# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address _publ_author_footnote ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; ; ? # Address 2 ; ; ? # Footnote 2 ; _publ_contact_author_address ; Department of Chemistry, Joseph Black Building, West Mains Road, University of Edinburgh, Edinburgh, EH9 3JJ, UK. ; _publ_contact_author_email komil@chemistry.uoc.gr _publ_contact_author_phone '+44 131 650 4806' #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_author_name 'Constantinos J. Milios' _publ_contact_letter ; ; _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; _publ_author_name C.Milios data_bk171ap _database_code_depnum_ccdc_archive 'CCDC 793021' #TrackingRef 'Complex_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H70 Mn6 N8 O18, 5.274(C2 H3 N)' _chemical_formula_sum 'C98.55 H85.82 Mn6 N13.27 O18' _chemical_formula_weight 2073.68 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 monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.608(6) _cell_length_b 19.100(9) _cell_length_c 16.182(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.07(4) _cell_angle_gamma 90.00 _cell_volume 4699(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 10933 _cell_measurement_theta_min 4.72 _cell_measurement_theta_max 27.23 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'Xcalibur PX KM4CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34378 _diffrn_reflns_av_R_equivalents 0.1646 _diffrn_reflns_av_sigmaI/netI 0.3176 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.70 _diffrn_reflns_theta_max 27.11 _reflns_number_total 10218 _reflns_number_gt 3645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.(2010)' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.(2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10218 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1705 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 0.652 _refine_ls_restrained_S_all 0.652 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.54384(4) 0.58553(3) 0.56172(4) 0.02062(17) Uani 1 1 d . . . Mn2 Mn 0.37207(4) 0.68354(3) 0.51843(4) 0.02268(17) Uani 1 1 d . . . Mn3 Mn 0.34553(4) 0.52370(3) 0.54737(4) 0.02245(17) Uani 1 1 d . . . O1 O 0.42150(16) 0.59401(11) 0.52307(16) 0.0201(7) Uani 1 1 d . . . O12 O 0.27012(18) 0.45325(12) 0.56324(18) 0.0251(8) Uani 1 1 d . . . O22 O 0.25700(17) 0.64699(12) 0.46704(17) 0.0242(7) Uani 1 1 d . . . N12 N 0.2444(2) 0.57588(16) 0.4780(2) 0.0219(9) Uani 1 1 d . . . C12 C 0.1987(3) 0.4318(2) 0.5064(3) 0.0254(11) Uani 1 1 d . . . C22 C 0.1446(3) 0.47809(19) 0.4482(3) 0.0224(10) Uani 1 1 d . . . C32 C 0.0682(3) 0.4512(2) 0.3939(3) 0.0255(11) Uani 1 1 d . . . H32 H 0.0303 0.4817 0.3558 0.031 Uiso 1 1 calc R . . C42 C 0.0476(3) 0.3801(2) 0.3958(3) 0.0278(12) Uani 1 1 d . . . H42 H -0.0043 0.3622 0.3595 0.033 Uiso 1 1 calc R . . C52 C 0.1041(3) 0.3357(2) 0.4515(3) 0.0316(13) Uani 1 1 d . . . H52 H 0.0906 0.2872 0.4517 0.038 Uiso 1 1 calc R . . C62 C 0.1779(3) 0.35999(19) 0.5055(3) 0.0288(12) Uani 1 1 d . . . H62 H 0.2153 0.3286 0.5426 0.035 Uiso 1 1 calc R . . C72 C 0.1668(3) 0.55182(19) 0.4402(3) 0.0215(11) Uani 1 1 d . . . C82 C 0.1039(3) 0.59968(19) 0.3846(3) 0.0186(10) Uani 1 1 d . . . C92 C 0.0315(3) 0.6264(2) 0.4089(3) 0.0316(12) Uani 1 1 d . . . H92 H 0.0211 0.6145 0.4628 0.038 Uiso 1 1 calc R . . C102 C -0.0270(3) 0.6711(2) 0.3549(3) 0.0353(13) Uani 1 1 d . . . H102 H -0.0760 0.6905 0.3725 0.042 Uiso 1 1 calc R . . C112 C -0.0128(3) 0.6862(2) 0.2771(3) 0.0317(12) Uani 1 1 d . . . H112 H -0.0527 0.7157 0.2396 0.038 Uiso 1 1 calc R . . C122 C 0.0589(3) 0.6590(2) 0.2524(3) 0.0314(12) Uani 1 1 d . . . H122 H 0.0683 0.6698 0.1978 0.038 Uiso 1 1 calc R . . C132 C 0.1171(3) 0.6164(2) 0.3057(3) 0.0259(11) Uani 1 1 d . . . H132 H 0.1668 0.5983 0.2881 0.031 Uiso 1 1 calc R . . O11 O 0.66418(17) 0.56341(12) 0.59331(18) 0.0222(7) Uani 1 1 d . . . O21 O 0.44532(17) 0.45984(12) 0.56404(17) 0.0212(7) Uani 1 1 d . . . N11 N 0.5221(2) 0.49101(14) 0.6093(2) 0.0186(8) Uani 1 1 d . . . C11 C 0.6990(3) 0.54002(19) 0.6727(3) 0.0178(10) Uani 1 1 d . . . C21 C 0.6593(3) 0.48351(19) 0.7095(3) 0.0176(10) Uani 1 1 d . . . C31 C 0.6992(3) 0.46301(19) 0.7915(3) 0.0219(11) Uani 1 1 d . . . H31 H 0.6724 0.4267 0.8170 0.026 Uiso 1 1 calc R . . C41 C 0.7746(3) 0.49226(19) 0.8374(3) 0.0253(11) Uani 1 1 d . . . H41 H 0.7999 0.4765 0.8932 0.030 Uiso 1 1 calc R . . C51 C 0.8139(3) 0.54564(19) 0.8008(3) 0.0254(11) Uani 1 1 d . . . H51 H 0.8666 0.5666 0.8317 0.031 Uiso 1 1 calc R . . C61 C 0.7764(3) 0.56828(19) 0.7196(3) 0.0238(11) Uani 1 1 d . . . H61 H 0.8047 0.6043 0.6952 0.029 Uiso 1 1 calc R . . C71 C 0.5760(3) 0.4528(2) 0.6643(3) 0.0207(11) Uani 1 1 d . . . C81 C 0.5560(3) 0.3776(2) 0.6812(3) 0.0220(11) Uani 1 1 d . . . C91 C 0.4752(3) 0.3577(2) 0.6950(3) 0.0374(13) Uani 1 1 d . . . H91 H 0.4302 0.3913 0.6946 0.045 Uiso 1 1 calc R . . C101 C 0.4617(4) 0.2871(2) 0.7096(3) 0.0436(14) Uani 1 1 d . . . H101 H 0.4071 0.2724 0.7204 0.052 Uiso 1 1 calc R . . C111 C 0.5257(4) 0.2385(2) 0.7088(3) 0.0500(15) Uani 1 1 d . . . H111 H 0.5150 0.1908 0.7194 0.060 Uiso 1 1 calc R . . C121 C 0.6041(4) 0.2573(2) 0.6931(3) 0.0468(15) Uani 1 1 d . . . H121 H 0.6478 0.2230 0.6915 0.056 Uiso 1 1 calc R . . C131 C 0.6198(3) 0.3280(2) 0.6793(3) 0.0274(11) Uani 1 1 d . . . H131 H 0.6748 0.3420 0.6687 0.033 Uiso 1 1 calc R . . O13 O 0.32511(18) 0.77172(12) 0.49195(17) 0.0288(8) Uani 1 1 d . . . O23 O 0.55913(16) 0.67652(12) 0.52103(16) 0.0215(7) Uani 1 1 d . . . N13 N 0.4937(2) 0.72336(16) 0.5271(2) 0.0228(9) Uani 1 1 d . . . C13 C 0.3632(3) 0.83319(18) 0.5186(3) 0.0229(11) Uani 1 1 d . . . C23 C 0.4550(3) 0.84409(19) 0.5339(3) 0.0194(11) Uani 1 1 d . . . C33 C 0.4868(3) 0.9118(2) 0.5593(2) 0.0268(11) Uani 1 1 d . . . H33 H 0.5482 0.9205 0.5690 0.032 Uiso 1 1 calc R . . C43 C 0.4320(3) 0.9652(2) 0.5705(3) 0.0314(12) Uani 1 1 d . . . H43 H 0.4554 1.0102 0.5875 0.038 Uiso 1 1 calc R . . C53 C 0.3425(3) 0.95357(19) 0.5569(3) 0.0291(12) Uani 1 1 d . . . H53 H 0.3043 0.9904 0.5648 0.035 Uiso 1 1 calc R . . C63 C 0.3089(3) 0.8885(2) 0.5320(3) 0.0273(12) Uani 1 1 d . . . H63 H 0.2474 0.8808 0.5235 0.033 Uiso 1 1 calc R . . C73 C 0.5174(3) 0.7896(2) 0.5279(3) 0.0210(11) Uani 1 1 d . . . C83 C 0.6103(3) 0.80608(18) 0.5276(3) 0.0194(11) Uani 1 1 d . . . C93 C 0.6813(3) 0.78341(18) 0.5918(3) 0.0235(11) Uani 1 1 d . . . H93 H 0.6702 0.7561 0.6373 0.028 Uiso 1 1 calc R . . C103 C 0.7664(3) 0.80012(18) 0.5899(3) 0.0262(11) Uani 1 1 d . . . H103 H 0.8132 0.7848 0.6345 0.031 Uiso 1 1 calc R . . C113 C 0.7850(3) 0.8389(2) 0.5238(3) 0.0302(12) Uani 1 1 d . . . H113 H 0.8442 0.8502 0.5232 0.036 Uiso 1 1 calc R . . C123 C 0.7173(3) 0.86101(19) 0.4592(3) 0.0280(12) Uani 1 1 d . . . H123 H 0.7295 0.8868 0.4130 0.034 Uiso 1 1 calc R . . C133 C 0.6301(3) 0.84541(18) 0.4616(3) 0.0223(11) Uani 1 1 d . . . H133 H 0.5836 0.8619 0.4174 0.027 Uiso 1 1 calc R . . O14 O 0.35744(17) 0.68117(14) 0.64335(17) 0.0272(7) Uani 1 1 d . A . O24 O 0.35197(18) 0.56532(13) 0.66804(18) 0.0279(8) Uani 1 1 d . A . C14 C 0.3572(3) 0.6294(2) 0.6921(3) 0.0296(12) Uani 1 1 d . . . C24 C 0.3612(3) 0.6436(2) 0.7848(3) 0.0371(13) Uani 0.637(4) 1 d P A 1 H24A H 0.4221 0.6556 0.8146 0.045 Uiso 0.637(4) 1 calc PR A 1 H24B H 0.3427 0.6016 0.8120 0.045 Uiso 0.637(4) 1 calc PR A 1 C34 C 0.2937(4) 0.7105(3) 0.7904(4) 0.034(2) Uani 0.637(4) 1 d P A 1 H34A H 0.2994 0.7238 0.8499 0.052 Uiso 0.637(4) 1 calc PR A 1 H34B H 0.2329 0.6965 0.7658 0.052 Uiso 0.637(4) 1 calc PR A 1 H34C H 0.3094 0.7505 0.7588 0.052 Uiso 0.637(4) 1 calc PR A 1 C240 C 0.3612(3) 0.6436(2) 0.7848(3) 0.0371(13) Uani 0.363(4) 1 d P A 2 H24C H 0.3021 0.6562 0.7929 0.045 Uiso 0.363(4) 1 calc PR A 2 H24D H 0.4016 0.6831 0.8049 0.045 Uiso 0.363(4) 1 calc PR A 2 C340 C 0.3993(8) 0.5675(6) 0.8425(8) 0.041(4) Uiso 0.363(4) 1 d P A 2 H34D H 0.4608 0.5591 0.8405 0.062 Uiso 0.363(4) 1 calc PR A 2 H34E H 0.3633 0.5274 0.8176 0.062 Uiso 0.363(4) 1 calc PR A 2 H34F H 0.3951 0.5734 0.9016 0.062 Uiso 0.363(4) 1 calc PR A 2 N4 N 0.3664(5) 0.4920(3) 0.9379(5) 0.074(3) Uani 0.637(4) 1 d P A 3 C7 C 0.4271(6) 0.4931(4) 0.9115(6) 0.056(3) Uani 0.637(4) 1 d P A 3 C8 C 0.5013(6) 0.4950(4) 0.8730(6) 0.089(4) Uani 0.637(4) 1 d P A 3 H8A H 0.4841 0.5169 0.8169 0.134 Uiso 0.637(4) 1 calc PR A 3 H8B H 0.5217 0.4471 0.8669 0.134 Uiso 0.637(4) 1 calc PR A 3 H8C H 0.5488 0.5222 0.9088 0.134 Uiso 0.637(4) 1 calc PR A 3 N1 N 0.5588(2) 0.63848(17) 0.6985(2) 0.0261(10) Uani 1 1 d . . . C1 C 0.5942(3) 0.6554(2) 0.7637(3) 0.0271(12) Uani 1 1 d . . . C2 C 0.6420(3) 0.6764(2) 0.8487(3) 0.0564(15) Uani 1 1 d . . . H2A H 0.6567 0.7263 0.8485 0.085 Uiso 1 1 calc R . . H2B H 0.6963 0.6489 0.8651 0.085 Uiso 1 1 calc R . . H2C H 0.6052 0.6681 0.8894 0.085 Uiso 1 1 calc R . . N2 N 0.0252(3) 0.8278(2) 0.5270(4) 0.0875(19) Uani 1 1 d . . . C3 C 0.0800(4) 0.7912(3) 0.5534(4) 0.0517(18) Uani 1 1 d . . . C4 C 0.1527(3) 0.7430(2) 0.5872(3) 0.0609(17) Uani 1 1 d . . . H4A H 0.1317 0.7054 0.6188 0.091 Uiso 1 1 calc R . . H4B H 0.2002 0.7686 0.6252 0.091 Uiso 1 1 calc R . . H4C H 0.1747 0.7229 0.5403 0.091 Uiso 1 1 calc R . . N3 N 0.1311(3) 0.5851(3) 0.7549(3) 0.0755(16) Uani 1 1 d . . . C5 C 0.1585(4) 0.5326(3) 0.7436(3) 0.0511(16) Uani 1 1 d . . . C6 C 0.1939(4) 0.4630(3) 0.7326(4) 0.078(2) Uani 1 1 d . . . H6A H 0.2270 0.4456 0.7875 0.117 Uiso 1 1 calc R . . H6B H 0.2330 0.4660 0.6931 0.117 Uiso 1 1 calc R . . H6C H 0.1454 0.4309 0.7098 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0221(4) 0.0121(3) 0.0249(4) 0.0000(3) -0.0003(3) -0.0013(3) Mn2 0.0239(4) 0.0134(3) 0.0276(5) -0.0011(3) -0.0009(4) 0.0007(3) Mn3 0.0229(4) 0.0158(3) 0.0267(4) -0.0003(3) 0.0016(4) -0.0010(3) O1 0.0244(17) 0.0075(13) 0.0265(18) -0.0007(13) 0.0017(15) -0.0015(13) O12 0.0218(18) 0.0192(15) 0.030(2) 0.0068(14) -0.0023(16) -0.0056(14) O22 0.0232(18) 0.0114(14) 0.034(2) 0.0045(14) -0.0012(16) -0.0034(13) N12 0.020(2) 0.019(2) 0.026(2) 0.0049(18) 0.0040(19) 0.0030(18) C12 0.026(3) 0.028(3) 0.024(3) -0.002(2) 0.010(3) -0.008(2) C22 0.023(3) 0.016(2) 0.026(3) 0.002(2) 0.002(2) 0.005(2) C32 0.019(3) 0.029(3) 0.027(3) -0.005(2) 0.001(2) -0.002(2) C42 0.023(3) 0.022(3) 0.035(3) -0.008(2) -0.001(3) -0.004(2) C52 0.035(3) 0.010(2) 0.052(4) 0.001(2) 0.013(3) -0.003(2) C62 0.030(3) 0.013(2) 0.041(3) 0.010(2) 0.003(3) -0.009(2) C72 0.018(3) 0.024(2) 0.021(3) -0.002(2) 0.000(2) 0.003(2) C82 0.012(3) 0.017(2) 0.023(3) -0.003(2) -0.004(2) -0.001(2) C92 0.035(3) 0.032(3) 0.028(3) 0.008(2) 0.009(3) -0.004(2) C102 0.031(3) 0.031(3) 0.046(4) 0.004(3) 0.012(3) 0.011(2) C112 0.030(3) 0.025(2) 0.036(3) 0.009(3) -0.003(3) -0.001(2) C122 0.034(3) 0.033(3) 0.024(3) -0.001(2) 0.000(3) -0.005(2) C132 0.022(3) 0.028(3) 0.026(3) -0.006(2) 0.003(3) 0.001(2) O11 0.0229(18) 0.0206(15) 0.021(2) -0.0009(14) 0.0006(16) -0.0034(13) O21 0.0149(16) 0.0221(15) 0.0237(19) 0.0004(14) -0.0018(15) -0.0049(13) N11 0.021(2) 0.0140(18) 0.019(2) -0.0049(17) -0.0003(19) -0.0018(16) C11 0.017(3) 0.023(2) 0.014(3) -0.005(2) 0.005(2) 0.005(2) C21 0.019(3) 0.014(2) 0.019(3) 0.002(2) 0.003(2) 0.005(2) C31 0.026(3) 0.016(2) 0.021(3) 0.001(2) 0.000(2) 0.003(2) C41 0.027(3) 0.016(2) 0.029(3) 0.000(2) -0.002(3) 0.008(2) C51 0.019(3) 0.024(2) 0.029(3) -0.012(2) -0.004(2) 0.001(2) C61 0.032(3) 0.011(2) 0.025(3) -0.004(2) 0.000(3) 0.004(2) C71 0.022(3) 0.023(2) 0.017(3) 0.000(2) 0.005(2) 0.001(2) C81 0.027(3) 0.020(2) 0.016(3) 0.003(2) -0.001(2) -0.007(2) C91 0.040(3) 0.039(3) 0.027(3) 0.011(3) -0.004(3) -0.002(3) C101 0.057(4) 0.039(3) 0.031(3) 0.013(3) 0.000(3) -0.031(3) C111 0.081(5) 0.026(3) 0.031(3) 0.004(3) -0.014(3) -0.016(3) C121 0.086(5) 0.020(3) 0.027(3) 0.006(2) -0.003(3) 0.005(3) C131 0.045(3) 0.016(2) 0.021(3) -0.006(2) 0.004(3) 0.000(2) O13 0.0313(19) 0.0097(14) 0.039(2) -0.0049(14) -0.0063(17) -0.0015(14) O23 0.0202(17) 0.0092(14) 0.034(2) 0.0002(14) 0.0031(15) 0.0001(13) N13 0.025(2) 0.021(2) 0.018(2) 0.0005(18) -0.0051(19) 0.0059(18) C13 0.034(3) 0.010(2) 0.022(3) 0.004(2) 0.001(2) 0.000(2) C23 0.022(3) 0.014(2) 0.021(3) 0.003(2) 0.002(2) -0.002(2) C33 0.024(3) 0.022(2) 0.032(3) -0.002(2) 0.000(2) 0.002(2) C43 0.038(3) 0.011(2) 0.045(3) -0.005(2) 0.009(3) -0.001(2) C53 0.042(3) 0.013(2) 0.031(3) 0.001(2) 0.004(3) -0.002(2) C63 0.031(3) 0.023(2) 0.025(3) 0.002(2) 0.000(2) 0.003(2) C73 0.030(3) 0.015(2) 0.016(3) 0.003(2) 0.003(2) 0.001(2) C83 0.030(3) 0.004(2) 0.022(3) -0.006(2) 0.003(2) -0.001(2) C93 0.028(3) 0.015(2) 0.026(3) -0.003(2) 0.003(3) -0.003(2) C103 0.029(3) 0.016(2) 0.029(3) -0.007(2) -0.002(3) 0.001(2) C113 0.032(3) 0.018(2) 0.041(4) -0.009(2) 0.008(3) 0.001(2) C123 0.034(3) 0.013(2) 0.037(3) 0.005(2) 0.010(3) -0.004(2) C133 0.024(3) 0.017(2) 0.024(3) -0.007(2) 0.001(2) -0.001(2) O14 0.0287(19) 0.0199(15) 0.032(2) -0.0050(16) 0.0048(17) -0.0036(15) O24 0.0335(19) 0.0223(16) 0.027(2) -0.0017(15) 0.0049(17) -0.0041(15) C14 0.015(3) 0.038(3) 0.035(3) -0.001(3) 0.004(3) -0.005(2) C24 0.049(4) 0.043(3) 0.024(3) -0.017(3) 0.018(3) -0.016(3) C34 0.044(5) 0.032(4) 0.029(5) -0.010(4) 0.014(4) 0.008(4) C240 0.049(4) 0.043(3) 0.024(3) -0.017(3) 0.018(3) -0.016(3) N4 0.032(5) 0.064(5) 0.119(8) 0.016(5) 0.003(5) 0.006(4) C7 0.033(6) 0.039(5) 0.092(9) 0.012(5) 0.003(6) 0.004(5) C8 0.059(7) 0.081(7) 0.140(10) 0.023(7) 0.049(7) 0.011(6) N1 0.025(2) 0.023(2) 0.028(3) 0.001(2) 0.001(2) 0.0010(18) C1 0.022(3) 0.026(3) 0.031(3) 0.002(2) 0.002(3) 0.012(2) C2 0.063(4) 0.053(3) 0.040(4) -0.007(3) -0.015(3) 0.023(3) N2 0.062(4) 0.056(3) 0.143(6) -0.010(4) 0.018(4) 0.008(3) C3 0.045(4) 0.035(3) 0.083(5) -0.009(3) 0.031(4) -0.007(3) C4 0.056(4) 0.045(3) 0.091(5) -0.015(3) 0.034(4) -0.011(3) N3 0.067(4) 0.085(4) 0.058(4) 0.002(3) -0.020(3) 0.015(3) C5 0.039(4) 0.069(4) 0.041(4) -0.006(4) -0.001(3) -0.019(4) C6 0.104(5) 0.056(4) 0.087(5) -0.018(4) 0.049(5) -0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.877(3) . ? Mn1 O11 1.880(3) . ? Mn1 O23 1.893(2) . ? Mn1 N11 2.021(3) . ? Mn1 O21 2.253(3) 3_666 ? Mn1 N1 2.397(4) . ? Mn1 Mn2 3.2146(14) . ? Mn2 O13 1.848(2) . ? Mn2 O1 1.871(2) . ? Mn2 O22 1.931(3) . ? Mn2 N13 2.020(3) . ? Mn2 O14 2.086(3) . ? Mn2 Mn3 3.1303(16) . ? Mn3 O12 1.844(3) . ? Mn3 O1 1.891(2) . ? Mn3 O21 1.948(3) . ? Mn3 N12 1.986(3) . ? Mn3 O24 2.090(3) . ? O12 C12 1.339(5) . ? O22 N12 1.390(3) . ? N12 C72 1.310(5) . ? C12 C62 1.408(5) . ? C12 C22 1.422(6) . ? C22 C32 1.408(6) . ? C22 C72 1.463(5) . ? C32 C42 1.398(5) . ? C32 H32 0.9500 . ? C42 C52 1.396(5) . ? C42 H42 0.9500 . ? C52 C62 1.360(6) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C72 C82 1.486(5) . ? C82 C92 1.376(5) . ? C82 C132 1.377(5) . ? C92 C102 1.402(6) . ? C92 H92 0.9500 . ? C102 C112 1.359(5) . ? C102 H102 0.9500 . ? C112 C122 1.373(5) . ? C112 H112 0.9500 . ? C122 C132 1.369(5) . ? C122 H122 0.9500 . ? C132 H132 0.9500 . ? O11 C11 1.353(5) . ? O21 N11 1.389(4) . ? O21 Mn1 2.253(3) 3_666 ? N11 C71 1.302(5) . ? C11 C61 1.383(5) . ? C11 C21 1.439(5) . ? C21 C31 1.390(5) . ? C21 C71 1.462(5) . ? C31 C41 1.361(5) . ? C31 H31 0.9500 . ? C41 C51 1.389(5) . ? C41 H41 0.9500 . ? C51 C61 1.382(5) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C71 C81 1.509(5) . ? C81 C131 1.380(5) . ? C81 C91 1.382(5) . ? C91 C101 1.394(5) . ? C91 H91 0.9500 . ? C101 C111 1.365(6) . ? C101 H101 0.9500 . ? C111 C121 1.352(6) . ? C111 H111 0.9500 . ? C121 C131 1.400(5) . ? C121 H121 0.9500 . ? C131 H131 0.9500 . ? O13 C13 1.343(4) . ? O23 N13 1.378(3) . ? N13 C73 1.317(4) . ? C13 C63 1.401(4) . ? C13 C23 1.413(5) . ? C23 C33 1.412(5) . ? C23 C73 1.444(5) . ? C33 C43 1.370(5) . ? C33 H33 0.9500 . ? C43 C53 1.382(6) . ? C43 H43 0.9500 . ? C53 C63 1.374(5) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C73 C83 1.485(5) . ? C83 C133 1.396(5) . ? C83 C93 1.404(5) . ? C93 C103 1.374(5) . ? C93 H93 0.9500 . ? C103 C113 1.385(5) . ? C103 H103 0.9500 . ? C113 C123 1.374(6) . ? C113 H113 0.9500 . ? C123 C133 1.402(5) . ? C123 H123 0.9500 . ? C133 H133 0.9500 . ? O14 C14 1.265(4) . ? O24 C14 1.281(4) . ? C14 C24 1.512(6) . ? C24 C34 1.671(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C340 H34D 0.9800 . ? C340 H34E 0.9800 . ? C340 H34F 0.9800 . ? N4 C7 1.125(8) . ? C7 C8 1.433(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N1 C1 1.122(5) . ? C1 C2 1.465(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N2 C3 1.112(6) . ? C3 C4 1.467(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N3 C5 1.123(6) . ? C5 C6 1.465(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O11 171.35(11) . . ? O1 Mn1 O23 90.21(11) . . ? O11 Mn1 O23 95.98(11) . . ? O1 Mn1 N11 87.61(12) . . ? O11 Mn1 N11 86.51(12) . . ? O23 Mn1 N11 176.34(12) . . ? O1 Mn1 O21 90.61(11) . 