# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Euan Brechin' 'Scott Dalgarno' 'Ross Inglis' _publ_contact_author_name 'Euan Brechin' _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_section_title ; A new family of Mn6 SMMs using phosphinate ligands ; # Attachment 'Complex 1.CIF' data_RI2223 _database_code_depnum_ccdc_archive 'CCDC 760677' #TrackingRef 'Complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common RI2223 _chemical_melting_point ? _chemical_formula_moiety 'C72 H74 Mn6 N6 O24 P2' _chemical_formula_sum 'C72 H74 Mn6 N6 O24 P2' _chemical_formula_weight 1798.96 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' P P 0.1023 0.0942 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.12(4) _cell_length_b 14.64(2) _cell_length_c 24.14(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.820(16) _cell_angle_gamma 90.00 _cell_volume 8240(24) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5396 _exptl_absorpt_correction_T_max 0.6604 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex 2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55360 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 30.32 _reflns_number_total 12230 _reflns_number_gt 9129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. The structure contained badly disordered methanol molecules that could not be modeled satisfac- torily. As this was the case, the data was processed with the routing SQUEEZE to remove this diffuse electron density. This dramatically impr- oved the agreement indices. The carbon atoms of one disordered methanol molecule were refined isotropically. ; _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^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12230 _refine_ls_number_parameters 499 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.106615(13) 1.171365(18) 0.107221(13) 0.01479(8) Uani 1 1 d . A . P1 P 0.18918(2) 1.01114(3) -0.01484(2) 0.01722(12) Uani 1 1 d . . . O1 O 0.13670(6) 1.22489(9) 0.18340(6) 0.0200(3) Uani 1 1 d . . . C1 C 0.14902(9) 1.31212(12) 0.19926(9) 0.0173(4) Uani 1 1 d . . . Mn2 Mn 0.071436(13) 0.989285(17) 0.021479(13) 0.01345(8) Uani 1 1 d . . . O2 O 0.04580(7) 1.30001(9) 0.01099(6) 0.0223(3) Uani 1 1 d . A . C2 C 0.13150(9) 1.38649(12) 0.15837(9) 0.0186(4) Uani 1 1 d . . . Mn3 Mn 0.032652(14) 1.192096(18) -0.036159(13) 0.01656(8) Uani 1 1 d . A . O3 O 0.05702(6) 0.86074(8) 0.01918(6) 0.0164(3) Uani 1 1 d . . . N3 N 0.12159(7) 0.97867(10) 0.10853(7) 0.0157(3) Uani 1 1 d . . . C3 C 0.14429(10) 1.47679(13) 0.17951(10) 0.0240(5) Uani 1 1 d . . . H3 H 0.1314 1.5261 0.1522 0.029 Uiso 1 1 calc R . . O4 O 0.12753(6) 1.05333(8) 0.14492(6) 0.0195(3) Uani 1 1 d . . . C4 C 0.17509(10) 1.49513(14) 0.23902(10) 0.0264(5) Uani 1 1 d . . . H4 H 0.1840 1.5562 0.2525 0.032 Uiso 1 1 calc R . . O5 O -0.01131(6) 1.26600(9) -0.10050(6) 0.0212(3) Uani 1 1 d . . . C5 C 0.19286(10) 1.42211(14) 0.27909(10) 0.0250(5) Uani 1 1 d . . . H5 H 0.2141 1.4340 0.3201 0.030 Uiso 1 1 calc R . . O6 O 0.00908(6) 0.99904(8) -0.05662(6) 0.0173(3) Uani 1 1 d . . . C6 C 0.17984(10) 1.33226(13) 0.25978(10) 0.0217(4) Uani 1 1 d . . . H6 H 0.1920 1.2838 0.2879 0.026 Uiso 1 1 calc R . . O7 O 0.13571(6) 0.96747(9) -0.01165(7) 0.0205(3) Uani 1 1 d . . . C7 C 0.09731(9) 1.37414(12) 0.09550(9) 0.0197(4) Uani 1 1 d . A . H7 H 0.0847 1.4272 0.0716 0.024 Uiso 1 1 calc R . . O8 O 0.19931(6) 1.11217(9) 0.00142(6) 0.0214(3) Uani 1 1 d . . . C8 C 0.09962(9) 0.80064(12) 0.04592(9) 0.0171(4) Uani 1 1 d . . . O9 O 0.01814(7) 1.17083(11) 0.11568(8) 0.0319(4) Uani 1 1 d D . . C9 C 0.14150(9) 0.81740(12) 0.10357(9) 0.0174(4) Uani 1 1 d . . . O10 O 0.19212(6) 1.19019(9) 0.09787(6) 0.0212(3) Uani 1 1 d D . . C10 C 0.18118(9) 0.74789(13) 0.13198(10) 0.0221(4) Uani 1 1 d . . . H10 H 0.2077 0.7572 0.1716 0.027 Uiso 1 1 calc R . . O11 O 0.10845(7) 1.21024(9) -0.06061(7) 0.0219(3) Uani 1 1 d D . . C11 C 0.18213(10) 0.66655(13) 0.10332(11) 0.0263(5) Uani 1 1 d . . . H11 H 0.2098 0.6211 0.1227 0.032 Uiso 1 1 calc R . . O12 O 0.07464(6) 1.11839(8) 0.02989(6) 0.0150(3) Uani 1 1 d . . . C12 C 0.14236(10) 0.65166(13) 0.04587(11) 0.0265(5) Uani 1 1 d . . . H12 H 0.1433 0.5961 0.0259 0.032 Uiso 1 1 calc R . . C13 C 0.10141(10) 0.71723(13) 0.01744(10) 0.0225(4) Uani 1 1 d . . . H13 H 0.0743 0.7058 -0.0216 0.027 Uiso 1 1 calc R . . C14 C 0.14552(9) 0.90391(12) 0.13463(9) 0.0185(4) Uani 1 1 d . . . H14 H 0.1669 0.9056 0.1764 0.022 Uiso 1 1 calc R . . C15 C -0.03383(9) 1.24718(14) -0.15881(9) 0.0200(4) Uani 1 1 d . . . C16 C -0.03862(9) 1.15701(14) -0.18217(9) 0.0192(4) Uani 1 1 d . . . C17 C -0.06498(10) 1.14288(15) -0.24440(9) 0.0242(5) Uani 1 1 d . . . H17 H -0.0686 1.0825 -0.2598 0.029 Uiso 1 1 calc R . . C18 C -0.08562(11) 1.21550(17) -0.28326(10) 0.0303(5) Uani 1 1 d . . . H18 H -0.1029 1.2054 -0.3250 0.036 Uiso 1 1 calc R . . C19 C -0.08061(11) 1.30438(16) -0.25996(10) 0.0317(5) Uani 1 1 d . . . H19 H -0.0950 1.3544 -0.2864 0.038 Uiso 1 1 calc R . . N20 N 0.08289(8) 1.29535(10) 0.06992(7) 0.0177(4) Uani 1 1 d . . . C20 C -0.05513(10) 1.32043(15) -0.19929(10) 0.0268(5) Uani 1 1 d . . . H20 H -0.0519 1.3812 -0.1846 0.032 Uiso 1 1 calc R . . N21 N 0.00672(7) 1.08114(10) -0.08725(7) 0.0162(3) Uani 1 1 d . . . C21 C -0.02147(9) 1.07726(13) -0.14445(9) 0.0188(4) Uani 1 1 d . A . H21 H -0.0313 1.0188 -0.1625 0.023 Uiso 1 1 calc R . . C22 C 0.25064(9) 0.94708(13) 0.03268(9) 0.0187(4) Uani 1 1 d . . . C23 C 0.30397(10) 0.99042(14) 0.05946(11) 0.0275(5) Uani 1 1 d . . . H23 H 0.3075 1.0538 0.0531 0.033 Uiso 1 1 calc R . . C24 C 0.35170(11) 0.94098(17) 