) 1.08997(19) 0.021(2) Uani 1 0 . C51 C 0.16397(14) -0.0983(3) 1.0588(2) 0.022(2) Uani 1 0 . C52 C 0.21035(14) -0.1137(3) 1.08189(19) 0.020(2) Uani 1 0 . C53 C 0.22797(16) -0.1987(3) 1.0963(2) 0.028(2) Uani 1 0 . C54 C 0.27140(16) -0.2107(3) 1.1199(2) 0.032(3) Uani 1 0 . C55 C 0.29659(15) -0.1367(3) 1.1289(2) 0.028(2) Uani 1 0 . C56 C 0.27748(14) -0.0533(3) 1.1130(2) 0.022(2) Uani 1 0 . N57 N 0.23521(11) -0.0412(2) 1.08970(15) 0.0173(17) Uani 1 0 . O58 O 0.16508(9) 0.2641(2) 1.11438(12) 0.0171(14) Uani 1 0 . C59 C 0.16327(16) 0.2868(4) 1.1640(2) 0.031(2) Uani 1 0 . C60 C 0.20760(16) 0.2964(3) 1.2187(2) 0.028(2) Uani 1 0 . C61 C 0.23139(14) 0.3757(3) 1.21575(19) 0.024(2) Uani 1 0 . C62 C 0.24509(16) 0.4453(4) 1.2553(2) 0.029(2) Uani 1 0 . C63 C 0.26816(17) 0.5156(4) 1.2524(2) 0.033(3) Uani 1 0 . C64 C 0.27712(17) 0.5142(3) 1.2092(2) 0.033(3) Uani 1 0 . C65 C 0.26226(15) 0.4450(3) 1.1697(2) 0.025(2) Uani 1 0 . N66 N 0.23932(11) 0.3773(2) 1.17214(15) 0.0174(16) Uani 1 0 . O67 O 0.10411(9) 0.1719(2) 0.95378(12) 0.0163(13) Uani 1 0 . C68 C 0.06221(14) 0.1754(3) 0.9031(2) 0.023(2) Uani 1 0 . C69 C 0.02958(14) 0.1923(3) 0.9207(2) 0.024(2) Uani 1 0 . C70 C 0.03542(14) 0.2826(3) 0.9487(2) 0.025(2) Uani 1 0 . C71 C 0.00484(15) 0.3501(4) 0.9218(2) 0.031(2) Uani 1 0 . C72 C 0.01187(17) 0.4318(4) 0.9489(2) 0.035(3) Uani 1 0 . C73 C 0.05001(17) 0.4469(4) 1.0018(2) 0.034(3) Uani 1 0 . C74 C 0.07910(15) 0.3769(3) 1.0248(2) 0.025(2) Uani 1 0 . N75 N 0.07261(12) 0.2963(3) 1.00049(16) 0.0220(18) Uani 1 0 . C76 C 0 0.3662(6) 0.75 0.090(6) Uani 1 0 . CL77 CL 0.03634(8) 0.30169(15) 0.74188(9) 0.1047(13) Uani 1 0 . C78 C -0.03411(15) 0.0937(3) 0.9822(2) 0.029(2) Uani 1 0 . CL79 CL -0.04616(4) 0.06801(11) 1.03596(6) 0.0421(7) Uani 1 0 . CL80 CL -0.06025(5) 0.19150(10) 0.94394(7) 0.0481(8) Uani 1 0 . C81 C 0.0330(2) 0.2991(4) 1.1121(3) 0.056(4) Uani 1 0 . CL82 CL 0.02380(7) 0.23386(12) 1.15823(10) 0.0784(14) Uani 1 0 . CL83 CL 0.06499(5) 0.39269(11) 1.15058(7) 0.0487(8) Uani 1 0 . C84 C 0.13893(18) 0.3058(4) 0.6970(2) 0.043(3) Uani 1 0 . CL85 CL 0.17244(5) 0.25488(13) 0.67714(7) 0.0568(8) Uani 1 0 . CL86 CL 0.11850(6) 0.40834(13) 0.66177(9) 0.0717(11) Uani 1 0 . H1 H 0.1025 -0.0309 0.921 0.0377 Uiso 1 0 . H2 H 0.0484 -0.1296 0.8512 0.0393 Uiso 1 0 . H3 H 0.0589 -0.2017 0.7846 0.0507 Uiso 1 0 . H4 H 0.1236 -0.184 0.7852 0.0463 Uiso 1 0 . H5 H 0.1755 -0.0841 0.8526 0.0406 Uiso 1 0 . H6 H 0.1834 0.5899 0.9532 0.0369 Uiso 1 0 . H7 H 0.1459 0.727 0.9259 0.0437 Uiso 1 0 . H8 H 0.1016 0.7644 0.9601 0.0442 Uiso 1 0 . H9 H 0.1001 0.6756 1.03 0.0428 Uiso 1 0 . H10 H 0.1379 0.5398 1.0584 0.0405 Uiso 1 0 . H11 H 0.0784 0.4416 0.9128 0.0364 Uiso 1 0 . H12 H 0.0323 0.5649 0.8792 0.0411 Uiso 1 0 . H13 H 0.0286 0.6574 0.8066 0.0393 Uiso 1 0 . H14 H 0.0689 0.6243 0.7646 0.0414 Uiso 1 0 . H15 H 0.1165 0.4999 0.7998 0.0354 Uiso 1 0 . H16 H 0.1464 0.1163 0.7457 0.0356 Uiso 1 0 . H17 H 0.1048 0.0269 0.6634 0.0395 Uiso 1 0 . H18 H 0.0384 -0.0293 0.644 0.0396 Uiso 1 0 . H19 H 0.015 0.0035 0.7076 0.042 Uiso 1 0 . H20 H 0.0572 0.0902 0.7901 0.036 Uiso 1 0 . H21 H 0.1738 -0.0346 1.1311 0.034 Uiso 1 0 . H22 H 0.1267 -0.0267 1.0795 0.034 Uiso 1 0 . H23 H 0.1518 -0.1528 1.0622 0.0345 Uiso 1 0 . H24 H 0.1499 -0.0829 1.0184 0.0345 Uiso 1 0 . H25 H 0.2096 -0.2494 1.0891 0.039 Uiso 1 0 . H26 H 0.284 -0.2698 1.1306 0.0416 Uiso 1 0 . H27 H 0.327 -0.1419 1.1463 0.0415 Uiso 1 0 . H28 H 0.2952 -0.0018 1.1189 0.0325 Uiso 1 0 . H29 H 0.1475 0.2417 1.1701 0.0417 Uiso 1 0 . H30 H 0.1484 0.3425 1.1571 0.0417 Uiso 1 0 . H31 H 0.2237 0.2426 1.2235 0.0393 Uiso 1 0 . H32 H 0.2051 0.3019 1.2521 0.0393 Uiso 1 0 . H33 H 0.2378 0.4454 1.2847 0.0387 Uiso 1 0 . H34 H 0.2789 0.5639 1.281 0.0465 Uiso 1 0 . H35 H 0.2929 0.5623 1.2055 0.0418 Uiso 1 0 . H36 H 0.2683 0.4456 1.1391 0.0365 Uiso 1 0 . H37 H 0.0608 0.2212 0.878 0.0351 Uiso 1 0 . H38 H 0.0562 0.1188 0.883 0.0351 Uiso 1 0 . H39 H 0.001 0.19 0.8862 0.0348 Uiso 1 0 . H40 H 0.0315 0.1469 0.9466 0.0348 Uiso 1 0 . H41 H -0.0212 0.3381 0.8838 0.0443 Uiso 1 0 . H42 H -0.0102 0.477 0.931 0.046 Uiso 1 0 . H43 H 0.0558 0.5045 1.0209 0.0447 Uiso 1 0 . H44 H 0.1058 0.3869 1.0615 0.0369 Uiso 1 0 . H45 H 0.0157 0.4055 0.7835 0.0824 Uiso 1 0 . H46 H -0.0036 0.1013 1 0.042 Uiso 1 0 . H47 H -0.0425 0.0445 0.955 0.042 Uiso 1 0 . H48 H 0.0475 0.2639 1.0971 0.0615 Uiso 1 0 . H49 H 0.0064 0.3188 1.0786 0.0615 Uiso 1 0 . H50 H 0.155 0.3154 0.7387 0.0519 Uiso 1 0 . H51 H 0.1157 0.2661 0.6882 0.0519 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 MN1 0.013(2) 0.0152(7) 0.0107(11) 0.0012(3) 0.0080(3) 0.0007(3) MN2 0.011(2) 0.0173(7) 0.0109(11) -0.0002(3) 0.0073(3) 0.0000(3) MN3 0.012(2) 0.0169(7) 0.0096(10) 0.0005(3) 0.0062(3) 0.0003(3) MN4 0.013(2) 0.0146(6) 0.0128(13) -0.0002(3) 0.0087(3) 0.0014(3) MN5 0.014(3) 0.0178(8) 0.0115(11) -0.0007(3) 0.0091(3) -0.0021(3) MN6 0.015(3) 0.0196(8) 0.0144(14) -0.0005(3) 0.0094(3) 0.0005(3) CL7 0.019(4) 0.0233(10) 0.0125(13) -0.0012(5) 0.0098(5) 0.0014(4) CL8 0.020(4) 0.0260(11) 0.024(2) -0.0009(5) 0.0156(5) 0.0019(5) O9 0.011(2) 0.0163(17) 0.0112(18) 0.0028(12) 0.0069(12) 0.0026(12) O10 0.014(3) 0.0163(17) 0.0128(19) 0.0000(12) 0.0084(13) 0.0003(13) O11 0.012(3) 0.0158(17) 0.0131(19) 0.0009(12) 0.0084(13) 0.0023(12) O12 0.016(3) 0.0159(17) 0.0117(18) 0.0002(12) 0.0094(13) 0.0009(12) O13 0.026(5) 0.023(2) 0.023(3) -0.0028(14) 0.0138(15) -0.0047(14) C14 0.014(3) 0.018(3) 0.037(5) 0.0099(18) 0.019(2) 0.020(2) O15 0.021(4) 0.023(2) 0.015(2) -0.0017(14) 0.0054(14) 0.0012(14) C16 0.024(5) 0.021(3) 0.019(3) 0.001(2) 0.009(2) 0.003(2) C17 0.027(5) 0.029(3) 0.024(4) -0.002(2) 0.014(2) 0.004(2) C18 0.027(5) 0.022(3) 0.033(4) -0.003(2) 0.017(2) 0.007(2) C19 0.039(8) 0.024(3) 0.037(5) -0.010(2) 0.011(3) 0.001(2) C20 0.045(9) 0.024(3) 0.026(4) -0.004(2) 0.016(3) -0.006(2) C21 0.032(6) 0.027(3) 0.029(4) 0.001(2) 0.019(2) 0.001(2) O22 0.020(4) 0.0203(18) 0.016(2) 0.0045(13) 0.0123(14) 0.0010(13) C23 0.015(3) 0.024(3) 0.011(2) -0.0017(19) 0.0044(19) -0.0042(19) O24 0.020(4) 0.0216(19) 0.018(2) 0.0052(13) 0.0131(14) 0.0043(14) C25 0.020(4) 0.022(3) 0.017(3) 0.0014(19) 0.009(2) -0.0023(19) C26 0.031(6) 0.027(3) 0.022(3) 0.001(2) 0.015(2) 0.001(2) C27 0.038(7) 0.024(3) 0.028(4) 0.005(2) 0.016(2) 0.004(2) C28 0.030(6) 0.024(3) 0.033(4) 0.010(2) 0.011(2) -0.001(2) C29 0.038(7) 0.022(3) 0.041(5) 0.007(2) 0.024(3) -0.006(2) C30 0.032(6) 0.024(3) 0.034(4) 0.001(2) 0.022(2) -0.003(2) O31 0.017(3) 0.0177(18) 0.019(2) 0.0028(13) 0.0109(14) 0.0024(13) C32 0.015(4) 0.024(3) 0.012(2) -0.0031(19) 0.0040(19) -0.0043(19) O33 0.014(3) 0.0222(19) 0.015(2) 0.0047(13) 0.0076(13) 0.0045(13) C34 0.012(3) 0.022(3) 0.014(3) -0.0014(18) 0.0029(18) -0.0023(19) C35 0.021(4) 0.025(3) 0.026(4) 0.001(2) 0.012(2) 0.003(2) C36 0.027(5) 0.028(3) 0.034(4) 0.007(2) 0.018(2) -0.000(2) C37 0.023(5) 0.027(3) 0.029(4) 0.010(2) 0.009(2) 0.002(2) C38 0.030(6) 