3_666 ? O11 Mn1 O21 83.38(11) . 3_666 ? O23 Mn1 O21 89.88(10) . 3_666 ? N11 Mn1 O21 93.09(10) . 3_666 ? O1 Mn1 N1 98.67(12) . . ? O11 Mn1 N1 87.76(13) . . ? O23 Mn1 N1 86.57(11) . . ? N11 Mn1 N1 90.85(12) . . ? O21 Mn1 N1 170.06(11) 3_666 . ? O1 Mn1 Mn2 30.87(7) . . ? O11 Mn1 Mn2 157.36(8) . . ? O23 Mn1 Mn2 63.51(8) . . ? N11 Mn1 Mn2 113.56(10) . . ? O21 Mn1 Mn2 104.86(8) 3_666 . ? N1 Mn1 Mn2 81.83(9) . . ? O13 Mn2 O1 168.76(12) . . ? O13 Mn2 O22 87.03(12) . . ? O1 Mn2 O22 91.25(11) . . ? O13 Mn2 N13 89.44(12) . . ? O1 Mn2 N13 88.21(12) . . ? O22 Mn2 N13 159.06(12) . . ? O13 Mn2 O14 96.89(12) . . ? O1 Mn2 O14 94.35(11) . . ? O22 Mn2 O14 96.57(11) . . ? N13 Mn2 O14 104.35(13) . . ? O13 Mn2 Mn3 149.83(9) . . ? O1 Mn2 Mn3 33.87(7) . . ? O22 Mn2 Mn3 64.54(7) . . ? N13 Mn2 Mn3 120.71(9) . . ? O14 Mn2 Mn3 77.68(7) . . ? O13 Mn2 Mn1 148.08(9) . . ? O1 Mn2 Mn1 30.99(8) . . ? O22 Mn2 Mn1 122.13(8) . . ? N13 Mn2 Mn1 58.65(9) . . ? O14 Mn2 Mn1 92.57(8) . . ? Mn3 Mn2 Mn1 62.06(3) . . ? O12 Mn3 O1 176.00(13) . . ? O12 Mn3 O21 92.26(11) . . ? O1 Mn3 O21 87.37(11) . . ? O12 Mn3 N12 89.65(13) . . ? O1 Mn3 N12 88.97(12) . . ? O21 Mn3 N12 154.28(12) . . ? O12 Mn3 O24 92.56(12) . . ? O1 Mn3 O24 91.39(11) . . ? O21 Mn3 O24 103.93(12) . . ? N12 Mn3 O24 101.60(12) . . ? O12 Mn3 Mn2 147.45(8) . . ? O1 Mn3 Mn2 33.46(7) . . ? O21 Mn3 Mn2 120.17(8) . . ? N12 Mn3 Mn2 62.70(10) . . ? O24 Mn3 Mn2 77.81(7) . . ? Mn2 O1 Mn1 118.13(12) . . ? Mn2 O1 Mn3 112.66(12) . . ? Mn1 O1 Mn3 120.53(13) . . ? C12 O12 Mn3 125.9(3) . . ? N12 O22 Mn2 116.3(2) . . ? C72 N12 O22 115.2(3) . . ? C72 N12 Mn3 128.4(3) . . ? O22 N12 Mn3 116.4(2) . . ? O12 C12 C62 117.4(4) . . ? O12 C12 C22 122.8(4) . . ? C62 C12 C22 119.8(4) . . ? C32 C22 C12 118.6(4) . . ? C32 C22 C72 118.7(4) . . ? C12 C22 C72 122.7(4) . . ? C42 C32 C22 120.5(4) . . ? C42 C32 H32 119.8 . . ? C22 C32 H32 119.8 . . ? C52 C42 C32 119.3(4) . . ? C52 C42 H42 120.4 . . ? C32 C42 H42 120.4 . . ? C62 C52 C42 121.8(4) . . ? C62 C52 H52 119.1 . . ? C42 C52 H52 119.1 . . ? C52 C62 C12 119.9(4) . . ? C52 C62 H62 120.0 . . ? C12 C62 H62 120.0 . . ? N12 C72 C22 120.6(4) . . ? N12 C72 C82 118.8(3) . . ? C22 C72 C82 120.5(4) . . ? C92 C82 C132 118.9(4) . . ? C92 C82 C72 121.9(4) . . ? C132 C82 C72 119.2(4) . . ? C82 C92 C102 120.6(4) . . ? C82 C92 H92 119.7 . . ? C102 C92 H92 119.7 . . ? C112 C102 C92 119.2(4) . . ? C112 C102 H102 120.4 . . ? C92 C102 H102 120.4 . . ? C102 C112 C122 120.3(4) . . ? C102 C112 H112 119.9 . . ? C122 C112 H112 119.9 . . ? C132 C122 C112 120.6(4) . . ? C132 C122 H122 119.7 . . ? C112 C122 H122 119.7 . . ? C122 C132 C82 120.4(4) . . ? C122 C132 H132 119.8 . . ? C82 C132 H132 119.8 . . ? C11 O11 Mn1 119.7(2) . . ? N11 O21 Mn3 111.85(19) . . ? N11 O21 Mn1 114.14(19) . 3_666 ? Mn3 O21 Mn1 109.67(13) . 3_666 ? C71 N11 O21 117.9(3) . . ? C71 N11 Mn1 128.5(3) . . ? O21 N11 Mn1 112.4(2) . . ? O11 C11 C61 120.4(4) . . ? O11 C11 C21 121.5(4) . . ? C61 C11 C21 118.1(4) . . ? C31 C21 C11 117.7(4) . . ? C31 C21 C71 121.4(4) . . ? C11 C21 C71 120.8(4) . . ? C41 C31 C21 123.4(4) . . ? C41 C31 H31 118.3 . . ? C21 C31 H31 118.3 . . ? C31 C41 C51 118.7(4) . . ? C31 C41 H41 120.7 . . ? C51 C41 H41 120.7 . . ? C61 C51 C41 120.2(4) . . ? C61 C51 H51 119.9 . . ? C41 C51 H51 119.9 . . ? C51 C61 C11 121.9(4) . . ? C51 C61 H61 119.1 . . ? C11 C61 H61 119.1 . . ? N11 C71 C21 118.7(4) . . ? N11 C71 C81 122.0(4) . . ? C21 C71 C81 119.3(4) . . ? C131 C81 C91 120.4(4) . . ? C131 C81 C71 117.9(4) . . ? C91 C81 C71 121.6(4) . . ? C81 C91 C101 118.1(4) . . ? C81 C91 H91 121.0 . . ? C101 C91 H91 121.0 . . ? C111 C101 C91 121.1(5) . . ? C111 C101 H101 119.5 . . ? C91 C101 H101 119.5 . . ? C121 C111 C101 121.1(5) . . ? C121 C111 H111 119.4 . . ? C101 C111 H111 119.4 . . ? C111 C121 C131 119.0(5) . . ? C111 C121 H121 120.5 . . ? C131 C121 H121 120.5 . . ? C81 C131 C121 120.3(4) . . ? C81 C131 H131 119.9 . . ? C121 C131 H131 119.9 . . ? C13 O13 Mn2 126.8(3) . . ? N13 O23 Mn1 114.7(2) . . ? C73 N13 O23 114.4(3) . . ? C73 N13 Mn2 128.3(3) . . ? O23 N13 Mn2 116.8(2) . . ? O13 C13 C63 118.0(4) . . ? O13 C13 C23 122.9(3) . . ? C63 C13 C23 119.1(4) . . ? C33 C23 C13 117.5(4) . . ? C33 C23 C73 118.8(4) . . ? C13 C23 C73 123.7(3) . . ? C43 C33 C23 122.2(4) . . ? C43 C33 H33 118.9 . . ? C23 C33 H33 118.9 . . ? C33 C43 C53 119.8(4) . . ? C33 C43 H43 120.1 . . ? C53 C43 H43 120.1 . . ? C63 C53 C43 119.8(4) . . ? C63 C53 H53 120.1 . . ? C43 C53 H53 120.1 . . ? C53 C63 C13 121.6(4) . . ? C53 C63 H63 119.2 . . ? C13 C63 H63 119.2 . . ? N13 C73 C23 120.0(4) . . ? N13 C73 C83 118.4(3) . . ? C23 C73 C83 121.5(3) . . ? C133 C83 C93 117.3(4) . . ? C133 C83 C73 120.1(4) . . ? C93 C83 C73 122.6(4) . . ? C103 C93 C83 121.1(4) . . ? C103 C93 H93 119.4 . . ? C83 C93 H93 119.4 . . ? C93 C103 C113 121.0(4) . . ? C93 C103 H103 119.5 . . ? C113 C103 H103 119.5 . . ? C123 C113 C103 119.4(4) . . ? C123 C113 H113 120.3 . . ? C103 C113 H113 120.3 . . ? C113 C123 C133 119.9(4) . . ? C113 C123 H123 120.0 . . ? C133 C123 H123 120.0 . . ? C83 C133 C123 121.3(4) . . ? C83 C133 H133 119.4 . . ? C123 C133 H133 119.4 . . ? C14 O14 Mn2 129.6(3) . . ? C14 O24 Mn3 129.3(3) . . ? O14 C14 O24 124.5(4) . . ? O14 C14 C24 118.2(4) . . ? O24 C14 C24 117.3(4) . . ? C14 C24 C34 107.8(4) . . ? C14 C24 H24A 110.1 . . ? C34 C24 H24A 110.1 . . ? C14 C24 H24B 110.1 . . ? C34 C24 H24B 110.1 . . ? H24A C24 H24B 108.5 . . ? H34D C340 H34E 109.5 . . ? H34D C340 H34F 109.5 . . ? H34E C340 H34F 109.5 . . ? N4 C7 C8 176.7(10) . . ? C1 N1 Mn1 156.1(4) . . ? N1 C1 C2 178.7(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 179.3(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 177.4(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mn1 Mn2 O13 -158.4(2) . . . . ? O11 Mn1 Mn2 O13 15.6(3) . . . . ? O23 Mn1 Mn2 O13 -11.1(2) . . . . ? N11 Mn1 Mn2 O13 166.43(19) . . . . ? O21 Mn1 Mn2 O13 -93.40(18) 3_666 . . . ? N1 Mn1 Mn2 O13 79.09(19) . . . . ? O11 Mn1 Mn2 O1 174.1(3) . . . . ? O23 Mn1 Mn2 O1 147.29(17) . . . . ? N11 Mn1 Mn2 O1 -35.13(17) . . . . ? O21 Mn1 Mn2 O1 65.03(16) 3_666 . . . ? N1 Mn1 Mn2 O1 -122.48(17) . . . . ? O1 Mn1 Mn2 O22 -5.25(17) . . . . ? O11 Mn1 Mn2 O22 168.8(2) . . . . ? O23 Mn1 Mn2 O22 142.04(13) . . . . ? N11 Mn1 Mn2 O22 -40.38(14) . . . . ? O21 Mn1 Mn2 O22 59.78(12) 3_666 . . . ? N1 Mn1 Mn2 O22 -127.73(12) . . . . ? O1 Mn1 Mn2 N13 -160.59(18) . . . . ? O11 Mn1 Mn2 N13 13.5(3) . . . . ? O23 Mn1 Mn2 N13 -13.29(14) . . . . ? N11 Mn1 Mn2 N13 164.28(15) . . . . ? O21 Mn1 Mn2 N13 -95.55(13) 3_666 . . . ? N1 Mn1 Mn2 N13 76.94(14) . . . . ? O1 Mn1 Mn2 O14 94.16(17) . . . . ? O11 Mn1 Mn2 O14 -91.8(2) . . . . ? O23 Mn1 Mn2 O14 -118.55(12) . . . . ? N11 Mn1 Mn2 O14 59.03(13) . . . . ? O21 Mn1 Mn2 O14 159.19(10) 3_666 . . . ? N1 Mn1 Mn2 O14 -28.31(11) . . . . ? O1 Mn1 Mn2 Mn3 19.56(14) . . . . ? O11 Mn1 Mn2 Mn3 -166.4(2) . . . . ? O23 Mn1 Mn2 Mn3 166.86(9) . . . . ? N11 Mn1 Mn2 Mn3 -15.56(10) . . . . ? O21 Mn1 Mn2 Mn3 84.60(7) 3_666 . . . ? N1 Mn1 Mn2 Mn3 -102.91(8) . . . . ? O13 Mn2 Mn3 O12 -13.0(3) . . . . ? O1 Mn2 Mn3 O12 -172.8(2) . . . . ? O22 Mn2 Mn3 O12 -34.1(2) . . . . ? N13 Mn2 Mn3 O12 169.0(2) . . . . ? O14 Mn2 Mn3 O12 69.5(2) . . . . ? Mn1 Mn2 Mn3 O12 169.13(18) . . . . ? O13 Mn2 Mn3 O1 159.9(2) . . . . ? O22 Mn2 Mn3 O1 138.80(17) . . . . ? N13 Mn2 Mn3 O1 -18.17(18) . . . . ? O14 Mn2 Mn3 O1 -117.68(17) . . . . ? Mn1 Mn2 Mn3 O1 -18.02(15) . . . . ? O13 Mn2 Mn3 O21 172.5(2) . . . . ? O1 Mn2 Mn3 O21 12.67(17) . . . . ? O22 Mn2 Mn3 O21 151.47(12) . . . . ? N13 Mn2 Mn3 O21 -5.50(15) . . . . ? O14 Mn2 Mn3 O21 -105.01(13) . . . . ? Mn1 Mn2 Mn3 O21 -5.35(9) . . . . ? O13 Mn2 Mn3 N12 21.8(2) . . . . ? O1 Mn2 Mn3 N12 -138.10(18) . . . . ? O22 Mn2 Mn3 N12 0.70(13) . . . . ? N13 Mn2 Mn3 N12 -156.27(15) . . . . ? O14 Mn2 Mn3 N12 104.22(13) . . . . ? Mn1 Mn2 Mn3 N12 -156.12(10) . . . . ? O13 Mn2 Mn3 O24 -88.3(2) . . . . ? O1 Mn2 Mn3 O24 111.84(17) . . . . ? O22 Mn2 Mn3 O24 -109.37(12) . . . . ? N13 Mn2 Mn3 O24 93.66(14) . . . . ? O14 Mn2 Mn3 O24 -5.85(11) . . . . ? Mn1 Mn2 Mn3 O24 93.81(9) . . . . ? O13 Mn2 O1 Mn1 94.6(6) . . . . ? O22 Mn2 O1 Mn1 175.55(15) . . . . ? N13 Mn2 O1 Mn1 16.50(16) . . . . ? O14 Mn2 O1 Mn1 -87.76(15) . . . . ? Mn3 Mn2 O1 Mn1 -147.9(2) . . . . ? O13 Mn2 O1 Mn3 -117.5(6) . . . . ? O22 Mn2 O1 Mn3 -36.51(14) . . . . ? N13 Mn2 O1 Mn3 164.44(15) . . . . ? O14 Mn2 O1 Mn3 60.18(15) . . . . ? Mn1 Mn2 O1 Mn3 147.9(2) . . . . ? O23 Mn1 O1 Mn2 -28.92(15) . . . . ? N11 Mn1 O1 Mn2 148.14(15) . . . . ? O21 Mn1 O1 Mn2 -118.80(14) 3_666 . . . ? N1 Mn1 O1 Mn2 57.64(16) . . . . ? O23 Mn1 O1 Mn3 -174.27(15) . . . . ? N11 Mn1 O1 Mn3 2.79(16) . . . . ? O21 Mn1 O1 Mn3 95.86(15) 3_666 . . . ? N1 Mn1 O1 Mn3 -87.70(15) . . . . ? Mn2 Mn1 O1 Mn3 -145.3(2) . . . . ? O21 Mn3 O1 Mn2 -169.05(15) . . . . ? N12 Mn3 O1 Mn2 36.41(15) . . . . ? O24 Mn3 O1 Mn2 -65.17(15) . . . . ? O21 Mn3 O1 Mn1 -21.97(15) . . . . ? N12 Mn3 O1 Mn1 -176.51(16) . . . . ? O24 Mn3 O1 Mn1 81.91(16) . . . . ? Mn2 Mn3 O1 Mn1 147.1(2) . . . . ? O21 Mn3 O12 C12 -119.2(3) . . . . ? N12 Mn3 O12 C12 35.1(3) . . . . ? O24 Mn3 O12 C12 136.7(3) . . . . ? Mn2 Mn3 O12 C12 65.6(4) . . . . ? O13 Mn2 O22 N12 -170.6(2) . . . . ? O1 Mn2 O22 N12 20.6(2) . . . . ? N13 Mn2 O22 N12 108.8(4) . . . . ? O14 Mn2 O22 N12 -74.0(2) . . . . ? Mn3 Mn2 O22 N12 -0.99(19) . . . . ? Mn1 Mn2 O22 N12 23.3(2) . . . . ? Mn2 O22 N12 C72 -177.8(3) . . . . ? Mn2 O22 N12 Mn3 1.6(3) . . . . ? O12 Mn3 N12 C72 -19.6(4) . . . . ? O1 Mn3 N12 C72 156.6(4) . . . . ? O21 Mn3 N12 C72 74.9(5) . . . . ? O24 Mn3 N12 C72 -112.1(4) . . . . ? Mn2 Mn3 N12 C72 178.3(4) . . . . ? O12 Mn3 N12 O22 161.2(2) . . . . ? O1 Mn3 N12 O22 -22.6(2) . . . . ? O21 Mn3 N12 O22 -104.4(3) . . . . ? O24 Mn3 N12 O22 68.6(2) . . . . ? Mn2 Mn3 N12 O22 -0.98(19) . . . . ? Mn3 O12 C12 C62 145.5(3) . . . . ? Mn3 O12 C12 C22 -34.4(5) . . . . ? O12 C12 C22 C32 -176.5(3) . . . . ? C62 C12 C22 C32 3.5(6) . . . . ? O12 C12 C22 C72 5.8(6) . . . . ? C62 C12 C22 C72 -174.1(4) . . . . ? C12 C22 C32 C42 -1.9(6) . . . . ? C72 C22 C32 C42 175.9(3) . . . . ? C22 C32 C42 C52 -0.6(6) . . . . ? C32 C42 C52 C62 1.4(7) . . . . ? C42 C52 C62 C12 0.3(7) . . . . ? O12 C12 C62 C52 177.3(4) . . . . ? C22 C12 C62 C52 -2.8(6) . . . . ? O22 N12 C72 C22 -178.8(3) . . . . ? Mn3 N12 C72 C22 1.9(6) . . . . ? O22 N12 C72 C82 5.0(5) . . . . ? Mn3 N12 C72 C82 -174.2(3) . . . . ? C32 C22 C72 N12 -167.7(4) . . . . ? C12 C22 C72 N12 10.0(6) . . . . ? C32 C22 C72 C82 8.4(6) . . . . ? C12 C22 C72 C82 -173.9(4) . . . . ? N12 C72 C82 C92 -106.7(5) . . . . ? C22 C72 C82 C92 77.1(5) . . . . ? N12 C72 C82 C132 75.0(5) . . . . ? C22 C72 C82 C132 -101.2(5) . . . . ? C132 C82 C92 C102 -1.3(6) . . . . ? C72 C82 C92 C102 -179.6(4) . . . . ? C82 C92 C102 C112 1.8(6) . . . . ? C92 C102 C112 C122 -1.1(7) . . . . ? C102 C112 C122 C132 -0.1(6) . . . . ? C112 C122 C132 C82 0.6(6) . . . . ? C92 C82 C132 C122 0.0(6) . . . . ? C72 C82 C132 C122 178.4(4) . . . . ? O23 Mn1 O11 C11 127.6(3) . . . . ? N11 Mn1 O11 C11 -49.7(3) . . . . ? O21 Mn1 O11 C11 -143.3(3) 3_666 . . . ? N1 Mn1 O11 C11 41.2(3) . . . . ? Mn2 Mn1 O11 C11 103.6(3) . . . . ? O12 Mn3 O21 N11 -141.6(2) . . . . ? O1 Mn3 O21 N11 42.4(2) . . . . ? N12 Mn3 O21 N11 124.6(3) . . . . ? O24 Mn3 O21 N11 -48.4(2) . . . . ? Mn2 Mn3 O21 N11 35.5(2) . . . . ? O12 Mn3 O21 Mn1 90.76(13) . . . 3_666 ? O1 Mn3 O21 Mn1 -85.25(12) . . . 3_666 ? N12 Mn3 O21 Mn1 -3.1(3) . . . 3_666 ? O24 Mn3 O21 Mn1 -176.03(10) . . . 3_666 ? Mn2 Mn3 O21 Mn1 -92.21(11) . . . 