0.09524(12) 0.0357(6) Uani 1 1 d . . . H24 H 0.3875 0.9710 0.1136 0.043 Uiso 1 1 calc R . . C25 C 0.34728(11) 0.84788(16) 0.10436(11) 0.0313(5) Uani 1 1 d . . . H25 H 0.3801 0.8143 0.1284 0.038 Uiso 1 1 calc R . . C26 C 0.29475(10) 0.80419(14) 0.07816(10) 0.0253(5) Uani 1 1 d . . . H26 H 0.2916 0.7407 0.0845 0.030 Uiso 1 1 calc R . . C27 C 0.24672(9) 0.85343(13) 0.04255(9) 0.0201(4) Uani 1 1 d . . . H27 H 0.2109 0.8232 0.0248 0.024 Uiso 1 1 calc R . . C28 C 0.18655(10) 0.99723(13) -0.09020(10) 0.0213(4) Uani 1 1 d . . . C29 C 0.15226(10) 0.92783(14) -0.12687(10) 0.0267(5) Uani 1 1 d . . . H29 H 0.1296 0.8898 -0.1124 0.032 Uiso 1 1 calc R . . C30 C 0.15167(11) 0.91501(16) -0.18460(11) 0.0335(6) Uani 1 1 d . . . H30 H 0.1289 0.8679 -0.2092 0.040 Uiso 1 1 calc R . . C31 C 0.18428(12) 0.97091(18) -0.20595(11) 0.0373(6) Uani 1 1 d . . . H31 H 0.1839 0.9615 -0.2450 0.045 Uiso 1 1 calc R . . C32 C 0.21744(11) 1.04055(17) -0.17084(11) 0.0322(6) Uani 1 1 d . . . H32 H 0.2392 1.0791 -0.1861 0.039 Uiso 1 1 calc R . . C33 C 0.21868(10) 1.05391(14) -0.11273(10) 0.0252(5) Uani 1 1 d . . . H33 H 0.2414 1.1015 -0.0887 0.030 Uiso 1 1 calc R . . C34 C 0.0056(3) 1.1847(4) 0.1666(3) 0.0753(16) Uiso 0.70 1 d P A 1 H34A H 0.0215 1.2434 0.1847 0.113 Uiso 0.70 1 calc PR A 1 H34B H 0.0226 1.1354 0.1952 0.113 Uiso 0.70 1 calc PR A 1 H34C H -0.0361 1.1849 0.1558 0.113 Uiso 0.70 1 calc PR A 1 C35 C 0.24517(11) 1.17635(18) 0.14741(11) 0.0353(6) Uani 1 1 d . A . H35A H 0.2385 1.1811 0.1848 0.053 Uiso 1 1 calc R . . H35B H 0.2729 1.2229 0.1467 0.053 Uiso 1 1 calc R . . H35C H 0.2603 1.1156 0.1445 0.053 Uiso 1 1 calc R . . C36 C 0.13037(11) 1.30061(13) -0.06230(11) 0.0283(5) Uani 1 1 d . . . H36A H 0.0998 1.3390 -0.0895 0.042 Uiso 1 1 calc R . . H36B H 0.1622 1.2972 -0.0764 0.042 Uiso 1 1 calc R . . H36C H 0.1440 1.3272 -0.0222 0.042 Uiso 1 1 calc R . . C34A C -0.0045(5) 1.2347(9) 0.1461(6) 0.089(4) Uiso 0.30 1 d P A 2 H34D H -0.0327 1.2039 0.1589 0.134 Uiso 0.30 1 calc PR A 2 H34E H -0.0231 1.2851 0.1191 0.134 Uiso 0.30 1 calc PR A 2 H34F H 0.0267 1.2587 0.1811 0.134 Uiso 0.30 1 calc PR A 2 H11S H 0.1357 1.1747 -0.0369 0.107 Uiso 1 1 d RD . . H10S H 0.1947 1.1688 0.0660 0.107 Uiso 1 1 d RD . . H9S H -0.0083 1.1402 0.0950 0.107 Uiso 1 1 d RD . . 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 0.01793(17) 0.01236(12) 0.01178(15) -0.00020(10) 0.00288(12) 0.00079(10) P1 0.0197(3) 0.0157(2) 0.0180(3) -0.00001(18) 0.0091(2) 0.00086(18) O1 0.0279(9) 0.0145(6) 0.0153(7) -0.0025(5) 0.0054(6) -0.0004(5) C1 0.0160(11) 0.0191(8) 0.0172(10) -0.0035(7) 0.0067(8) -0.0007(7) Mn2 0.01484(17) 0.01215(12) 0.01165(15) 0.00050(9) 0.00293(12) 0.00023(10) O2 0.0281(9) 0.0161(6) 0.0147(7) 0.0003(5) -0.0013(6) 0.0055(6) C2 0.0198(11) 0.0178(8) 0.0179(10) -0.0022(7) 0.0068(8) 0.0021(7) Mn3 0.01995(18) 0.01430(13) 0.01210(15) 0.00167(10) 0.00209(12) 0.00185(11) O3 0.0163(8) 0.0136(5) 0.0167(7) 0.0006(5) 0.0029(6) 0.0002(5) N3 0.0176(9) 0.0131(6) 0.0148(8) -0.0005(6) 0.0041(7) -0.0009(6) C3 0.0285(13) 0.0172(8) 0.0253(11) -0.0036(8) 0.0089(10) -0.0002(8) O4 0.0270(9) 0.0134(6) 0.0136(7) -0.0021(5) 0.0023(6) -0.0007(5) C4 0.0322(14) 0.0203(9) 0.0245(12) -0.0095(8) 0.0079(10) -0.0057(8) O5 0.0252(8) 0.0204(6) 0.0138(7) 0.0034(5) 0.0026(6) 0.0036(6) C5 0.0267(13) 0.0273(10) 0.0189(11) -0.0063(8) 0.0061(9) -0.0038(9) O6 0.0199(8) 0.0146(6) 0.0145(7) 0.0030(5) 0.0029(6) -0.0004(5) C6 0.0236(12) 0.0211(9) 0.0187(10) -0.0018(7) 0.0060(9) 0.0004(8) O7 0.0202(8) 0.0203(6) 0.0232(8) -0.0005(6) 0.0106(6) 0.0001(6) C7 0.0256(12) 0.0143(8) 0.0180(10) 0.0004(7) 0.0067(8) 0.0049(7) O8 0.0262(9) 0.0173(6) 0.0236(8) -0.0006(5) 0.0127(7) 0.0006(6) C8 0.0169(11) 0.0146(8) 0.0205(10) 0.0017(7) 0.0078(8) 0.0009(7) O9 0.0264(10) 0.0434(9) 0.0307(9) -0.0172(7) 0.0160(8) -0.0095(7) C9 0.0170(11) 0.0163(8) 0.0186(10) 0.0019(7) 0.0063(8) 0.0000(7) O10 0.0179(8) 0.0247(7) 0.0180(8) 0.0002(5) 0.0033(6) 0.0018(6) C10 0.0178(11) 0.0211(9) 0.0235(11) 0.0065(8) 0.0032(9) 0.0022(8) O11 0.0257(9) 0.0168(6) 0.0227(8) 0.0032(5) 0.0085(6) -0.0035(6) C11 0.0218(12) 0.0185(9) 0.0368(13) 0.0056(8) 0.0089(10) 0.0065(8) O12 0.0175(8) 0.0130(5) 0.0127(7) 0.0018(5) 0.0034(5) 0.0022(5) C12 0.0306(13) 0.0163(8) 0.0335(13) -0.0011(8) 0.0131(10) 0.0038(8) C13 0.0222(12) 0.0197(8) 0.0236(11) -0.0032(8) 0.0064(9) 0.0005(8) C14 0.0188(11) 0.0177(8) 0.0175(10) 0.0020(7) 0.0052(8) -0.0010(7) C15 0.0171(11) 0.0270(9) 0.0149(10) 0.0073(8) 0.0049(8) 0.0030(8) C16 0.0157(11) 0.0287(9) 0.0129(10) 0.0043(8) 0.0048(8) -0.0008(8) C17 0.0241(12) 0.0321(10) 0.0153(10) 0.0002(8) 0.0061(9) -0.0026(9) C18 0.0307(14) 0.0456(13) 0.0111(10) 0.0073(9) 0.0039(9) 0.0024(11) C19 0.0339(15) 0.0390(12) 0.0193(12) 0.0136(9) 0.0066(10) 0.0094(10) N20 0.0207(10) 0.0185(7) 0.0107(8) 0.0000(6) 0.0023(7) 0.0028(6) C20 0.0272(13) 0.0306(10) 0.0208(11) 0.0071(8) 0.0070(10) 0.0061(9) N21 0.0180(9) 0.0161(7) 0.0132(8) 0.0028(6) 0.0045(7) 0.0001(6) C21 0.0171(11) 0.0229(9) 0.0158(10) -0.0006(7) 0.0054(8) -0.0016(8) C22 0.0232(12) 0.0185(8) 0.0177(10) -0.0009(7) 0.0112(9) -0.0010(7) C23 0.0240(13) 0.0250(10) 0.0338(13) 0.0016(9) 0.0110(10) -0.0023(9) C24 0.0226(14) 0.0377(12) 0.0440(16) -0.0037(11) 0.0092(12) -0.0037(10) C25 0.0241(13) 0.0405(12) 0.0278(13) 0.0029(10) 0.0080(10) 0.0091(10) C26 0.0320(14) 0.0217(9) 0.0249(12) 0.0043(8) 0.0137(10) 0.0070(9) C27 0.0215(12) 0.0198(8) 0.0211(11) 0.0006(7) 0.0102(9) 0.0005(8) C28 0.0224(12) 0.0223(9) 0.0195(11) 0.0028(7) 0.0081(9) 0.0081(8) C29 0.0289(14) 0.0230(9) 0.0268(12) 0.0005(8) 0.0090(10) 0.0064(9) C30 0.0391(16) 