0.030(3) 0.022(3) 0.007(2) 0.011(2) 0.007(2) C39 0.021(5) 0.029(3) 0.018(3) 0.004(2) 0.007(2) 0.000(2) O40 0.014(3) 0.0238(19) 0.0120(19) -0.0002(13) 0.0062(13) -0.0016(13) C41 0.020(4) 0.015(2) 0.018(3) 0.0017(19) 0.012(2) 0.0024(18) O42 0.017(3) 0.0236(19) 0.0101(18) -0.0017(14) 0.0062(13) -0.0014(13) C43 0.023(5) 0.017(2) 0.015(3) 0.0000(19) 0.008(2) 0.0024(18) C44 0.026(5) 0.026(3) 0.021(3) -0.005(2) 0.014(2) -0.002(2) C45 0.041(8) 0.031(3) 0.014(3) -0.003(2) 0.014(2) -0.004(2) C46 0.037(7) 0.028(3) 0.014(3) -0.008(2) 0.008(2) -0.008(2) C47 0.029(6) 0.031(3) 0.025(4) -0.009(2) 0.009(2) -0.005(2) C48 0.024(5) 0.027(3) 0.020(3) -0.002(2) 0.012(2) -0.001(2) O49 0.016(3) 0.0186(18) 0.021(3) -0.0005(13) 0.0123(14) 0.0033(13) C50 0.022(5) 0.026(3) 0.019(3) 0.001(2) 0.013(2) 0.007(2) C51 0.021(5) 0.018(3) 0.024(3) -0.0014(19) 0.011(2) 0.005(2) C52 0.025(5) 0.020(3) 0.017(3) -0.000(2) 0.012(2) 0.0021(19) C53 0.033(6) 0.020(3) 0.035(4) -0.001(2) 0.020(2) 0.003(2) C54 0.037(7) 0.025(3) 0.036(5) 0.009(2) 0.021(3) 0.011(2) C55 0.026(5) 0.032(3) 0.031(4) 0.005(2) 0.018(2) 0.006(2) C56 0.022(5) 0.024(3) 0.022(3) -0.000(2) 0.014(2) 0.004(2) N57 0.020(4) 0.019(2) 0.017(3) 0.0024(16) 0.0123(17) 0.0023(16) O58 0.016(3) 0.026(2) 0.016(2) -0.0017(13) 0.0123(14) -0.0035(13) C59 0.035(7) 0.045(4) 0.027(4) -0.010(3) 0.026(2) -0.011(2) C60 0.034(7) 0.039(3) 0.020(3) -0.003(2) 0.020(2) -0.003(2) C61 0.022(5) 0.033(3) 0.017(3) 0.002(2) 0.011(2) -0.002(2) C62 0.034(7) 0.039(3) 0.023(3) 0.001(2) 0.020(2) -0.006(2) C63 0.043(8) 0.030(3) 0.030(4) -0.001(2) 0.022(3) -0.014(2) C64 0.048(9) 0.023(3) 0.037(5) -0.009(2) 0.030(3) -0.010(2) C65 0.030(6) 0.029(3) 0.021(3) -0.002(2) 0.018(2) -0.005(2) N66 0.018(4) 0.022(2) 0.013(2) 0.0012(16) 0.0087(16) 0.0010(16) O67 0.011(2) 0.0243(19) 0.014(2) -0.0007(13) 0.0069(13) 0.0012(13) C68 0.016(4) 0.034(3) 0.019(3) -0.002(2) 0.008(2) -0.000(2) C69 0.015(3) 0.036(3) 0.019(3) -0.001(2) 0.007(2) 0.004(2) C70 0.021(4) 0.034(3) 0.027(4) 0.003(2) 0.016(2) 0.004(2) C71 0.021(5) 0.043(4) 0.031(4) 0.007(2) 0.013(2) 0.009(2) C72 0.031(6) 0.038(4) 0.049(6) 0.016(2) 0.029(3) 0.017(3) C73 0.042(8) 0.036(3) 0.041(5) 0.003(3) 0.032(3) 0.001(3) C74 0.029(6) 0.027(3) 0.029(4) 0.001(2) 0.022(2) -0.001(2) N75 0.021(4) 0.028(3) 0.023(3) 0.0000(18) 0.0156(18) 0.0019(18) C76 0.054(12) 0.026(5) 0.098(13) 0 -0.024(6) 0 CL77 0.13(2) 0.072(3) 0.048(5) 0.0328(14) 0.0015(12) -0.0172(10) C78 0.024(5) 0.033(3) 0.035(4) 0.001(2) 0.019(2) 0.001(2) CL79 0.033(6) 0.063(3) 0.029(3) 0.0057(7) 0.0153(6) 0.0043(7) CL80 0.056(10) 0.0369(16) 0.070(7) 0.0194(7) 0.0468(9) 0.0158(8) C81 0.077(15) 0.047(4) 0.050(6) 0.013(4) 0.038(4) -0.009(3) CL82 0.105(19) 0.052(2) 0.121(12) -0.0262(11) 0.0897(15) -0.0304(12) CL83 0.057(10) 0.047(2) 0.061(6) 0.0085(8) 0.0439(9) 0.0069(8) C84 0.036(7) 0.057(4) 0.027(4) 0.005(3) 0.011(3) 0.005(3) CL85 0.045(8) 0.077(3) 0.041(4) 0.0099(8) 0.0174(7) -0.0127(8) CL86 0.076(14) 0.063(3) 0.085(8) 0.0215(10) 0.0479(12) 0.0273(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN1 O9 1.911(3) . . no MN1 O9 2.311(3) . 8_557 no MN1 O11 1.918(3) . . no MN1 O12 1.909(3) . 8_557 no MN1 O13 2.225(3) . . no MN1 O22 1.952(3) . 8_557 no MN2 O9 1.852(3) . . no MN2 O10 1.965(3) . . no MN2 O15 2.359(3) . . no MN2 O31 2.096(3) . . no MN2 O40 2.044(3) . . no MN2 O67 1.890(3) . . no MN3 CL7 2.6282(12) . . no MN3 O9 2.088(3) . 8_557 no MN3 O11 1.912(3) . . no MN3 O12 1.923(3) . . no MN3 O33 1.962(3) . 8_557 no MN3 O42 1.946(3) . 8_557 no MN4 CL7 2.6480(12) . . no MN4 O10 1.942(3) . . no MN4 O11 1.903(3) . . no MN4 O15 2.181(3) . . no MN4 O49 1.884(3) . . no MN4 N57 2.097(4) . . no MN5 CL7 2.7899(13) . . no MN5 O10 1.934(3) . . no MN5 O12 1.859(3) . . no MN5 O24 2.118(3) . . no MN5 O58 1.895(3) . . no MN5 N66 2.100(4) . . no MN6 CL8 2.4241(12) . . no MN6 O10 2.261(3) . . no MN6 O49 2.222(3) . . no MN6 O58 2.148(3) . . no MN6 O67 2.154(3) . . no MN6 N75 2.329(4) . . no CL77 C76 1.753(5) . . no CL77 C76 1.753(5) . 3_556 no CL79 C78 1.772(5) . . no CL80 C78 1.754(5) . . no CL82 C81 1.751(7) . . no CL83 C81 1.768(7) . . no CL85 C84 1.756(6) . . no CL86 C84 1.748(6) . . no O13 C14 1.238(5) . . no O15 C14 1.223(5) . . no O22 C23 1.274(5) . . no O24 C23 1.250(5) . . no O31 C32 1.249(5) . . no O31 C32 1.249(5) . . no O33 C32 1.281(5) . . no O40 C41 1.269(5) . . no O42 C41 1.266(5) . . no O49 C50 1.413(5) . . no O58 C59 1.419(5) . . no O67 C68 1.422(5) . . no N57 C52 1.359(6) . . no N57 C56 1.346(5) . . no N66 C61 1.356(6) . . no N66 C65 1.341(6) . . no N75 C70 1.360(6) . . no N75 C74 1.331(6) . . no C14 C16 1.544(6) . . no C16 C17 1.386(6) . . no C16 C21 1.405(6) . . no C17 C18 1.420(7) . . no C17 H1 0.961(5) . . no C18 C19 1.342(7) . . no C18 H2 0.962(5) . . no C19 C20 1.424(7) . . no C19 H3 0.973(5) . . no C20 C21 1.360(7) . . no C20 H4 0.970(5) . . no C21 H5 0.963(5) . . no C23 C25 1.494(6) . . no C25 C26 1.397(6) . . no C25 C30 1.390(6) . . no C26 C27 1.380(7) . . no C26 H6 0.966(5) . . no C27 C28 1.379(7) . . no C27 H7 0.963(5) . . no C28 C29 1.376(7) . . no C28 H8 0.962(5) . . no C29 C30 1.376(7) . . no C29 H9 0.967(5) . . no C30 H10 0.954(5) . . no C32 C34 1.500(6) . . no C34 C35 1.388(6) . . no C34 C39 1.384(6) . . no C35 C36 1.375(6) . . no C35 H11 0.960(5) . . no C36 C37 1.391(7) . . no C36 H12 0.960(5) . . no C37 C38 1.382(7) . . no C37 H13 0.959(5) . . no C38 C39 1.391(7) . . no C38 H14 0.976(5) . . no C39 H15 0.975(5) . . no C41 C43 1.493(6) . . no C43 C44 1.398(6) . . no C43 C48 1.390(6) . . no C44 C45 1.377(6) . . no C44 H16 0.959(4) . . no C45 C46 1.381(7) . . no C45 H17 0.960(5) . . no C46 C47 1.392(7) . . no C46 H18 0.961(5) . . no C47 C48 1.382(7) . . no C47 H19 0.960(5) . . no C48 H20 0.957(5) . . no C50 C51 1.512(6) . . no C50 H21 0.961(4) . . no C50 H22 0.961(4) . . no C51 C52 1.492(6) . . no C51 H23 0.956(4) . . no C51 H24 0.956(5) . . no C52 C53 1.384(6) . . no C53 C54 1.383(7) . . no C53 H25 0.963(5) . . no C54 C55 1.379(7) . . no C54 H26 0.967(5) . . no C55 C56 1.382(7) . . no C55 H27 0.960(5) . . no C56 H28 0.966(5) . . no C59 C60 1.523(7) . . no C59 H29 0.958(5) . . no C59 H30 0.958(5) . . no C60 C61 1.498(7) . . no C60 H31 0.965(5) . . no C60 H32 0.958(4) . . no C61 C62 1.381(7) . . no C62 C63 1.376(7) . . no C62 H33 0.964(4) . . no C63 C64 1.371(7) . . no C63 H34 0.976(5) . . no C64 C65 1.374(7) . . no C64 H35 0.960(5) . . no C65 H36 0.961(4) . . no C68 C69 1.526(6) . . no C68 H37 0.947(5) . . no C68 H38 0.965(5) . . no C69 C70 1.505(7) . . no C69 H39 0.969(4) . . no C69 H40 0.951(5) . . no C70 C71 1.395(7) . . no C71 C72 1.374(8) . . no C71 H41 0.982(5) . . no C72 C73 1.394(8) . . no C72 H42 0.968(5) . . no C73 C74 1.385(7) . . no C73 H43 0.967(5) . . no C74 H44 0.971(5) . . no C76 H45 0.972(6) . . no C76 H45 0.972(6) . 