3_666 ? Mn3 O21 N11 C71 141.8(3) . . . . ? Mn1 O21 N11 C71 -93.0(3) 3_666 . . . ? Mn3 O21 N11 Mn1 -49.6(2) . . . . ? Mn1 O21 N11 Mn1 75.6(2) 3_666 . . . ? O1 Mn1 N11 C71 -164.7(3) . . . . ? O11 Mn1 N11 C71 21.6(3) . . . . ? O21 Mn1 N11 C71 104.8(3) 3_666 . . . ? N1 Mn1 N11 C71 -66.1(3) . . . . ? Mn2 Mn1 N11 C71 -147.5(3) . . . . ? O1 Mn1 N11 O21 28.2(2) . . . . ? O11 Mn1 N11 O21 -145.5(2) . . . . ? O21 Mn1 N11 O21 -62.3(2) 3_666 . . . ? N1 Mn1 N11 O21 126.8(2) . . . . ? Mn2 Mn1 N11 O21 45.4(2) . . . . ? Mn1 O11 C11 C61 -132.5(3) . . . . ? Mn1 O11 C11 C21 50.1(4) . . . . ? O11 C11 C21 C31 -179.7(3) . . . . ? C61 C11 C21 C31 2.9(5) . . . . ? O11 C11 C21 C71 -4.5(5) . . . . ? C61 C11 C21 C71 178.1(3) . . . . ? C11 C21 C31 C41 -1.9(5) . . . . ? C71 C21 C31 C41 -177.1(4) . . . . ? C21 C31 C41 C51 0.3(6) . . . . ? C31 C41 C51 C61 0.1(5) . . . . ? C41 C51 C61 C11 1.1(6) . . . . ? O11 C11 C61 C51 -180.0(3) . . . . ? C21 C11 C61 C51 -2.6(5) . . . . ? O21 N11 C71 C21 176.9(3) . . . . ? Mn1 N11 C71 C21 10.5(6) . . . . ? O21 N11 C71 C81 -1.7(6) . . . . ? Mn1 N11 C71 C81 -168.2(3) . . . . ? C31 C21 C71 N11 149.0(4) . . . . ? C11 C21 C71 N11 -26.0(6) . . . . ? C31 C21 C71 C81 -32.3(5) . . . . ? C11 C21 C71 C81 152.6(3) . . . . ? N11 C71 C81 C131 129.9(4) . . . . ? C21 C71 C81 C131 -48.8(6) . . . . ? N11 C71 C81 C91 -47.8(6) . . . . ? C21 C71 C81 C91 133.6(4) . . . . ? C131 C81 C91 C101 2.0(6) . . . . ? C71 C81 C91 C101 179.6(4) . . . . ? C81 C91 C101 C111 -1.2(7) . . . . ? C91 C101 C111 C121 -0.5(8) . . . . ? C101 C111 C121 C131 1.3(8) . . . . ? C91 C81 C131 C121 -1.2(6) . . . . ? C71 C81 C131 C121 -178.9(4) . . . . ? C111 C121 C131 C81 -0.4(7) . . . . ? O1 Mn2 O13 C13 -108.9(6) . . . . ? O22 Mn2 O13 C13 169.7(3) . . . . ? N13 Mn2 O13 C13 -31.0(3) . . . . ? O14 Mn2 O13 C13 73.4(3) . . . . ? Mn3 Mn2 O13 C13 150.7(2) . . . . ? Mn1 Mn2 O13 C13 -32.8(4) . . . . ? O1 Mn1 O23 N13 34.6(2) . . . . ? O11 Mn1 O23 N13 -151.5(2) . . . . ? O21 Mn1 O23 N13 125.2(2) 3_666 . . . ? N1 Mn1 O23 N13 -64.1(2) . . . . ? Mn2 Mn1 O23 N13 18.5(2) . . . . ? Mn1 O23 N13 C73 157.3(3) . . . . ? Mn1 O23 N13 Mn2 -30.4(3) . . . . ? O13 Mn2 N13 C73 10.7(4) . . . . ? O1 Mn2 N13 C73 179.8(4) . . . . ? O22 Mn2 N13 C73 90.9(5) . . . . ? O14 Mn2 N13 C73 -86.2(4) . . . . ? Mn3 Mn2 N13 C73 -170.2(3) . . . . ? Mn1 Mn2 N13 C73 -170.4(4) . . . . ? O13 Mn2 N13 O23 -160.4(2) . . . . ? O1 Mn2 N13 O23 8.6(2) . . . . ? O22 Mn2 N13 O23 -80.2(4) . . . . ? O14 Mn2 N13 O23 102.6(2) . . . . ? Mn3 Mn2 N13 O23 18.6(3) . . . . ? Mn1 Mn2 N13 O23 18.46(19) . . . . ? Mn2 O13 C13 C63 -146.9(3) . . . . ? Mn2 O13 C13 C23 32.9(6) . . . . ? O13 C13 C23 C33 178.1(3) . . . . ? C63 C13 C23 C33 -2.1(6) . . . . ? O13 C13 C23 C73 -4.3(7) . . . . ? C63 C13 C23 C73 175.5(4) . . . . ? C13 C23 C33 C43 1.1(6) . . . . ? C73 C23 C33 C43 -176.7(4) . . . . ? C23 C33 C43 C53 0.2(7) . . . . ? C33 C43 C53 C63 -0.3(7) . . . . ? C43 C53 C63 C13 -0.8(7) . . . . ? O13 C13 C63 C53 -178.1(4) . . . . ? C23 C13 C63 C53 2.1(6) . . . . ? O23 N13 C73 C23 179.8(3) . . . . ? Mn2 N13 C73 C23 8.5(6) . . . . ? O23 N13 C73 C83 -3.6(5) . . . . ? Mn2 N13 C73 C83 -174.9(3) . . . . ? C33 C23 C73 N13 161.7(4) . . . . ? C13 C23 C73 N13 -15.9(7) . . . . ? C33 C23 C73 C83 -14.8(6) . . . . ? C13 C23 C73 C83 167.6(4) . . . . ? N13 C73 C83 C133 120.0(4) . . . . ? C23 C73 C83 C133 -63.5(5) . . . . ? N13 C73 C83 C93 -59.8(5) . . . . ? C23 C73 C83 C93 116.7(4) . . . . ? C133 C83 C93 C103 0.7(5) . . . . ? C73 C83 C93 C103 -179.4(3) . . . . ? C83 C93 C103 C113 -1.0(6) . . . . ? C93 C103 C113 C123 0.0(6) . . . . ? C103 C113 C123 C133 1.4(6) . . . . ? C93 C83 C133 C123 0.6(5) . . . . ? C73 C83 C133 C123 -179.3(3) . . . . ? C113 C123 C133 C83 -1.7(6) . . . . ? O13 Mn2 O14 C14 161.0(3) . . . . ? O1 Mn2 O14 C14 -18.5(4) . . . . ? O22 Mn2 O14 C14 73.2(4) . . . . ? N13 Mn2 O14 C14 -107.8(4) . . . . ? Mn3 Mn2 O14 C14 11.1(3) . . . . ? Mn1 Mn2 O14 C14 -49.5(3) . . . . ? O12 Mn3 O24 C14 -144.0(4) . . . . ? O1 Mn3 O24 C14 35.4(4) . . . . ? O21 Mn3 O24 C14 123.0(3) . . . . ? N12 Mn3 O24 C14 -53.8(4) . . . . ? Mn2 Mn3 O24 C14 4.6(3) . . . . ? Mn2 O14 C14 O24 -12.0(6) . . . . ? Mn2 O14 C14 C24 169.4(3) . . . . ? Mn3 O24 C14 O14 1.7(6) . . . . ? Mn3 O24 C14 C24 -179.8(3) . . . . ? O14 C14 C24 C34 42.6(5) . . . . ? O24 C14 C24 C34 -136.0(4) . . . . ? O1 Mn1 N1 C1 174.1(9) . . . . ? O11 Mn1 N1 C1 -0.1(9) . . . . ? O23 Mn1 N1 C1 -96.2(9) . . . . ? N11 Mn1 N1 C1 86.4(9) . . . . ? Mn2 Mn1 N1 C1 -160.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.48 _refine_diff_density_min -0.52 _refine_diff_density_rms 0.071 # Attachment 'Complex_2.cif' data_bk170ap _database_code_depnum_ccdc_archive 'CCDC 793022' #TrackingRef 'Complex_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H88 Mn6 N6 O22' _chemical_formula_sum 'C92 H88 Mn6 N6 O22' _chemical_formula_weight 1959.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.004(5) _cell_length_b 12.887(5) _cell_length_c 26.360(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.58(3) _cell_angle_gamma 90.00 _cell_volume 4328(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 12557 _cell_measurement_theta_min 4.68 _cell_measurement_theta_max 30.14 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'Xcalibur PX KM4CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30246 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.1257 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 30.14 _reflns_number_total 12349 _reflns_number_gt 6849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.(2010)' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.(2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12349 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.52516(3) 0.61710(2) 0.481984(11) 0.01420(8) Uani 1 1 d . . . Mn2 Mn 0.56222(3) 0.59292(2) 0.607812(11) 0.01537(8) Uani 1 1 d . . . Mn3 Mn 0.37943(3) 0.74493(3) 0.545437(11) 0.01609(8) Uani 1 1 d . . . O1 O 0.49285(10) 0.65740(10) 0.54599(5) 0.0137(3) Uani 1 1 d . . . O11 O 0.53430(11) 0.55929(10) 0.41718(5) 0.0150(3) Uani 1 1 d . . . O21 O 0.34346(11) 0.74724(11) 0.47180(5) 0.0192(3) Uani 1 1 d . . . N11 N 0.41764(13) 0.71614(12) 0.44480(6) 0.0149(4) Uani 1 1 d . . . C11 C 0.54182(16) 0.62229(16) 0.37716(7) 0.0142(5) Uani 1 1 d . . . C21 C 0.47543(16) 0.70891(15) 0.36417(7) 0.0144(5) Uani 1 1 d . . . C31 C 0.48373(16) 0.76612(16) 0.31973(7) 0.0169(5) Uani 1 1 d . . . H31 H 0.4385 0.8238 0.3100 0.020 Uiso 1 1 calc R . . C41 C 0.55604(17) 0.74065(17) 0.28978(8) 0.0205(5) Uani 1 1 d . . . H41 H 0.5610 0.7808 0.2601 0.025 Uiso 1 1 calc R . . C51 C 0.62087(18) 0.65618(17) 0.30352(8) 0.0218(5) Uani 1 1 d . . . H51 H 0.6712 0.6386 0.2833 0.026 Uiso 1 1 calc R . . C61 C 0.61337(17) 0.59688(16) 0.34640(7) 0.0193(5) Uani 1 1 d . . . H61 H 0.6576 0.5381 0.3549 0.023 Uiso 1 1 calc R . . C71 C 0.39974(16) 0.74182(15) 0.39561(7) 0.0143(4) Uani 1 1 d . . . C81 C 0.30649(16) 0.80433(16) 0.37206(8) 0.0158(5) Uani 1 1 d . . . C91 C 0.24187(17) 0.76916(16) 0.32658(8) 0.0179(5) Uani 1 1 d . . . H91 H 0.2585 0.7065 0.3110 0.021 Uiso 1 1 calc R . . C101 C 0.15379(18) 0.82494(17) 0.30398(8) 0.0247(6) Uani 1 1 d . . . H101 H 0.1088 0.7992 0.2737 0.030 Uiso 1 1 calc R . . C111 C 0.13111(18) 0.91752(17) 0.32523(8) 0.0252(6) Uani 1 1 d . . . H111 H 0.0711 0.9562 0.3093 0.030 Uiso 1 1 calc R . . C121 C 0.19571(18) 0.95454(17) 0.36993(8) 0.0224(5) Uani 1 1 d . . . H121 H 0.1805 1.0191 0.3842 0.027 Uiso 1 1 calc R . . C131 C 0.28207(16) 0.89771(16) 0.39371(7) 0.0182(5) Uani 1 1 d . . . H131 H 0.3250 0.9223 0.4249 0.022 Uiso 1 1 calc R . . O12 O 0.26266(11) 0.82723(11) 0.54343(5) 0.0206(4) Uani 1 1 d . . . O22 O 0.46235(11) 0.64757(11) 0.64526(5) 0.0186(3) Uani 1 1 d . . . N12 N 0.37963(13) 0.70640(13) 0.61959(6) 0.0158(4) Uani 1 1 d . . . C12 C 0.19965(17) 0.84093(16) 0.57662(8) 0.0182(5) Uani 1 1 d . . . C22 C 0.21809(17) 0.79569(16) 0.62658(8) 0.0179(5) Uani 1 1 d . . . C32 C 0.14519(18) 0.81716(17) 0.65844(8) 0.0233(5) Uani 1 1 d . . . H32 H 0.1558 0.7869 0.6919 0.028 Uiso 1 1 calc R . . C42 C 0.06004(18) 0.87990(17) 0.64270(9) 0.0276(6) Uani 1 1 d . . . H42 H 0.0128 0.8931 0.6652 0.033 Uiso 1 1 calc R . . C52 C 0.04268(18) 0.92458(17) 0.59334(8) 0.0245(6) Uani 1 1 d . . . H52 H -0.0163 0.9683 0.5821 0.029 Uiso 1 1 calc R . . C62 C 0.11130(17) 0.90484(16) 0.56133(8) 0.0210(5) Uani 1 1 d . . . H62 H 0.0988 0.9352 0.5278 0.025 Uiso 1 1 calc R . . C72 C 0.30860(17) 0.73005(16) 0.64674(7) 0.0161(5) Uani 1 1 d . . . C82 C 0.32114(17) 0.69074(17) 0.70113(8) 0.0197(5) Uani 1 1 d . . . C92 C 0.38122(18) 0.74451(19) 0.74183(8) 0.0288(6) Uani 1 1 d . . . H92 H 0.4188 0.8046 0.7353 0.035 Uiso 1 1 calc R . . C102 C 0.3868(2) 0.7107(2) 0.79249(9) 0.0399(7) Uani 1 1 d . . . H102 H 0.4281 0.7477 0.8205 0.048 Uiso 1 1 calc R . . C112 C 0.3323(2) 0.6236(2) 0.80184(9) 0.0392(7) Uani 1 1 d . . . H112 H 0.3363 0.6004 0.8364 0.047 Uiso 1 1 calc R . . C122 C 0.2719(2) 0.56983(19) 0.76149(9) 0.0336(7) Uani 1 1 d . . . H122 H 0.2349 0.5094 0.7682 0.040 Uiso 1 1 calc R . . C132 C 0.26509(18) 0.60397(18) 0.71093(8) 0.0253(6) Uani 1 1 d . . . H132 H 0.2221 0.5679 0.6831 0.030 Uiso 1 1 calc R . . O13 O 0.64075(11) 0.52479(10) 0.66595(5) 0.0176(3) Uani 1 1 d . . . O23 O 0.60982(10) 0.50423(10) 0.51682(5) 0.0142(3) Uani 1 1 d . . . N13 N 0.65974(13) 0.52941(12) 0.56694(6) 0.0137(4) Uani 1 1 d . . . C13 C 0.74451(18) 0.51489(15) 0.67526(8) 0.0182(5) Uani 1 1 d . . . C23 C 0.80544(17) 0.50747(16) 0.63639(8) 0.0167(5) Uani 1 1 d . . . C33 C 0.91537(18) 0.50153(16) 0.65135(8) 0.0224(5) Uani 1 1 d . . . H33 H 0.9565 0.5004 0.6254 0.027 Uiso 1 1 calc R . . C43 C 0.96506(19) 0.49728(16) 0.70275(8) 0.0252(5) Uani 1 1 d . . . H43 H 1.0395 0.4946 0.7121 0.030 Uiso 1 1 calc R . . C53 C 0.90426(19) 0.49698(16) 0.74064(8) 0.0259(6) Uani 1 1 d . . . H53 H 0.9373 0.4899 0.7760 0.031 Uiso 1 1 calc R . . C63 C 0.79714(18) 0.50675(16) 0.72736(8) 0.0202(5) Uani 1 1 d . . . H63 H 0.7574 0.5080 0.7539 0.024 Uiso 1 1 calc R . . C73 C 0.75684(17) 0.49974(16) 0.58127(8) 0.0153(5) Uani 1 1 d . . . C83 C 0.81574(16) 0.45606(16) 0.54306(8) 0.0173(5) Uani 1 1 d . . . C93 C 0.87013(17) 0.36311(17) 0.55298(8) 0.0217(5) Uani 1 1 d . . . H93 H 0.8708 0.3276 0.5846 0.026 Uiso 1 1 calc R . . C103 C 0.92336(17) 0.32184(18) 0.51711(9) 0.0266(6) Uani 1 1 d . . . H103 H 0.9594 0.2576 0.5239 0.032 Uiso 1 1 calc R . . C113 C 0.92397(17) 0.37419(19) 0.47139(9) 0.0269(6) Uani 1 1 d . . . H113 H 0.9615 0.3464 0.4471 0.032 Uiso 1 1 calc R . . C123 C 0.87086(17) 0.46584(18) 0.46100(8) 0.0240(6) Uani 1 1 d . . . H123 H 0.8713 0.5011 0.4294 0.029 Uiso 1 1 calc R . . C133 C 0.81620(17) 0.50772(17) 0.49640(8) 0.0208(5) Uani 1 1 d . . . H133 H 0.7792 0.5713 0.4889 0.025 Uiso 1 1 calc R . . O14 O 0.67090(11) 0.72548(10) 0.62389(5) 0.0207(4) Uani 1 1 d . . . H14 H 0.6739 0.7663 0.5985 0.031 Uiso 1 1 d R . . C14 C 0.69647(19) 0.78611(17) 0.67040(8) 0.0283(6) Uani 1 1 d . . . H14A H 0.6606 0.7566 0.6969 0.034 Uiso 1 1 calc R . . H14B H 0.6709 0.8580 0.6631 0.034 Uiso 1 1 calc R . . C24 C 0.81219(19) 0.78786(17) 0.69109(9) 0.0357(7) Uani 1 1 d . . . H24A H 0.8271 0.8281 0.7233 0.053 Uiso 1 1 calc R . . H24B H 0.8476 0.8199 0.6655 0.053 Uiso 1 1 calc R . . H24C H 0.8378 0.7167 0.6980 0.053 Uiso 1 1 calc R . . O15 O 0.65354(11) 0.71911(10) 0.48189(5) 0.0186(3) Uani 1 1 d . . . O25 O 0.67373(11) 0.84699(10) 0.54097(5) 0.0200(4) Uani 1 1 d . . . C15 C 0.69998(17) 0.79760(17) 0.50384(8) 0.0185(5) Uani 1 1 d . . . C25 C 0.79622(18) 0.83588(18) 0.48531(9) 0.0280(6) Uani 1 1 d . . . H25A H 0.7920 0.9124 0.4822 0.034 Uiso 1 1 calc R . . H25B H 0.8590 0.8192 0.5121 0.034 Uiso 1 1 calc R . . C35 C 0.81191(18) 0.79194(18) 0.43436(8) 0.0299(6) Uani 1 1 d . . . H35A H 0.8783 0.8175 0.4270 0.045 Uiso 1 1 calc R . . H35B H 0.7539 0.8138 0.4067 0.045 Uiso 1 1 calc R . . H35C H 0.8137 0.7160 0.4363 0.045 Uiso 1 1 calc R . . O16 O 0.48094(11) 0.87519(11) 0.55582(5) 0.0264(4) Uani 1 1 d . . . H16 H 0.5413 0.8627 0.5487 0.040 Uiso 1 1 d R . . C16 C 0.44824(19) 0.98151(17) 0.55560(8) 0.0270(6) Uani 1 1 d . . . H16A H 0.3818 0.9908 0.5301 0.032 Uiso 1 1 calc R . . H16B H 0.5022 1.0266 0.5453 0.032 Uiso 1 1 calc R . . C26 C 0.4327(2) 1.0119(2) 0.60787(10) 0.0458(8) Uani 1 1 d . . . H26A H 0.4114 1.0848 0.6074 0.069 Uiso 1 1 calc R . . H26B H 0.4986 1.0025 0.6331 0.069 Uiso 1 1 calc R . . H26C H 0.3780 0.9683 0.6176 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01476(18) 0.01750(19) 0.01089(15) -0.00061(13) 0.00388(13) 0.00066(15) Mn2 0.01636(18) 0.0193(2) 0.01099(15) -0.00096(13) 0.00410(14) 0.00069(15) Mn3 0.01651(18) 0.0197(2) 0.01340(15) -0.00095(14) 0.00622(13) 0.00164(15) O1 0.0146(8) 0.0171(9) 0.0100(7) -0.0002(6) 0.0043(6) 0.0011(6) O11 0.0174(8) 0.0183(9) 0.0101(7) 0.0008(6) 0.0044(6) -0.0006(7) O21 0.0186(8) 0.0272(9) 0.0145(7) 0.0018(6) 0.0096(6) 0.0077(7) N11 0.0139(10) 0.0183(11) 0.0143(9) -0.0021(7) 0.0073(8) 0.0013(8) C11 0.0151(12) 0.0162(13) 0.0114(10) -0.0027(9) 0.0026(9) -0.0051(10) C21 0.0147(12) 0.0158(13) 0.0127(10) -0.0034(8) 0.0029(9) -0.0033(9) C31 0.0208(12) 0.0158(13) 0.0138(10) -0.0018(9) 0.0027(9) -0.0018(10) C41 0.0253(13) 0.0225(14) 0.0151(10) 0.0030(10) 0.0074(10) -0.0019(11) C51 0.0266(14) 0.0260(14) 0.0169(11) -0.0007(9) 0.0145(11) 0.0009(11) C61 0.0198(13) 0.0214(14) 0.0182(11) 0.0009(9) 0.0075(10) 0.0038(10) C71 0.0169(12) 0.0128(12) 0.0136(10) 0.0007(9) 0.0040(9) -0.0029(10) C81 0.0163(12) 0.0173(13) 0.0156(11) 0.0038(9) 0.0078(10) -0.0008(10) C91 0.0202(13) 0.0179(13) 0.0176(11) -0.0001(9) 0.0083(10) 0.0011(10) C101 0.0219(14) 0.0296(15) 0.0214(12) -0.0009(10) 0.0014(11) -0.0001(11) C111 0.0182(13) 0.0305(15) 0.0278(13) 0.0046(11) 0.0069(11) 0.0082(11) C121 0.0255(14) 0.0188(14) 0.0259(12) 0.0010(10) 0.0120(11) 0.0041(11) C131 0.0191(13) 0.0206(14) 0.0162(10) 0.0010(9) 0.0067(9) 0.0005(10) O12 0.0187(9) 0.0287(10) 0.0172(8) 0.0011(6) 0.0102(7) 0.0057(7) O22 0.0200(9) 0.0231(9) 0.0143(7) 0.0012(6) 0.0072(7) 0.0047(7) N12 0.0162(10) 0.0159(11) 0.0157(9) -0.0028(7) 0.0045(8) 0.0000(8) C12 0.0201(13) 0.0146(13) 0.0217(12) -0.0059(9) 0.0087(10) -0.0036(10) C22 0.0208(13) 0.0161(13) 0.0186(11) -0.0045(9) 0.0085(10) -0.0033(10) C32 0.0273(15) 0.0252(14) 0.0205(12) -0.0036(10) 0.0126(11) -0.0042(11) C42 0.0277(15) 0.0266(15) 0.0338(14) -0.0021(11) 0.0191(12) 0.0057(12) C52 0.0218(14) 0.0199(14) 0.0343(14) -0.0029(10) 0.0114(11) 0.0014(11) C62 0.0221(13) 0.0202(14) 0.0219(11) -0.0003(10) 0.0069(10) 0.0000(10) C72 0.0189(12) 0.0173(13) 0.0141(10) -0.0070(9) 0.0085(9) -0.0049(10) C82 0.0180(13) 0.0265(14) 0.0167(11) -0.0024(10) 0.0081(10) 0.0052(11) C92 0.0256(14) 0.0387(16) 0.0236(12) -0.0071(11) 0.0083(11) 0.0037(12) C102 0.0341(17) 0.067(2) 0.0168(12) -0.0122(13) 0.0011(12) 0.0141(15) C112 0.0401(18) 0.061(2) 0.0203(13) 0.0112(13) 0.0147(13) 0.0253(15) C122 0.0391(17) 0.0399(17) 0.0276(14) 0.0065(12) 0.0206(13) 0.0110(13) C132 0.0280(14) 0.0319(16) 0.0198(11) -0.0001(10) 0.0137(11) 0.0073(12) O13 0.0185(9) 0.0212(9) 0.0132(7) 0.0014(6) 0.0036(7) 0.0021(7) O23 0.0127(8) 0.0185(8) 0.0112(7) -0.0024(6) 0.0020(6) 0.0011(6) N13 0.0137(10) 0.0162(10) 0.0107(8) -0.0009(7) 0.0011(8) -0.0031(8) C13 0.0234(14) 0.0113(13) 0.0180(11) -0.0005(9) -0.0009(10) -0.0001(10) C23 0.0181(13) 0.0151(12) 0.0156(11) -0.0004(9) 0.0000(9) 0.0009(10) C33 0.0217(14) 0.0231(14) 0.0211(12) -0.0033(10) 0.0014(10) -0.0020(11) C43 0.0202(13) 0.0252(14) 0.0256(13) -0.0013(10) -0.0062(11) 0.0005(11) C53 0.0353(16) 0.0225(14) 0.0151(11) -0.0011(10) -0.0069(11) 0.0019(12) C63 0.0291(14) 0.0169(13) 0.0143(11) -0.0005(9) 0.0033(10) -0.0005(11) C73 0.0173(13) 0.0126(12) 0.0165(11) 0.0002(9) 0.0047(9) -0.0022(10) C83 0.0109(12) 0.0222(14) 0.0181(11) -0.0044(9) 0.0013(9) -0.0016(10) C93 0.0166(13) 0.0249(14) 0.0223(12) -0.0006(10) 0.0004(10) -0.0012(11) C103 0.0183(14) 0.0258(15) 0.0353(14) -0.0099(11) 0.0043(11) 0.0024(11) C113 0.0168(13) 0.0367(16) 0.0288(13) -0.0144(11) 0.0083(11) -0.0017(12) C123 0.0195(13) 0.0335(16) 0.0203(12) -0.0023(10) 0.0072(11) -0.0046(11) C133 0.0153(13) 0.0248(14) 0.0221(12) -0.0022(10) 0.0030(10) -0.0016(10) O14 0.0263(9) 0.0216(9) 0.0130(7) 0.0003(6) 0.0011(7) -0.0046(7) C14 0.0343(16) 0.0303(15) 0.0193(12) -0.0083(10) 0.0031(11) -0.0075(12) C24 0.0413(17) 0.0201(15) 0.0368(15) 0.0021(11) -0.0132(13) -0.0046(12) O15 0.0166(9) 0.0205(9) 0.0196(8) -0.0024(6) 0.0059(7) -0.0049(7) O25 0.0260(9) 0.0192(9) 0.0161(8) -0.0012(6) 0.0070(7) 0.0002(7) C15 0.0157(12) 0.0208(14) 0.0185(11) 0.0053(10) 0.0022(10) -0.0008(10) C25 0.0218(14) 0.0289(15) 0.0349(14) -0.0018(11) 0.0093(12) -0.0066(11) C35 0.0248(14) 0.0413(17) 0.0264(13) 0.0084(11) 0.0120(11) 0.0000(12) O16 0.0213(9) 0.0167(9) 0.0440(10) -0.0026(7) 0.0136(8) 0.0026(7) C16 0.0255(14) 0.0226(15) 0.0305(14) 0.0025(10) -0.0005(11) -0.0003(11) C26 0.049(2) 0.0427(19) 0.0479(17) -0.0197(14) 0.0149(15) -0.0097(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O11 1.8891(14) . ? Mn1 O1 1.8914(13) . ? Mn1 O23 1.9405(15) . ? Mn1 N11 1.9986(18) . ? Mn1 O15 2.1253(15) . ? Mn1 O23 2.3556(15) 3_666 ? Mn1 