0.0318(11) 0.0224(12) -0.0032(9) 0.0031(11) 0.0108(10) C31 0.0505(18) 0.0453(13) 0.0176(12) 0.0057(10) 0.0143(12) 0.0244(12) C32 0.0368(15) 0.0406(12) 0.0248(12) 0.0129(10) 0.0181(11) 0.0149(11) C33 0.0278(13) 0.0268(10) 0.0234(11) 0.0062(8) 0.0122(10) 0.0070(9) C35 0.0226(13) 0.0519(14) 0.0244(13) -0.0068(10) 0.0008(10) 0.0073(11) C36 0.0371(15) 0.0175(9) 0.0347(13) 0.0006(8) 0.0184(11) -0.0061(9) _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 1.880(4) . ? Mn1 O12 1.902(4) . ? Mn1 O4 1.933(3) . ? Mn1 N20 2.015(3) . ? Mn1 O10 2.258(3) . ? Mn1 O9 2.306(4) . ? P1 O7 1.515(2) . ? P1 O8 1.527(2) . ? P1 C22 1.806(3) . ? P1 C28 1.807(5) . ? O1 C1 1.336(3) . ? C1 C6 1.407(4) . ? C1 C2 1.425(3) . ? Mn2 O12 1.900(3) . ? Mn2 O3 1.913(3) . ? Mn2 O6 1.958(3) . ? Mn2 N3 2.015(4) . ? Mn2 O7 2.075(3) . ? Mn2 O6 2.473(3) 5_575 ? O2 N20 1.383(3) . ? O2 Mn3 1.903(3) . ? C2 C3 1.411(3) . ? C2 C7 1.451(4) . ? Mn3 O5 1.878(3) . ? Mn3 O12 1.889(3) . ? Mn3 N21 1.997(3) . ? Mn3 O11 2.209(3) . ? O3 C8 1.350(3) . ? N3 C14 1.294(3) . ? N3 O4 1.375(3) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.399(4) . ? C4 H4 0.9500 . ? O5 C15 1.336(4) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? O6 N21 1.401(2) . ? O6 Mn2 2.473(3) 5_575 ? C6 H6 0.9500 . ? C7 N20 1.295(3) . ? C7 H7 0.9500 . ? C8 C13 1.410(3) . ? C8 C9 1.420(4) . ? O9 C34 1.393(7) . ? O9 C34A 1.431(11) . ? O9 H9S 0.8033 . ? C9 C10 1.411(3) . ? C9 C14 1.456(3) . ? O10 C35 1.436(3) . ? O10 H10S 0.8550 . ? C10 C11 1.382(3) . ? C10 H10 0.9500 . ? O11 C36 1.439(3) . ? O11 H11S 0.8800 . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.415(3) . ? C15 C16 1.423(3) . ? C16 C17 1.414(4) . ? C16 C21 1.444(3) . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 C19 1.405(4) . ? C18 H18 0.9500 . ? C19 C20 1.383(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? N21 C21 1.298(4) . ? C21 H21 0.9500 . ? C22 C27 1.401(3) . ? C22 C23 1.404(3) . ? C23 C24 1.392(4) . ? C23 H23 0.9500 . ? C24 C25 1.392(4) . ? C24 H24 0.9500 . ? C25 C26 1.389(4) . ? C25 H25 0.9500 . ? C26 C27 1.394(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.401(3) . ? C28 C29 1.411(3) . ? C29 C30 1.401(4) . ? C29 H29 0.9500 . ? C30 C31 1.386(4) . ? C30 H30 0.9500 . ? C31 C32 1.388(4) . ? C31 H31 0.9500 . ? C32 C33 1.405(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 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 O12 178.78(6) . . ? O1 Mn1 O4 88.40(12) . . ? O12 Mn1 O4 92.25(12) . . ? O1 Mn1 N20 90.35(12) . . ? O12 Mn1 N20 88.96(12) . . ? O4 Mn1 N20 177.69(7) . . ? O1 Mn1 O10 89.74(10) . . ? O12 Mn1 O10 91.26(10) . . ? O4 Mn1 O10 93.10(8) . . ? N20 Mn1 O10 88.84(8) . . ? O1 Mn1 O9 87.99(10) . . ? O12 Mn1 O9 90.93(10) . . ? O4 Mn1 O9 93.29(8) . . ? N20 Mn1 O9 84.72(8) . . ? O10 Mn1 O9 173.15(6) . . ? O7 P1 O8 117.49(9) . . ? O7 P1 C22 108.25(13) . . ? O8 P1 C22 108.56(11) . . ? O7 P1 C28 107.59(10) . . ? O8 P1 C28 107.95(9) . . ? C22 P1 C28 106.48(13) . . ? C1 O1 Mn1 130.14(13) . . ? O1 C1 C6 118.50(17) . . ? O1 C1 C2 123.6(2) . . ? C6 C1 C2 117.9(2) . . ? O12 Mn2 O3 169.07(6) . . ? O12 Mn2 O6 90.99(6) . . ? O3 Mn2 O6 88.21(6) . . ? O12 Mn2 N3 88.86(6) . . ? O3 Mn2 N3 89.58(6) . . ? O6 Mn2 N3 167.51(7) . . ? O12 Mn2 O7 100.73(6) . . ? O3 Mn2 O7 90.20(7) . . ? O6 Mn2 O7 95.65(16) . . ? N3 Mn2 O7 96.65(15) . . ? O12 Mn2 O6 84.38(5) . 5_575 ? O3 Mn2 O6 84.71(6) . 5_575 ? O6 Mn2 O6 82.06(16) . 5_575 ? N3 Mn2 O6 85.50(14) . 5_575 ? O7 Mn2 O6 174.47(5) . 5_575 ? N20 O2 Mn3 118.38(13) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 C7 117.52(18) . . ? C1 C2 C7 122.66(19) . . ? O5 Mn3 O12 177.73(6) . . ? O5 Mn3 O2 86.23(14) . . ? O12 Mn3 O2 92.93(14) . . ? O5 Mn3 N21 90.08(14) . . ? O12 Mn3 N21 90.47(14) . . ? O2 Mn3 N21 171.55(7) . . ? O5 Mn3 O11 90.57(12) . . ? O12 Mn3 O11 91.60(12) . . ? O2 Mn3 O11 94.86(9) . . ? N21 Mn3 O11 92.78(10) . . ? C8 O3 Mn2 121.29(14) . . ? C14 N3 O4 116.2(2) . . ? C14 N3 Mn2 124.76(14) . . ? O4 N3 Mn2 118.83(14) . . ? C4 C3 C2 121.5(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? N3 O4 Mn1 117.64(17) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C15 O5 Mn3 129.87(15) . . ? C6 C5 C4 121.0(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? N21 O6 Mn2 115.63(13) . . ? N21 O6 Mn2 104.02(12) . 5_575 ? Mn2 O6 Mn2 97.94(16) . 5_575 ? C5 C6 C1 121.02(19) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? P1 O7 Mn2 141.80(10) . . ? N20 C7 C2 124.18(18) . . ? N20 C7 H7 117.9 . . ? C2 C7 H7 117.9 . . ? O3 C8 C13 119.6(2) . . ? O3 C8 C9 121.53(17) . . ? C13 C8 C9 118.77(19) . . ? C34 O9 C34A 35.7(5) . . ? C34 O9 Mn1 128.2(3) . . ? C34A O9 Mn1 128.6(5) . . ? C34A O9 H9S 106.9 . . ? Mn1 O9 H9S 123.2 . . ? C10 C9 C8 118.94(18) . . ? C10 C9 C14 118.4(2) . . ? C8 C9 C14 122.64(18) . . ? C35 O10 Mn1 121.48(19) . . ? C35 O10 H10S 110.0 . . ? Mn1 O10 H10S 115.9 . . ? C11 C10 C9 121.2(2) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C36 O11 Mn3 119.66(13) . . ? C36 O11 H11S 110.4 . . ? Mn3 O11 H11S 107.2 . . ? C10 C11 C12 119.6(2) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? Mn3 O12 Mn2 119.34(10) . . ? Mn3 O12 Mn1 119.68(13) . . ? Mn2 O12 Mn1 119.76(8) . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 120.7(2) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? N3 C14 C9 123.7(2) . . ? N3 C14 H14 118.2 . . ? C9 C14 H14 118.2 . . ? O5 C15 C20 118.3(2) . . ? O5 C15 C16 123.31(17) . . ? C20 C15 C16 118.3(2) . . ? C17 C16 C15 119.62(19) . . ? C17 C16 C21 117.6(2) . . ? C15 C16 C21 122.6(2) . . ? C18 C17 C16 121.1(2) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 119.0(2) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 121.3(2) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C7 N20 O2 114.13(16) . . ? C7 N20 Mn1 127.26(17) . . ? O2 N20 Mn1 118.58(12) . . ? C19 C20 C15 120.7(2) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C21 N21 O6 115.04(17) . . ? C21 N21 Mn3 128.06(14) . . ? O6 N21 Mn3 115.59(18) . . ? N21 C21 C16 123.52(19) . . ? N21 C21 H21 118.2 . . ? C16 C21 H21 118.2 . . ? C27 C22 C23 118.6(2) . . ? C27 C22 P1 121.24(17) . . ? C23 C22 P1 120.12(17) . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.0(2) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.8(2) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C33 C28 C29 119.2(2) . . ? C33 C28 P1 120.89(18) . . ? C29 C28 P1 119.87(18) . . ? C30 C29 C28 119.9(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.1(2) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.7(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 119.8(2) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 120.2(2) . . ? C28 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? O9 C34 H34A 109.5 . . ? O9 C34 H34B 109.5 . . ? O9 C34 H34C 109.5 . . ? O10 C35 H35A 109.5 . . ? O10 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O10 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O11 C36 H36A 109.5 . . ? O11 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O11 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O9 C34A H34D 109.5 . . ? O9 C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? O9 C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.32 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.572 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.091 # Attachment 'Complex 2.CIF' data_RI2361 _database_code_depnum_ccdc_archive 'CCDC 760678' #TrackingRef 'Complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common RI2361 _chemical_melting_point ? _chemical_formula_moiety 'C78 H86 Mn6 N6 O24 P2, 3(C H4 O)' _chemical_formula_sum 'C81 H98 Mn6 N6 O27 P2' _chemical_formula_weight 1979.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.14(2) _cell_length_b 12.80(2) _cell_length_c 29.09(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.571(19) _cell_angle_gamma 90.00 _cell_volume 8519(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4088 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6498 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex 2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75431 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.39 _reflns_number_total 9545 _reflns_number_gt 6864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. A number of restraints were applied due to disorder present in methanol molecules of crystallis- ation. ; _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^)+(0.0409P)^2^+7.3305P] 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 9545 _refine_ls_number_parameters 568 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.003 _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 0.139425(17) 0.15309(3) 0.034298(14) 0.01294(10) Uani 1 1 d . . . O4 O 0.06694(7) 0.22156(14) 0.03894(6) 0.0161(4) Uani 1 1 d . . . C1 C 0.38337(11) 0.3406(2) 0.07602(9) 0.0145(6) Uani 1 1 d . . . Mn2 Mn 0.265329(16) 0.27278(3) 0.055783(14) 0.01171(10) Uani 1 1 d . . . O7 O 0.18467(7) 0.26877(14) 0.05700(6) 0.0128(4) Uani 1 1 d . . . C2 C 0.43994(11) 0.3024(2) 0.08537(9) 0.0155(6) Uani 1 1 d . . . H2 H 0.4501 0.2407 0.0702 0.019 Uiso 1 1 calc R . . Mn3 Mn 0.143831(16) 0.39008(3) 0.069059(14) 0.01322(10) Uani 1 1 d . . . O5 O 0.09956(7) 0.03660(14) 0.00992(6) 0.0161(4) Uani 1 1 d . . . C3 C 0.48160(12) 0.3525(2) 0.11625(10) 0.0192(6) Uani 1 1 d . . . H3 H 0.5203 0.3256 0.1221 0.023 Uiso 1 1 calc R . . P4 P 0.27999(3) 0.16866(6) 0.16578(3) 0.01537(16) Uani 1 1 d . . . O3 O 0.09993(7) 0.50593(14) 0.07987(7) 0.0168(4) Uani 1 1 d . . . C4 C 0.46748(12) 0.4417(2) 0.13870(10) 0.0183(6) Uani 1 1 d . . . H4 H 0.4960 0.4758 0.1604 0.022 Uiso 1 1 calc R . . O1 O 0.34447(7) 0.29063(14) 0.04432(6) 0.0134(4) Uani 1 1 d . . . C5 C 0.41183(11) 0.4809(2) 0.12935(10) 0.0174(6) Uani 1 1 d . . . H5 H 0.4024 0.5427 0.1447 0.021 Uiso 1 1 calc R . . O10 O 0.16528(8) 0.36252(15) 0.14557(7) 0.0195(4) Uani 1 1 d D . . C6 C 0.36867(11) 0.4328(2) 0.09797(9) 0.0139(6) Uani 1 1 d . . . O2 O 0.21282(7) 0.47286(14) 0.07031(7) 0.0151(4) Uani 1 1 d . . . C7 C 0.31062(11) 0.4797(2) 0.08947(9) 0.0143(6) Uani 1 1 d . . . O6 O 0.25918(7) 0.14539(14) 0.01999(6) 0.0133(4) Uani 1 1 d . . . C8 C 0.30253(12) 0.5941(2) 0.09513(11) 0.0212(7) Uani 1 1 d . . . H8A H 0.2767 0.6214 0.0680 0.032 Uiso 1 1 calc R . . H8B H 0.3405 0.6292 0.0978 0.032 Uiso 1 1 calc R . . H8C H 0.2851 0.6070 0.1233 0.032 Uiso 1 1 calc R . . O12 O 0.11652(8) 0.40491(14) -0.00790(6) 0.0167(4) Uani 1 1 d D . . C9 C 0.06486(11) 0.5045(2) 0.11216(10) 0.0174(6) Uani 1 1 d . . . O11 O 0.14348(8) 0.09157(15) 0.10484(6) 0.0183(4) Uani 1 1 d D . . C10 C 0.06291(12) 0.5928(2) 0.13968(10) 0.0223(7) Uani 1 1 d . . . H10 H 0.0865 0.6515 0.1349 0.027 Uiso 1 1 calc R . . O13 O 0.14818(10) 0.11813(19) 0.23819(8) 0.0373(6) Uani 1 1 d D . . N11 N 0.26510(9) 0.42155(17) 0.07695(8) 0.0136(5) Uani 1 1 d . . . C11 C 0.02763(13) 0.5972(2) 0.17368(12) 0.0298(8) Uani 1 1 d . . . H11 H 0.0268 0.6586 0.1920 0.036 Uiso 1 1 calc R . . N12 N 0.07170(9) 0.30551(17) 0.06835(8) 0.0146(5) Uani 1 1 d . . . C12 C -0.00684(14) 0.5121(3) 0.18127(12) 0.0352(8) Uani 1 1 d . . . H12 H -0.0307 0.5141 0.2052 0.042 Uiso 1 1 calc R . . O9 O 0.21632(8) 