3_556 no C78 H46 0.966(5) . . no C78 H47 0.967(5) . . no C81 H48 0.977(6) . . no C81 H49 0.963(7) . . no C84 H50 0.968(5) . . no C84 H51 0.960(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 MN1 O9 83.27(11) . . 8_557 no O9 MN1 O11 91.33(12) . . . no O9 MN1 O11 79.83(11) 8_557 . . no O9 MN1 O12 83.30(12) . . 8_557 no O9 MN1 O12 91.07(11) 8_557 . 8_557 no O9 MN1 O13 96.71(12) . . . no O9 MN1 O13 179.31(11) 8_557 . . no O9 MN1 O22 178.19(13) . . 8_557 no O9 MN1 O22 98.51(11) 8_557 . 8_557 no O11 MN1 O12 169.94(12) . . 8_557 no O11 MN1 O13 99.48(12) . . . no O11 MN1 O22 89.31(12) . . 8_557 no O12 MN1 O13 89.61(12) 8_557 . . no O12 MN1 O22 96.32(12) 8_557 . 8_557 no O13 MN1 O22 81.51(12) . . 8_557 no O9 MN2 O10 90.76(12) . . . no O9 MN2 O15 93.58(12) . . . no O9 MN2 O31 91.05(12) . . . no O9 MN2 O40 94.87(12) . . . no O9 MN2 O67 173.92(12) . . . no O10 MN2 O15 79.80(11) . . . no O10 MN2 O31 112.75(12) . . . no O10 MN2 O40 161.08(12) . . . no O10 MN2 O67 83.35(12) . . . no O15 MN2 O31 166.59(11) . . . no O15 MN2 O40 81.83(11) . . . no O15 MN2 O67 83.93(12) . . . no O31 MN2 O40 85.24(12) . . . no O31 MN2 O67 92.60(12) . . . no O40 MN2 O67 90.27(12) . . . no CL7 MN3 O9 157.06(8) . . 8_557 no CL7 MN3 O11 80.84(8) . . . no CL7 MN3 O12 84.25(9) . . . no CL7 MN3 O33 100.54(9) . . 8_557 no CL7 MN3 O42 94.85(9) . . 8_557 no O9 MN3 O11 85.95(11) 8_557 . . no O9 MN3 O12 78.41(11) 8_557 . . no O9 MN3 O33 98.09(11) 8_557 . 8_557 no O9 MN3 O42 99.52(12) 8_557 . 8_557 no O11 MN3 O12 95.50(12) . . . no O11 MN3 O33 89.90(12) . . 8_557 no O11 MN3 O42 173.84(12) . . 8_557 no O12 MN3 O33 173.31(12) . . 8_557 no O12 MN3 O42 88.40(12) . . 8_557 no O33 MN3 O42 86.55(12) 8_557 . 8_557 no CL7 MN4 O10 90.63(9) . . . no CL7 MN4 O11 80.46(9) . . . no CL7 MN4 O15 170.36(9) . . . no CL7 MN4 O49 95.44(9) . . . no CL7 MN4 N57 92.08(10) . . . no O10 MN4 O11 93.79(12) . . . no O10 MN4 O15 84.98(12) . . . no O10 MN4 O49 82.88(12) . . . no O10 MN4 N57 174.18(13) . . . no O11 MN4 O15 91.25(12) . . . no O11 MN4 O49 174.72(13) . . . no O11 MN4 N57 91.74(13) . . . no O15 MN4 O49 92.53(12) . . . no O15 MN4 N57 93.10(13) . . . no O49 MN4 N57 91.74(13) . . . no CL7 MN5 O10 86.67(9) . . . no CL7 MN5 O12 80.86(9) . . . no CL7 MN5 O24 171.16(9) . . . no CL7 MN5 O58 94.37(10) . . . no CL7 MN5 N66 89.11(10) . . . no O10 MN5 O12 92.30(12) . . . no O10 MN5 O24 100.02(12) . . . no O10 MN5 O58 83.88(12) . . . no O10 MN5 N66 173.67(13) . . . no O12 MN5 O24 93.03(12) . . . no O12 MN5 O58 174.08(13) . . . no O12 MN5 N66 91.68(13) . . . no O24 MN5 O58 92.09(12) . . . no O24 MN5 N66 84.67(13) . . . no O58 MN5 N66 91.75(13) . . . no CL8 MN6 O10 158.28(8) . . . no CL8 MN6 O49 92.07(8) . . . no CL8 MN6 O58 101.42(8) . . . no CL8 MN6 O67 123.88(8) . . . no CL8 MN6 N75 88.29(9) . . . no O10 MN6 O49 68.78(10) . . . no O10 MN6 O58 70.92(10) . . . no O10 MN6 O67 70.95(10) . . . no O10 MN6 N75 111.67(12) . . . no O49 MN6 O58 93.65(11) . . . no O49 MN6 O67 98.10(11) . . . no O49 MN6 N75 175.15(13) . . . no O58 MN6 O67 132.41(11) . . . no O58 MN6 N75 91.02(13) . . . no O67 MN6 N75 77.72(12) . . . no MN3 CL7 MN4 76.38(3) . . . no MN3 CL7 MN5 73.83(3) . . . no MN4 CL7 MN5 71.74(3) . . . no MN1 O9 MN1 96.73(11) 8_557 . . no MN1 O9 MN2 125.59(14) 8_557 . . no MN1 O9 MN2 123.56(15) . . . no MN1 O9 MN3 87.96(10) 8_557 . 8_557 no MN1 O9 MN3 96.13(11) . . 8_557 no MN2 O9 MN3 118.23(14) . . 8_557 no MN2 O10 MN4 105.59(13) . . . no MN2 O10 MN5 134.10(15) . . . no MN2 O10 MN6 99.35(12) . . . no MN4 O10 MN5 110.71(13) . . . no MN4 O10 MN6 102.27(12) . . . no MN5 O10 MN6 99.40(11) . . . no MN1 O11 MN3 106.03(13) . . . no MN1 O11 MN4 124.68(14) . . . no MN3 O11 MN4 117.54(14) . . . no MN1 O12 MN3 101.97(13) 8_557 . . no MN1 O12 MN5 128.32(15) 8_557 . . no MN3 O12 MN5 118.91(15) . . . no MN1 O13 C14 116.5(3) . . . no MN2 O15 MN4 86.44(11) . . . no MN2 O15 C14 112.0(3) . . . no MN4 O15 C14 134.9(3) . . . no MN1 O22 C23 133.2(3) 8_557 . . no MN5 O24 C23 131.6(3) . . . no MN2 O31 C32 134.6(3) . . . no MN3 O33 C32 129.8(3) 8_557 . . no MN2 O40 C41 138.2(3) . . . no MN3 O42 C41 128.1(3) 8_557 . . no MN4 O49 MN6 105.66(13) . . . no MN4 O49 C50 125.2(3) . . . no MN6 O49 C50 127.1(2) . . . no MN5 O58 MN6 104.77(12) . . . no MN5 O58 C59 128.0(3) . . . no MN6 O58 C59 127.0(3) . . . no MN2 O67 MN6 105.69(13) . . . no MN2 O67 C68 123.2(3) . . . no MN6 O67 C68 127.4(2) . . . no MN4 N57 C52 122.3(3) . . . no MN4 N57 C56 118.9(3) . . . no C52 N57 C56 118.9(4) . . . no MN5 N66 C61 123.0(3) . . . no MN5 N66 C65 117.0(3) . . . no C61 N66 C65 119.2(4) . . . no MN6 N75 C70 119.4(3) . . . no MN6 N75 C74 122.9(3) . . . no C70 N75 C74 117.7(4) . . . no O13 C14 O15 127.6(5) . . . no O13 C14 C16 116.4(4) . . . no O15 C14 C16 115.8(4) . . . no C14 C16 C17 119.8(4) . . . no C14 C16 C21 121.3(4) . . . no C17 C16 C21 118.9(4) . . . no C16 C17 C18 120.1(4) . . . no C16 C17 H1 119.6(5) . . . no C18 C17 H1 120.2(5) . . . no C17 C18 C19 118.9(4) . . . no C17 C18 H2 120.5(5) . . . no C19 C18 H2 120.6(5) . . . no C18 C19 C20 122.5(5) . . . no C18 C19 H3 118.6(6) . . . no C20 C19 H3 118.9(6) . . . no C19 C20 C21 117.6(5) . . . no C19 C20 H4 120.4(5) . . . no C21 C20 H4 122.0(5) . . . no C16 C21 C20 121.9(5) . . . no C16 C21 H5 118.5(5) . . . no C20 C21 H5 119.5(5) . . . no O22 C23 O24 125.7(4) . . . no O22 C23 C25 116.1(4) . . . no O24 C23 C25 118.2(4) . . . no C23 C25 C26 121.2(4) . . . no C23 C25 C30 120.2(4) . . . no C26 C25 C30 118.5(4) . . . no C25 C26 C27 120.3(4) . . . no C25 C26 H6 119.6(5) . . . no C27 C26 H6 120.1(5) . . . no C26 C27 C28 120.0(5) . . . no C26 C27 H7 120.8(5) . . . no C28 C27 H7 119.2(5) . . . no C27 C28 C29 120.3(5) . . . no C27 C28 H8 119.5(5) . . . no C29 C28 H8 120.1(5) . . . no C28 C29 C30 119.9(5) . . . no C28 C29 H9 119.5(5) . . . no C30 C29 H9 120.6(5) . . . no C25 C30 C29 120.8(5) . . . no C25 C30 H10 119.1(5) . . . no C29 C30 H10 120.1(5) . . . no O31 C32 O33 126.3(4) . . . no O31 C32 C34 117.3(4) . . . no O33 C32 C34 116.4(4) . . . no C32 C34 C35 118.8(4) . . . no C32 C34 C39 121.2(4) . . . no C35 C34 C39 119.9(4) . . . no C34 C35 C36 120.3(4) . . . no C34 C35 H11 119.6(4) . . . no C36 C35 H11 120.0(5) . . . no C35 C36 C37 119.8(4) . . . no C35 C36 H12 120.1(5) . . . no C37 C36 H12 120.1(5) . . . no C36 C37 C38 120.2(4) . . . no C36 C37 H13 119.4(5) . . . no C38 C37 H13 120.4(5) . . . no C37 C38 C39 119.8(4) . . . no C37 C38 H14 119.5(5) . . . no C39 C38 H14 120.7(5) . . . no C34 C39 C38 119.9(4) . . . no C34 C39 H15 120.0(4) . . . no C38 C39 H15 120.1(5) . . . no O40 C41 O42 125.9(4) . . . no O40 C41 C43 117.4(4) . . . no O42 C41 C43 116.7(4) . . . no C41 C43 C44 119.5(4) . . . no C41 C43 C48 121.0(4) . . . no C44 C43 C48 119.5(4) . . . no C43 C44 C45 120.2(4) . . . no C43 C44 H16 118.7(4) . . . no C45 C44 H16 121.0(5) . . . no C44 C45 C46 119.9(4) . . . no C44 C45 H17 119.3(5) . . . no C46 C45 H17 120.7(5) . . . no C45 C46 C47 120.5(4) . . . no C45 C46 H18 