Mn3 3.2210(10) . ? Mn2 O13 1.8799(15) . ? Mn2 O1 1.8894(14) . ? Mn2 O22 1.9161(14) . ? Mn2 N13 1.9970(17) . ? Mn2 O14 2.2034(15) . ? Mn2 O11 2.3505(15) 3_666 ? Mn3 O12 1.8442(15) . ? Mn3 O1 1.8545(14) . ? Mn3 O21 1.9034(14) . ? Mn3 N12 2.0163(17) . ? Mn3 O16 2.1189(16) . ? O11 C11 1.350(2) . ? O11 Mn2 2.3505(15) 3_666 ? O21 N11 1.3688(19) . ? N11 C71 1.313(2) . ? C11 C61 1.390(3) . ? C11 C21 1.411(3) . ? C21 C31 1.407(3) . ? C21 C71 1.471(3) . ? C31 C41 1.383(3) . ? C31 H31 0.9500 . ? C41 C51 1.380(3) . ? C41 H41 0.9500 . ? C51 C61 1.384(3) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C71 C81 1.484(3) . ? C81 C91 1.394(3) . ? C81 C131 1.396(3) . ? C91 C101 1.382(3) . ? C91 H91 0.9500 . ? C101 C111 1.375(3) . ? C101 H101 0.9500 . ? C111 C121 1.387(3) . ? C111 H111 0.9500 . ? C121 C131 1.381(3) . ? C121 H121 0.9500 . ? C131 H131 0.9500 . ? O12 C12 1.325(2) . ? O22 N12 1.378(2) . ? N12 C72 1.313(2) . ? C12 C62 1.405(3) . ? C12 C22 1.416(3) . ? C22 C32 1.414(3) . ? C22 C72 1.460(3) . ? C32 C42 1.367(3) . ? C32 H32 0.9500 . ? C42 C52 1.399(3) . ? C42 H42 0.9500 . ? C52 C62 1.369(3) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C72 C82 1.498(3) . ? C82 C92 1.380(3) . ? C82 C132 1.387(3) . ? C92 C102 1.393(3) . ? C92 H92 0.9500 . ? C102 C112 1.376(3) . ? C102 H102 0.9500 . ? C112 C122 1.375(3) . ? C112 H112 0.9500 . ? C122 C132 1.389(3) . ? C122 H122 0.9500 . ? C132 H132 0.9500 . ? O13 C13 1.328(2) . ? O23 N13 1.3884(19) . ? O23 Mn1 2.3556(15) 3_666 ? N13 C73 1.301(3) . ? C13 C63 1.410(3) . ? C13 C23 1.419(3) . ? C23 C33 1.407(3) . ? C23 C73 1.467(3) . ? C33 C43 1.380(3) . ? C33 H33 0.9500 . ? C43 C53 1.393(3) . ? C43 H43 0.9500 . ? C53 C63 1.372(3) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C73 C83 1.493(3) . ? C83 C93 1.389(3) . ? C83 C133 1.400(3) . ? C93 C103 1.385(3) . ? C93 H93 0.9500 . ? C103 C113 1.382(3) . ? C103 H103 0.9500 . ? C113 C123 1.368(3) . ? C113 H113 0.9500 . ? C123 C133 1.391(3) . ? C123 H123 0.9500 . ? C133 H133 0.9500 . ? O14 C14 1.435(2) . ? O14 H14 0.8582 . ? C14 C24 1.494(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O15 C15 1.258(2) . ? O25 C15 1.271(2) . ? C15 C25 1.514(3) . ? C25 C35 1.509(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O16 C16 1.434(2) . ? O16 H16 0.8584 . ? C16 C26 1.484(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mn1 O1 168.65(6) . . ? O11 Mn1 O23 89.98(6) . . ? O1 Mn1 O23 89.44(6) . . ? O11 Mn1 N11 88.46(7) . . ? O1 Mn1 N11 90.19(6) . . ? O23 Mn1 N11 170.20(6) . . ? O11 Mn1 O15 92.92(6) . . ? O1 Mn1 O15 98.42(6) . . ? O23 Mn1 O15 95.34(6) . . ? N11 Mn1 O15 94.40(7) . . ? O11 Mn1 O23 86.13(6) . 3_666 ? O1 Mn1 O23 82.57(6) . 3_666 ? O23 Mn1 O23 81.35(6) . 3_666 ? N11 Mn1 O23 88.89(7) . 3_666 ? O15 Mn1 O23 176.55(5) . 3_666 ? O11 Mn1 Mn3 145.25(5) . . ? O1 Mn1 Mn3 30.36(4) . . ? O23 Mn1 Mn3 118.34(4) . . ? N11 Mn1 Mn3 60.10(5) . . ? O15 Mn1 Mn3 103.21(5) . . ? O23 Mn1 Mn3 79.33(4) 3_666 . ? O13 Mn2 O1 174.70(6) . . ? O13 Mn2 O22 93.74(6) . . ? O1 Mn2 O22 91.55(6) . . ? O13 Mn2 N13 87.05(7) . . ? O1 Mn2 N13 87.70(7) . . ? O22 Mn2 N13 176.47(7) . . ? O13 Mn2 O14 89.01(6) . . ? O1 Mn2 O14 90.10(6) . . ? O22 Mn2 O14 95.21(6) . . ? N13 Mn2 O14 88.24(6) . . ? O13 Mn2 O11 90.62(6) . 3_666 ? O1 Mn2 O11 89.41(6) . 3_666 ? O22 Mn2 O11 94.14(6) . 3_666 ? N13 Mn2 O11 82.41(6) . 3_666 ? O14 Mn2 O11 170.65(5) . 3_666 ? O12 Mn3 O1 177.38(7) . . ? O12 Mn3 O21 85.95(6) . . ? O1 Mn3 O21 92.85(6) . . ? O12 Mn3 N12 90.58(7) . . ? O1 Mn3 N12 89.79(7) . . ? O21 Mn3 N12 160.86(7) . . ? O12 Mn3 O16 92.07(7) . . ? O1 Mn3 O16 90.40(7) . . ? O21 Mn3 O16 97.96(6) . . ? N12 Mn3 O16 100.98(7) . . ? O12 Mn3 Mn1 147.79(5) . . ? O1 Mn3 Mn1 31.03(4) . . ? O21 Mn3 Mn1 61.85(5) . . ? N12 Mn3 Mn1 119.41(5) . . ? O16 Mn3 Mn1 93.21(5) . . ? Mn3 O1 Mn2 121.03(7) . . ? Mn3 O1 Mn1 118.60(7) . . ? Mn2 O1 Mn1 119.70(7) . . ? C11 O11 Mn1 119.80(12) . . ? C11 O11 Mn2 113.65(11) . 3_666 ? Mn1 O11 Mn2 117.11(6) . 3_666 ? N11 O21 Mn3 118.11(11) . . ? C71 N11 O21 115.85(16) . . ? C71 N11 Mn1 127.82(14) . . ? O21 N11 Mn1 115.38(11) . . ? O11 C11 C61 118.42(19) . . ? O11 C11 C21 121.91(17) . . ? C61 C11 C21 119.57(18) . . ? C31 C21 C11 118.12(18) . . ? C31 C21 C71 119.34(19) . . ? C11 C21 C71 122.53(18) . . ? C41 C31 C21 121.7(2) . . ? C41 C31 H31 119.1 . . ? C21 C31 H31 119.1 . . ? C51 C41 C31 119.13(19) . . ? C51 C41 H41 120.4 . . ? C31 C41 H41 120.4 . . ? C41 C51 C61 120.7(2) . . ? C41 C51 H51 119.7 . . ? C61 C51 H51 119.7 . . ? C51 C61 C11 120.7(2) . . ? C51 C61 H61 119.6 . . ? C11 C61 H61 119.6 . . ? N11 C71 C21 118.53(19) . . ? N11 C71 C81 121.20(18) . . ? C21 C71 C81 120.26(17) . . ? C91 C81 C131 119.0(2) . . ? C91 C81 C71 118.95(19) . . ? C131 C81 C71 122.06(19) . . ? C101 C91 C81 120.4(2) . . ? C101 C91 H91 119.8 . . ? C81 C91 H91 119.8 . . ? C111 C101 C91 120.2(2) . . ? C111 C101 H101 119.9 . . ? C91 C101 H101 119.9 . . ? C101 C111 C121 120.1(2) . . ? C101 C111 H111 119.9 . . ? C121 C111 H111 119.9 . . ? C131 C121 C111 120.1(2) . . ? C131 C121 H121 119.9 . . ? C111 C121 H121 119.9 . . ? C121 C131 C81 120.2(2) . . ? C121 C131 H131 119.9 . . ? C81 C131 H131 119.9 . . ? C12 O12 Mn3 132.26(13) . . ? N12 O22 Mn2 119.50(11) . . ? C72 N12 O22 115.19(16) . . ? C72 N12 Mn3 127.38(15) . . ? O22 N12 Mn3 117.43(11) . . ? O12 C12 C62 117.84(19) . . ? O12 C12 C22 123.2(2) . . ? C62 C12 C22 118.97(19) . . ? C32 C22 C12 117.6(2) . . ? C32 C22 C72 118.99(19) . . ? C12 C22 C72 123.42(19) . . ? C42 C32 C22 122.3(2) . . ? C42 C32 H32 118.8 . . ? C22 C32 H32 118.8 . . ? C32 C42 C52 119.7(2) . . ? C32 C42 H42 120.2 . . ? C52 C42 H42 120.2 . . ? C62 C52 C42 119.5(2) . . ? C62 C52 H52 120.2 . . ? C42 C52 H52 120.2 . . ? C52 C62 C12 121.9(2) . . ? C52 C62 H62 119.0 . . ? C12 C62 H62 119.0 . . ? N12 C72 C22 122.68(18) . . ? N12 C72 C82 119.32(19) . . ? C22 C72 C82 117.98(17) . . ? C92 C82 C132 119.8(2) . . ? C92 C82 C72 120.7(2) . . ? C132 C82 C72 119.4(2) . . ? C82 C92 C102 120.0(2) . . ? C82 C92 H92 120.0 . . ? C102 C92 H92 120.0 . . ? C112 C102 C92 119.8(2) . . ? C112 C102 H102 120.1 . . ? C92 C102 H102 120.1 . . ? C122 C112 C102 120.5(2) . . ? C122 C112 H112 119.8 . . ? C102 C112 H112 119.8 . . ? C112 C122 C132 119.9(2) . . ? C112 C122 H122 120.0 . . ? C132 C122 H122 120.0 . . ? C82 C132 C122 120.0(2) . . ? C82 C132 H132 120.0 . . ? C122 C132 H132 120.0 . . ? C13 O13 Mn2 124.13(13) . . ? N13 O23 Mn1 112.80(11) . . ? N13 O23 Mn1 110.48(10) . 3_666 ? Mn1 O23 Mn1 98.65(6) . 3_666 ? C73 N13 O23 116.68(16) . . ? C73 N13 Mn2 130.42(14) . . ? O23 N13 Mn2 112.51(12) . . ? O13 C13 C63 117.6(2) . . ? O13 C13 C23 124.53(19) . . ? C63 C13 C23 117.8(2) . . ? C33 C23 C13 119.0(2) . . ? C33 C23 C73 119.04(19) . . ? C13 C23 C73 121.9(2) . . ? C43 C33 C23 121.8(2) . . ? C43 C33 H33 119.1 . . ? C23 C33 H33 119.1 . . ? C33 C43 C53 118.9(2) . . ? C33 C43 H43 120.6 . . ? C53 C43 H43 120.6 . . ? C63 C53 C43 120.7(2) . . ? C63 C53 H53 119.7 . . ? C43 C53 H53 119.7 . . ? C53 C63 C13 121.7(2) . . ? C53 C63 H63 119.2 . . ? C13 C63 H63 119.2 . . ? N13 C73 C23 117.89(19) . . ? N13 C73 C83 120.97(19) . . ? C23 C73 C83 121.11(19) . . ? C93 C83 C133 118.93(19) . . ? C93 C83 C73 120.61(19) . . ? C133 C83 C73 120.45(19) . . ? C103 C93 C83 120.5(2) . . ? C103 C93 H93 119.7 . . ? C83 C93 H93 119.7 . . ? C113 C103 C93 119.9(2) . . ? C113 C103 H103 120.0 . . ? C93 C103 H103 120.0 . . ? C123 C113 C103 120.3(2) . . ? C123 C113 H113 119.8 . . ? C103 C113 H113 119.8 . . ? C113 C123 C133 120.4(2) . . ? C113 C123 H123 119.8 . . ? C133 C123 H123 119.8 . . ? C123 C133 C83 119.9(2) . . ? C123 C133 H133 120.1 . . ? C83 C133 H133 120.1 . . ? C14 O14 Mn2 128.03(12) . . ? C14 O14 H14 107.1 . . ? Mn2 O14 H14 116.9 . . ? O14 C14 C24 111.33(18) . . ? O14 C14 H14A 109.4 . . ? C24 C14 H14A 109.4 . . ? O14 C14 H14B 109.4 . . ? C24 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C15 O15 Mn1 143.28(13) . . ? O15 C15 O25 125.36(19) . . ? O15 C15 C25 117.72(19) . . ? O25 C15 C25 116.90(19) . . ? C35 C25 C15 115.65(19) . . ? C35 C25 H25A 108.4 . . ? C15 C25 H25A 108.4 . . ? C35 C25 H25B 108.4 . . ? C15 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C25 C35 H35A 109.5 . . ? C25 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C25 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C16 O16 Mn3 125.43(13) . . ? C16 O16 H16 117.5 . . ? Mn3 O16 H16 113.4 . . ? O16 C16 C26 110.09(19) . . ? O16 C16 H16A 109.6 . . ? C26 C16 H16A 109.6 . . ? O16 C16 H16B 109.6 . . ? C26 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? C16 C26 H26A 109.5 . . ? C16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Mn1 Mn3 O12 -15.08(12) . . . . ? O1 Mn1 Mn3 O12 -175.53(12) . . . . ? O23 Mn1 Mn3 O12 -156.02(10) . . . . ? N11 Mn1 Mn3 O12 12.90(10) . . . . ? O15 Mn1 Mn3 O12 100.38(10) . . . . ? O23 Mn1 Mn3 O12 -82.02(10) 3_666 . . . ? O11 Mn1 Mn3 O1 160.45(11) . . . . ? O23 Mn1 Mn3 O1 19.51(9) . . . . ? N11 Mn1 Mn3 O1 -171.57(10) . . . . ? O15 Mn1 Mn3 O1 -84.09(9) . . . . ? O23 Mn1 Mn3 O1 93.52(9) 3_666 . . . ? O11 Mn1 Mn3 O21 -16.80(9) . . . . ? O1 Mn1 Mn3 O21 -177.25(9) . . . . ? O23 Mn1 Mn3 O21 -157.74(7) . . . . ? N11 Mn1 Mn3 O21 11.18(7) . . . . ? O15 Mn1 Mn3 O21 98.66(7) . . . . ? O23 Mn1 Mn3 O21 -83.73(6) 3_666 . . . ? O11 Mn1 Mn3 N12 141.37(9) . . . . ? O1 Mn1 Mn3 N12 -19.07(10) . . . . ? O23 Mn1 Mn3 N12 0.44(7) . . . . ? N11 Mn1 Mn3 N12 169.35(8) . . . . ? O15 Mn1 Mn3 N12 -103.17(7) . . . . ? O23 Mn1 Mn3 N12 74.44(7) 3_666 . . . ? O11 Mn1 Mn3 O16 -114.12(9) . . . . ? O1 Mn1 Mn3 O16 85.43(9) . . . . ? O23 Mn1 Mn3 O16 104.94(7) . . . . ? N11 Mn1 Mn3 O16 -86.14(7) . . . . ? O15 Mn1 Mn3 O16 1.34(6) . . . . ? O23 Mn1 Mn3 O16 178.95(5) 3_666 . . . ? O21 Mn3 O1 Mn2 -168.25(8) . . . . ? N12 Mn3 O1 Mn2 -7.21(9) . . . . ? O16 Mn3 O1 Mn2 93.76(9) . . . . ? Mn1 Mn3 O1 Mn2 -170.67(14) . . . . ? O21 Mn3 O1 Mn1 2.43(8) . . . . ? N12 Mn3 O1 Mn1 163.46(8) . . . . ? O16 Mn3 O1 Mn1 -95.57(8) . . . . ? O22 Mn2 O1 Mn3 4.72(9) . . . . ? N13 Mn2 O1 Mn3 -178.73(9) . . . . ? O14 Mn2 O1 Mn3 -90.50(8) . . . . ? O11 Mn2 O1 Mn3 98.84(8) 3_666 . . . ? O22 Mn2 O1 Mn1 -165.85(8) . . . . ? N13 Mn2 O1 Mn1 10.70(8) . . . . ? O14 Mn2 O1 Mn1 98.93(8) . . . . ? O11 Mn2 O1 Mn1 -71.73(8) 3_666 . . . ? O11 Mn1 O1 Mn3 -75.8(3) . . . . ? O23 Mn1 O1 Mn3 -162.90(8) . . . . ? N11 Mn1 O1 Mn3 7.30(8) . . . . ? O15 Mn1 O1 Mn3 101.78(8) . . . . ? O23 Mn1 O1 Mn3 -81.56(8) 3_666 . . . ? O11 Mn1 O1 Mn2 95.0(3) . . . . ? O23 Mn1 O1 Mn2 7.90(8) . . . . ? N11 Mn1 O1 Mn2 178.10(8) . . . . ? O15 Mn1 O1 Mn2 -87.42(9) . . . . ? O23 Mn1 O1 Mn2 89.24(8) 3_666 . . . ? Mn3 Mn1 O1 Mn2 170.80(14) . . . . ? O1 Mn1 O11 C11 129.5(3) . . . . ? O23 Mn1 O11 C11 -143.49(14) . . . . ? N11 Mn1 O11 C11 46.19(14) . . . . ? O15 Mn1 O11 C11 -48.15(14) . . . . ? O23 Mn1 O11 C11 135.18(14) 3_666 . . . ? Mn3 Mn1 O11 C11 70.19(16) . . . . ? O1 Mn1 O11 Mn2 -14.8(3) . . . 3_666 ? O23 Mn1 O11 Mn2 72.18(8) . . . 3_666 ? N11 Mn1 O11 Mn2 -98.14(8) . . . 3_666 ? O15 Mn1 O11 Mn2 167.52(7) . . . 3_666 ? O23 Mn1 O11 Mn2 -9.15(7) 3_666 . . 3_666 ? Mn3 Mn1 O11 Mn2 -74.14(10) . . . 3_666 ? O12 Mn3 O21 N11 164.77(13) . . . . ? O1 Mn3 O21 N11 -17.57(13) . . . . ? N12 Mn3 O21 N11 -115.2(2) . . . . ? O16 Mn3 O21 N11 73.24(13) . . . . ? Mn1 Mn3 O21 N11 -16.15(10) . . . . ? Mn3 O21 N11 C71 -164.31(14) . . . . ? Mn3 O21 N11 Mn1 25.95(16) . . . . ? O11 Mn1 N11 C71 -19.07(18) . . . . ? O1 Mn1 N11 C71 172.20(17) . . . . ? O15 Mn1 N11 C71 73.74(18) . . . . ? O23 Mn1 N11 C71 -105.23(18) 3_666 . . . ? Mn3 Mn1 N11 C71 176.45(19) . . . . ? O11 Mn1 N11 O21 149.23(13) . . . . ? O1 Mn1 N11 O21 -19.50(13) . . . . ? O15 Mn1 N11 O21 -117.96(12) . . . . ? O23 Mn1 N11 O21 63.07(12) 3_666 . . . ? Mn3 Mn1 N11 O21 -15.25(10) . . . . ? Mn1 O11 C11 C61 136.61(16) . . . . ? Mn2 O11 C11 C61 -77.9(2) 3_666 . . . ? Mn1 O11 C11 C21 -47.1(2) . . . . ? Mn2 O11 C11 C21 98.43(19) 3_666 . . . ? O11 C11 C21 C31 -175.64(17) . . . . ? C61 C11 C21 C31 0.7(3) . . . . ? O11 C11 C21 C71 5.2(3) . . . . ? C61 C11 C21 C71 -178.48(19) . . . . ? C11 C21 C31 C41 -1.4(3) . . . . ? C71 C21 C31 C41 177.79(19) . . . . ? C21 C31 C41 C51 0.8(3) . . . . ? C31 C41 C51 C61 0.6(3) . . . . ? C41 C51 C61 C11 -1.3(3) . . . . ? O11 C11 C61 C51 177.07(19) . . . . ? C21 C11 C61 C51 0.6(3) . . . . ? O21 N11 C71 C21 -178.80(16) . . . . ? Mn1 N11 C71 C21 -10.5(3) . . . . ? O21 N11 C71 C81 2.3(3) . . . . ? Mn1 N11 C71 C81 170.58(14) . . . . ? C31 C21 C71 N11 -154.73(19) . . . . ? C11 C21 C71 N11 24.4(3) . . . . ? C31 C21 C71 C81 24.2(3) . . . . ? C11 C21 C71 C81 -156.7(2) . . . . ? N11 C71 C81 C91 -129.2(2) . . . . ? C21 C71 C81 C91 51.9(3) . . . . ? N11 C71 C81 C131 51.5(3) . . . . ? C21 C71 C81 C131 -127.4(2) . . . . ? C131 C81 C91 C101 -1.4(3) . . . . ? C71 C81 C91 C101 179.28(18) . . . . ? C81 C91 C101 C111 2.2(3) . . . . ? C91 C101 C111 C121 -1.0(3) . . . . ? C101 C111 C121 C131 -1.0(3) . . . . ? C111 C121 C131 C81 1.9(3) . . . . ? C91 C81 C131 C121 -0.7(3) . . . . ? C71 C81 C131 C121 178.66(18) . . . . ? O21 Mn3 O12 C12 153.51(18) . . . . ? N12 Mn3 O12 C12 -7.65(18) . . . . ? O16 Mn3 O12 C12 -108.65(18) . . . . ? Mn1 Mn3 O12 C12 151.99(14) . . . . ? O13 Mn2 O22 N12 -178.63(13) . . . . ? O1 Mn2 O22 N12 1.78(13) . . . . ? O14 Mn2 O22 N12 92.02(13) . . . . ? O11 Mn2 O22 N12 -87.73(13) 3_666 . . . ? Mn2 O22 N12 C72 172.21(13) . . . . ? Mn2 O22 N12 Mn3 -7.08(18) . . . . ? O12 Mn3 N12 C72 6.50(17) . . . . ? O1 Mn3 N12 C72 -170.91(17) . . . . ? O21 Mn3 N12 C72 -72.8(3) . . . . ? O16 Mn3 N12 C72 98.72(17) . . . . ? Mn1 Mn3 N12 C72 -161.21(15) . . . . ? O12 Mn3 N12 O22 -174.31(13) . . . . ? O1 Mn3 N12 O22 8.28(13) . . . . ? O21 Mn3 N12 O22 106.4(2) . . . . ? O16 Mn3 N12 O22 -82.09(14) . . . . ? Mn1 Mn3 N12 O22 17.98(15) . . . . ? Mn3 O12 C12 C62 -175.27(15) . . . . ? Mn3 O12 C12 C22 5.7(3) . . . . ? O12 C12 C22 C32 179.48(18) . . . . ? C62 C12 C22 C32 0.4(3) . . . . ? O12 C12 C22 C72 0.4(3) . . . . ? C62 C12 C22 C72 -178.6(2) . . . . ? C12 C22 C32 C42 -0.7(3) . . . . ? C72 C22 C32 C42 178.4(2) . . . . ? C22 C32 C42 C52 0.5(3) . . . . ? C32 C42 C52 C62 0.0(3) . . . . ? C42 C52 C62 C12 -0.3(3) . . . . ? O12 C12 C62 C52 -179.08(19) . . . . ? C22 C12 C62 C52 0.0(3) . . . . ? O22 N12 C72 C22 177.19(18) . . . . ? Mn3 N12 C72 C22 -3.6(3) . . . . ? O22 N12 C72 C82 -1.3(3) . . . . ? Mn3 N12 C72 C82 177.87(14) . . . . ? C32 C22 C72 N12 179.90(19) . . . . ? C12 C22 C72 N12 -1.1(3) . . . . ? C32 C22 C72 C82 -1.6(3) . . . . ? C12 C22 C72 C82 177.46(19) . . . . ? N12 C72 C82 C92 85.4(3) . . . . ? C22 C72 C82 C92 -93.2(3) . . . . ? N12 C72 C82 C132 -99.7(2) . . . . ? C22 C72 C82 C132 81.7(3) . . . . ? C132 C82 C92 C102 1.0(3) . . . . ? C72 C82 C92 C102 175.9(2) . . . . ? C82 C92 C102 C112 0.0(4) . . . . ? C92 C102 C112 C122 -0.3(4) . . . . ? C102 C112 C122 C132 -0.5(4) . . . . ? C92 C82 C132 C122 -1.8(3) . . . . ? C72 C82 C132 C122 -176.73(19) . . . . ? C112 C122 C132 C82 1.5(3) . . . . ? O22 Mn2 O13 C13 -144.43(15) . . . . ? N13 Mn2 O13 C13 39.02(15) . . . . ? O14 Mn2 O13 C13 -49.27(15) . . . . ? O11 Mn2 O13 C13 121.39(15) 3_666 . . . ? O11 Mn1 O23 N13 157.30(11) . . . . ? O1 Mn1 O23 N13 -34.03(11) . . . . ? O15 Mn1 O23 N13 64.37(11) . . . . ? O23 Mn1 O23 N13 -116.61(12) 3_666 . . . ? Mn3 Mn1 O23 N13 -43.75(12) . . . . ? O11 Mn1 O23 Mn1 -86.09(6) . . . 