0.18022(15) 0.17237(6) 0.0175(4) Uani 1 1 d . . . C13 C -0.00607(13) 0.4254(3) 0.15404(11) 0.0279(7) Uani 1 1 d . . . H13 H -0.0307 0.3682 0.1588 0.033 Uiso 1 1 calc R . . O8 O 0.29387(8) 0.19889(15) 0.11894(6) 0.0170(4) Uani 1 1 d . . . C14 C 0.02956(11) 0.4176(2) 0.11948(10) 0.0173(6) Uani 1 1 d . . . N15 N 0.21377(9) 0.08053(17) 0.02850(7) 0.0126(5) Uani 1 1 d . . . C15 C 0.02808(11) 0.3235(2) 0.09067(10) 0.0176(6) Uani 1 1 d . . . C16 C -0.02309(12) 0.2516(2) 0.08742(11) 0.0257(7) Uani 1 1 d . . . H16A H -0.0198 0.1979 0.0640 0.039 Uiso 1 1 calc R . . H16B H -0.0592 0.2915 0.0785 0.039 Uiso 1 1 calc R . . H16C H -0.0239 0.2183 0.1176 0.039 Uiso 1 1 calc R . . C17 C 0.11599(12) -0.0591(2) 0.02255(9) 0.0150(6) Uani 1 1 d . . . C18 C 0.07221(12) -0.1335(2) 0.02417(10) 0.0199(6) Uani 1 1 d . . . H18 H 0.0324 -0.1139 0.0160 0.024 Uiso 1 1 calc R . . C19 C 0.08594(13) -0.2340(2) 0.03732(11) 0.0253(7) Uani 1 1 d . . . H19 H 0.0556 -0.2836 0.0383 0.030 Uiso 1 1 calc R . . C20 C 0.14362(13) -0.2642(2) 0.04921(11) 0.0261(7) Uani 1 1 d . . . H20 H 0.1529 -0.3339 0.0588 0.031 Uiso 1 1 calc R . . C21 C 0.18731(13) -0.1930(2) 0.04706(11) 0.0232(7) Uani 1 1 d . . . H21 H 0.2269 -0.2146 0.0546 0.028 Uiso 1 1 calc R . . C22 C 0.17516(11) -0.0890(2) 0.03396(9) 0.0152(6) Uani 1 1 d . . . C23 C 0.22421(11) -0.0181(2) 0.03102(9) 0.0157(6) Uani 1 1 d . . . C24 C 0.28474(11) -0.0592(2) 0.03148(11) 0.0201(6) Uani 1 1 d . . . H24A H 0.3083 -0.0071 0.0179 0.030 Uiso 1 1 calc R . . H24B H 0.2832 -0.1238 0.0133 0.030 Uiso 1 1 calc R . . H24C H 0.3025 -0.0736 0.0636 0.030 Uiso 1 1 calc R . . C25 C 0.30110(12) 0.0350(2) 0.17745(10) 0.0184(6) Uani 1 1 d . . . C26 C 0.34732(13) 0.0073(3) 0.21072(11) 0.0263(7) Uani 1 1 d . . . H26 H 0.3688 0.0602 0.2288 0.032 Uiso 1 1 calc R . . C27 C 0.36295(14) -0.0965(2) 0.21820(12) 0.0313(8) Uani 1 1 d . . . H27 H 0.3947 -0.1145 0.2414 0.038 Uiso 1 1 calc R . . C28 C 0.33257(14) -0.1726(3) 0.19213(12) 0.0317(8) Uani 1 1 d . . . H28 H 0.3436 -0.2437 0.1968 0.038 Uiso 1 1 calc R . . C29 C 0.28625(14) -0.1468(2) 0.15926(12) 0.0303(8) Uani 1 1 d . . . H29 H 0.2649 -0.2001 0.1414 0.036 Uiso 1 1 calc R . . C30 C 0.27040(13) -0.0431(2) 0.15192(11) 0.0244(7) Uani 1 1 d . . . H30 H 0.2381 -0.0256 0.1291 0.029 Uiso 1 1 calc R . . C31 C 0.32483(12) 0.2420(2) 0.20927(9) 0.0168(6) Uani 1 1 d . . . C32 C 0.37939(12) 0.2770(2) 0.20098(10) 0.0220(7) Uani 1 1 d . . . H32 H 0.3913 0.2652 0.1715 0.026 Uiso 1 1 calc R . . C33 C 0.41593(13) 0.3282(3) 0.23516(11) 0.0277(7) Uani 1 1 d . . . H33 H 0.4528 0.3529 0.2292 0.033 Uiso 1 1 calc R . . C34 C 0.39906(13) 0.3438(3) 0.27816(11) 0.0285(7) Uani 1 1 d . . . H34 H 0.4246 0.3788 0.3019 0.034 Uiso 1 1 calc R . . C35 C 0.34540(14) 0.3091(3) 0.28694(11) 0.0295(7) Uani 1 1 d . . . H35 H 0.3341 0.3197 0.3167 0.035 Uiso 1 1 calc R . . C36 C 0.30805(13) 0.2589(2) 0.25251(10) 0.0230(7) Uani 1 1 d . . . H36 H 0.2708 0.2359 0.2584 0.028 Uiso 1 1 calc R . . C37 C 0.19778(14) 0.4385(2) 0.17462(11) 0.0307(8) Uani 1 1 d . . . H37A H 0.2372 0.4442 0.1664 0.046 Uiso 1 1 calc R . . H37B H 0.2004 0.4170 0.2072 0.046 Uiso 1 1 calc R . . H37C H 0.1781 0.5063 0.1703 0.046 Uiso 1 1 calc R . . C38 C 0.09402(13) 0.0487(3) 0.12264(11) 0.0294(8) Uani 1 1 d . . . H38A H 0.0807 0.0982 0.1445 0.044 Uiso 1 1 calc R . . H38B H 0.1052 -0.0172 0.1387 0.044 Uiso 1 1 calc R . . H38C H 0.0624 0.0359 0.0969 0.044 Uiso 1 1 calc R . . C39 C 0.06710(13) 0.4577(3) -0.03192(11) 0.0293(8) Uani 1 1 d . . . H39A H 0.0317 0.4174 -0.0294 0.044 Uiso 1 1 calc R . . H39B H 0.0715 0.4651 -0.0648 0.044 Uiso 1 1 calc R . . H39C H 0.0640 0.5271 -0.0182 0.044 Uiso 1 1 calc R . . C40 C 0.18626(15) 0.0548(3) 0.26762(11) 0.0342(8) Uani 1 1 d D . . H40A H 0.2122 0.0987 0.2893 0.051 Uiso 1 1 calc R . . H40B H 0.2096 0.0126 0.2491 0.051 Uiso 1 1 calc R . . H40C H 0.1637 0.0086 0.2851 0.051 Uiso 1 1 calc R . . C41 C 0.4928(12) 0.6625(7) 0.2463(16) 0.081(6) Uani 0.50 1 d PDU A -1 H41A H 0.4928 0.6662 0.2799 0.122 Uiso 0.50 1 calc PR A -1 H41B H 0.4530 0.6500 0.2305 0.122 Uiso 0.50 1 calc PR A -1 H41C H 0.5073 0.7286 0.2354 0.122 Uiso 0.50 1 calc PR A -1 O14 O 0.5310(2) 0.5766(6) 0.2358(3) 0.100(3) Uani 0.50 1 d PDU A -1 H14 H 0.5661 0.5934 0.2441 0.120 Uiso 0.50 1 calc PR A -1 H11O H 0.1668 0.1215 0.1255 0.120 Uiso 1 1 d RD . . H10O H 0.1780 0.3045 0.1547 0.120 Uiso 1 1 d RD . . H12O H 0.1288 0.3558 -0.0225 0.120 Uiso 1 1 d RD . . H13O H 0.1674 0.1641 0.2236 0.120 Uiso 1 1 d RD . . 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 0.0123(2) 0.0099(2) 0.0169(2) -0.00100(17) 0.00322(16) -0.00153(16) O4 0.0142(9) 0.0124(10) 0.0215(10) -0.0044(8) 0.0022(8) -0.0015(8) C1 0.0133(13) 0.0165(15) 0.0141(14) 0.0038(11) 0.0035(11) -0.0021(11) Mn2 0.01107(19) 0.0096(2) 0.0149(2) -0.00077(17) 0.00347(16) -0.00094(16) O7 0.0125(9) 0.0113(10) 0.0150(10) -0.0012(8) 0.0030(7) -0.0007(7) C2 0.0161(13) 0.0119(14) 0.0191(15) -0.0005(12) 0.0047(11) 0.0001(11) Mn3 0.0121(2) 0.0101(2) 0.0182(2) -0.00062(17) 0.00457(16) -0.00042(16) O5 0.0156(9) 0.0114(10) 0.0210(11) -0.0011(8) 0.0020(8) -0.0012(8) C3 0.0137(13) 0.0218(16) 0.0215(16) 0.0008(13) 0.0006(12) 0.0005(12) P4 0.0154(3) 0.0151(4) 0.0156(4) 0.0009(3) 0.0024(3) -0.0005(3) O3 0.0159(9) 0.0135(10) 0.0226(11) 0.0015(8) 0.0082(8) 0.0029(8) C4 0.0165(14) 0.0181(16) 0.0196(15) -0.0010(12) 0.0002(11) -0.0046(12) O1 0.0120(9) 0.0140(10) 0.0142(10) -0.0012(8) 0.0018(7) -0.0023(8) C5 0.0191(14) 0.0113(14) 0.0229(16) -0.0008(12) 0.0064(12) -0.0010(11) O10 0.0225(10) 0.0179(11) 0.0178(11) -0.0027(8) 0.0018(8) 0.0024(8) C6 