120.9(5) . . . no C47 C46 H18 118.6(5) . . . no C46 C47 C48 119.7(4) . . . no C46 C47 H19 121.0(5) . . . no C48 C47 H19 119.3(5) . . . no C43 C48 C47 120.1(4) . . . no C43 C48 H20 120.2(5) . . . no C47 C48 H20 119.7(5) . . . no O49 C50 C51 112.7(3) . . . no O49 C50 H21 109.5(4) . . . no O49 C50 H22 109.9(4) . . . no C51 C50 H21 108.2(4) . . . no C51 C50 H22 108.8(4) . . . no H21 C50 H22 107.7(4) . . . no C50 C51 C52 113.1(4) . . . no C50 C51 H23 109.4(4) . . . no C50 C51 H24 108.2(4) . . . no C52 C51 H23 108.6(4) . . . no C52 C51 H24 108.9(4) . . . no H23 C51 H24 108.4(4) . . . no N57 C52 C51 118.0(4) . . . no N57 C52 C53 120.6(4) . . . no C51 C52 C53 121.4(4) . . . no C52 C53 C54 120.3(4) . . . no C52 C53 H25 119.4(5) . . . no C54 C53 H25 120.3(5) . . . no C53 C54 C55 118.8(5) . . . no C53 C54 H26 120.8(5) . . . no C55 C54 H26 120.4(5) . . . no C54 C55 C56 118.9(4) . . . no C54 C55 H27 121.4(5) . . . no C56 C55 H27 119.7(5) . . . no N57 C56 C55 122.5(4) . . . no N57 C56 H28 119.0(4) . . . no C55 C56 H28 118.5(4) . . . no O58 C59 C60 112.3(4) . . . no O58 C59 H29 109.3(4) . . . no O58 C59 H30 109.2(4) . . . no C60 C59 H29 109.5(5) . . . no C60 C59 H30 108.3(4) . . . no H29 C59 H30 108.1(5) . . . no C59 C60 C61 112.3(4) . . . no C59 C60 H31 108.5(4) . . . no C59 C60 H32 109.7(4) . . . no C61 C60 H31 109.3(4) . . . no C61 C60 H32 109.3(4) . . . no H31 C60 H32 107.5(5) . . . no N66 C61 C60 117.4(4) . . . no N66 C61 C62 120.0(4) . . . no C60 C61 C62 122.6(4) . . . no C61 C62 C63 120.9(4) . . . no C61 C62 H33 119.4(5) . . . no C63 C62 H33 119.6(5) . . . no C62 C63 C64 118.0(4) . . . no C62 C63 H34 121.5(5) . . . no C64 C63 H34 120.4(5) . . . no C63 C64 C65 119.8(5) . . . no C63 C64 H35 120.4(5) . . . no C65 C64 H35 119.8(5) . . . no N66 C65 C64 122.0(4) . . . no N66 C65 H36 119.1(4) . . . no C64 C65 H36 118.9(5) . . . no O67 C68 C69 109.7(4) . . . no O67 C68 H37 109.8(4) . . . no O67 C68 H38 108.7(4) . . . no C69 C68 H37 110.4(4) . . . no C69 C68 H38 109.7(4) . . . no H37 C68 H38 108.5(4) . . . no C68 C69 C70 112.3(4) . . . no C68 C69 H39 109.1(4) . . . no C68 C69 H40 110.2(4) . . . no C70 C69 H39 108.0(4) . . . no C70 C69 H40 109.4(4) . . . no H39 C69 H40 107.8(4) . . . no N75 C70 C69 116.8(4) . . . no N75 C70 C71 121.6(5) . . . no C69 C70 C71 121.6(4) . . . no C70 C71 C72 119.3(5) . . . no C70 C71 H41 119.0(5) . . . no C72 C71 H41 121.7(5) . . . no C71 C72 C73 119.7(5) . . . no C71 C72 H42 118.7(6) . . . no C73 C72 H42 121.7(6) . . . no C72 C73 C74 117.3(5) . . . no C72 C73 H43 120.6(5) . . . no C74 C73 H43 122.1(5) . . . no N75 C74 C73 124.4(5) . . . no N75 C74 H44 117.7(5) . . . no C73 C74 H44 117.9(5) . . . no CL77 C76 CL77 113.3(5) . . 3_556 no CL77 C76 CL77 113.3(5) 3_556 . . no CL77 C76 H45 109.42(10) . . 3_556 no CL77 C76 H45 109.42(10) 3_556 . . no CL77 C76 H45 109.31(9) . . . no CL77 C76 H45 109.31(9) 3_556 . 3_556 no CL77 C76 H45 109.31(9) . . . no CL77 C76 H45 109.31(9) 3_556 . 3_556 no H45 C76 H45 105.8(9) . . 3_556 no H45 C76 H45 105.8(9) 3_556 . . no CL79 C78 CL80 111.5(3) . . . no CL79 C78 H46 110.1(4) . . . no CL79 C78 H47 110.0(4) . . . no CL80 C78 H46 109.1(4) . . . no CL80 C78 H47 109.3(4) . . . no H46 C78 H47 106.8(4) . . . no CL82 C81 CL83 109.8(3) . . . no CL82 C81 H48 110.5(5) . . . no CL82 C81 H49 111.0(6) . . . no CL83 C81 H48 109.2(6) . . . no CL83 C81 H49 110.0(5) . . . no H48 C81 H49 106.2(6) . . . no CL85 C84 CL86 112.5(3) . . . no CL85 C84 H50 109.0(4) . . . no CL85 C84 H51 109.4(5) . . . no CL86 C84 H50 109.1(5) . . . no CL86 C84 H51 109.6(4) . . . no H50 C84 H51 107.1(5) . . . no data_MSC99079 _database_code_CSD 154916 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C104 H104 Cl12 Mn12 N6 O32' _chemical_formula_moiety 'C92 H76 Cl4 Mn12 N6 O30, 4(C H2 Cl2), 2(C4 H10 O)' _chemical_formula_weight 3034.68 _cell_length_a 14.2602(12) _cell_length_b 14.8241(12) _cell_length_c 15.7931(14) _cell_angle_alpha 94.558(2) _cell_angle_beta 92.773(2) _cell_angle_gamma 114.916(2) _cell_volume 3005.9(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 5116 _cell_measurement_theta_min 5.731 _cell_measurement_theta_max 55.207 _cell_measurement_temperature 113 _exptl_crystal_colour brown _exptl_crystal_description 'rectangular plate' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1530 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.5972 _exptl_absorpt_correction_T_max 0.7860 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _diffrn_ambient_temperature 113 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '3-circle diffractometer with fixed chi of 54.75 degrees' _diffrn_measurement_type 'Bruker' _diffrn_measurement_method 'phi and omega scans' _diffrn_measurement_details ; 0.3 degree frames were measured with a counting time of 30.1 seconds each. ; _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_detector_details ; The detector was operated in 4x4 "binning" mode. ; _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_reflns_number 28667 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_measured_fraction_theta_max 0.97 _diffrn_reflns_theta_full 27.725 _diffrn_measured_fraction_theta_full 0.97 _diffrn_reflns_theta_min 2.109 _diffrn_reflns_theta_max 27.725 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _reflns_number_total 13844 _reflns_number_gt 9258 _reflns_threshold_expression I>2.0\s(I) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.295 0.729 'International Tables Vol. IV (1974) Table 2.2B' Cl Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 9578 _refine_ls_number_parameters 743 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.00000018(5) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.0698 _refine_ls_goodness_of_fit_ref 1.5743 _refine_ls_shift/su_max 0.0059 _refine_diff_density_max 1.79 _refine_diff_density_min -1.65 _refine_special_details ;In the final cycles of full matrix refinement the non-hydrogen atoms were refined using anisotropic thermal parameters, with the exception of C(83) and C(84), the half weight atoms in the one arm of the diethyl ether, which remained isotropic. The hydrogen atoms were fixed. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT and XTEL, local package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly Mn1 Mn 0.58477(5) -0.03669(5) 0.86628(5) 0.0142(2) Uani 1 0 . Mn2 Mn 0.48240(5) -0.25691(5) 0.96943(5) 0.0144(2) Uani 1 0 . Mn3 Mn 0.42082(5) 0.02513(5) 0.94290(5) 0.0134(2) Uani 1 0 . Mn4 Mn 0.70739(5) 0.19083(5) 0.96348(5) 0.0139(2) Uani 1 0 . Mn5 Mn 0.33590(5) -0.19916(5) 0.84298(5) 0.0140(2) Uani 1 0 . Mn6 Mn 0.23479(5) -0.41382(5) 0.92456(5) 0.0163(3) Uani 1 0 . Cl7 Cl 0.22286(8) -0.11155(8) 0.90136(8) 0.0185(4) Uani 1 0 . Cl8 Cl 0.17698(10) -0.56081(8) 0.81656(9) 0.0267(4) Uani 1 0 . O9 O 0.5742(2) -0.1234(2) 0.9731(2) 0.0141(11) Uani 1 0 . O10 O 0.3582(2) -0.2368(2) 0.9531(2) 0.0138(11) Uani 1 0 . O11 O 0.5956(2) 0.0575(2) 0.9612(2) 0.0141(11) Uani 1 0 . O12 O 0.4412(2) -0.0684(2) 0.8606(2) 0.0141(11) Uani 1 0 . O13 O 0.6111(3) 0.0676(2) 0.7712(2) 0.0216(13) Uani 1 0 . C14 C 0.6212(3) 0.1568(3) 0.7779(3) 0.0187(17) Uani 1 0 . O15 O 0.6491(2) 0.2154(2) 0.8476(2) 0.0204(13) Uani 1 0 . C16 C 0.5974(4) 0.1964(4) 0.6987(4) 0.025(2) Uani 1 0 . C17 C 0.6128(5) 0.2970(5) 0.7031(4) 0.040(3) Uani 1 0 . C18 C 0.5871(7) 0.3326(6) 0.6313(6) 0.065(4) Uani 1 0 . C19 C 0.5470(6) 0.2702(7) 0.5551(5) 0.064(4) Uani 1 0 . C20 C 0.5328(6) 0.1694(6) 0.5522(5) 0.058(3) Uani 1 0 . C21 C 0.5588(5) 0.1345(5) 0.6226(4) 0.039(2) Uani 1 0 . O22 O 0.5773(3) -0.1335(2) 0.7707(2) 0.0240(13) Uani 1 0 . C23 C 0.5158(4) -0.2266(3) 0.7630(3) 0.0173(16) Uani 1 0 . O24 O 0.4406(2) -0.2686(2) 0.8032(2) 0.0223(13) Uani 1 0 . C25 C 0.5474(4) -0.2905(3) 0.6993(3) 0.0223(18) Uani 1 0 . C26 C 0.4786(4) -0.3928(4) 0.6777(4) 0.029(2) Uani 1 0 . C27 C 0.5063(5) -0.4520(4) 0.6219(4) 0.039(2) Uani 1 0 . C28 C 0.6020(5) -0.4116(4) 0.5863(4) 0.042(2) Uani 1 0 . C29 C 0.6697(5) -0.3114(5) 0.6085(4) 0.041(2) Uani 1 0 . C30 C 0.6425(4) -0.2503(4) 0.6637(4) 0.029(2) Uani 1 0 . O31 O 0.4648(2) 0.2618(2) 0.9046(2) 0.0191(12) Uani 1 0 . C32 C 0.4170(3) 0.1897(3) 0.8482(3) 0.0175(17) Uani 1 0 . O33 O 0.4102(2) 0.0999(2) 0.8501(2) 0.0175(12) Uani 1 0 . C34 C 0.3615(4) 0.2053(3) 0.7710(3) 0.0198(17) Uani 1 0 . C35 C 0.3557(4) 0.2960(3) 0.7667(4) 0.0239(18) Uani 1 0 . C36 C 0.3042(4) 0.3120(4) 0.6965(4) 0.032(2) Uani 1 0 . C37 C 0.2585(5) 0.2365(5) 0.6298(4) 0.043(3) Uani 1 0 . C38 C 0.2642(6) 0.1461(5) 0.6343(5) 0.057(3) Uani 1 0 . C39 C 0.3146(5) 0.1296(4) 0.7047(4) 0.038(2) Uani 1 0 . O40 O 0.7344(2) -0.0100(2) 0.8775(2) 0.0191(12) Uani 1 0 . C41 C 0.8135(4) 0.0741(3) 0.8876(3) 0.0189(17) Uani 1 0 . O42 O 0.8106(2) 0.1581(2) 0.9045(2) 0.0193(12) Uani 1 0 . C43 C 0.9178(4) 0.0745(3) 0.8784(4) 0.0224(18) Uani 1 0 . C44 C 1.0019(4) 0.1605(4) 0.8632(4) 0.0259(19) Uani 1 0 . C45 C 1.0987(4) 0.1609(4) 0.8553(4) 0.031(2) Uani 1 0 . C46 C 1.1123(4) 0.0740(4) 0.8647(5) 0.041(3) Uani 1 0 . C47 C 1.0287(5) -0.0104(5) 0.8815(6) 0.058(4) Uani 1 0 . C48 C 0.9321(5) -0.0113(4) 0.8870(6) 0.051(3) Uani 1 0 . N49 N 0.5845(3) -0.3093(3) 0.9213(3) 0.0171(14) Uani 1 0 . C50 C 0.6838(4) -0.2536(3) 0.9064(4) 0.0221(18) Uani 1 0 . C51 C 0.7418(4) -0.2957(4) 0.8688(4) 0.029(2) Uani 1 0 . C52 C 0.7003(4) -0.3985(4) 0.8474(4) 0.035(2) Uani 1 0 . C53 C 0.5999(4) -0.4558(4) 0.8629(4) 0.030(2) Uani 1 0 . C54 C 0.5419(4) -0.4095(3) 0.8991(3) 0.0187(17) Uani 1 0 . C55 C 0.4289(4) -0.4627(3) 0.9134(4) 0.0261(19) Uani 1 0 . O56 O 0.3912(2) -0.3972(2) 0.9523(2) 0.0171(12) Uani 1 0 . N57 N 0.3025(3) -0.1899(3) 0.7191(3) 0.0187(14) Uani 1 0 . C58 C 0.3454(4) -0.1084(4) 0.6760(4) 0.029(2) Uani 1 0 . C59 C 0.3154(5) -0.1113(4) 0.5917(4) 0.034(2) Uani 1 0 . C60 C 0.2388(5) -0.2002(5) 0.5490(4) 0.044(3) Uani 1 0 . C61 C 0.1948(4) -0.2834(4) 0.5928(4) 0.034(2) Uani 1 0 . C62 C 0.2285(4) -0.2766(4) 0.6790(4) 0.0277(19) Uani 1 0 . C63 C 0.1885(4) -0.3613(4) 0.7327(4) 0.0257(19) Uani 1 0 . O64 O 0.2233(2) -0.3275(2) 0.8195(2) 0.0188(12) Uani 1 0 . N65 N 0.1414(3) -0.5185(3) 1.0177(3) 0.0197(15) Uani 1 0 . C66 C 0.1129(4) -0.6190(3) 1.0090(4) 0.0230(18) Uani 1 0 . C67 C 0.0408(4) -0.6836(3) 1.0577(4) 0.025(2) Uani 1 0 . C68 C -0.0042(4) -0.6451(4) 1.1175(4) 0.0207(18) Uani 1 0 . C69 C 0.0260(4) -0.5422(3) 1.1279(4) 0.0206(18) Uani 1 0 . C70 C 0.0985(3) -0.4817(3) 1.0767(3) 0.0182(17) Uani 1 0 . C71 C 0.1294(4) -0.3700(3) 1.0855(3) 0.0210(17) Uani 1 0 . O72 O 0.1923(2) -0.3260(2) 1.0195(2) 0.0189(12) Uani 1 0 . C73 C 0.7955(6) 0.0506(6) 0.6730(5) 0.061(3) Uani 1 0 . Cl74 Cl 0.86153(18) 0.18233(17) 0.67393(15) 0.0724(10) Uani 1 0 . Cl75 Cl 0.7473(2) -0.01276(18) 0.57245(15) 0.0896(12) Uani 1 0 . C76 C 0.0882(6) -0.6286(6) 0.5877(6) 0.070(3) Uani 1 0 . Cl77 Cl -0.00451(17) -0.58230(15) 0.59374(15) 0.0775(9) Uani 1 0 . Cl78 Cl 0.21110(18) -0.54101(16) 0.56342(14) 0.0738(10) Uani 1 0 . C79 C 0.1029(9) -0.6109(9) 1.3445(7) 0.102(6) Uani 1 0 . C80 C 0.0441(7) -0.7312(8) 1.3172(6) 0.075(5) Uani 1 0 . O81 O 0.0434(6) -0.7713(6) 1.3957(5) 0.117(4) Uani 1 0 . C82 C -0.0149(11) -0.8810(11) 1.3844(9) 0.113(4) Uiso 1 0 . C83 C 0.0090(19) -0.9113(18) 1.4544(16) 0.099(7) Uiso 0.5 0 . C84 C 0.0285(15) -0.9304(15) 1.3563(13) 0.076(5) Uiso 0.5 0 . H1 H 0.6419 0.3405 0.7562 0.0497 Uiso 1 0 . H2 H 0.5997 0.4025 0.6342 0.0709 Uiso 1 0 . H3 H 0.529 0.294 0.5033 0.0715 Uiso 1 0 . H4 H 0.5049 0.1253 0.4999 0.0629 Uiso 1 0 . H5 H 0.5498 0.0668 0.6211 0.0464 Uiso 1 0 . H6 H 0.4136 -0.4204 0.7035 0.0386 Uiso 1 0 . H7 H 0.4595 -0.5212 0.6053 0.0444 Uiso 1 0 . H8 H 0.6228 -0.4521 0.5484 0.0477 Uiso 1 0 . H9 H 0.7372 -0.2827 0.5861 0.0456 Uiso 1 0 . H10 H 0.6877 -0.1814 0.6778 0.0384 Uiso 1 0 . H11 H 0.3878 0.3482 0.8137 0.0344 Uiso 1 0 . H12 H 0.2993 0.3747 0.6947 0.0407 Uiso 1 0 . H13 H 0.2238 0.2478 0.5805 0.047 Uiso 1 0 . H14 H 0.2325 0.0936 0.5878 0.0548 Uiso 1 0 . H15 H 0.3177 0.0664 0.708 0.0418 Uiso 1 0 . H16 H 0.9938 0.2206 0.859 0.0351 Uiso 1 0 . H17 H 1.1562 0.2212 0.8435 0.0404 Uiso 1 0 . H18 H 1.1801 0.0753 0.8609 0.0465 Uiso 1 0 . H19 H 1.0386 -0.07 0.8892 0.0615 Uiso 1 0 . H20 H 0.8723 -0.0734 0.896 0.0529 Uiso 1 0 . H21 H 0.7131 -0.1829 0.9222 0.0323 Uiso 1 0 . H22 H 0.8123 -0.2549 0.8569 0.0381 Uiso 1 0 . H23 H 0.7403 -0.429 0.8209 0.0386 Uiso 1 0 . H24 H 0.5707 -0.5274 0.8505 0.0344 Uiso 1 0 . H25 H 0.4193 -0.5147 0.9492 0.0318 Uiso 1 0 . H26 H 0.3891 -0.4932 0.86 0.0318 Uiso 1 0 . H27 H 0.398 -0.0472 0.705 0.0365 Uiso 1 0 . H28 H 0.3462 -0.0523 0.5615 0.0456 Uiso 1 0 . H29 H 0.2165 -0.2053 0.489 0.051 Uiso 1 0 . H30 H 0.1428 -0.3441 0.5649 0.0427 Uiso 1 0 . H31 H 0.1153 -0.3903 0.7265 0.0356 Uiso 1 0 . H32 H 0.2127 -0.4097 0.7142 0.0356 Uiso 1 0 . H33 H 0.143 -0.6467 0.9676 0.0335 Uiso 1 0 . H34 H 0.0226 -0.7535 1.0499 0.033 Uiso 1 0 . H35 H -0.0538 -0.6885 1.1518 0.0332 Uiso 1 0 . H36 H -0.0039 -0.5132 1.1685 0.0315 Uiso 1 0 . H37 H 0.0689 -0.3583 1.0826 0.0298 Uiso 1 0 . H38 H 0.1677 -0.341 1.1398 0.0298 Uiso 1 0 . H39 H 0.7369 0.0342 0.7071 0.0643 Uiso 1 0 . H40 H 0.8402 0.0247 0.6975 0.0643 Uiso 1 0 . H41 H 0.0652 -0.6854 0.5463 0.065 Uiso 1 0 . H42 H 0.0989 -0.6505 0.6426 0.065 Uiso 1 0 . H43 H 0.1724 -0.5932 1.3687 0.1025 Uiso 1 0 . H44 H 0.0671 -0.5905 1.3845 0.1025 Uiso 1 0 . H45 H 0.1087 -0.5746 1.2954 0.1025 Uiso 1 0 . H46 H 0.0803 -0.7527 1.2757 0.0773 Uiso 1 0 . H47 H -0.025 -0.7499 1.2911 0.0773 Uiso 1 0 . H48 H 0.0003 -0.9133 1.3361 0.1295 Uiso 0.5 0 . H49 H -0.091 -0.9009 1.3766 0.1295 Uiso 0.5 0 . H50 H -0.0786 -0.9 1.3458 0.1295 Uiso 0.5 0 . H51 H -0.0395 -0.906 1.4376 0.1295 Uiso 0.5 0 . H52 H -0.0317 -0.9841 1.4525 0.1051 Uiso 0.5 0 . H53 H -0.0143 -0.8828 1.5018 0.1051 Uiso 0.5 0 . H54 H 0.0773 -0.8947 1.4614 0.1051 Uiso 0.5 0 . H55 H -0.0102 -0.9978 1.3486 0.0832 Uiso 0.5 0 . H56 H 0.0915 -0.912 1.3923 0.0832 Uiso 0.5 0 . H57 H 0.0518 -0.9067 1.3005 0.0832 Uiso 0.5 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn1 0.0072(4) 0.0054(3) 0.0248(12) 0.0011(2) 0.0013(3) -0.0027(3) Mn2 0.0072(4) 0.0038(3) 0.0271(13) 0.0007(2) -0.0004(3) -0.0027(3) Mn3 0.0082(4) 0.0044(3) 0.0229(11) 0.0011(2) -0.0008(3) -0.0020(3) Mn4 0.0072(4) 0.0040(3) 0.0257(12) 0.0000(2) 0.0017(3) -0.0023(3) Mn5 0.0076(4) 0.0054(3) 0.0230(11) -0.0002(2) -0.0009(3) -0.0030(3) Mn6 0.0093(4) 0.0064(4) 0.0270(13) 0.0005(3) 0.0003(3) -0.0025(3) Cl7 0.0084(5) 0.0108(6) 0.0308(15) 0.0032(4) -0.0001(5) -0.0017(5) Cl8 0.0245(9) 0.0109(6) 0.0320(16) 0.0050(5) -0.0033(5) -0.0057(5) O9 0.0082(15) 0.0062(14) 0.023(2) 0.0006(12) 0.0007(13) -0.0019(13) O10 0.0073(14) 0.0063(14) 0.023(2) 0.0017(11) 0.0001(13) -0.0023(13) O11 0.0070(14) 0.0064(14) 0.025(2) 0.0010(12) 0.0007(13) -0.0006(13) O12 0.0072(14) 0.0076(14) 0.023(2) 0.0016(12) 0.0012(13) -0.0017(13) O13 0.0153(17) 0.0116(16) 0.032(3) 0.0047(13) 0.0026(15) -0.0012(15) C14 0.006(2) 0.016(2) 0.032(3) 0.0021(17) 0.006(2) 0.003(2) O15 0.0140(17) 0.0119(16) 0.032(3) 0.0058(13) 0.0003(15) 0.0020(15) C16 0.014(2) 0.025(3) 0.037(4) 0.010(2) 0.008(2) 0.008(2) C17 0.041(4) 0.034(3) 0.043(4) 0.022(3) 0.007(3) 0.014(3) C18 0.073(6) 0.059(5) 0.075(7) 0.045(5) 0.021(5) 0.039(5) C19 0.058(5) 0.085(7) 0.050(6) 0.043(5) 0.010(4) 0.029(5) C20 0.044(4) 0.073(6) 0.039(5) 0.026(4) 0.002(3) 0.005(4) C21 0.032(3) 0.045(4) 0.030(4) 0.019(3) 0.003(3) 0.005(3) O22 0.0173(18) 0.0099(16) 0.037(3) 0.0033(13) 0.0055(16) -0.0023(15) C23 0.015(2) 0.008(2) 0.020(3) -0.0019(17) -0.0074(19) -0.0025(18) O24 0.0128(17) 0.0154(17) 0.031(3) 0.0065(13) 0.0010(15) -0.0033(15) C25 0.021(2) 0.015(2) 0.023(3) 0.0092(19) 0.001(2) -0.002(2) C26 0.026(3) 0.020(3) 0.030(4) 0.005(2) 0.005(2) -0.001(2) C27 0.040(4) 0.015(3) 0.046(4) 0.012(2) 0.004(3) -0.006(3) C28 0.051(4) 0.023(3) 0.035(4) 0.021(3) 0.008(3) -0.005(3) C29 0.039(4) 0.035(3) 0.038(4) 0.020(3) 0.013(3) 0.001(3) C30 0.028(3) 0.018(3) 0.034(4) 0.008(2) 0.006(2) 0.002(2) O31 0.0134(16) 0.0069(15) 0.029(2) 0.0010(12) -0.0007(14) -0.0040(14) C32 0.010(2) 0.012(2) 0.027(3) 0.0037(17) 0.0060(19) 0.002(2) O33 0.0138(16) 0.0081(15) 0.025(2) 0.0042(12) 0.0001(14) -0.0015(14) C34 0.013(2) 0.013(2) 0.028(3) 0.0049(18) 0.002(2) -0.001(2) C35 0.022(3) 0.012(2) 0.031(3) 0.0059(19) 0.001(2) -0.001(2) C36 0.034(3) 0.018(3) 0.041(4) 0.013(2) 0.009(3) 0.007(2) C37 0.041(4) 0.044(4) 0.033(4) 0.027(3) -0.002(3) 0.003(3) C38 0.054(4) 0.040(4) 0.043(5) 0.029(3) -0.013(3) -0.018(3) C39 0.038(3) 0.025(3) 0.031(4) 0.018(2) -0.011(3) -0.008(2) O40 0.0098(15) 0.0071(15) 0.035(3) 0.0013(12) 0.0048(14) -0.0016(14) C41 0.012(2) 0.013(2) 0.027(3) 0.0041(18) 0.003(2) 0.001(2) O42 0.0111(16) 0.0087(15) 0.034(3) 0.0039(12) 0.0050(14) -0.0011(14) C43 0.009(2) 0.012(2) 0.043(4) 0.0038(18) 0.007(2) 0.001(2) C44 0.015(2) 0.015(2) 0.045(4) 0.0061(19) 0.007(2) 0.002(2) C45 0.016(3) 0.022(3) 0.055(5) 0.005(2) 0.013(3) 0.007(3) C46 0.018(3) 0.028(3) 0.080(6) 0.012(2) 0.019(3) 0.012(3) C47 0.028(3) 0.027(3) 0.146(11) 0.019(3) 0.032(4) 0.039(4) C48 0.020(3) 0.019(3) 0.132(10) 0.008(2) 0.028(4) 0.027(4) N49 0.0137(19) 0.0094(18) 0.024(3) 0.0051(15) 0.0001(17) 0.0005(16) C50 0.010(2) 0.012(2) 0.041(4) 0.0017(18) 0.003(2) 0.002(2) C51 0.014(2) 0.019(3) 0.052(5) 0.007(2) 0.007(2) 0.006(3) C52 0.025(3) 0.025(3) 0.043(4) 0.018(2) 0.003(2) -0.005(3) C53 0.018(3) 0.013(2) 0.046(4) 0.008(2) 0.001(2) -0.007(2) C54 0.016(2) 0.010(2) 0.023(3) 0.0045(18) -0.001(2) -0.0011(19) C55 0.014(2) 0.009(2) 0.045(4) 0.0054(18) -0.003(2) -0.005(2) O56 0.0107(15) 0.0050(14) 0.030(2) 0.0010(12) 0.0007(14) -0.0024(14) N57 0.015(2) 0.0094(18) 0.023(3) 0.0033(15) -0.0014(17) -0.0039(16) C58 0.028(3) 0.015(2) 0.032(4) 0.006(2) 0.000(2) -0.004(2) C59 0.037(3) 0.023(3) 0.033(4) 0.006(2) -0.006(3) 0.004(2) C60 0.051(4) 0.035(4) 0.025(4) 0.009(3) -0.012(3) -0.002(3) C61 0.029(3) 0.019(3) 0.041(4) 0.003(2) -0.010(3) -0.003(2) C62 0.019(3) 0.016(2) 0.035(4) 0.006(2) -0.004(2) -0.006(2) C63 0.021(3) 0.014(2) 0.032(4) 0.001(2) -0.005(2) -0.001(2) O64 0.0103(15) 0.0083(15) 0.028(2) -0.0003(12) -0.0032(14) -0.0055(14) N65 0.013(2) 0.0097(19) 0.031(3) 0.0024(15) 0.0003(18) -0.0002(17) C66 0.019(2) 0.012(2) 0.034(4) 0.0064(19) 0.003(2) 0.002(2) C67 0.019(3) 0.008(2) 0.047(4) 0.0010(19) -0.003(2) 0.006(2) C68 0.013(2) 0.013(2) 0.035(4) -0.0029(18) 0.004(2) 0.007(2) C69 0.014(2) 0.012(2) 0.033(3) 0.0022(18) 0.004(2) 0.003(2) C70 0.008(2) 0.009(2) 0.032(3) 0.0004(17) -0.0066(19) -0.001(2) C71 0.012(2) 0.012(2) 0.030(3) 0.0012(18) 0.003(2) -0.004(2) O72 0.0127(16) 0.0063(15) 0.031(3) -0.0003(12) 0.0054(14) -0.0023(14) C73 0.064(5) 0.063(5) 0.046(5) 0.038(4) 0.013(4) 0.010(4) Cl74 0.067(2) 0.070(2) 0.064(3) 0.0175(11) -0.0078(11) 0.0139(11) Cl75 0.122(4) 0.067(2) 0.050(3) 0.0378(15) -0.0049(13) 0.0085(11) C76 0.046(4) 0.045(4) 0.079(7) 0.016(3) -0.004(4) -0.026(4) Cl77 0.060(2) 0.054(2) 0.081(4) 0.0249(10) -0.0259(11) -0.0158(11) Cl78 0.071(2) 0.067(2) 0.063(3) 0.0342(11) 0.0131(11) 0.0039(11) C79 0.107(9) 0.109(10) 0.075(8) 0.059(7) 0.016(6) 0.024(6) C80 0.062(6) 0.120(9) 0.055(6) 0.054(6) 0.009(4) 0.048(6) O81 0.105(7) 0.100(7) 0.119(9) 0.051(5) 0.011(5) 0.009(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O9 2.175(3) . . no Mn1 O11 1.920(3) . . no Mn1 O12 1.894(3) . . no Mn1 O13 2.172(4) . . no Mn1 O22 1.965(4) . . no Mn1 O40 1.996(3) . . no Mn2 O9 1.851(3) . . no Mn2 O10 1.924(3) . . no Mn2 O31 2.110(4) . 2_657 no Mn2 O56 1.920(3) . . no Mn2 N49 2.066(4) . . no Mn3 Cl7 2.7010(12) . . no Mn3 O9 1.867(3) . 2_657 no Mn3 O11 1.984(3) . 2_657 no Mn3 O11 2.329(3) . . no Mn3 O12 1.945(3) . . no Mn3 O33 1.943(3) . . no Mn4 Cl7 2.8470(15) . 2_657 no Mn4 Cl7 2.8470(15) . 2_657 no Mn4 O10 1.895(3) . 2_657 no Mn4 O11 1.944(3) . . no Mn4 O15 2.095(4) . . no Mn4 O42 1.984(3) . . no Mn4 O72 1.896(3) . 