3_666 ? O1 Mn1 O23 Mn1 82.58(6) . . . 3_666 ? O15 Mn1 O23 Mn1 -179.02(5) . . . 3_666 ? O23 Mn1 O23 Mn1 0.0 3_666 . . 3_666 ? Mn3 Mn1 O23 Mn1 72.86(5) . . . 3_666 ? Mn1 O23 N13 C73 -137.70(14) . . . . ? Mn1 O23 N13 C73 112.95(16) 3_666 . . . ? Mn1 O23 N13 Mn2 48.73(13) . . . . ? Mn1 O23 N13 Mn2 -60.61(12) 3_666 . . . ? O13 Mn2 N13 C73 -26.98(18) . . . . ? O1 Mn2 N13 C73 152.29(18) . . . . ? O14 Mn2 N13 C73 62.12(18) . . . . ? O11 Mn2 N13 C73 -118.01(18) 3_666 . . . ? O13 Mn2 N13 O23 145.46(12) . . . . ? O1 Mn2 N13 O23 -35.27(11) . . . . ? O14 Mn2 N13 O23 -125.44(11) . . . . ? O11 Mn2 N13 O23 54.43(11) 3_666 . . . ? Mn2 O13 C13 C63 151.85(14) . . . . ? Mn2 O13 C13 C23 -31.0(3) . . . . ? O13 C13 C23 C33 177.40(19) . . . . ? C63 C13 C23 C33 -5.5(3) . . . . ? O13 C13 C23 C73 -6.2(3) . . . . ? C63 C13 C23 C73 170.93(19) . . . . ? C13 C23 C33 C43 3.4(3) . . . . ? C73 C23 C33 C43 -173.05(19) . . . . ? C23 C33 C43 C53 1.2(3) . . . . ? C33 C43 C53 C63 -3.7(3) . . . . ? C43 C53 C63 C13 1.5(3) . . . . ? O13 C13 C63 C53 -179.56(19) . . . . ? C23 C13 C63 C53 3.1(3) . . . . ? O23 N13 C73 C23 -168.72(16) . . . . ? Mn2 N13 C73 C23 3.5(3) . . . . ? O23 N13 C73 C83 9.4(3) . . . . ? Mn2 N13 C73 C83 -178.47(14) . . . . ? C33 C23 C73 N13 -164.07(19) . . . . ? C13 C23 C73 N13 19.5(3) . . . . ? C33 C23 C73 C83 17.9(3) . . . . ? C13 C23 C73 C83 -158.52(19) . . . . ? N13 C73 C83 C93 -130.0(2) . . . . ? C23 C73 C83 C93 48.0(3) . . . . ? N13 C73 C83 C133 49.4(3) . . . . ? C23 C73 C83 C133 -132.6(2) . . . . ? C133 C83 C93 C103 -0.4(3) . . . . ? C73 C83 C93 C103 178.96(19) . . . . ? C83 C93 C103 C113 1.1(3) . . . . ? C93 C103 C113 C123 -1.0(3) . . . . ? C103 C113 C123 C133 0.4(3) . . . . ? C113 C123 C133 C83 0.2(3) . . . . ? C93 C83 C133 C123 -0.2(3) . . . . ? C73 C83 C133 C123 -179.61(19) . . . . ? O13 Mn2 O14 C14 -57.24(17) . . . . ? O1 Mn2 O14 C14 127.99(16) . . . . ? O22 Mn2 O14 C14 36.42(17) . . . . ? N13 Mn2 O14 C14 -144.31(17) . . . . ? Mn2 O14 C14 C24 124.72(17) . . . . ? O11 Mn1 O15 C15 166.5(2) . . . . ? O1 Mn1 O15 C15 -13.0(2) . . . . ? O23 Mn1 O15 C15 -103.2(2) . . . . ? N11 Mn1 O15 C15 77.9(2) . . . . ? Mn3 Mn1 O15 C15 17.6(2) . . . . ? Mn1 O15 C15 O25 0.0(4) . . . . ? Mn1 O15 C15 C25 178.93(16) . . . . ? O15 C15 C25 C35 13.9(3) . . . . ? O25 C15 C25 C35 -167.02(19) . . . . ? O12 Mn3 O16 C16 -4.13(15) . . . . ? O1 Mn3 O16 C16 175.01(14) . . . . ? O21 Mn3 O16 C16 82.08(15) . . . . ? N12 Mn3 O16 C16 -95.12(15) . . . . ? Mn1 Mn3 O16 C16 144.09(14) . . . . ? Mn3 O16 C16 C26 84.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O25 0.86 1.84 2.695(2) 175.7 . O16 H16 O25 0.86 1.79 2.639(2) 172.6 . _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.44 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.077 # Attachment 'Complex_3.cif' data_EB8125 _database_code_depnum_ccdc_archive 'CCDC 793023' #TrackingRef 'Complex_3.cif' _audit_creation_date 08-08-04 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8125 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _exptl_crystal_recrystallization_method ; Diffusion of Et~2~O into MeCN/MeOH solution. ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Checkcif alerts 912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1491 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 6 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 2 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 6 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 5041 5035 6 23.01 0.550 0.999 6715 6709 6 25.24 0.600 0.999 8719 8711 8 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.996 11082 11041 41 29.84 0.700 0.928 13843 12843 1000 30.56 0.715 0.898 14670 13171 1499 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.02 097_ALERT_2_C Maximum (Positive) Residual Density ............ 1.98 e/A** 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 44.00 A**3 There is a single peak of electron density. This could be a partially- occupied water molecule. The output from Platon SQUEEZE indicates that the total amount of residual electron density is about 12e, equivalent to a single water molecule. However this has not beem modelled, nor has the SQUEEZE output been applied. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.96 Ratio 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 8 No action. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 13.8863(4) _cell_length_b 14.4013(4) _cell_length_c 15.7519(5) _cell_angle_alpha 116.3910(10) _cell_angle_beta 90.639(2) _cell_angle_gamma 117.4650(10) _cell_volume 2409.38(13) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C104 H100 Mn6 N6 O22 # Dc = 1.46 Fooo = 1092.00 Mu = 8.39 M = 1057.77 # Found Formula = C104 H100 Mn6 N6 O22 # Dc = 1.46 FOOO = 1092.00 Mu = 8.39 M = 1057.77 _chemical_formula_sum 'C104 H100 Mn6 N6 O22' _chemical_formula_moiety 'C104 H100 Mn6 N6 O22' _chemical_compound_source 'Ross Inglis, RI1308' _chemical_formula_weight 2115.53 _cell_measurement_reflns_used 9907 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _cell_measurement_temperature 150 _exptl_crystal_description rod _exptl_crystal_colour 'dark brown' _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 0.839 # Sheldrick geometric approximatio 0.89 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.89 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 31740 _reflns_number_total 13171 _diffrn_reflns_av_R_equivalents 0.049 # Number of reflections with Friedels Law is 13171 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14780 _diffrn_reflns_theta_min 1.976 _diffrn_reflns_theta_max 30.560 _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 27.504 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min -19 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 1.22 _oxford_diffrn_Wilson_scale 133.58 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.98 _refine_diff_density_max 1.98 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 13140 _refine_ls_number_restraints 0 _refine_ls_number_parameters 622 _oxford_refine_ls_R_factor_ref 0.0962 _refine_ls_wR_factor_ref 0.1652 _refine_ls_goodness_of_fit_ref 0.9012 _refine_ls_shift/su_max 0.000551 # The values computed from all data _oxford_reflns_number_all 13140 _refine_ls_R_factor_all 0.0962 _refine_ls_wR_factor_all 0.1652 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9837 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_gt 0.1322 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.89405(5) 0.93192(5) 0.53298(4) 0.0147 1.0000 Uani . . . . . . . Mn2 Mn 0.78258(5) 0.66228(5) 0.34366(4) 0.0169 1.0000 Uani . . . . . . . Mn3 Mn 1.03891(5) 0.79901(5) 0.47639(4) 0.0162 1.0000 Uani . . . . . . . O4 O 0.9021(2) 0.7931(2) 0.45284(19) 0.0160 1.0000 Uani . . . . . . . O5 O 0.8837(2) 1.0734(2) 0.5900(2) 0.0181 1.0000 Uani . . . . . . . C6 C 0.8004(3) 1.0719(4) 0.6325(3) 0.0197 1.0000 Uani . . . . . . . C7 C 0.8264(4) 1.1766(4) 0.7214(3) 0.0243 1.0000 Uani . . . . . . . C8 C 0.7443(4) 1.1819(4) 0.7686(3) 0.0271 1.0000 Uani . . . . . . . C9 C 0.6337(4) 1.0829(4) 0.7285(4) 0.0301 1.0000 Uani . . . . . . . C10 C 0.6070(3) 0.9802(4) 0.6408(3) 0.0230 1.0000 Uani . . . . . . . C11 C 0.6892(3) 0.9720(4) 0.5898(3) 0.0187 1.0000 Uani . . . . . . . C12 C 0.6545(3) 0.8607(3) 0.4962(3) 0.0177 1.0000 Uani . . . . . . . N13 N 0.7305(3) 0.8366(3) 0.4633(2) 0.0185 1.0000 Uani . . . . . . . O14 O 0.6960(2) 0.7382(3) 0.3714(2) 0.0221 1.0000 Uani . . . . . . . C15 C 0.5335(3) 0.7751(4) 0.4423(3) 0.0227 1.0000 Uani . . . . . . . C16 C 0.4687(4) 0.8140(5) 0.4179(4) 0.0361 1.0000 Uani . . . . . . . C17 C 0.3531(4) 0.7357(7) 0.3762(4) 0.0486 1.0000 Uani . . . . . . . C18 C 0.3015(4) 0.6205(6) 0.3593(4) 0.0492 1.0000 Uani . . . . . . . C19 C 0.3654(5) 0.5799(5) 0.3819(5) 0.0486 1.0000 Uani . . . . . . . C20 C 0.4811(4) 0.6566(4) 0.4236(4) 0.0359 1.0000 Uani . . . . . . . O21 O 0.6735(3) 0.5445(3) 0.2251(2) 0.0258 1.0000 Uani . . . . . . . C22 C 0.6642(3) 0.4490(4) 0.1478(3) 0.0223 1.0000 Uani . . . . . . . C23 C 0.5667(4) 0.3762(4) 0.0682(3) 0.0247 1.0000 Uani . . . . . . . C24 C 0.5482(4) 0.2709(4) -0.0118(3) 0.0316 1.0000 Uani . . . . . . . C25 C 0.6259(4) 0.2350(5) -0.0160(4) 0.0371 1.0000 Uani . . . . . . . C26 C 0.7239(4) 0.3082(4) 0.0584(3) 0.0352 1.0000 Uani . . . . . . . C27 C 0.7471(4) 0.4178(4) 0.1410(3) 0.0267 1.0000 Uani . . . . . . . C28 C 0.8555(3) 0.4935(4) 0.2147(3) 0.0216 1.0000 Uani . . . . . . . N29 N 0.8810(3) 0.5923(3) 0.2960(2) 0.0191 1.0000 Uani . . . . . . . O30 O 0.9861(2) 0.6507(2) 0.35634(19) 0.0198 1.0000 Uani . . . . . . . C31 C 0.9403(4) 0.4554(4) 0.1933(3) 0.0262 1.0000 Uani . . . . . . . C32 C 1.0095(4) 0.4890(4) 0.1367(3) 0.0324 1.0000 Uani . . . . . . . C33 C 1.0820(4) 0.4456(5) 0.1090(4) 0.0375 1.0000 Uani . . . . . . . C34 C 1.0835(4) 0.3682(5) 0.1369(4) 0.0389 1.0000 Uani . . . . . . . C35 C 1.0144(4) 0.3342(5) 0.1933(4) 0.0365 1.0000 Uani . . . . . . . C36 C 0.9431(4) 0.3791(4) 0.2224(3) 0.0299 1.0000 Uani . . . . . . . O37 O 1.1747(2) 0.8096(3) 0.5084(2) 0.0218 1.0000 Uani . . . . . . . C38 C 1.2247(3) 0.8475(4) 0.5999(3) 0.0198 1.0000 Uani . . . . . . . C39 C 1.2817(4) 0.7930(4) 0.6115(3) 0.0274 1.0000 Uani . . . . . . . C40 C 1.3346(4) 0.8265(4) 0.7030(4) 0.0310 1.0000 Uani . . . . . . . C41 C 1.3312(4) 0.9155(4) 0.7873(3) 0.0291 1.0000 Uani . . . . . . . C42 C 1.2782(4) 0.9720(4) 0.7786(3) 0.0244 1.0000 Uani . . . . . . . C43 C 1.2249(3) 0.9412(3) 0.6850(3) 0.0177 1.0000 Uani . . . . . . . C44 C 1.1720(3) 1.0065(3) 0.6796(3) 0.0166 1.0000 Uani . . . . . . . N45 N 1.0972(3) 0.9578(3) 0.5994(2) 0.0177 1.0000 Uani . . . . . . . O46 O 1.0577(2) 1.0269(2) 0.59119(19) 0.0159 1.0000 Uani . . . . . . . C47 C 1.2037(4) 1.1267(4) 0.7654(3) 0.0228 1.0000 Uani . . . . . . . C48 C 1.3164(4) 1.2191(4) 0.8101(3) 0.0243 1.0000 Uani . . . . . . . C49 C 1.3443(4) 1.3289(4) 0.8928(3) 0.0324 1.0000 Uani . . . . . . . C50 C 1.2620(5) 1.3451(4) 0.9311(3) 0.0344 1.0000 Uani . . . . . . . C51 C 1.1500(5) 1.2542(5) 0.8875(3) 0.0349 1.0000 Uani . . . . . . . C52 C 1.1207(4) 1.1452(4) 0.8043(3) 0.0269 1.0000 Uani . . . . . . . O53 O 0.8645(2) 0.9061(3) 0.6533(2) 0.0210 1.0000 Uani . . . . . . . C54 C 0.8112(3) 0.8241(4) 0.6726(3) 0.0207 1.0000 Uani . . . . . . . O55 O 0.7821(3) 0.7139(3) 0.6186(2) 0.0284 1.0000 Uani . . . . . . . C56 C 0.7821(3) 0.8596(4) 0.7714(3) 0.0184 1.0000 Uani . . . . . . . C57 C 0.8511(4) 0.8465(4) 0.8376(3) 0.0267 1.0000 Uani . . . . . . . C58 C 0.8226(4) 0.8798(5) 0.9373(3) 0.0306 1.0000 Uani . . . . . . . C59 C 0.6559(4) 0.7743(4) 0.7555(3) 0.0270 1.0000 Uani . . . . . . . C60 C 0.6264(4) 0.8060(5) 0.8546(3) 0.0306 1.0000 Uani . . . . . . . C61 C 0.6976(4) 0.7933(5) 0.9187(4) 0.0328 1.0000 Uani . . . . . . . C62 C 0.8078(4) 0.9906(4) 0.8235(3) 0.0262 1.0000 Uani . . . . . . . C63 C 0.7794(4) 1.0231(4) 0.9229(3) 0.0330 1.0000 Uani . . . . . . . C64 C 0.6532(4) 0.9373(5) 0.9055(4) 0.0369 1.0000 Uani . . . . . . . C65 C 0.8489(4) 1.0106(5) 0.9884(3) 0.0380 1.0000 Uani . . . . . . . O66 O 0.7163(3) 0.5727(3) 0.4260(2) 0.0289 1.0000 Uani . . . . . . . C67 C 0.6177(5) 0.4592(5) 0.3945(4) 0.0470 1.0000 Uani . . . . . . . O68 O 0.9704(3) 0.7125(3) 0.5684(2) 0.0242 1.0000 Uani . . . . . . . C69 C 0.9506(5) 0.5944(4) 0.5368(4) 0.0340 1.0000 Uani . . . . . . . H71 H 0.8997 1.2425 0.7480 0.0250 1.0000 Uiso R . . . . . . H81 H 0.7620 1.2523 0.8276 0.0304 1.0000 Uiso R . . . . . . H91 H 0.5778 1.0852 0.7604 0.0370 1.0000 Uiso R . . . . . . H101 H 0.5328 0.9133 0.6150 0.0270 1.0000 Uiso R . . . . . . H161 H 0.5036 0.8920 0.4281 0.0448 1.0000 Uiso R . . . . . . H171 H 0.3103 0.7621 0.3606 0.0621 1.0000 Uiso R . . . . . . H181 H 0.2244 0.5704 0.3332 0.0442 1.0000 Uiso R . . . . . . H191 H 0.3307 0.5020 0.3706 0.0448 1.0000 Uiso R . . . . . . H201 H 0.5235 0.6290 0.4397 0.0405 1.0000 Uiso R . . . . . . H231 H 0.5129 0.3984 0.0711 0.0251 1.0000 Uiso R . . . . . . H241 H 0.4821 0.2237 -0.0631 0.0275 1.0000 Uiso R . . . . . . H251 H 0.6114 0.1614 -0.0698 0.0332 1.0000 Uiso R . . . . . . H261 H 0.7762 0.2847 0.0542 0.0341 1.0000 Uiso R . . . . . . H321 H 1.0079 0.5405 0.1174 0.0329 1.0000 Uiso R . . . . . . H331 H 1.1281 0.4694 0.0728 0.0407 1.0000 Uiso R . . . . . . H341 H 1.1315 0.3397 0.1182 0.0402 1.0000 Uiso R . . . . . . H351 H 1.0140 0.2810 0.2113 0.0407 1.0000 Uiso R . . . . . . H361 H 0.8963 0.3557 0.2589 0.0331 1.0000 Uiso R . . . . . . H391 H 1.2832 0.7329 0.5556 0.0319 1.0000 Uiso R . . . . . . H401 H 1.3726 0.7896 0.7095 0.0391 1.0000 Uiso R . . . . . . H411 H 1.3645 0.9352 0.8493 0.0339 1.0000 Uiso R . . . . . . H421 H 1.2761 1.0311 0.8350 0.0260 1.0000 Uiso R . . . . . . H481 H 1.3726 1.2079 0.7842 0.0257 1.0000 Uiso R . . . . . . H491 H 1.4194 1.3908 0.9214 0.0320 1.0000 Uiso R . . . . . . H501 H 1.2828 1.4190 0.9878 0.0360 1.0000 Uiso R . . . . . . H511 H 1.0937 1.2659 0.9138 0.0397 1.0000 Uiso R . . . . . . H521 H 1.0447 1.0837 0.7744 0.0293 1.0000 Uiso R . . . . . . H571 H 0.9302 0.9013 0.8473 0.0322 1.0000 Uiso R . . . . . . H572 H 0.8336 0.7626 0.8041 0.0318 1.0000 Uiso R . . . . . . H581 H 0.8670 0.8727 0.9795 0.0357 1.0000 Uiso R . . . . . . H591 H 0.6404 0.6927 0.7241 0.0278 1.0000 Uiso R . . . . . . H592 H 0.6114 0.7800 0.7127 0.0283 1.0000 Uiso R . . . . . . H601 H 0.5454 0.7497 0.8425 0.0320 1.0000 Uiso R . . . . . . H611 H 0.6783 0.8119 0.9807 0.0381 1.0000 Uiso R . . . . . . H612 H 0.6812 0.7096 0.8855 0.0380 1.0000 Uiso R . . . . . . H622 H 0.8883 1.0448 0.8360 0.0313 1.0000 Uiso R . . . . . . H621 H 0.7651 1.0000 0.7824 0.0308 1.0000 Uiso R . . . . . . H631 H 0.7955 1.1071 0.9553 0.0369 1.0000 Uiso R . . . . . . H642 H 0.6343 0.9576 0.9679 0.0450 1.0000 Uiso R . . . . . . H641 H 0.6095 0.9470 0.8650 0.0446 1.0000 Uiso R . . . . . . H651 H 0.9281 1.0650 0.9988 0.0341 1.0000 Uiso R . . . . . . H652 H 0.8315 1.0315 1.0513 0.0342 1.0000 Uiso R . . . . . . H691 H 0.9243 0.5698 0.5830 0.0550 1.0000 Uiso R . . . . . . H693 H 1.0193 0.5960 0.5303 0.0551 1.0000 Uiso R . . . . . . H692 H 0.8956 0.5377 0.4741 0.0550 1.0000 Uiso R . . . . . . H681 H 0.9149 0.7109 0.5834 0.0364 1.0000 Uiso R . . . . . . H673 H 0.5899 0.4162 0.3253 0.0537 1.0000 Uiso R . . . . . . H672 H 0.6364 0.4132 0.4130 0.0536 1.0000 Uiso R . . . . . . H671 H 0.5612 0.4699 0.4249 0.0534 1.0000 Uiso R . . . . . . H661 H 0.7356 0.6157 0.4850 0.0324 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0138(2) 0.0136(3) 0.0127(2) 0.0034(2) 0.00299(19) 0.0074(2) Mn2 0.0165(3) 0.0151(3) 0.0119(2) 0.0016(2) 0.0005(2) 0.0084(2) Mn3 0.0163(3) 0.0156(3) 0.0120(2) 0.0024(2) 0.0009(2) 0.0094(2) O4 0.0153(12) 0.0151(12) 0.0127(12) 0.0031(10) 0.0010(9) 0.0083(10) O5 0.0178(13) 0.0159(12) 0.0175(13) 0.0051(10) 0.0051(10) 0.0097(11) C6 0.0203(18) 0.0207(18) 0.0197(18) 0.0094(15) 0.0074(14) 0.0126(16) C7 0.0209(19) 0.0189(18) 0.024(2) 0.0051(16) 0.0068(16) 0.0098(16) C8 0.028(2) 0.025(2) 0.023(2) 