0.0130(13) 0.0121(14) 0.0167(14) 0.0006(11) 0.0024(11) -0.0022(11) O2 0.0098(9) 0.0108(10) 0.0245(11) 0.0000(8) 0.0021(8) 0.0012(7) C7 0.0165(13) 0.0102(14) 0.0170(14) -0.0002(11) 0.0053(11) -0.0023(11) O6 0.0128(9) 0.0120(10) 0.0157(10) -0.0001(8) 0.0045(8) -0.0051(7) C8 0.0199(14) 0.0122(15) 0.0309(18) -0.0018(13) 0.0020(13) -0.0003(12) O12 0.0169(9) 0.0159(11) 0.0171(10) 0.0015(8) 0.0022(8) 0.0021(8) C9 0.0144(13) 0.0182(15) 0.0197(15) 0.0008(12) 0.0031(11) 0.0035(12) O11 0.0176(10) 0.0194(11) 0.0187(11) 0.0016(9) 0.0047(8) -0.0051(8) C10 0.0239(15) 0.0178(16) 0.0265(17) -0.0030(13) 0.0077(13) 0.0005(13) O13 0.0390(13) 0.0407(15) 0.0319(14) 0.0015(11) 0.0044(11) -0.0034(12) N11 0.0114(11) 0.0146(12) 0.0155(12) -0.0005(10) 0.0044(9) 0.0014(9) C11 0.0339(18) 0.0224(18) 0.036(2) -0.0109(15) 0.0138(15) 0.0012(14) N12 0.0161(11) 0.0104(12) 0.0172(12) -0.0030(10) 0.0021(9) 0.0015(9) C12 0.0385(19) 0.032(2) 0.041(2) -0.0097(16) 0.0263(16) -0.0030(16) O9 0.0168(10) 0.0181(11) 0.0175(10) -0.0007(8) 0.0026(8) -0.0006(8) C13 0.0288(17) 0.0248(18) 0.0335(19) -0.0020(15) 0.0163(14) -0.0028(14) O8 0.0175(10) 0.0163(10) 0.0173(10) 0.0017(8) 0.0032(8) -0.0002(8) C14 0.0162(13) 0.0139(15) 0.0220(16) -0.0011(12) 0.0038(12) -0.0001(11) N15 0.0150(11) 0.0099(12) 0.0134(12) -0.0009(9) 0.0039(9) -0.0042(9) C15 0.0139(13) 0.0177(16) 0.0218(16) 0.0031(12) 0.0049(12) 0.0013(11) C16 0.0210(15) 0.0219(17) 0.0360(19) -0.0070(14) 0.0101(13) -0.0047(13) C17 0.0214(14) 0.0113(14) 0.0134(14) -0.0042(11) 0.0060(11) -0.0024(11) C18 0.0203(14) 0.0152(15) 0.0254(17) -0.0039(12) 0.0070(12) -0.0060(12) C19 0.0283(16) 0.0164(16) 0.0336(18) -0.0032(14) 0.0124(14) -0.0109(13) C20 0.0344(18) 0.0093(15) 0.0381(19) 0.0000(13) 0.0171(15) -0.0034(13) C21 0.0273(16) 0.0140(15) 0.0305(18) -0.0001(13) 0.0118(14) -0.0015(13) C22 0.0185(14) 0.0106(14) 0.0181(15) 0.0001(11) 0.0077(11) -0.0023(11) C23 0.0180(14) 0.0127(15) 0.0169(15) 0.0005(11) 0.0048(11) 0.0011(11) C24 0.0179(14) 0.0143(15) 0.0300(17) 0.0031(13) 0.0098(12) 0.0004(12) C25 0.0202(14) 0.0156(15) 0.0212(16) 0.0040(12) 0.0084(12) 0.0000(12) C26 0.0216(15) 0.0258(18) 0.0307(18) 0.0050(14) 0.0011(13) -0.0006(13) C27 0.0258(17) 0.0242(18) 0.043(2) 0.0124(16) 0.0024(15) 0.0058(14) C28 0.0330(18) 0.0194(18) 0.046(2) 0.0116(16) 0.0169(16) 0.0077(14) C29 0.0376(19) 0.0169(17) 0.037(2) -0.0029(15) 0.0083(16) -0.0026(14) C30 0.0267(16) 0.0201(17) 0.0264(17) 0.0011(13) 0.0039(13) 0.0015(13) C31 0.0173(14) 0.0147(15) 0.0177(15) 0.0022(12) 0.0005(11) 0.0015(11) C32 0.0206(14) 0.0247(17) 0.0196(16) 0.0038(13) -0.0002(12) -0.0005(13) C33 0.0167(15) 0.035(2) 0.0298(18) 0.0035(15) -0.0010(13) -0.0076(14) C34 0.0282(17) 0.0321(19) 0.0228(17) -0.0060(14) -0.0042(13) -0.0019(14) C35 0.0316(17) 0.036(2) 0.0206(17) -0.0076(15) 0.0020(13) -0.0008(15) C36 0.0206(15) 0.0259(17) 0.0226(16) -0.0025(13) 0.0034(12) -0.0025(13) C37 0.0368(19) 0.0258(19) 0.0282(19) -0.0078(15) 0.0007(15) 0.0013(15) C38 0.0291(17) 0.034(2) 0.0259(18) 0.0067(15) 0.0074(14) -0.0109(15) C39 0.0254(16) 0.0265(18) 0.0326(19) -0.0014(15) -0.0072(14) 0.0109(14) C40 0.045(2) 0.031(2) 0.0257(19) 0.0032(15) 0.0038(15) -0.0042(16) C41 0.049(12) 0.071(6) 0.127(13) 0.009(11) 0.024(11) -0.006(7) O14 0.042(4) 0.118(6) 0.140(7) -0.052(6) 0.010(4) 0.000(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 O5 1.839(3) . ? Mn1 O7 1.875(3) . ? Mn1 O4 1.915(2) . ? Mn1 N15 1.984(3) . ? Mn1 O11 2.187(3) . ? Mn1 O1 2.478(3) 7 ? Mn1 Mn3 3.194(4) . ? O4 N12 1.367(3) . ? C1 O1 1.350(3) . ? C1 C2 1.386(4) . ? C1 C6 1.408(4) . ? Mn2 O7 1.873(2) . ? Mn2 O1 1.924(2) . ? Mn2 O6 1.928(3) . ? Mn2 N11 2.001(4) . ? Mn2 O8 2.084(3) . ? Mn2 O6 2.430(3) 7 ? O7 Mn3 1.878(3) . ? C2 C3 1.375(4) . ? Mn3 O3 1.850(3) . ? Mn3 O2 1.912(2) . ? Mn3 N12 1.987(3) . ? Mn3 O10 2.235(3) . ? Mn3 O12 2.242(3) . ? O5 C17 1.318(4) . ? C3 C4 1.378(4) . ? P4 O8 1.497(2) . ? P4 O9 1.521(2) . ? P4 C31 1.780(3) . ? P4 C25 1.798(4) . ? O3 C9 1.330(3) . ? C4 C5 1.371(4) . ? O1 Mn1 2.478(3) 7 ? C5 C6 1.392(4) . ? O10 C37 1.426(4) . ? C6 C7 1.458(4) . ? O2 N11 1.365(3) . ? C7 N11 1.296(3) . ? C7 C8 1.489(4) . ? O6 N15 1.390(3) . ? O6 Mn2 2.430(3) 7 ? O12 C39 1.419(3) . ? C9 C10 1.390(4) . ? C9 C14 1.415(4) . ? O11 C38 1.434(3) . ? C10 C11 1.374(4) . ? O13 C40 1.393(4) . ? C11 C12 1.387(5) . ? N12 C15 1.300(3) . ? C12 C13 1.365(5) . ? C13 C14 1.396(4) . ? C14 C15 1.464(4) . ? N15 C23 1.286(4) . ? C15 C16 1.491(4) . ? C17 C18 1.396(4) . ? C17 C22 1.413(4) . ? C18 C19 1.366(4) . ? C19 C20 1.383(4) . ? C20 C21 1.369(4) . ? C21 C22 1.401(4) . ? C22 C23 1.465(4) . ? C23 C24 1.494(4) . ? C25 C30 1.377(4) . ? C25 C26 1.378(4) . ? C26 C27 1.385(5) . ? C27 C28 1.363(5) . ? C28 C29 1.366(5) . ? C29 C30 1.385(5) . ? C31 C36 1.387(4) . ? C31 C32 1.394(4) . ? C32 C33 1.372(4) . ? C33 C34 1.379(5) . ? C34 C35 1.378(4) . ? C35 C36 1.380(4) . ? C41 O14 1.471(17) . ? 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 O5 Mn1 O7 175.81(8) . . ? O5 Mn1 O4 90.21(11) . . ? O7 Mn1 O4 93.62(11) . . ? O5 Mn1 N15 88.82(12) . . ? O7 Mn1 N15 87.34(12) . . ? O4 Mn1 N15 178.91(9) . . ? O5 Mn1 O11 91.08(10) . . ? O7 Mn1 O11 90.58(10) . . ? O4 Mn1 O11 90.81(8) . . ? N15 Mn1 O11 89.70(9) . . ? O5 Mn1 O1 90.89(9) . 7 ? O7 Mn1 O1 86.72(9) . 7 ? O4 Mn1 O1 100.71(8) . 7 ? N15 Mn1 O1 78.81(8) . 7 ? O11 Mn1 O1 168.30(7) . 