2_657 no Mn5 Cl7 2.6178(13) . . no Mn5 O10 1.920(3) . . no Mn5 O12 1.874(3) . . no Mn5 O24 2.229(3) . . no Mn5 O64 1.895(3) . . no Mn5 N57 2.019(4) . . no Mn6 Cl8 2.4692(14) . . no Mn6 O10 2.455(3) . . no Mn6 O56 2.156(3) . . no Mn6 O64 2.215(4) . . no Mn6 O72 2.180(3) . . no Mn6 N65 2.271(4) . . no Cl74 C73 1.773(8) . . no Cl75 C73 1.730(8) . . no Cl77 C76 1.731(8) . . no Cl78 C76 1.769(8) . . no O13 C14 1.263(6) . . no O15 C14 1.281(6) . . no O22 C23 1.278(5) . . no O24 C23 1.227(6) . . no O31 C32 1.256(6) . . no O33 C32 1.296(5) . . no O40 C41 1.272(5) . . no O42 C41 1.270(5) . . no O56 C55 1.410(6) . . no O64 C63 1.412(6) . . no O72 C71 1.423(6) . . no O81 C80 1.415(10) . . no O81 C82 1.473(14) . . no N49 C50 1.349(6) . . no N49 C54 1.354(6) . . no N57 C58 1.359(7) . . no N57 C62 1.353(6) . . no N65 C66 1.362(6) . . no N65 C70 1.341(6) . . no C14 C16 1.506(8) . . no C16 C17 1.408(8) . . no C16 C21 1.388(8) . . no C17 C18 1.384(10) . . no C17 H1 0.972(7) . . no C18 C19 1.393(12) . . no C18 H2 0.972(8) . . no C19 C20 1.416(11) . . no C19 H3 0.980(8) . . no C20 C21 1.363(9) . . no C20 H4 0.965(7) . . no C21 H5 0.954(6) . . no C23 C25 1.539(7) . . no C25 C26 1.417(7) . . no C25 C30 1.398(7) . . no C26 C27 1.380(8) . . no C26 H6 0.968(5) . . no C27 C28 1.406(9) . . no C27 H7 0.965(5) . . no C28 C29 1.393(8) . . no C28 H8 0.958(5) . . no C29 C30 1.391(8) . . no C29 H9 0.971(6) . . no C30 H10 0.951(5) . . no C32 C34 1.507(7) . . no C34 C35 1.389(7) . . no C34 C39 1.384(7) . . no C35 C36 1.391(8) . . no C35 H11 0.967(5) . . no C36 C37 1.384(8) . . no C36 H12 0.964(5) . . no C37 C38 1.384(9) . . no C37 H13 0.966(6) . . no C38 C39 1.389(9) . . no C38 H14 0.964(6) . . no C39 H15 0.962(5) . . no C41 C43 1.500(6) . . no C43 C44 1.382(6) . . no C43 C48 1.386(7) . . no C44 C45 1.390(7) . . no C44 H16 0.953(5) . . no C45 C46 1.398(8) . . no C45 H17 0.964(5) . . no C46 C47 1.373(8) . . no C46 H18 0.964(5) . . no C47 C48 1.377(8) . . no C47 H19 0.968(6) . . no C48 H20 0.983(6) . . no C50 C51 1.360(7) . . no C50 H21 0.957(5) . . no C51 C52 1.389(7) . . no C51 H22 0.967(5) . . no C52 C53 1.369(7) . . no C52 H23 0.956(5) . . no C53 C54 1.393(7) . . no C53 H24 0.963(5) . . no C54 C55 1.504(6) . . no C55 H25 0.960(5) . . no C55 H26 0.957(5) . . no C58 C59 1.371(8) . . no C58 H27 0.960(5) . . no C59 C60 1.399(8) . . no C59 H28 0.973(6) . . no C60 C61 1.386(9) . . no C60 H29 0.972(6) . . no C61 C62 1.402(8) . . no C61 H30 0.947(5) . . no C62 C63 1.495(8) . . no C63 H31 0.944(5) . . no C63 H32 0.950(5) . . no C66 C67 1.389(7) . . no C66 H33 0.956(5) . . no C67 C68 1.382(8) . . no C67 H34 0.952(5) . . no C68 C69 1.392(7) . . no C68 H35 0.958(5) . . no C69 C70 1.393(7) . . no C69 H36 0.957(5) . . no C70 C71 1.515(6) . . no C70 C71 1.515(6) . . no C71 H37 0.949(5) . . no C71 H38 0.959(5) . . no C73 H39 0.970(8) . . no C73 H40 0.954(8) . . no C76 H41 0.949(7) . . no C76 H42 0.976(9) . . no C79 C80 1.629(15) . . no C79 H43 0.962(11) . . no C79 H44 0.940(11) . . no C79 H45 0.966(10) . . no C80 H46 0.967(9) . . no C80 H47 0.965(8) . . no C82 C83 1.31(2) . . no C82 C84 1.21(2) . . no C82 H48 0.952(14) . . no C82 H49 0.996(14) . . no C82 H50 0.990(14) . . no C82 H51 0.967(14) . . no C83 C84 1.61(3) . . no C83 H51 0.77(2) . . no C83 H52 0.98(2) . . no C83 H53 0.97(2) . . no C83 H54 0.90(2) . . no C84 H48 0.64(2) . . no C84 H55 0.91(2) . . no C84 H56 0.96(2) . . no C84 H57 0.99(2) . . no H48 H57 0.92263(6) . . no H49 H50 0.52469(4) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Mn1 O11 78.29(13) . . . no O9 Mn1 O12 92.21(13) . . . no O9 Mn1 O13 172.00(12) . . . no O9 Mn1 O22 100.80(14) . . . no O9 Mn1 O40 84.14(13) . . . no O11 Mn1 O12 84.57(13) . . . no O11 Mn1 O13 95.35(13) . . . no O11 Mn1 O22 178.33(14) . . . no O11 Mn1 O40 95.34(13) . . . no O12 Mn1 O13 91.99(13) . . . no O12 Mn1 O22 96.89(14) . . . no O12 Mn1 O40 176.29(14) . . . no O13 Mn1 O22 85.44(14) . . . no O13 Mn1 O40 91.72(13) . . . no O22 Mn1 O40 83.16(14) . . . no O9 Mn2 O10 95.99(13) . . . no O9 Mn2 O31 91.01(13) . . 2_657 no O9 Mn2 O56 173.34(15) . . . no O9 Mn2 N49 94.41(14) . . . no O10 Mn2 O31 117.69(14) . . 2_657 no O10 Mn2 O56 85.47(13) . . . no O10 Mn2 N49 149.36(16) . . . no O31 Mn2 O56 94.06(14) 2_657 . . no O31 Mn2 N49 90.80(15) 2_657 . . no O56 Mn2 N49 81.22(14) . . . no Cl7 Mn3 O9 110.38(10) . . 2_657 no Cl7 Mn3 O11 80.64(9) . . 2_657 no Cl7 Mn3 O11 147.56(8) . . . no Cl7 Mn3 O12 79.13(9) . . . no Cl7 Mn3 O33 90.55(10) . . . no O9 Mn3 O11 84.57(14) 2_657 . 2_657 no O9 Mn3 O11 97.00(12) 2_657 . . no O9 Mn3 O12 170.15(13) 2_657 . . no O9 Mn3 O33 93.32(14) 2_657 . . no O11 Mn3 O11 85.14(12) 2_657 . . no O11 Mn3 O12 94.78(13) 2_657 . . no O11 Mn3 O12 73.16(12) . . . no O11 Mn3 O33 169.55(13) 2_657 . . no O11 Mn3 O33 105.30(13) . . . no O12 Mn3 O33 89.02(14) . . . no Cl7 Mn4 O10 86.04(10) 2_657 . 2_657 no Cl7 Mn4 O11 77.51(10) 2_657 . . no Cl7 Mn4 O15 165.97(9) 2_657 . . no Cl7 Mn4 O42 81.18(11) 2_657 . . no Cl7 Mn4 O72 100.28(12) 2_657 . 2_657 no O10 Mn4 O11 88.68(13) 2_657 . . no O10 Mn4 O15 104.16(14) 2_657 . . no O10 Mn4 O42 162.53(14) 2_657 . . no O10 Mn4 O72 82.66(13) 2_657 . 2_657 no O11 Mn4 O15 92.90(13) . . . no O11 Mn4 O42 100.04(13) . . . no O11 Mn4 O72 171.21(14) . . 2_657 no O15 Mn4 O42 90.59(14) . . . no O15 Mn4 O72 90.70(14) . . 2_657 no O42 Mn4 O72 87.93(13) . . 2_657 no Cl7 Mn5 O10 92.35(10) . . . no Cl7 Mn5 O12 82.57(10) . . . no Cl7 Mn5 O24 175.28(10) . . . no Cl7 Mn5 O64 94.83(10) . . . no Cl7 Mn5 N57 94.83(12) . . . no O10 Mn5 O12 96.62(14) . . . no O10 Mn5 O24 84.00(13) . . . no O10 Mn5 O64 87.31(14) . . . no O10 Mn5 N57 168.11(14) . . . no O12 Mn5 O24 94.85(13) . . . no O12 Mn5 O64 175.36(15) . . . no O12 Mn5 N57 93.69(15) . . . no O24 Mn5 O64 88.00(13) . . . no O24 Mn5 N57 89.26(15) . . . no O64 Mn5 N57 82.67(15) . . . no Cl8 Mn6 O10 142.53(9) . . . no Cl8 Mn6 O56 97.33(9) . . . no Cl8 Mn6 O64 87.10(9) . . . no Cl8 Mn6 O72 147.77(9) . . . no Cl8 Mn6 N65 87.92(11) . . . no O10 Mn6 O56 68.55(11) . . . no O10 Mn6 O64 68.42(11) . . . no O10 Mn6 O72 65.07(11) . . . no O10 Mn6 N65 128.61(13) . . . no O56 Mn6 O64 112.00(12) . . . no O56 Mn6 O72 111.95(13) . . . no O56 Mn6 N65 104.41(14) . . . no O64 Mn6 O72 93.82(13) . . . no O64 Mn6 N65 143.59(14) . . . no O72 Mn6 N65 72.41(13) . . . no Mn3 Cl7 Mn4 76.69(4) . . 2_657 no Mn3 Cl7 Mn5 75.47(4) . . . no Mn4 Cl7 Mn5 70.27(4) 2_657 . . no Mn1 O9 Mn2 122.69(16) . . . no Mn1 O9 Mn3 96.06(13) . . 2_657 no Mn2 O9 Mn3 123.20(17) . . 2_657 no Mn2 O10 Mn4 127.68(18) . . 2_657 no Mn2 O10 Mn5 114.56(16) . . . no Mn2 O10 Mn6 97.44(12) . . . no Mn4 O10 Mn5 111.33(15) 2_657 . . no Mn4 O10 Mn6 100.81(13) 2_657 . . no Mn5 O10 Mn6 96.79(13) . . . no Mn1 O11 Mn3 100.96(14) . . 2_657 no Mn1 O11 Mn3 93.61(12) . . . no Mn1 O11 Mn4 116.03(16) . . . no Mn3 O11 Mn3 94.86(12) 2_657 . . no Mn3 O11 Mn4 122.51(17) 2_657 . . no Mn3 O11 Mn4 122.95(14) . . . no Mn1 O12 Mn3 108.20(15) . . . no Mn1 O12 Mn5 123.93(16) . . . no Mn3 O12 Mn5 116.95(16) . . . no Mn1 O13 C14 130.7(3) . . . no Mn4 O15 C14 126.9(3) . . . no Mn1 O22 C23 124.5(3) . . . no Mn5 O24 C23 123.0(3) . . . no Mn2 O31 C32 127.9(3) 2_657 . . no Mn3 O33 C32 132.8(3) . . . no Mn1 O40 C41 128.2(3) . . . no Mn4 O42 C41 129.7(3) . . . no Mn2 O56 Mn6 108.46(14) . . . no Mn2 O56 C55 118.0(3) . . . no Mn6 O56 C55 122.9(3) . . . no Mn5 O64 Mn6 106.15(15) . . . no Mn5 O64 C63 116.3(3) . . . no Mn6 O64 C63 129.0(3) . . . no Mn4 O72 Mn6 111.45(15) 2_657 . . no Mn4 O72 C71 120.6(3) 2_657 . . no Mn6 O72 C71 122.1(3) . . . no C80 O81 C82 110.8(9) . . . no Mn2 N49 C50 126.6(3) . . . no Mn2 N49 C54 114.0(3) . . . no C50 N49 C54 119.3(4) . . . no Mn5 N57 C58 127.0(3) . . . no Mn5 N57 C62 112.9(4) . . . no C58 N57 C62 120.1(5) . . . no Mn6 N65 C66 123.9(4) . . . no Mn6 N65 C70 117.3(3) . . . no C66 N65 C70 117.9(4) . . . no O13 C14 O15 