0.0087(16) 0.0110(17) 0.0131(18) C9 0.029(2) 0.034(2) 0.030(2) 0.0154(19) 0.0170(19) 0.019(2) C10 0.0198(18) 0.029(2) 0.0209(19) 0.0114(16) 0.0124(15) 0.0138(17) C11 0.0233(18) 0.0186(17) 0.0168(17) 0.0073(14) 0.0063(14) 0.0142(15) C12 0.0203(17) 0.0182(17) 0.0131(16) 0.0064(13) 0.0018(13) 0.0105(15) N13 0.0187(15) 0.0151(14) 0.0149(14) 0.0026(12) 0.0018(12) 0.0087(12) O14 0.0198(13) 0.0211(14) 0.0155(13) 0.0016(11) 0.0003(10) 0.0110(12) C15 0.0147(17) 0.0240(19) 0.0219(19) 0.0067(15) 0.0022(14) 0.0096(15) C16 0.028(2) 0.047(3) 0.040(3) 0.025(2) 0.009(2) 0.021(2) C17 0.023(2) 0.093(5) 0.039(3) 0.041(3) 0.009(2) 0.030(3) C18 0.018(2) 0.062(4) 0.034(3) 0.013(3) 0.0016(19) 0.008(2) C19 0.033(3) 0.029(3) 0.053(3) 0.008(2) 0.014(3) 0.007(2) C20 0.027(2) 0.028(2) 0.047(3) 0.014(2) 0.014(2) 0.014(2) O21 0.0223(14) 0.0232(15) 0.0178(13) -0.0011(11) -0.0024(11) 0.0130(12) C22 0.0218(19) 0.0211(19) 0.0187(18) 0.0071(15) 0.0037(15) 0.0101(16) C23 0.0196(18) 0.028(2) 0.0172(18) 0.0064(16) 0.0036(15) 0.0105(16) C24 0.024(2) 0.030(2) 0.020(2) 0.0021(17) -0.0025(16) 0.0093(18) C25 0.029(2) 0.031(2) 0.025(2) -0.0032(18) -0.0013(18) 0.013(2) C26 0.033(2) 0.032(2) 0.023(2) -0.0035(18) -0.0019(18) 0.021(2) C27 0.024(2) 0.024(2) 0.0195(19) 0.0024(16) -0.0012(15) 0.0123(17) C28 0.0230(19) 0.0192(18) 0.0149(17) 0.0023(14) 0.0004(14) 0.0117(16) N29 0.0232(16) 0.0228(16) 0.0079(13) 0.0043(12) 0.0025(12) 0.0130(14) O30 0.0200(13) 0.0167(12) 0.0132(12) 0.0001(10) -0.0034(10) 0.0101(11) C31 0.026(2) 0.0193(19) 0.0166(18) -0.0041(14) -0.0034(15) 0.0131(17) C32 0.034(2) 0.028(2) 0.025(2) 0.0037(18) 0.0053(18) 0.018(2) C33 0.033(3) 0.037(3) 0.033(3) 0.009(2) 0.012(2) 0.021(2) C34 0.034(3) 0.037(3) 0.031(2) 0.000(2) 0.004(2) 0.025(2) C35 0.040(3) 0.033(2) 0.031(2) 0.005(2) 0.003(2) 0.027(2) C36 0.031(2) 0.029(2) 0.026(2) 0.0068(18) 0.0065(18) 0.021(2) O37 0.0208(13) 0.0278(15) 0.0129(12) 0.0049(11) 0.0026(10) 0.0150(12) C38 0.0174(17) 0.0253(19) 0.0167(17) 0.0088(15) 0.0029(14) 0.0130(15) C39 0.029(2) 0.027(2) 0.025(2) 0.0063(17) 0.0055(17) 0.0198(18) C40 0.032(2) 0.035(2) 0.033(2) 0.015(2) 0.0052(19) 0.023(2) C41 0.034(2) 0.031(2) 0.023(2) 0.0113(18) -0.0010(17) 0.019(2) C42 0.030(2) 0.024(2) 0.0136(17) 0.0071(15) -0.0002(15) 0.0128(17) C43 0.0149(16) 0.0199(17) 0.0143(16) 0.0061(14) 0.0006(13) 0.0088(14) C44 0.0172(16) 0.0141(16) 0.0136(16) 0.0049(13) 0.0063(13) 0.0066(14) N45 0.0190(15) 0.0153(14) 0.0143(14) 0.0042(12) 0.0017(12) 0.0090(13) O46 0.0173(12) 0.0140(12) 0.0147(12) 0.0029(10) 0.0016(10) 0.0111(10) C47 0.029(2) 0.0189(18) 0.0116(16) 0.0011(14) 0.0000(14) 0.0123(16) C48 0.023(2) 0.024(2) 0.0193(18) 0.0083(16) 0.0019(15) 0.0104(17) C49 0.040(3) 0.0184(19) 0.024(2) 0.0057(16) -0.0079(18) 0.0095(19) C50 0.049(3) 0.023(2) 0.020(2) 0.0020(17) 0.0028(19) 0.019(2) C51 0.041(3) 0.034(2) 0.022(2) 0.0058(19) 0.0115(19) 0.021(2) C52 0.030(2) 0.027(2) 0.0172(18) 0.0075(16) 0.0100(16) 0.0143(18) O53 0.0217(14) 0.0240(14) 0.0159(13) 0.0114(11) 0.0083(11) 0.0097(12) C54 0.0190(18) 0.0227(19) 0.0151(17) 0.0070(14) 0.0037(14) 0.0096(15) O55 0.0403(18) 0.0230(15) 0.0201(14) 0.0086(12) 0.0156(13) 0.0173(14) C56 0.0229(18) 0.0201(18) 0.0137(16) 0.0088(14) 0.0091(14) 0.0119(15) C57 0.026(2) 0.033(2) 0.023(2) 0.0145(18) 0.0081(16) 0.0167(19) C58 0.029(2) 0.039(3) 0.019(2) 0.0140(18) 0.0004(16) 0.014(2) C59 0.026(2) 0.030(2) 0.0189(19) 0.0103(17) 0.0036(16) 0.0120(18) C60 0.026(2) 0.036(2) 0.023(2) 0.0128(19) 0.0064(17) 0.0122(19) C61 0.033(2) 0.039(3) 0.025(2) 0.021(2) 0.0157(19) 0.014(2) C62 0.032(2) 0.022(2) 0.023(2) 0.0115(16) 0.0108(17) 0.0127(18) C63 0.044(3) 0.027(2) 0.022(2) 0.0084(18) 0.0144(19) 0.019(2) C64 0.039(3) 0.048(3) 0.028(2) 0.015(2) 0.018(2) 0.029(2) C65 0.034(3) 0.036(3) 0.017(2) 0.0040(18) 0.0060(18) 0.009(2) O66 0.0275(16) 0.0199(14) 0.0192(14) 0.0052(12) 0.0017(12) 0.0026(12) C67 0.048(3) 0.027(3) 0.033(3) 0.009(2) 0.008(2) 0.002(2) O68 0.0283(15) 0.0212(14) 0.0225(14) 0.0089(12) 0.0074(12) 0.0145(13) C69 0.043(3) 0.030(2) 0.036(3) 0.020(2) 0.013(2) 0.021(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3835(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . O46 2_776 2.306(3) yes Mn1 . Mn1 2_776 3.1844(12) yes Mn1 . Mn2 . 3.2290(8) yes Mn1 . Mn3 . 3.2526(8) yes Mn1 . O4 . 1.890(3) yes Mn1 . O5 . 1.904(3) yes Mn1 . N13 . 1.994(3) yes Mn1 . O46 . 1.962(3) yes Mn1 . O53 . 2.098(3) yes Mn2 . O4 . 1.853(3) yes Mn2 . O14 . 1.906(3) yes Mn2 . O21 . 1.847(3) yes Mn2 . N29 . 2.016(3) yes Mn2 . O66 . 2.147(3) yes Mn3 . O5 2_776 2.353(3) yes Mn3 . O4 . 1.886(3) yes Mn3 . O30 . 1.900(3) yes Mn3 . O37 . 1.864(3) yes Mn3 . N45 . 1.989(3) yes Mn3 . O68 . 2.258(3) yes O5 . C6 . 1.338(5) yes C6 . C7 . 1.406(5) yes C6 . C11 . 1.405(5) yes C7 . C8 . 1.381(6) yes C7 . H71 . 0.926 no C8 . C9 . 1.396(6) yes C8 . H81 . 0.938 no C9 . C10 . 1.379(6) yes C9 . H91 . 0.935 no C10 . C11 . 1.422(5) yes C10 . H101 . 0.939 no C11 . C12 . 1.465(5) yes C12 . N13 . 1.301(5) yes C12 . C15 . 1.480(5) yes N13 . O14 . 1.366(4) yes C15 . C16 . 1.384(6) yes C15 . C20 . 1.390(7) yes C16 . C17 . 1.388(7) yes C16 . H161 . 0.926 no C17 . C18 . 1.359(10) yes C17 . H171 . 0.920 no C18 . C19 . 1.382(9) yes C18 . H181 . 0.922 no C19 . C20 . 1.388(7) yes C19 . H191 . 0.919 no C20 . H201 . 0.934 no O21 . C22 . 1.317(5) yes C22 . C23 . 1.410(6) yes C22 . C27 . 1.406(6) yes C23 . C24 . 1.374(6) yes C23 . H231 . 0.933 no C24 . C25 . 1.385(7) yes C24 . H241 . 0.937 no C25 . C26 . 1.371(6) yes C25 . H251 . 0.939 no C26 . C27 . 1.409(6) yes C26 . H261 . 0.925 no C27 . C28 . 1.457(5) yes C28 . N29 . 1.303(5) yes C28 . C31 . 1.497(6) yes N29 . O30 . 1.367(4) yes C31 . C32 . 1.388(7) yes C31 . C36 . 1.381(7) yes C32 . C33 . 1.394(7) yes C32 . H321 . 0.926 no C33 . C34 . 1.376(8) yes C33 . H331 . 0.913 no C34 . C35 . 1.387(8) yes C34 . H341 . 0.922 no C35 . C36 . 1.394(6) yes C35 . H351 . 0.926 no C36 . H361 . 0.920 no O37 . C38 . 1.337(5) yes C38 . C39 . 1.406(6) yes C38 . C43 . 1.416(5) yes C39 . C40 . 1.371(6) yes C39 . H391 . 0.930 no C40 . C41 . 1.397(6) yes C40 . H401 . 0.936 no C41 . C42 . 1.369(6) yes C41 . H411 . 0.934 no C42 . C43 . 1.417(5) yes C42 . H421 . 0.931 no C43 . C44 . 1.462(5) yes C44 . N45 . 1.296(5) yes C44 . C47 . 1.490(5) yes N45 . O46 . 1.387(4) yes C47 . C48 . 1.392(6) yes C47 . C52 . 1.388(6) yes C48 . C49 . 1.392(6) yes C48 . H481 . 0.931 no C49 . C50 . 1.364(7) yes C49 . H491 . 0.927 no C50 . C51 . 1.380(7) yes C50 . H501 . 0.937 no C51 . C52 . 1.384(6) yes C51 . H511 . 0.937 no C52 . H521 . 0.936 no O53 . C54 . 1.246(5) yes C54 . O55 . 1.267(5) yes C54 . C56 . 1.531(5) yes C56 . C57 . 1.537(6) yes C56 . C59 . 1.540(6) yes C56 . C62 . 1.535(6) yes C57 . C58 . 1.540(6) yes C57 . H571 . 0.971 no C57 . H572 . 0.978 no C58 . C61 . 1.522(7) yes C58 . C65 . 1.530(7) yes C58 . H581 . 0.971 no C59 . C60 . 1.539(6) yes C59 . H591 . 0.958 no C59 . H592 . 0.965 no C60 . C61 . 1.530(7) yes C60 . C64 . 1.534(7) yes C60 . H601 . 0.988 no C61 . H611 . 0.967 no C61 . H612 . 0.980 no C62 . C63 . 1.536(6) yes C62 . H622 . 0.976 no C62 . H621 . 0.965 no C63 . C64 . 1.537(7) yes C63 . C65 . 1.526(8) yes C63 . H631 . 0.986 no C64 . H642 . 0.971 no C64 . H641 . 0.972 no C65 . H651 . 0.968 no C65 . H652 . 0.968 no O66 . C67 . 1.412(6) yes O66 . H661 . 0.805 no C67 . H673 . 0.944 no C67 . H672 . 0.958 no C67 . H671 . 0.961 no O68 . C69 . 1.424(5) yes O68 . H681 . 0.803 no C69 . H691 . 0.952 no C69 . H693 . 0.952 no C69 . H692 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O46 2_776 Mn1 . Mn1 2_776 37.76(6) yes O46 2_776 Mn1 . Mn2 . 78.25(6) yes Mn1 2_776 Mn1 . Mn2 . 98.47(3) yes O46 2_776 Mn1 . Mn3 . 85.26(6) yes Mn1 2_776 Mn1 . Mn3 . 68.38(2) yes Mn2 . Mn1 . Mn3 . 60.393(17) yes O46 2_776 Mn1 . O4 . 82.71(11) yes Mn1 2_776 Mn1 . O4 . 84.73(9) yes Mn2 . Mn1 . O4 . 30.05(8) yes Mn3 . Mn1 . O4 . 30.50(8) yes O46 2_776 Mn1 . O5 . 86.24(11) yes Mn1 2_776 Mn1 . O5 . 88.76(9) yes Mn2 . Mn1 . O5 . 143.00(9) yes Mn3 . Mn1 . O5 . 151.77(9) yes O4 . Mn1 . O5 . 168.37(12) yes O46 2_776 Mn1 . N13 . 91.08(12) yes Mn1 2_776 Mn1 . N13 . 128.84(11) yes Mn2 . Mn1 . N13 . 59.56(9) yes Mn3 . Mn1 . N13 . 119.27(9) yes O4 . Mn1 . N13 . 88.87(12) yes O46 2_776 Mn1 . O46 . 83.82(11) yes Mn1 2_776 Mn1 . O46 . 46.05(8) yes Mn2 . Mn1 . O46 . 118.59(8) yes Mn3 . Mn1 . O46 . 59.94(7) yes O4 . Mn1 . O46 . 90.00(11) yes O46 2_776 Mn1 . O53 . 175.07(10) yes Mn1 2_776 Mn1 . O53 . 137.44(8) yes Mn2 . Mn1 . O53 . 105.20(8) yes Mn3 . Mn1 . O53 . 93.38(8) yes O4 . Mn1 . O53 . 98.52(12) yes O5 . Mn1 . N13 . 87.73(12) yes O5 . Mn1 . O46 . 92.41(11) yes N13 . Mn1 . O46 . 174.88(13) yes O5 . Mn1 . O53 . 92.80(12) yes N13 . Mn1 . O53 . 93.71(13) yes O46 . Mn1 . O53 . 91.40(11) yes Mn1 . Mn2 . O4 . 30.70(8) yes Mn1 . Mn2 . O14 . 62.00(8) yes O4 . Mn2 . O14 . 92.67(12) yes Mn1 . Mn2 . O21 . 147.39(10) yes O4 . Mn2 . O21 . 171.33(14) yes O14 . Mn2 . O21 . 86.86(12) yes Mn1 . Mn2 . N29 . 119.08(10) yes O4 . Mn2 . N29 . 89.22(12) yes O14 . Mn2 . N29 . 169.35(14) yes O21 . Mn2 . N29 . 89.70(13) yes Mn1 . Mn2 . O66 . 94.27(8) yes O4 . Mn2 . O66 . 90.67(12) yes O14 . Mn2 . O66 . 94.85(14) yes O21 . Mn2 . O66 . 98.00(14) yes N29 . Mn2 . O66 . 95.61(14) yes O5 2_776 Mn3 . Mn1 . 80.17(7) yes O5 2_776 Mn3 . O4 . 88.86(11) yes Mn1 . Mn3 . O4 . 30.55(8) yes O5 2_776 Mn3 . O30 . 96.25(11) yes Mn1 . Mn3 . O30 . 121.33(9) yes O4 . Mn3 . O30 . 91.45(11) yes O5 2_776 Mn3 . O37 . 92.88(12) yes Mn1 . Mn3 . O37 . 146.72(9) yes O4 . Mn3 . O37 . 176.26(12) yes O30 . Mn3 . O37 . 91.66(12) yes O5 2_776 Mn3 . N45 . 81.50(12) yes Mn1 . Mn3 . N45 . 58.66(10) yes O4 . Mn3 . N45 . 88.79(12) yes O30 . Mn3 . N45 . 177.73(14) yes O37 . Mn3 . N45 . 88.19(13) yes O5 2_776 Mn3 . O68 . 167.86(10) yes Mn1 . Mn3 . O68 . 91.51(8) yes O4 . Mn3 . O68 . 88.35(12) yes O30 . Mn3 . O68 . 95.64(12) yes O37 . Mn3 . O68 . 89.27(13) yes N45 . Mn3 . O68 . 86.63(12) yes Mn1 . O4 . Mn3 . 118.95(13) yes Mn1 . O4 . Mn2 . 119.24(14) yes Mn3 . O4 . Mn2 . 121.33(14) yes Mn3 2_776 O5 . Mn1 . 115.98(13) yes Mn3 2_776 O5 . C6 . 119.9(2) yes Mn1 . O5 . C6 . 118.7(2) yes O5 . C6 . C7 . 117.7(4) yes O5 . C6 . C11 . 122.5(3) yes C7 . C6 . C11 . 119.8(4) yes C6 . C7 . C8 . 120.8(4) yes C6 . C7 . H71 . 119.0 no C8 . C7 . H71 . 120.2 no C7 . C8 . C9 . 120.4(4) yes C7 . C8 . H81 . 120.4 no C9 . C8 . H81 . 119.2 no C8 . C9 . C10 . 119.3(4) yes C8 . C9 . H91 . 121.0 no C10 . C9 . H91 . 119.7 no C9 . C10 . C11 . 121.8(4) yes C9 . C10 . H101 . 118.8 no C11 . C10 . H101 . 119.3 no C10 . C11 . C6 . 117.9(3) yes C10 . C11 . C12 . 118.9(4) yes C6 . C11 . C12 . 123.2(4) yes C11 . C12 . N13 . 119.3(3) yes C11 . C12 . C15 . 119.8(3) yes N13 . C12 . C15 . 120.9(3) yes Mn1 . N13 . C12 . 126.2(3) yes Mn1 . N13 . O14 . 116.5(2) yes C12 . N13 . O14 . 117.2(3) yes N13 . O14 . Mn2 . 117.2(2) yes C12 . C15 . C16 . 121.0(4) yes C12 . C15 . C20 . 119.8(4) yes C16 . C15 . C20 . 118.9(4) yes C15 . C16 . C17 . 120.3(5) yes C15 . C16 . H161 . 119.3 no C17 . C16 . H161 . 120.4 no C16 . C17 . C18 . 120.8(6) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 119.1 no C17 . C18 . C19 . 119.5(5) yes C17 . C18 . H181 . 119.7 no C19 . C18 . H181 . 120.9 no C18 . C19 . C20 . 120.6(6) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 119.7 no C15 . C20 . C19 . 119.8(5) yes C15 . C20 . H201 . 120.0 no C19 . C20 . H201 . 120.1 no Mn2 . O21 . C22 . 133.0(3) yes O21 . C22 . C23 . 117.9(4) yes O21 . C22 . C27 . 123.0(4) yes C23 . C22 . C27 . 119.1(4) yes C22 . C23 . C24 . 120.7(4) yes C22 . C23 . H231 . 119.5 no C24 . C23 . H231 . 119.7 no C23 . C24 . C25 . 120.5(4) yes C23 . C24 . H241 . 118.9 no C25 . C24 . H241 . 120.7 no C24 . C25 . C26 . 119.4(4) yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 120.6 no C25 . C26 . C27 . 122.0(4) yes C25 . C26 . H261 . 118.9 no C27 . C26 . H261 . 119.0 no C26 . C27 . C22 . 118.0(4) yes C26 . C27 . C28 . 118.8(4) yes C22 . C27 . C28 . 123.2(4) yes C27 . C28 . N29 . 122.6(4) yes C27 . C28 . C31 . 117.5(3) yes N29 . C28 . C31 . 119.8(4) yes Mn2 . N29 . C28 . 127.9(3) yes Mn2 . N29 . O30 . 117.9(2) yes C28 . N29 . O30 . 114.2(3) yes N29 . O30 . Mn3 . 119.9(2) yes C28 . C31 . C32 . 119.3(4) yes C28 . C31 . C36 . 120.3(4) yes C32 . C31 . C36 . 120.2(4) yes C31 . C32 . C33 . 119.9(5) yes C31 . C32 . H321 . 120.2 no C33 . C32 . H321 . 119.8 no C32 . C33 . C34 . 119.8(5) yes C32 . C33 . H331 . 119.2 no C34 . C33 . H331 . 121.1 no C33 . C34 . C35 . 120.5(5) yes C33 . C34 . H341 . 119.3 no C35 . C34 . H341 . 120.3 no C34 . C35 . C36 . 119.9(5) yes C34 . C35 . H351 . 120.9 no C36 . C35 . H351 . 119.3 no C35 . C36 . C31 . 119.8(5) yes C35 . C36 . H361 . 120.1 no C31 . C36 . H361 . 120.1 no Mn3 . O37 . C38 . 122.6(2) yes O37 . C38 . C39 . 118.0(4) yes O37 . C38 . C43 . 123.2(4) yes C39 . C38 . C43 . 118.8(4) yes C38 . C39 . C40 . 121.4(4) yes C38 . C39 . H391 . 118.8 no C40 . C39 . H391 . 119.7 no C39 . C40 . C41 . 120.0(4) yes C39 . C40 . H401 . 120.5 no C41 . C40 . H401 . 119.5 no C40 . C41 . C42 . 120.0(4) yes C40 . C41 . H411 . 119.5 no C42 . C41 . H411 . 120.5 no C41 . C42 . C43 . 121.3(4) yes C41 . C42 . H421 . 119.6 no C43 . C42 . H421 . 119.1 no C42 . C43 . C38 . 118.4(4) yes C42 . C43 . C44 . 119.2(3) yes C38 . C43 . C44 . 122.4(3) yes C43 . C44 . N45 . 118.8(3) yes C43 . C44 . C47 . 120.2(3) yes N45 . C44 . C47 . 121.0(4) yes Mn3 . N45 . C44 . 128.8(3) yes Mn3 . N45 . O46 . 113.0(2) yes C44 . N45 . O46 . 118.0(3) yes Mn1 2_776 O46 . N45 . 112.2(2) yes Mn1 2_776 O46 . Mn1 . 96.18(11) yes N45 . O46 . Mn1 . 111.9(2) yes C44 . C47 . C48 . 120.6(4) yes C44 . C47 . C52 . 119.9(4) yes C48 . C47 . C52 . 119.4(4) yes C47 . C48 . C49 . 119.6(4) yes C47 . C48 . H481 . 120.1 no C49 . C48 . H481 . 120.3 no C48 . C49 . C50 . 120.3(4) yes C48 . C49 . H491 . 119.3 no C50 . C49 . H491 . 120.4 no C49 . C50 . C51 . 120.6(4) yes C49 . C50 . H501 . 118.9 no C51 . C50 . H501 . 120.5 no C50 . C51 . C52 . 119.8(5) yes C50 . C51 . H511 . 120.3 no C52 . C51 . H511 . 119.8 no C47 . C52 . C51 . 120.2(4) yes C47 . C52 . H521 . 120.0 no C51 . C52 . H521 . 119.8 no Mn1 . O53 . C54 . 141.0(3) yes O53 . C54 . O55 . 125.4(4) yes O53 . C54 . C56 . 117.7(3) yes O55 . C54 . C56 . 116.9(4) yes C54 . C56 . C57 . 108.8(3) yes C54 . C56 . C59 . 110.1(3) yes C57 . C56 . C59 . 108.4(3) yes C54 . C56 . C62 . 111.7(3) yes C57 . C56 . C62 . 109.3(3) yes C59 . C56 . C62 . 108.4(3) yes C56 . C57 . C58 . 110.2(4) yes C56 . C57 . H571 . 107.2 no C58 . C57 . H571 . 110.3 no C56 . C57 . H572 . 108.7 no C58 . C57 . H572 . 110.3 no H571 . C57 . H572 . 110.1 no C57 . C58 . C61 . 108.6(4) yes C57 . C58 . C65 . 109.7(4) yes C61 . C58 . C65 . 109.8(4) yes C57 . C58 . H581 . 110.3 no C61 . C58 . H581 . 109.6 no C65 . C58 . H581 . 108.8 no C56 . C59 . C60 . 110.6(3) yes C56 . C59 . H591 . 108.3 no C60 . C59 . H591 . 109.0 no C56 . C59 . H592 . 109.4 no C60 . C59 . H592 . 110.8 no H591 . C59 . H592 . 108.7 no C59 . C60 . C61 . 108.7(4) yes C59 . C60 . C64 . 108.9(4) yes C61 . C60 . C64 . 109.8(4) yes C59 . C60 . H601 . 109.1 no C61 . C60 . H601 . 110.1 no C64 . C60 . H601 . 