7 ? O5 Mn1 Mn3 151.94(7) . . ? O7 Mn1 Mn3 31.71(7) . . ? O4 Mn1 Mn3 61.98(7) . . ? N15 Mn1 Mn3 118.96(8) . . ? O11 Mn1 Mn3 92.86(8) . . ? O1 Mn1 Mn3 90.81(7) 7 . ? N12 O4 Mn1 114.44(15) . . ? O1 C1 C2 118.8(2) . . ? O1 C1 C6 121.7(2) . . ? C2 C1 C6 119.5(2) . . ? O7 Mn2 O1 169.72(8) . . ? O7 Mn2 O6 89.62(7) . . ? O1 Mn2 O6 90.13(8) . . ? O7 Mn2 N11 88.39(8) . . ? O1 Mn2 N11 89.24(8) . . ? O6 Mn2 N11 165.27(9) . . ? O7 Mn2 O8 99.02(8) . . ? O1 Mn2 O8 91.25(8) . . ? O6 Mn2 O8 94.62(12) . . ? N11 Mn2 O8 100.10(11) . . ? O7 Mn2 O6 86.01(7) . 7 ? O1 Mn2 O6 83.75(7) . 7 ? O6 Mn2 O6 83.46(11) . 7 ? N11 Mn2 O6 81.85(10) . 7 ? O8 Mn2 O6 174.62(7) . 7 ? Mn2 O7 Mn1 121.38(10) . . ? Mn2 O7 Mn3 120.78(10) . . ? Mn1 O7 Mn3 116.63(12) . . ? C3 C2 C1 120.9(3) . . ? O3 Mn3 O7 176.96(8) . . ? O3 Mn3 O2 91.78(12) . . ? O7 Mn3 O2 91.11(12) . . ? O3 Mn3 N12 87.50(13) . . ? O7 Mn3 N12 89.61(12) . . ? O2 Mn3 N12 179.19(9) . . ? O3 Mn3 O10 90.19(8) . . ? O7 Mn3 O10 90.70(8) . . ? O2 Mn3 O10 90.44(8) . . ? N12 Mn3 O10 89.20(9) . . ? O3 Mn3 O12 91.24(8) . . ? O7 Mn3 O12 87.61(8) . . ? O2 Mn3 O12 94.73(8) . . ? N12 Mn3 O12 85.66(8) . . ? O10 Mn3 O12 174.59(7) . . ? O3 Mn3 Mn1 145.30(8) . . ? O7 Mn3 Mn1 31.67(7) . . ? O2 Mn3 Mn1 121.29(8) . . ? N12 Mn3 Mn1 59.49(8) . . ? O10 Mn3 Mn1 99.05(7) . . ? O12 Mn3 Mn1 76.89(6) . . ? C17 O5 Mn1 122.57(19) . . ? C2 C3 C4 120.2(3) . . ? O8 P4 O9 115.65(11) . . ? O8 P4 C31 109.22(14) . . ? O9 P4 C31 109.41(13) . . ? O8 P4 C25 109.19(12) . . ? O9 P4 C25 108.06(12) . . ? C31 P4 C25 104.75(15) . . ? C9 O3 Mn3 121.13(17) . . ? C5 C4 C3 119.4(3) . . ? C1 O1 Mn2 119.54(16) . . ? C1 O1 Mn1 108.43(16) . 7 ? Mn2 O1 Mn1 118.20(8) . 7 ? C4 C5 C6 122.0(3) . . ? C37 O10 Mn3 120.11(19) . . ? C5 C6 C1 118.0(2) . . ? C5 C6 C7 118.9(3) . . ? C1 C6 C7 123.1(2) . . ? N11 O2 Mn3 117.15(17) . . ? N11 C7 C6 120.1(3) . . ? N11 C7 C8 119.0(2) . . ? C6 C7 C8 120.9(2) . . ? N15 O6 Mn2 113.94(15) . . ? N15 O6 Mn2 109.78(14) . 7 ? Mn2 O6 Mn2 96.54(11) . 7 ? C39 O12 Mn3 128.20(17) . . ? O3 C9 C10 118.1(3) . . ? O3 C9 C14 123.0(3) . . ? C10 C9 C14 118.9(3) . . ? C38 O11 Mn1 123.48(17) . . ? C11 C10 C9 121.4(3) . . ? C7 N11 O2 115.5(2) . . ? C7 N11 Mn2 126.35(19) . . ? O2 N11 Mn2 117.19(16) . . ? C10 C11 C12 120.0(3) . . ? C15 N12 O4 117.1(2) . . ? C15 N12 Mn3 127.8(2) . . ? O4 N12 Mn3 115.06(16) . . ? C13 C12 C11 119.2(3) . . ? C12 C13 C14 122.4(3) . . ? P4 O8 Mn2 146.82(12) . . ? C13 C14 C9 117.9(3) . . ? C13 C14 C15 120.3(3) . . ? C9 C14 C15 121.7(3) . . ? C23 N15 O6 117.1(2) . . ? C23 N15 Mn1 127.79(18) . . ? O6 N15 Mn1 115.07(18) . . ? N12 C15 C14 118.5(2) . . ? N12 C15 C16 121.9(3) . . ? C14 C15 C16 119.6(2) . . ? O5 C17 C18 117.5(3) . . ? O5 C17 C22 123.1(2) . . ? C18 C17 C22 119.4(3) . . ? C19 C18 C17 120.8(3) . . ? C18 C19 C20 120.6(3) . . ? C21 C20 C19 119.6(3) . . ? C20 C21 C22 121.6(3) . . ? C21 C22 C17 118.0(2) . . ? C21 C22 C23 118.6(3) . . ? C17 C22 C23 123.4(3) . . ? N15 C23 C22 118.1(2) . . ? N15 C23 C24 120.9(2) . . ? C22 C23 C24 121.0(3) . . ? C30 C25 C26 118.5(3) . . ? C30 C25 P4 119.0(2) . . ? C26 C25 P4 122.5(2) . . ? C25 C26 C27 120.9(3) . . ? C28 C27 C26 119.8(3) . . ? C27 C28 C29 120.2(3) . . ? C28 C29 C30 120.1(3) . . ? C25 C30 C29 120.5(3) . . ? C36 C31 C32 119.4(3) . . ? C36 C31 P4 120.9(2) . . ? C32 C31 P4 119.6(2) . . ? C33 C32 C31 120.3(3) . . ? C32 C33 C34 120.0(3) . . ? C35 C34 C33 120.4(3) . . ? C34 C35 C36 120.0(3) . . ? C35 C36 C31 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.507 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.090 # Attachment 'Complex 3.CIF' data_RI2229 _database_code_depnum_ccdc_archive 'CCDC 760679' #TrackingRef 'Complex 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common RI2229 _chemical_melting_point ? _chemical_formula_moiety 'C84 H98 Mn6 N6 O24 P2' _chemical_formula_sum 'C84 H98 Mn6 N6 O24 P2' _chemical_formula_weight 1967.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.745(6) _cell_length_b 12.618(2) _cell_length_c 27.229(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.539(8) _cell_angle_gamma 90.00 _cell_volume 8528(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6836 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex 2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99808 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.50 _reflns_number_total 10644 _reflns_number_gt 8121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. One ethyl group of a ligand on Mn3 is disordered over two positions. This has been successfully model- ed but causes a short contact as found in the chceckcif file. ; _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^)+(0.0323P)^2^+16.8642P] 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 10644 _refine_ls_number_parameters 575 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.111476(13) 0.89035(3) 0.070933(13) 0.01625(8) Uani 1 1 d . . . P1 P 0.12784(2) 1.23240(5) 0.14555(2) 0.01698(12) Uani 1 1 d . . . O1 O 0.15409(6) 0.82622(13) 0.04248(6) 0.0205(3) Uani 1 1 d . . . N1 N 0.09874(7) 1.00895(15) 0.01870(7) 0.0171(4) Uani 1 1 d . . . C1 C 0.19124(9) 0.8828(2) 0.03596(9) 0.0212(5) Uani 1 1 d . . . O2 O 0.04776(6) 1.05514(12) -0.00125(6) 0.0168(3) Uani 1 1 d . . . N2 N 0.11099(7) 0.78363(15) 0.16135(7) 0.0180(4) Uani 1 1 d . . . C2 C 0.18321(9) 0.9890(2) 0.01696(9) 0.0218(5) Uani 1 1 d . . . Mn3 Mn 0.024548(13) 1.07782(3) 0.056052(12) 0.01474(8) Uani 1 1 d . . . O3 O 0.04403(6) 0.83080(13) 0.20693(6) 0.0227(4) Uani 1 1 d . . . N3 N -0.01070(7) 1.07669(15) 0.10688(7) 0.0170(4) Uani 1 1 d . A . C3 C 0.22588(10) 1.0421(2) 0.01273(9) 0.0269(5) Uani 1 1 d . . . H3 H 0.2210 1.1134 0.0003 0.032 Uiso 1 1 calc R . . O4 O 0.11974(6) 0.76930(13) 0.11585(6) 0.0220(3) Uani 1 1 d . . . C4 C 0.27452(10) 0.9926(2) 0.02623(10) 0.0317(6) Uani 1 1 d . . . H4 H 