124.5(5) . . . no O13 C14 C16 117.8(5) . . . no O15 C14 C16 117.7(4) . . . no C14 C16 C17 119.2(5) . . . no C14 C16 C21 120.7(5) . . . no C17 C16 C21 120.1(6) . . . no C16 C17 C18 119.3(7) . . . no C16 C17 H1 119.6(6) . . . no C18 C17 H1 121.1(6) . . . no C17 C18 C19 120.7(7) . . . no C17 C18 H2 119.0(9) . . . no C19 C18 H2 120.3(8) . . . no C18 C19 C20 118.9(7) . . . no C18 C19 H3 122.1(9) . . . no C20 C19 H3 119.0(9) . . . no C19 C20 C21 120.5(7) . . . no C19 C20 H4 119.9(8) . . . no C21 C20 H4 119.7(8) . . . no C16 C21 C20 120.5(6) . . . no C16 C21 H5 118.6(6) . . . no C20 C21 H5 121.0(7) . . . no O22 C23 O24 127.4(5) . . . no O22 C23 C25 113.6(4) . . . no O24 C23 C25 118.8(4) . . . no C23 C25 C26 118.7(4) . . . no C23 C25 C30 121.5(4) . . . no C26 C25 C30 119.9(5) . . . no C25 C26 C27 119.6(5) . . . no C25 C26 H6 119.4(5) . . . no C27 C26 H6 121.0(5) . . . no C26 C27 C28 120.5(5) . . . no C26 C27 H7 120.7(6) . . . no C28 C27 H7 118.8(6) . . . no C27 C28 C29 119.6(5) . . . no C27 C28 H8 121.5(6) . . . no C29 C28 H8 118.9(6) . . . no C28 C29 C30 120.6(5) . . . no C28 C29 H9 120.8(6) . . . no C30 C29 H9 118.6(6) . . . no C25 C30 C29 119.8(5) . . . no C25 C30 H10 119.3(5) . . . no C29 C30 H10 120.9(6) . . . no O31 C32 O33 125.3(5) . . . no O31 C32 C34 119.3(4) . . . no O33 C32 C34 115.4(4) . . . no C32 C34 C35 119.8(4) . . . no C32 C34 C39 120.8(4) . . . no C35 C34 C39 119.4(5) . . . no C34 C35 C36 120.9(5) . . . no C34 C35 H11 118.8(5) . . . no C36 C35 H11 120.3(5) . . . no C35 C36 C37 119.6(5) . . . no C35 C36 H12 120.2(6) . . . no C37 C36 H12 120.2(6) . . . no C36 C37 C38 119.5(6) . . . no C36 C37 H13 119.8(6) . . . no C38 C37 H13 120.8(6) . . . no C37 C38 C39 121.1(6) . . . no C37 C38 H14 119.5(7) . . . no C39 C38 H14 119.4(6) . . . no C34 C39 C38 119.6(5) . . . no C34 C39 H15 119.5(5) . . . no C38 C39 H15 120.9(5) . . . no O40 C41 O42 124.8(4) . . . no O40 C41 C43 117.7(4) . . . no O42 C41 C43 117.4(4) . . . no C41 C43 C44 120.9(4) . . . no C41 C43 C48 120.4(4) . . . no C44 C43 C48 118.7(5) . . . no C43 C44 C45 120.9(5) . . . no C43 C44 H16 119.6(5) . . . no C45 C44 H16 119.5(5) . . . no C44 C45 C46 119.8(5) . . . no C44 C45 H17 119.7(5) . . . no C46 C45 H17 120.4(5) . . . no C45 C46 C47 118.8(5) . . . no C45 C46 H18 119.5(5) . . . no C47 C46 H18 121.7(6) . . . no C46 C47 C48 121.2(6) . . . no C46 C47 H19 118.6(6) . . . no C48 C47 H19 120.1(6) . . . no C43 C48 C47 120.6(5) . . . no C43 C48 H20 119.2(6) . . . no C47 C48 H20 120.2(6) . . . no N49 C50 C51 121.5(4) . . . no N49 C50 H21 118.7(5) . . . no C51 C50 H21 119.8(5) . . . no C50 C51 C52 120.0(5) . . . no C50 C51 H22 120.9(5) . . . no C52 C51 H22 119.1(5) . . . no C51 C52 C53 118.9(5) . . . no C51 C52 H23 120.8(5) . . . no C53 C52 H23 120.3(5) . . . no C52 C53 C54 119.4(4) . . . no C52 C53 H24 120.0(5) . . . no C54 C53 H24 120.7(5) . . . no N49 C54 C53 120.9(4) . . . no N49 C54 C55 114.5(4) . . . no C53 C54 C55 124.5(4) . . . no O56 C55 C54 112.0(4) . . . no O56 C55 H25 108.8(5) . . . no O56 C55 H26 109.0(4) . . . no C54 C55 H25 109.5(4) . . . no C54 C55 H26 109.5(5) . . . no H25 C55 H26 107.9(4) . . . no N57 C58 C59 121.5(5) . . . no N57 C58 H27 119.6(6) . . . no C59 C58 H27 118.9(5) . . . no C58 C59 C60 119.3(5) . . . no C58 C59 H28 120.8(5) . . . no C60 C59 H28 119.9(6) . . . no C59 C60 C61 119.4(6) . . . no C59 C60 H29 121.5(6) . . . no C61 C60 H29 119.1(6) . . . no C60 C61 C62 119.1(5) . . . no C60 C61 H30 120.4(6) . . . no C62 C61 H30 120.5(6) . . . no N57 C62 C61 120.6(5) . . . no N57 C62 C63 115.2(5) . . . no C61 C62 C63 124.2(5) . . . no O64 C63 C62 110.9(4) . . . no O64 C63 H31 109.0(5) . . . no O64 C63 H32 109.1(5) . . . no C62 C63 H31 108.8(5) . . . no C62 C63 H32 109.0(5) . . . no H31 C63 H32 109.9(5) . . . no N65 C66 C67 122.5(5) . . . no N65 C66 H33 119.1(5) . . . no C67 C66 H33 118.4(5) . . . no C66 C67 C68 119.2(4) . . . no C66 C67 H34 120.3(6) . . . no C68 C67 H34 120.5(5) . . . no C67 C68 C69 118.6(5) . . . no C67 C68 H35 120.3(5) . . . no C69 C68 H35 121.1(5) . . . no C68 C69 C70 119.3(5) . . . no C68 C69 H36 120.7(5) . . . no C70 C69 H36 119.9(5) . . . no N65 C70 C69 122.5(4) . . . no N65 C70 C71 117.7(4) . . . no C69 C70 C71 119.8(4) . . . no O72 C71 C70 109.9(4) . . . no O72 C71 H37 110.2(5) . . . no O72 C71 H38 109.5(4) . . . no C70 C71 H37 109.5(4) . . . no C70 C71 H38 108.9(5) . . . no H37 C71 H38 108.7(5) . . . no Cl74 C73 Cl75 114.0(4) . . . no Cl74 C73 H39 109.7(6) . . . no Cl74 C73 H40 110.6(6) . . . no Cl75 C73 H39 107.0(6) . . . no Cl75 C73 H40 107.9(6) . . . no H39 C73 H40 107.5(7) . . . no Cl77 C76 Cl78 114.4(5) . . . no Cl77 C76 H41 110.6(6) . . . no Cl77 C76 H42 109.2(6) . . . no Cl78 C76 H41 108.2(6) . . . no Cl78 C76 H42 106.9(6) . . . no H41 C76 H42 107.2(8) . . . no C80 C79 H43 109.6(9) . . . no C80 C79 H44 110.9(10) . . . no C80 C79 H45 110.9(10) . . . no H43 C79 H44 109.3(11) . . . no H43 C79 H45 107.1(11) . . . no H44 C79 H45 108.9(11) . . . no O81 C80 C79 103.1(8) . . . no O81 C80 H46 112.8(8) . . . no O81 C80 H47 112.3(8) . . . no C79 C80 H46 111.4(8) . . . no C79 C80 H47 110.7(9) . . . no H46 C80 H47 106.7(9) . . . no O81 C82 C83 105.4(15) . . . no O81 C82 C84 118.1(15) . . . no O81 C82 H48 114.5(12) . . . no O81 C82 H49 110.9(12) . . . no O81 C82 H50 109.5(12) . . . no O81 C82 H51 111.0(12) . . . no C83 C82 C84 79.4(16) . . . no C83 C82 H48 110.2(17) . . . no C83 C82 H49 110.5(16) . . . no C83 C82 H50 135.7(17) . . . no C83 C82 H51 35.5(12) . . . no C84 C82 H48 31.7(10) . . . no C84 C82 H49 125.1(17) . . . no C84 C82 H50 106.3(16) . . . no C84 C82 H51 106.2(16) . . . no H48 C82 H49 105.5(13) . . . no H48 C82 H50 79.1(10) . . . no H48 C82 H51 129.8(15) . . . no H49 C82 H50 30.6(4) . . . no H49 C82 H51 76.1(10) . . . no H50 C82 H51 104.8(13) . . . no C82 C83 C84 47.8(12) . . . no C82 C83 H51 47.1(15) . . . no C82 C83 H52 109(2) . . . no C82 C83 H53 108(2) . . . no C82 C83 H54 111(2) . . . no C84 C83 H51 87(2) . . . no C84 C83 H52 87.4(18) . . . no C84 C83 H53 156(2) . . . no C84 C83 H54 81.2(18) . . . no H51 C83 H52 90(2) . . . no H51 C83 H53 72.5(19) . . . no H51 C83 H54 155(3) . . . no H52 C83 H53 105(2) . . . no H52 C83 H54 111(2) . . . no H53 C83 H54 112(2) . . . no C82 C84 C83 52.9(13) . . . no C82 C84 H48 51.1(16) . . . no C82 C84 H55 116(2) . . . no C82 C84 H56 107.7(19) . . . no C82 C84 H57 106.6(19) . . . no C83 C84 H48 103(2) . . . no C83 C84 H55 97.9(17) . . . no C83 C84 H56 70.1(15) . . . no C83 C84 H57 152(2) . . . no H48 C84 H55 104(2) . . . no H48 C84 H56 144(3) . . . no H48 C84 H57 64.5(16) . . . no H55 C84 H56 112(2) . . . no H55 C84 H57 109(2) . . . no H56 C84 H57 104.9(18) . . . no C82 H48 C84 97.2(19) . . . no C82 H48 H57 142.6(8) . . . no C84 H48 H57 76.5(18) . . . no C82 H49 H50 74.1(8) . . . no C82 H50 H49 75.2(8) . . . no C82 H51 C83 97.3(19) . . . no C84 H57 H48 39.0(12) . . . no