110.3 no C60 . C61 . C58 . 110.2(4) yes C60 . C61 . H611 . 108.8 no C58 . C61 . H611 . 109.8 no C60 . C61 . H612 . 109.6 no C58 . C61 . H612 . 109.5 no H611 . C61 . H612 . 108.8 no C56 . C62 . C63 . 110.0(4) yes C56 . C62 . H622 . 108.4 no C63 . C62 . H622 . 108.3 no C56 . C62 . H621 . 110.0 no C63 . C62 . H621 . 110.4 no H622 . C62 . H621 . 109.7 no C62 . C63 . C64 . 109.4(4) yes C62 . C63 . C65 . 110.1(4) yes C64 . C63 . C65 . 109.4(4) yes C62 . C63 . H631 . 109.2 no C64 . C63 . H631 . 108.6 no C65 . C63 . H631 . 110.1 no C63 . C64 . C60 . 109.4(4) yes C63 . C64 . H642 . 109.9 no C60 . C64 . H642 . 109.2 no C63 . C64 . H641 . 109.0 no C60 . C64 . H641 . 110.7 no H642 . C64 . H641 . 108.7 no C58 . C65 . C63 . 109.4(4) yes C58 . C65 . H651 . 109.5 no C63 . C65 . H651 . 108.6 no C58 . C65 . H652 . 109.6 no C63 . C65 . H652 . 110.3 no H651 . C65 . H652 . 109.4 no Mn2 . O66 . C67 . 128.6(3) yes Mn2 . O66 . H661 . 116.2 no C67 . O66 . H661 . 111.6 no O66 . C67 . H673 . 109.8 no O66 . C67 . H672 . 108.7 no H673 . C67 . H672 . 108.6 no O66 . C67 . H671 . 110.5 no H673 . C67 . H671 . 110.0 no H672 . C67 . H671 . 109.2 no Mn3 . O68 . C69 . 119.3(3) yes Mn3 . O68 . H681 . 116.6 no C69 . O68 . H681 . 105.4 no O68 . C69 . H691 . 110.8 no O68 . C69 . H693 . 108.7 no H691 . C69 . H693 . 109.5 no O68 . C69 . H692 . 109.5 no H691 . C69 . H692 . 109.3 no H693 . C69 . H692 . 109.0 no # Attachment 'Complex_4.cif' data_eb9037 _database_code_depnum_ccdc_archive 'CCDC 793024' #TrackingRef 'Complex_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Ross Inglis' _exptl_crystal_recrystallization_method 'Diffusion of Et2O into EtOH solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H96 Mn6 N6 O22, 0.5(C2 H6 O1)' _chemical_formula_sum 'C97 H99 Mn6 N6 O22.50' _chemical_formula_weight 2038.46 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7188(4) _cell_length_b 14.4624(5) _cell_length_c 14.9900(5) _cell_angle_alpha 95.712(2) _cell_angle_beta 116.428(2) _cell_angle_gamma 110.512(2) _cell_volume 2375.90(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8153 _cell_measurement_theta_min 2.5435 _cell_measurement_theta_max 26.4405 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1053 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7184 _exptl_absorpt_correction_T_max 0.8746 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30950 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9711 _reflns_number_gt 7795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; #========================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #========================================================================== Format: alert-number_ALERT_alert-type_alert-level text 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.00 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.02 Ratio 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O1E 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2E 360_ALERT_2_C Short C(sp3)-C(sp3) Bond C2E - C3E ... 1.36 Ang. This is an ethanol ligand bound by its oxygen. ADP's are consistent with thermal motion expected. 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C27C 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C23C 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C26C This is a benzene ring which is free to rotate about its axis, some motion is expected. 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2D This is the central atom in a tBu group. 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2F 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2F' 301_ALERT_3_G Note Main Residue Disorder .................... 3.00 Perc. 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 37.00 Deg. C2F -O1F -C2F' 1.555 1.555 1.555 This is a disordered ethanol ligand, motion is expected to increase towards the end of the chain. 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 29 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 97 The data collection strategy used was to collect fully complete data to 2TH= 53deg. Some higher angle data were collected in the process and these have been included in the refinement. Please refer to the completeness statistics below #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 4974 4973 1 23.01 0.550 0.999 6629 6623 6 25.24 0.600 0.997 8601 8572 29 #----------------------------------------------------------- ACTA Min. Res. --- 26.50 0.628 0.987 9837 9711 126 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2 731_ALERT_1_C Bond Calc 0.84(4), Rep 0.836(10) ...... 4.00 su-Ra O1E -H1E 1.555 1.555 731_ALERT_1_C Bond Calc 0.84(3), Rep 0.836(10) ...... 3.00 su-Ra O1F -H1F 1.555 1.555 These are O-H distances which have been treated with DFIX. 061_ALERT_4_C Tmax/Tmin Range Test RR' too Large ............. 0.87 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. The crystal was a rather irregular shape, being a fragment of a larger block; this precluded integration methods for correcting for absorption. 077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C3S 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 43.10 Deg. C3S -O1S -H3SC 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 22.80 Deg. H1SB -O1S -H3SC 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 43.90 Deg. O1S -C3S -H1SB 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 40.40 Deg. H1SB -C3S -H3SC 1.555 1.555 1.555 302_ALERT_4_G Note Anion/Solvent Disorder .................... 25.00 Perc. The solvent EtOH is disordered over the inversion centre, an occupancy of 0.5 overall was assigned to reduced the thermal parameters to more acceptable values. 152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? 154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 200 Deg. Values have been carried through electronically and have not changed. The volume alert is likely a rounding error. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 23 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken ; _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^)+(0.0570P)^2^+2.2261P] 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 9711 _refine_ls_number_parameters 620 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Mn1 Mn 0.42252(4) 0.04530(3) 0.03126(3) 0.02676(12) Uani 1 1 d . . . Mn2 Mn 0.30541(4) -0.02981(3) -0.22088(3) 0.02916(13) Uani 1 1 d . . . Mn3 Mn 0.16180(4) -0.15280(3) -0.11294(3) 0.02935(13) Uani 1 1 d . A . O123 O 0.29062(19) -0.04188(15) -0.10240(15) 0.0283(5) Uani 1 1 d . . . C1A C 0.5526(3) 0.1573(2) 0.2410(2) 0.0320(7) Uani 1 1 d . . . O1A O 0.56355(19) 0.10869(16) 0.16685(15) 0.0301(5) Uani 1 1 d . . . O2A O 0.2364(2) -0.12244(16) 0.03558(16) 0.0331(5) Uani 1 1 d . . . C2A C 0.4583(3) 0.1074(3) 0.2593(2) 0.0336(7) Uani 1 1 d . . . C3A C 0.4560(3) 0.1617(3) 0.3406(2) 0.0413(8) Uani 1 1 d . . . H3A H 0.3943 0.1281 0.3555 0.050 Uiso 1 1 calc R . . C4A C 0.5404(3) 0.2619(3) 0.3992(3) 0.0496(10) Uani 1 1 d . . . H4A H 0.5361 0.2974 0.4531 0.060 Uiso 1 1 calc R . . C5A C 0.6318(3) 0.3111(3) 0.3794(3) 0.0484(9) Uani 1 1 d . . . H5A H 0.6903 0.3806 0.4198 0.058 Uiso 1 1 calc R . . C6A C 0.6385(3) 0.2589(3) 0.3005(2) 0.0382(8) Uani 1 1 d . . . H6A H 0.7016 0.2928 0.2873 0.046 Uiso 1 1 calc R . . C21A C 0.3605(3) 0.0024(2) 0.1938(2) 0.0313(7) Uani 1 1 d . . . N22A N 0.3279(2) -0.02563(19) 0.09606(19) 0.0305(6) Uani 1 1 d . . . C23A C 0.3031(3) -0.0660(3) 0.2420(2) 0.0354(7) Uani 1 1 d . . . C24A C 0.1783(3) -0.1221(3) 0.1944(3) 0.0493(9) Uani 1 1 d . . . H24A H 0.1259 -0.1198 0.1277 0.059 Uiso 1 1 calc R . . C25A C 0.1310(4) -0.1816(4) 0.2451(3) 0.0677(13) Uani 1 1 d . . . H25A H 0.0455 -0.2201 0.2129 0.081 Uiso 1 1 calc R . . C26A C 0.2065(5) -0.1855(4) 0.3418(4) 0.0709(14) Uani 1 1 d . . . H26A H 0.1730 -0.2252 0.3766 0.085 Uiso 1 1 calc R . . C27A C 0.3298(4) -0.1321(3) 0.3878(3) 0.0587(11) Uani 1 1 d . . . H27A H 0.3819 -0.1368 0.4533 0.070 Uiso 1 1 calc R . . C28A C 0.3786(4) -0.0714(3) 0.3391(3) 0.0436(8) Uani 1 1 d . . . H28A H 0.4641 -0.0331 0.3720 0.052 Uiso 1 1 calc R . . C1B C 0.3668(3) 0.0866(3) -0.3431(2) 0.0344(7) Uani 1 1 d . . . O1B O 0.3322(2) -0.00679(17) -0.33065(16) 0.0362(5) Uani 1 1 d . . . O2B O 0.52364(19) 0.09211(15) -0.02886(15) 0.0282(5) Uani 1 1 d . . . C2B C 0.4502(3) 0.1799(3) -0.2588(2) 0.0339(7) Uani 1 1 d . . . C3B C 0.4768(3) 0.2745(3) -0.2815(3) 0.0416(8) Uani 1 1 d . . . H3B H 0.5302 0.3374 -0.2255 0.050 Uiso 1 1 calc R . . C4B C 0.4276(4) 0.2785(3) -0.3829(3) 0.0489(9) Uani 1 1 d . . . H4B H 0.4459 0.3433 -0.3965 0.059 Uiso 1 1 calc R . . C5B C 0.3515(4) 0.1871(3) -0.4646(3) 0.0502(10) Uani 1 1 d . . . H5B H 0.3194 0.1894 -0.5346 0.060 Uiso 1 1 calc R . . C6B C 0.3213(3) 0.0925(3) -0.4460(3) 0.0431(8) Uani 1 1 d . . . H6B H 0.2692 0.0306 -0.5033 0.052 Uiso 1 1 calc R . . C21B C 0.5098(3) 0.1797(2) -0.1500(2) 0.0308(7) Uani 1 1 d . . . N22B N 0.4593(2) 0.09822(19) -0.12785(18) 0.0287(6) Uani 1 1 d . . . C23B C 0.6258(3) 0.2687(2) -0.0691(2) 0.0324(7) Uani 1 1 d . . . C24B C 0.6412(3) 0.3107(3) 0.0271(3) 0.0403(8) Uani 1 1 d . . . H24B H 0.5781 0.2810 0.0415 0.048 Uiso 1 1 calc R . . C25B C 0.7492(4) 0.3962(3) 0.1019(3) 0.0477(9) Uani 1 1 d . . . H25B H 0.7591 0.4254 0.1667 0.057 Uiso 1 1 calc R . . C26B C 0.8419(3) 0.4388(3) 0.0821(3) 0.0493(10) Uani 1 1 d . . . H26B H 0.9154 0.4970 0.1333 0.059 Uiso 1 1 calc R . . C27B C 0.8277(3) 0.3966(3) -0.0118(3) 0.0454(9) Uani 1 1 d . . . H27B H 0.8917 0.4257 -0.0251 0.055 Uiso 1 1 calc R . . C28B C 0.7202(3) 0.3114(3) -0.0873(3) 0.0394(8) Uani 1 1 d . . . H28B H 0.7115 0.2824 -0.1516 0.047 Uiso 1 1 calc R . . O1C O 0.0356(2) -0.26435(17) -0.12302(17) 0.0412(6) Uani 1 1 d . . . C1C C -0.0426(3) -0.3543(2) -0.1964(2) 0.0329(7) Uani 1 1 d . . . C2C C -0.0570(3) -0.3777(3) -0.2956(2) 0.0355(7) Uani 1 1 d . . . O2C O 0.1616(2) -0.15526(17) -0.30818(16) 0.0362(5) Uani 1 1 d . . . C3C C -0.1383(4) -0.4789(3) -0.3642(3) 0.0541(10) Uani 1 1 d . . . H3C H -0.1464 -0.4965 -0.4308 0.065 Uiso 1 1 calc R . . C4C C -0.2060(4) -0.5529(3) -0.3380(3) 0.0640(12) Uani 1 1 d . . . H4C H -0.2595 -0.6209 -0.3855 0.077 Uiso 1 1 calc R . . C5C C -0.1959(4) -0.5279(3) -0.2418(3) 0.0526(10) Uani 1 1 d . . . H5C H -0.2453 -0.5780 -0.2244 0.063 Uiso 1 1 calc R . . C6C C -0.1148(3) -0.4308(3) -0.1714(3) 0.0395(8) Uani 1 1 d . . . H6C H -0.1073 -0.4150 -0.1049 0.047 Uiso 1 1 calc R . . C21C C 0.0105(3) -0.3023(2) -0.3300(2) 0.0310(7) Uani 1 1 d . . . N22C N 0.1062(2) -0.2155(2) -0.26364(19) 0.0311(6) Uani 1 1 d . . . C23C C -0.0333(3) -0.3246(2) -0.4445(2) 0.0343(7) Uani 1 1 d . . . C24C C 0.0227(3) -0.3549(3) -0.4884(3) 0.0465(9) Uani 1 1 d . . . H24C H 0.0965 -0.3580 -0.4452 0.056 Uiso 1 1 calc R . . C25C C -0.0274(4) -0.3816(3) -0.5966(3) 0.0526(10) Uani 1 1 d . . . H25C H 0.0129 -0.4024 -0.6262 0.063 Uiso 1 1 calc R . . C26C C -0.1321(4) -0.3781(3) -0.6592(3) 0.0553(11) Uani 1 1 d . . . H26C H -0.1659 -0.3965 -0.7328 0.066 Uiso 1 1 calc R . . C27C C -0.1890(5) -0.3481(5) -0.6164(3) 0.095(2) Uani 1 1 d . . . H27C H -0.2627 -0.3449 -0.6601 0.114 Uiso 1 1 calc R . . C28C C -0.1399(5) -0.3218(5) -0.5086(3) 0.0791(17) Uani 1 1 d . . . H28C H -0.1811 -0.3018 -0.4795 0.095 Uiso 1 1 calc R . . C1D C 0.3033(3) 0.2011(2) -0.0086(2) 0.0345(7) Uani 1 1 d . . . C2D C 0.3306(3) 0.3160(3) 0.0199(3) 0.0483(9) Uani 1 1 d . . . O11D O 0.1962(2) 0.13834(18) -0.08033(19) 0.0439(6) Uani 1 1 d . . . O12D O 0.3885(2) 0.17730(16) 0.03640(17) 0.0353(5) Uani 1 1 d . . . C21D C 0.2241(5) 0.3273(4) 0.0145(5) 0.0880(18) Uani 1 1 d . . . H21A H 0.1516 0.2850 -0.0542 0.132 Uiso 1 1 calc R . . H21B H 0.2398 0.4002 0.0249 0.132 Uiso 1 1 calc R . . H21C H 0.2112 0.3041 0.0693 0.132 Uiso 1 1 calc R . . C22D C 0.3507(5) 0.3556(4) -0.0654(4) 0.0792(15) Uani 1 1 d . . . H22A H 0.4207 0.3493 -0.0628 0.119 Uiso 1 1 calc R . . H22B H 0.3660 0.4284 -0.0532 0.119 Uiso 1 1 calc R . . H22C H 0.2782 0.3142 -0.1343 0.119 Uiso 1 1 calc R . . C23D C 0.4472(4) 0.3786(3) 0.1245(3) 0.0713(14) Uani 1 1 d . . . H23A H 0.5137 0.3682 0.1237 0.107 Uiso 1 1 calc R . . H23B H 0.4368 0.3557 0.1804 0.107 Uiso 1 1 calc R . . H23C H 0.4663 0.4523 0.1368 0.107 Uiso 1 1 calc R . . O1E O 0.2036(2) 0.06590(18) -0.25314(17) 0.0378(5) Uani 1 1 d D . . H1E H 0.196(4) 0.085(3) -0.203(2) 0.057 Uiso 1 1 d D . . C2E C 0.0956(5) 0.0414(5) -0.3505(3) 0.0803(16) Uani 1 1 d . . . H2E1 H 0.1190 0.0519 -0.4037 0.096 Uiso 1 1 calc R . . H2E2 H 0.0417 -0.0334 -0.3715 0.096 Uiso 1 1 calc R . . C3E C 0.0293(7) 0.0939(6) -0.3553(5) 0.154(4) Uani 1 1 d . . . H3E1 H -0.0398 0.0707 -0.4267 0.231 Uiso 1 1 calc R . . H3E2 H 0.0804 0.1684 -0.3354 0.231 Uiso 1 1 calc R . . H3E3 H -0.0005 0.0806 -0.3071 0.231 Uiso 1 1 calc R . . O1F O 0.0669(2) -0.06047(18) -0.1324(2) 0.0422(6) Uani 1 1 d D . . H1F H 0.115(3) 0.0024(11) -0.112(3) 0.063 Uiso 1 1 d D . . C2F C -0.0345(7) -0.0819(5) -0.1236(9) 0.060(2) Uani 0.710(17) 1 d P A 1 H2F1 H -0.0342 -0.0162 -0.0973 0.072 Uiso 0.710(17) 1 calc PR A 1 H2F2 H -0.0320 -0.1210 -0.0726 0.072 Uiso 0.710(17) 1 calc PR A 1 C3F C -0.1473(8) -0.1438(8) -0.2268(10) 0.110(5) Uani 0.710(17) 1 d P A 1 H3F1 H -0.2182 -0.1586 -0.2193 0.165 Uiso 0.710(17) 1 calc PR A 1 H3F2 H -0.1477 -0.2091 -0.2524 0.165 Uiso 0.710(17) 1 calc PR A 1 H3F3 H -0.1503 -0.1045 -0.2768 0.165 Uiso 0.710(17) 1 calc PR A 1 C2F' C -0.0662(17) -0.0894(13) -0.1938(18) 0.053(5) Uani 0.290(17) 1 d P A 2 H2F3 H -0.1081 -0.1542 -0.2519 0.064 Uiso 0.290(17) 1 calc PR A 2 H2F4 H -0.0785 -0.0340 -0.2245 0.064 Uiso 0.290(17) 1 calc PR A 2 C3F' C -0.120(2) -0.105(2) -0.126(2) 0.099(9) Uani 0.290(17) 1 d P A 2 H3F4 H -0.2077 -0.1265 -0.1679 0.148 Uiso 0.290(17) 1 calc PR A 2 H3F5 H -0.0822 -0.0392 -0.0706 0.148 Uiso 0.290(17) 1 calc PR A 2 H3F6 H -0.1059 -0.1579 -0.0934 0.148 Uiso 0.290(17) 1 calc PR A 2 O1S O 0.4415(11) 0.4647(11) 0.4570(11) 0.143(5) Uiso 0.25 1 d P B -1 H1SB H 0.4488 0.4154 0.4289 0.215 Uiso 0.25 1 d PR B -1 C2S C 0.4415(11) 0.4647(11) 0.4570(11) 0.143(5) Uiso 0.25 1 d P B -1 H2SA H 0.3920 0.4536 0.4881 0.172 Uiso 0.25 1 d PR B -1 H2SB H 0.4298 0.5173 0.4253 0.172 Uiso 0.25 1 d PR B -1 C3S C 0.416(2) 0.4390(18) 0.3669(19) 0.092(7) Uiso 0.25 1 d P B -1 H3SA H 0.3388 0.4413 0.3341 0.138 Uiso 0.25 1 d PR B -1 H3SB H 0.4453 0.4420 0.3195 0.138 Uiso 0.25 1 d PR B -1 H3SC H 0.4061 0.3757 0.3847 0.138 Uiso 0.25 1 d PR B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0293(2) 0.0238(2) 0.0180(2) 0.00207(17) 0.00830(19) 0.00855(19) Mn2 0.0318(3) 0.0263(2) 0.0190(2) 0.00356(18) 0.0095(2) 0.0080(2) Mn3 0.0327(3) 0.0238(2) 0.0205(2) 0.00178(18) 0.0107(2) 0.0066(2) O123 0.0309(11) 0.0261(11) 0.0192(10) 0.0030(8) 0.0099(9) 0.0087(9) C1A 0.0348(17) 0.0359(17) 0.0169(14) 0.0028(13) 0.0068(13) 0.0170(15) O1A 0.0319(11) 0.0300(11) 0.0191(10) 0.0021(8) 0.0092(9) 0.0108(9) O2A 0.0368(12) 0.0245(11) 0.0235(11) 0.0016(9) 0.0122(10) 0.0047(9) C2A 0.0357(17) 0.0347(17) 0.0209(15) 0.0029(13) 0.0090(14) 0.0145(14) C3A 0.043(2) 0.045(2) 0.0254(16) -0.0001(15) 0.0155(15) 0.0154(17) C4A 0.049(2) 0.050(2) 0.0301(18) -0.0092(16) 0.0165(17) 0.0137(19) C5A 0.046(2) 0.039(2) 0.0327(19) -0.0119(15) 0.0103(17) 0.0094(17) C6A 0.0328(18) 0.0361(18) 0.0274(16) -0.0028(14) 0.0084(14) 0.0092(15) C21A 0.0322(17) 0.0364(17) 0.0232(15) 0.0047(13) 0.0126(13) 0.0167(14) N22A 0.0311(14) 0.0265(13) 0.0250(13) 0.0021(11) 0.0105(11) 0.0105(11) C23A 0.0414(19) 0.0363(18) 0.0255(16) 0.0047(13) 0.0175(15) 0.0151(15) C24A 0.044(2) 0.061(2) 0.0325(19) 0.0062(17) 0.0185(17) 0.0157(19) C25A 0.054(3) 0.077(3) 0.049(3) 0.008(2) 0.032(2) 0.002(2) C26A 0.079(3) 0.070(3) 0.056(3) 0.019(2) 0.045(3) 0.011(3) C27A 0.076(3) 0.063(3) 0.036(2) 0.0219(19) 0.029(2) 0.027(2) C28A 0.050(2) 0.049(2) 0.0309(18) 0.0106(16) 0.0209(17) 0.0217(18) C1B 0.0341(17) 0.0422(19) 0.0311(17) 0.0135(14) 0.0188(15) 0.0180(15) O1B 0.0422(13) 0.0357(12) 0.0256(11) 0.0071(9) 0.0170(10) 0.0131(10) O2B 0.0333(11) 0.0253(10) 0.0190(10) 0.0052(8) 0.0092(9) 0.0118(9) C2B 0.0342(17) 0.0406(18) 0.0296(16) 0.0145(14) 0.0176(14) 0.0167(15) C3B 0.041(2) 0.042(2) 0.043(2) 0.0189(16) 0.0225(17) 0.0181(16) C4B 0.053(2) 0.056(2) 0.050(2) 0.032(2) 0.030(2) 0.028(2) C5B 0.058(2) 0.077(3) 0.037(2) 0.033(2) 0.0300(19) 0.040(2) C6B 0.046(2) 0.060(2) 0.0275(17) 0.0155(16) 0.0204(16) 0.0258(19) C21B 0.0344(17) 0.0285(16) 0.0303(16) 0.0100(13) 0.0161(14) 0.0151(14) N22B 0.0341(14) 0.0273(13) 0.0207(12) 0.0066(10) 0.0112(11) 0.0136(11) C23B 0.0366(17) 0.0249(15) 0.0294(16) 0.0100(13) 0.0129(14) 0.0124(14) C24B 0.042(2) 0.0287(17) 0.0404(19) 0.0073(15) 0.0177(16) 0.0115(15) C25B 0.053(2) 0.0319(19) 0.039(2) 0.0025(15) 0.0155(18) 0.0126(17) C26B 0.042(2) 0.0280(18) 0.049(2) 0.0061(16) 0.0071(18) 0.0085(16) C27B 0.0342(19) 0.0357(19) 0.055(2) 0.0190(17) 0.0165(17) 0.0107(15) C28B 0.0397(19) 0.0329(18) 0.0413(19) 0.0157(15) 0.0180(16) 0.0145(15) O1C 0.0476(14) 0.0306(12) 0.0276(12) 0.0013(10) 0.0194(11) 0.0010(11) C1C 0.0315(17) 0.0277(16) 0.0288(16) 0.0039(13) 0.0117(14) 0.0087(13) C2C 0.0297(17) 0.0339(17) 0.0273(16) 0.0021(13) 0.0100(14) 0.0064(14) O2C 0.0390(13) 0.0327(12) 0.0223(11) 0.0047(9) 0.0133(10) 0.0053(10) C3C 0.052(2) 0.046(2) 0.0332(19) -0.0040(17) 0.0174(18) 0.0002(18) C4C 0.058(3) 0.042(2) 0.045(2) -0.0060(18) 0.019(2) -0.0109(19) C5C 0.045(2) 0.043(2) 0.044(2) 0.0087(17) 0.0194(18) -0.0011(17) C6C 0.0395(19) 0.0370(18) 0.0320(17) 0.0072(15) 0.0175(16) 0.0088(15) C21C 0.0283(16) 0.0308(16) 0.0224(15) 0.0006(12) 0.0080(13) 0.0100(13) N22C 0.0333(14) 0.0318(14) 0.0231(13) 0.0053(11) 0.0120(11) 0.0135(12) C23C 0.0343(17) 0.0304(16) 0.0229(15) 0.0007(13) 0.0080(14) 0.0097(14) C24C 0.038(2) 0.063(2) 0.0300(18) 0.0080(17) 0.0129(16) 0.0221(18) C25C 0.059(3) 0.056(2) 0.034(2) 0.0003(17) 0.0240(19) 0.021(2) C26C 0.072(3) 0.055(2) 0.0236(17) 0.0043(16) 0.0132(19) 0.030(2) C27C 0.095(4) 0.164(6) 0.029(2) 0.014(3) 0.009(2) 0.095(4) C28C 0.083(3) 0.137(5) 0.035(2) 0.017(3) 0.021(2) 0.082(4) C1D 0.0406(19) 0.0314(17) 0.0284(16) 0.0067(14) 0.0163(15) 0.0151(15) C2D 0.046(2) 0.0270(18) 0.056(2) 0.0070(16) 0.0152(19) 0.0165(16) O11D 0.0391(14) 0.0348(13) 0.0414(14) 0.0032(11) 0.0116(12) 0.0141(11) O12D 0.0397(13) 0.0291(12) 0.0320(12) 0.0065(9) 0.0143(10) 0.0161(10) C21D 0.075(3) 0.048(3) 0.133(5) 0.004(3) 0.046(4) 0.035(3) C22D 0.098(4) 0.048(3) 0.075(3) 0.031(2) 0.034(3) 0.025(3) C23D 0.078(3) 0.036(2) 0.059(3) -0.0098(19) 0.010(2) 0.023(2) O1E 0.0381(13) 0.0417(13) 0.0277(12) 0.0095(10) 0.0125(11) 0.0178(11) C2E 0.074(3) 0.125(5) 0.034(2) 0.014(3) 0.008(2) 0.066(3) C3E 0.130(6) 0.187(8) 0.086(5) -0.012(5) -0.019(4) 0.123(6) O1F 0.0331(13) 0.0320(13) 0.0510(15) 0.0072(11) 0.0178(12) 0.0102(11) C2F 0.051(5) 0.055(4) 0.083(7) 0.015(4) 0.039(5) 0.027(3) C3F 0.036(5) 0.082(6) 0.156(12) 0.023(7) 0.012(5) 0.022(5) C2F' 0.041(11) 0.049(9) 0.060(12) 0.019(9) 0.024(10) 0.012(8) C3F' 0.090(18) 0.13(2) 0.092(18) 0.048(16) 0.054(15) 0.050(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O123 1.8840(19) . ? Mn1 O1A 1.897(2) . ? Mn1 O2B 1.942(2) . ? Mn1 N22A 2.017(3) . ? Mn1 O12D 2.120(2) . ? Mn1 O2B 2.353(2) 2_655 ? Mn1 Mn3 3.2214(6) . ? Mn2 O1B 1.875(2) . ? Mn2 O123 1.893(2) . ? Mn2 O2C 1.902(2) . ? Mn2 N22B 1.989(3) . ? Mn2 O1E 2.233(2) . ? Mn2 O1A 2.348(2) 2_655 ? Mn3 O1C 1.840(2) . ? Mn3 O123 1.853(2) . ? Mn3 O2A 1.913(2) . ? Mn3 N22C 2.020(2) . ? Mn3 O1F 2.127(2) . ? C1A O1A 1.349(4) . ? C1A C6A 1.390(4) . ? C1A C2A 1.403(5) . ? O1A Mn2 2.348(2) 2_655 ? O2A N22A 1.364(3) . ? C2A C3A 1.402(4) . ? C2A C21A 1.474(4) . ? C3A C4A 1.370(5) . ? C3A H3A 0.9500 . ? C4A C5A 1.384(6) . ? C4A H4A 0.9500 . ? C5A C6A 1.395(5) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C21A N22A 1.298(4) . ? C21A C23A 1.491(5) . ? C23A C24A 1.387(5) . ? C23A C28A 1.390(5) . ? C24A C25A 1.385(6) . ? C24A H24A 0.9500 . ? C25A C26A 1.377(6) . ? C25A H25A 0.9500 . ? C26A C27A 1.369(6) . ? C26A H26A 0.9500 . ? C27A C28A 1.378(5) . ? C27A H27A 0.9500 . ? C28A H28A 0.9500 . ? C1B O1B 1.328(4) . ? C1B C6B 1.409(4) . ? C1B C2B 1.420(5) . ? O2B N22B 1.380(3) . ? O2B Mn1 2.352(2) 2_655 ? C2B C3B 1.405(5) . ? C2B C21B 1.465(4) . ? C3B C4B 1.379(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.382(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.379(5) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C21B N22B 1.300(4) . ? C21B C23B 1.482(4) . ? C23B C28B 1.386(5) . ? C23B C24B 1.399(5) . ? C24B C25B 1.394(5) . ? C24B H24B 0.9500 . ? C25B C26B 1.381(6) . ? C25B H25B 0.9500 . ? C26B C27B 1.376(6) . ? C26B H26B 0.9500 . ? C27B C28B 1.391(5) . ? C27B H27B 0.9500 . ? C28B H28B 0.9500 . ? O1C C1C 1.320(4) . ? C1C C2C 1.399(5) . ? C1C C6C 1.411(5) . ? C2C C3C 1.407(5) . ? C2C C21C 1.463(5) . ? O2C N22C 1.374(3) . ? C3C C4C 1.369(6) . ? C3C H3C 0.9500 . ? C4C C5C 1.382(6) . ? C4C H4C 0.9500 . ? C5C C6C 1.374(5) . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? C21C N22C 1.312(4) . ? C21C C23C 1.499(4) . ? C23C C24C 1.358(5) . ? C23C C28C 1.365(5) . ? C24C C25C 1.395(5) . ? C24C H24C 0.9500 . ? C25C C26C 1.344(6) . ? C25C H25C 0.9500 . ? C26C C27C 1.356(6) . ? C26C H26C 0.9500 . ? C27C C28C 1.392(6) . ? C27C H27C 0.9500 . ? C28C H28C 0.9500 . ? C1D O12D 1.252(4) . ? C1D O11D 1.266(4) . ? C1D C2D 1.537(4) . ? C2D C21D 1.494(6) . ? C2D C23D 1.519(5) . ? C2D C22D 1.545(6) . ? C21D H21A 0.9800 . ? C21D H21B 0.9800 . ? C21D H21C 0.9800 . ? C22D H22A 0.9800 . ? C22D H22B 0.9800 . ? C22D H22C 0.9800 . ? C23D H23A 0.9800 . ? C23D H23B 0.9800 . ? C23D H23C 0.9800 . ? O1E C2E 1.433(4) . ? O1E H1E 0.836(10) . ? C2E C3E 1.359(7) . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? C3E H3E1 0.9800 . ? C3E H3E2 0.9800 . ? C3E H3E3 0.9800 . ? O1F C2F 1.384(8) . ? O1F C2F' 1.499(18) . ? O1F H1F 0.836(10) . ? C2F C3F 1.488(17) . ? C2F H2F1 0.9900 . ? C2F H2F2 0.9900 . ? C3F H3F1 0.9800 . ? C3F H3F2 0.9800 . ? C3F H3F3 0.9800 . ? C2F' C3F' 1.50(4) . ? C2F' H2F3 0.9900 . ? C2F' H2F4 0.9900 . ? C3F' H3F4 0.9800 . ? C3F' H3F5 0.9800 . ? C3F' H3F6 0.9800 . ? O1S C3S 1.21(2) . ? O1S H1SB 0.8500 . ? C2S H2SA 0.9600 . ? C2S H2SB 0.9600 . ? C3S H3SA 0.9600 . ? C3S H3SB 0.9600 . ? C3S H3SC 0.9601 . ? 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 O123 Mn1 O1A 167.72(9) . . ? O123 Mn1 O2B 89.74(9) . . ? O1A Mn1 O2B 89.46(9) . . ? O123 Mn1 N22A 89.78(9) . . ? O1A Mn1 N22A 88.63(10) . . ? O2B Mn1 N22A 168.78(9) . . ? O123 Mn1 O12D 99.75(9) . . ? O1A Mn1 O12D 92.53(9) . . ? O2B Mn1 O12D 94.31(9) . . ? N22A Mn1 O12D 96.82(10) . . ? O123 Mn1 O2B 83.05(8) . 2_655 ? O1A Mn1 O2B 84.71(8) . 2_655 ? O2B Mn1 O2B 81.88(8) . 2_655 ? N22A Mn1 O2B 86.93(9) . 2_655 ? O12D Mn1 O2B 175.30(8) . 2_655 ? O123 Mn1 Mn3 30.19(6) . . ? O1A Mn1 Mn3 144.48(7) . . ? O2B Mn1 Mn3 117.86(6) . . ? N22A Mn1 Mn3 60.02(7) . . ? O12D Mn1 Mn3 106.48(6) . . ? O2B Mn1 Mn3 77.84(5) 2_655 . ? O1B Mn2 O123 174.97(9) . . ? O1B Mn2 O2C 93.15(10) . . ? O123 Mn2 O2C 91.88(9) . . ? O1B Mn2 N22B 87.10(10) . . ? O123 Mn2 N22B 87.88(9) . . ? O2C Mn2 N22B 177.79(10) . . ? O1B Mn2 O1E 89.62(9) . . ? O123 Mn2 O1E 89.96(9) . . ? O2C Mn2 O1E 92.70(10) . . ? N22B Mn2 O1E 89.49(9) . . ? O1B Mn2 O1A 91.89(9) . 2_655 ? O123 Mn2 O1A 87.81(8) . 2_655 ? O2C Mn2 O1A 95.47(9) . 2_655 ? N22B Mn2 O1A 82.33(9) . 2_655 ? O1E Mn2 O1A 171.59(8) . 2_655 ? O1C Mn3 O123 178.91(10) . . ? O1C Mn3 O2A 87.11(10) . . ? O123 Mn3 O2A 92.72(9) . . ? O1C Mn3 N22C 90.38(10) . . ? O123 Mn3 N22C 89.46(10) . . ? O2A Mn3 N22C 162.31(10) . . ? O1C Mn3 O1F 91.76(10) . . ? O123 Mn3 O1F 89.33(9) . . ? O2A Mn3 O1F 97.52(10) . . ? N22C Mn3 O1F 100.06(10) . . ? O1C Mn3 Mn1 149.09(7) . . ? O123 Mn3 Mn1 30.74(6) . . ? O2A Mn3 Mn1 61.99(7) . . ? N22C Mn3 Mn1 118.84(8) . . ? O1F Mn3 Mn1 92.64(6) . . ? Mn3 O123 Mn1 119.07(11) . . ? Mn3 O123 Mn2 120.85(10) . . ? Mn1 O123 Mn2 119.09(11) . . ? O1A C1A C6A 118.2(3) . . ? O1A C1A C2A 121.5(3) . . ? C6A C1A C2A 120.3(3) . . ? C1A O1A Mn1 115.96(18) . . ? C1A O1A Mn2 117.05(17) . 2_655 ? Mn1 O1A Mn2 118.23(9) . 2_655 ? N22A O2A Mn3 117.77(17) . . ? C3A C2A C1A 118.2(3) . . ? C3A C2A C21A 119.5(3) . . ? C1A C2A C21A 122.3(3) . . ? C4A C3A C2A 121.7(4) . . ? C4A C3A H3A 119.2 . . ? C2A C3A H3A 119.2 . . ? C3A C4A C5A 119.8(3) . . ? C3A C4A H4A 120.1 . . ? C5A C4A H4A 120.1 . . ? C4A C5A C6A 120.2(3) . . ? C4A C5A H5A 119.9 . . ? C6A C5A H5A 119.9 . . ? C1A C6A C5A 119.9(3) . . ? C1A C6A H6A 120.0 . . ? C5A C6A H6A 120.0 . . ? N22A C21A C2A 117.8(3) . . ? N22A C21A C23A 123.1(3) . . ? C2A C21A C23A 119.1(3) . . ? C21A N22A O2A 117.6(3) . . ? C21A N22A Mn1 125.9(2) . . ? O2A N22A Mn1 114.91(18) . . ? C24A C23A C28A 119.5(3) . . ? C24A C23A C21A 122.3(3) . . ? C28A C23A C21A 118.1(3) . . ? C25A C24A C23A 119.3(4) . . ? C25A C24A H24A 120.3 . . ? C23A C24A H24A 120.3 . . ? C26A C25A C24A 120.7(4) . . ? C26A C25A H25A 119.7 . . ? C24A C25A H25A 119.7 . . ? C27A C26A C25A 120.1(4) . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C28A 120.0(4) . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C27A C28A C23A 120.3(4) . . ? C27A C28A H28A 119.8 . . ? C23A C28A H28A 119.8 . . ? O1B C1B C6B 117.7(3) . . ? O1B C1B C2B 123.8(3) . . ? C6B C1B C2B 118.5(3) . . ? C1B O1B Mn2 121.7(2) . . ? N22B O2B Mn1 112.15(16) . . ? N22B O2B Mn1 112.27(15) . 2_655 ? Mn1 O2B Mn1 98.11(8) . 2_655 ? C3B C2B C1B 118.6(3) . . ? C3B C2B C21B 119.6(3) . . ? C1B C2B C21B 121.8(3) . . ? C4B C3B C2B 121.7(4) . . ? C4B C3B H3B 119.1 . . ? C2B C3B H3B 119.1 . . ? C3B C4B C5B 119.3(4) . . ? C3B C4B H4B 120.4 . . ? C5B C4B H4B 120.4 . . ? C6B C5B C4B 121.0(3) . . ? C6B C5B H5B 119.5 . . ? C4B C5B H5B 119.5 . . ? C5B C6B C1B 120.8(3) . . ? C5B C6B H6B 119.6 . . ? C1B C6B H6B 119.6 . . ? N22B C21B C2B 117.9(3) . . ? N22B C21B C23B 121.5(3) . . ? C2B C21B C23B 120.6(3) . . ? C21B N22B O2B 117.7(2) . . ? C21B N22B Mn2 129.4(2) . . ? O2B N22B Mn2 112.68(17) . . ? C28B C23B C24B 119.1(3) . . ? C28B C23B C21B 120.8(3) . . ? C24B C23B C21B 120.1(3) . . ? C25B C24B C23B 119.9(4) . . ? C25B C24B H24B 120.1 . . ? C23B C24B H24B 120.1 . . ? C26B C25B C24B 120.4(4) . . ? C26B C25B H25B 119.8 . . ? C24B C25B H25B 119.8 . . ? C27B C26B C25B 119.9(3) . . ? C27B C26B H26B 120.1 . . ? C25B C26B H26B 120.1 . . ? C26B C27B C28B 120.4(4) . . ? C26B C27B H27B 119.8 . . ? C28B C27B H27B 119.8 . . ? C23B C28B C27B 120.4(3) . . ? C23B C28B H28B 119.8 . . ? C27B C28B H28B 119.8 . . ? C1C O1C Mn3 131.6(2) . . ? O1C C1C C2C 124.1(3) . . ? O1C C1C C6C 116.9(3) . . ? C2C C1C C6C 119.0(3) . . ? C1C C2C C3C 118.3(3) . . ? C1C C2C C21C 122.9(3) . . ? C3C C2C C21C 118.9(3) . . ? N22C O2C Mn2 119.14(17) . . ? C4C C3C C2C 122.0(4) . . ? C4C C3C H3C 119.0 . . ? C2C C3C H3C 119.0 . . ? C3C C4C C5C 119.5(4) . . ? C3C C4C H4C 120.2 . . ? C5C C4C H4C 120.2 . . ? C6C C5C C4C 120.2(4) . . ? C6C C5C H5C 119.9 . . ? C4C C5C H5C 119.9 . . ? C5C C6C C1C 120.9(3) . . ? C5C C6C H6C 119.5 . . ? C1C C6C H6C 119.5 . . ? N22C C21C C2C 121.7(3) . . ? N22C C21C C23C 119.7(3) . . ? C2C C21C C23C 118.6(3) . . ? C21C N22C O2C 114.3(2) . . ? C21C N22C Mn3 127.3(2) . . ? O2C N22C Mn3 117.61(18) . . ? C24C C23C C28C 118.4(3) . . ? C24C C23C C21C 123.4(3) . . ? C28C C23C C21C 118.0(3) . . ? C23C C24C C25C 120.6(3) . . ? C23C C24C H24C 119.7 . . ? C25C C24C H24C 119.7 . . ? C26C C25C C24C 120.7(4) . . ? C26C C25C H25C 119.7 . . ? C24C C25C H25C 119.7 . . ? C25C C26C C27C 119.4(4) . . ? C25C C26C H26C 120.3 . . ? C27C C26C H26C 120.3 . . ? C26C C27C C28C 120.3(4) . . ? C26C C27C H27C 119.8 . . ? C28C C27C H27C 119.8 . . ? C23C C28C C27C 120.6(4) . . ? C23C C28C H28C 119.7 . . ? C27C C28C H28C 119.7 . . ? O12D C1D O11D 125.1(3) . . ? O12D C1D C2D 118.3(3) . . ? O11D C1D C2D 116.5(3) . . ? C21D C2D C23D 112.9(4) . . ? C21D C2D C1D 110.8(3) . . ? C23D C2D C1D 111.6(3) . . ? C21D C2D C22D 108.3(4) . . ? C23D C2D C22D 107.6(4) . . ? C1D C2D C22D 105.2(3) . . ? C1D O12D Mn1 139.4(2) . . ? C2D C21D H21A 109.5 . . ? C2D C21D H21B 109.5 . . ? H21A C21D H21B 109.5 . . ? C2D C21D H21C 109.5 . . ? H21A C21D H21C 109.5 . . ? H21B C21D H21C 109.5 . . ? C2D C22D H22A 109.5 . . ? C2D C22D H22B 109.5 . . ? H22A C22D H22B 109.5 . . ? C2D C22D H22C 109.5 . . ? H22A C22D H22C 109.5 . . ? H22B C22D H22C 109.5 . . ? C2D C23D H23A 109.5 . . ? C2D C23D H23B 109.5 . . ? H23A C23D H23B 109.5 . . ? C2D C23D H23C 109.5 . . ? H23A C23D H23C 109.5 . . ? H23B C23D H23C 109.5 . . ? C2E O1E Mn2 123.9(2) . . ? C2E O1E H1E 111(3) . . ? Mn2 O1E H1E 112(3) . . ? C3E C2E O1E 118.6(4) . . ? C3E C2E H2E1 107.7 . . ? O1E C2E H2E1 107.7 . . ? C3E C2E H2E2 107.7 . . ? O1E C2E H2E2 107.7 . . ? H2E1 C2E H2E2 107.1 . . ? C2E C3E H3E1 109.5 . . ? C2E C3E H3E2 109.5 . . ? H3E1 C3E H3E2 109.5 . . ? C2E C3E H3E3 109.5 . . ? H3E1 C3E H3E3 109.5 . . ? H3E2 C3E H3E3 109.5 . . ? C2F O1F C2F' 37.0(7) . . ? C2F O1F Mn3 126.2(4) . . ? C2F' O1F Mn3 131.0(7) . . ? C2F O1F H1F 115(3) . . ? C2F' O1F H1F 117(3) . . ? Mn3 O1F H1F 111(3) . . ? O1F C2F C3F 110.4(9) . . ? O1F C2F H2F1 109.6 . . ? C3F C2F H2F1 109.6 . . ? O1F C2F H2F2 109.6 . . ? C3F C2F H2F2 109.6 . . ? H2F1 C2F H2F2 108.1 . . ? C2F C3F H3F1 109.5 . . ? C2F C3F H3F2 109.5 . . ? H3F1 C3F H3F2 109.5 . . ? C2F C3F H3F3 109.5 . . ? H3F1 C3F H3F3 109.5 . . ? H3F2 C3F H3F3 109.5 . . ? O1F C2F' C3F' 111(2) . . ? O1F C2F' H2F3 109.5 . . ? C3F' C2F' H2F3 109.5 . . ? O1F C2F' H2F4 109.5 . . ? C3F' C2F' H2F4 109.5 . . ? H2F3 C2F' H2F4 108.1 . . ? C2F' C3F' H3F4 109.5 . . ? C2F' C3F' H3F5 109.5 . . ? H3F4 C3F' H3F5 109.5 . . ? C2F' C3F' H3F6 109.5 . . ? H3F4 C3F' H3F6 109.5 . . ? H3F5 C3F' H3F6 109.5 . . ? C3S O1S H1SB 54.0 . . ? C3S O1S H2SA 131.8 . . ? H1SB O1S H2SA 122.2 . . ? C3S O1S H2SB 69.7 . . ? H1SB O1S H2SB 122.3 . . ? H2SA O1S H2SB 103.5 . . ? C3S O1S H3SC 43.1 . . ? H1SB O1S H3SC 22.8 . . ? H2SA O1S H3SC 111.7 . . ? H2SB O1S H3SC 111.8 . . ? O1S C3S H1SB 43.9 . . ? O1S C3S H2SB 45.6 . . ? H1SB C3S H2SB 88.8 . . ? O1S C3S H3SA 98.2 . . ? H1SB C3S H3SA 126.1 . . ? H2SB C3S H3SA 74.3 . . ? O1S C3S H3SB 146.4 . . ? H1SB C3S H3SB 121.9 . . ? H2SB C3S H3SB 124.2 . . ? H3SA C3S H3SB 109.5 . . ? O1S C3S H3SC 77.3 . . ? H1SB C3S H3SC 40.4 . . ? H2SB C3S H3SC 121.7 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.923 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.075