0.3032 1.0305 0.0242 0.038 Uiso 1 1 calc R . . O5 O -0.02896(6) 1.17539(12) 0.00938(6) 0.0178(3) Uani 1 1 d . . . C5 C 0.28141(10) 0.8873(2) 0.04273(10) 0.0322(6) Uani 1 1 d . . . H5 H 0.3144 0.8524 0.0507 0.039 Uiso 1 1 calc R . . O6 O -0.00428(6) 0.98729(13) 0.13747(6) 0.0209(3) Uani 1 1 d . . . C6 C 0.24058(10) 0.8328(2) 0.04769(9) 0.0270(5) Uani 1 1 d . . . H6 H 0.2459 0.7609 0.0591 0.032 Uiso 1 1 calc R . . O7 O 0.16256(6) 1.14076(12) 0.17810(6) 0.0197(3) Uani 1 1 d . . . C7 C 0.13108(9) 1.04287(18) -0.00053(8) 0.0185(5) Uani 1 1 d . . . O8 O 0.07747(6) 1.20563(12) 0.09418(6) 0.0194(3) Uani 1 1 d . . . C8 C 0.11648(10) 1.13504(18) -0.03925(9) 0.0216(5) Uani 1 1 d . . . H8A H 0.0779 1.1307 -0.0657 0.026 Uiso 1 1 calc R . . H8B H 0.1379 1.1322 -0.0602 0.026 Uiso 1 1 calc R . . O9 O 0.18257(6) 0.97305(13) 0.13330(6) 0.0220(4) Uani 1 1 d D . . C9 C 0.12737(11) 1.2403(2) -0.00774(10) 0.0282(6) Uani 1 1 d . . . H9A H 0.1047 1.2448 0.0113 0.042 Uiso 1 1 calc R . . H9B H 0.1190 1.2994 -0.0336 0.042 Uiso 1 1 calc R . . H9C H 0.1654 1.2438 0.0191 0.042 Uiso 1 1 calc R . . O10 O 0.11709(7) 1.00041(15) 0.21472(6) 0.0333(4) Uani 1 1 d D . . C10 C 0.07865(9) 0.77352(19) 0.24917(9) 0.0214(5) Uani 1 1 d . . . O11 O 0.00232(7) 0.77602(14) 0.08830(7) 0.0285(4) Uani 1 1 d D . . C11 C 0.12021(9) 0.71258(18) 0.24667(9) 0.0201(5) Uani 1 1 d . . . C12 C 0.15334(10) 0.65178(19) 0.29291(9) 0.0251(5) Uani 1 1 d . . . H12 H 0.1814 0.6103 0.2917 0.030 Uiso 1 1 calc R . . C13 C 0.14623(11) 0.6508(2) 0.33988(10) 0.0294(6) Uani 1 1 d . . . H13 H 0.1694 0.6102 0.3708 0.035 Uiso 1 1 calc R . . C14 C 0.10479(11) 0.7099(2) 0.34141(10) 0.0277(6) Uani 1 1 d . . . H14 H 0.0992 0.7085 0.3734 0.033 Uiso 1 1 calc R . . C15 C 0.07154(10) 0.7706(2) 0.29710(9) 0.0250(5) Uani 1 1 d . . . H15 H 0.0435 0.8109 0.2990 0.030 Uiso 1 1 calc R . . C16 C 0.12918(9) 0.70788(18) 0.19754(9) 0.0188(5) Uani 1 1 d . . . C17 C 0.15726(10) 0.61420(19) 0.18802(10) 0.0229(5) Uani 1 1 d . . . H17A H 0.1383 0.5942 0.1488 0.028 Uiso 1 1 calc R . . H17B H 0.1545 0.5536 0.2097 0.028 Uiso 1 1 calc R . . C18 C 0.21662(10) 0.6331(2) 0.20320(10) 0.0300(6) Uani 1 1 d . . . H18A H 0.2197 0.6883 0.1794 0.045 Uiso 1 1 calc R . . H18B H 0.2328 0.5673 0.1983 0.045 Uiso 1 1 calc R . . H18C H 0.2355 0.6559 0.2416 0.045 Uiso 1 1 calc R . . C19 C -0.04246(9) 1.25798(18) 0.03227(9) 0.0191(5) Uani 1 1 d . . . C20 C -0.05189(9) 1.24710(19) 0.07916(9) 0.0199(5) Uani 1 1 d . A . C21 C -0.06962(9) 1.3366(2) 0.09687(10) 0.0255(5) Uani 1 1 d . . . H21 H -0.0770 1.3301 0.1276 0.031 Uiso 1 1 calc R . . C22 C -0.07671(10) 1.4332(2) 0.07154(10) 0.0295(6) Uani 1 1 d . . . H22 H -0.0889 1.4924 0.0845 0.035 Uiso 1 1 calc R . . C23 C -0.06587(11) 1.4435(2) 0.02658(10) 0.0315(6) Uani 1 1 d . . . H23 H -0.0698 1.5104 0.0092 0.038 Uiso 1 1 calc R . . C24 C -0.04946(10) 1.35691(19) 0.00717(10) 0.0253(5) Uani 1 1 d . . . H24 H -0.0428 1.3647 -0.0239 0.030 Uiso 1 1 calc R . . C25 C -0.04298(9) 1.14788(19) 0.11013(9) 0.0196(5) Uani 1 1 d D . . C26 C -0.0698(4) 1.1415(10) 0.1475(4) 0.023(2) Uani 0.50 1 d PDU A 1 H26A H -0.0619 1.2068 0.1699 0.028 Uiso 0.50 1 calc PR A 1 H26B H -0.0548 1.0806 0.1728 0.028 Uiso 0.50 1 calc PR A 1 C27 C -0.13078(19) 1.1282(4) 0.11462(19) 0.0267(11) Uani 0.50 1 d PDU A 1 H27A H -0.1451 1.1841 0.0868 0.040 Uiso 0.50 1 calc PR A 1 H27B H -0.1476 1.1332 0.1394 0.040 Uiso 0.50 1 calc PR A 1 H27C H -0.1387 1.0587 0.0966 0.040 Uiso 0.50 1 calc PR A 1 C28 C 0.16964(9) 1.31936(19) 0.12808(9) 0.0198(5) Uani 1 1 d . . . C29 C 0.14939(10) 1.41293(19) 0.09912(9) 0.0234(5) Uani 1 1 d . . . H29 H 0.1128 1.4316 0.0881 0.028 Uiso 1 1 calc R . . C30 C 0.18181(10) 1.4792(2) 0.08612(10) 0.0262(5) Uani 1 1 d . . . H30 H 0.1675 1.5430 0.0664 0.031 Uiso 1 1 calc R . . C31 C 0.23493(10) 1.4522(2) 0.10187(10) 0.0300(6) Uani 1 1 d . . . H31 H 0.2574 1.4979 0.0934 0.036 Uiso 1 1 calc R . . C32 C 0.25533(11) 1.3595(2) 0.12978(12) 0.0377(7) Uani 1 1 d . . . H32 H 0.2917 1.3405 0.1399 0.045 Uiso 1 1 calc R . . C33 C 0.22308(10) 1.2934(2) 0.14333(11) 0.0323(6) Uani 1 1 d . . . H33 H 0.2377 1.2299 0.1632 0.039 Uiso 1 1 calc R . . C34 C 0.10936(9) 1.30842(18) 0.19071(9) 0.0183(5) Uani 1 1 d . . . C35 C 0.14107(10) 1.30442(19) 0.24761(9) 0.0224(5) Uani 1 1 d . . . H35 H 0.1725 1.2615 0.2625 0.027 Uiso 1 1 calc R . . C36 C 0.12700(10) 1.3626(2) 0.28236(10) 0.0261(5) Uani 1 1 d . . . H36 H 0.1488 1.3593 0.3209 0.031 Uiso 1 1 calc R . . C37 C 0.08146(10) 1.4252(2) 0.26119(10) 0.0281(6) Uani 1 1 d . . . H37 H 0.0718 1.4647 0.2852 0.034 Uiso 1 1 calc R . . C38 C 0.04975(10) 1.4305(2) 0.20492(10) 0.0279(6) Uani 1 1 d . . . H38 H 0.0185 1.4740 0.1904 0.034 Uiso 1 1 calc R . . C39 C 0.06351(9) 1.37227(19) 0.16985(10) 0.0232(5) Uani 1 1 d . . . H39 H 0.0415 1.3759 0.1313 0.028 Uiso 1 1 calc R . . C40 C 0.23027(10) 0.9247(2) 0.17214(12) 0.0390(7) Uani 1 1 d . . . H40A H 0.2256 0.9036 0.2044 0.058 Uiso 1 1 calc R . . H40B H 0.2602 0.9750 0.1832 0.058 Uiso 1 1 calc R . . H40C H 0.2381 0.8619 0.1558 0.058 Uiso 1 1 calc R . . C41 C 0.13003(19) 1.0183(3) 0.26775(12) 0.0786(15) Uani 1 1 d . . . H41A H 0.1258 1.0939 0.2732 0.118 Uiso 1 1 calc R . . H41B H 0.1675 0.9973 0.2905 0.118 Uiso 1 1 calc R . . H41C H 0.1063 0.9768 0.2783 0.118 Uiso 1 1 calc R . . C42 C 0.00336(12) 0.6675(2) 0.10277(12) 0.0396(7) Uani 1 1 d . . . H42A H 0.0365 0.6344 0.1055 0.059 Uiso 1 1 calc R . . H42B H -0.0280 0.6311 0.0746 0.059 Uiso 1 1 calc R . . H42C H 0.0023 0.6621 0.1382 0.059 Uiso 1 1 calc R . . C27A C -0.0308(2) 1.1454(5) 0.2078(2) 0.0415(15) Uani 0.50 1 d PDU A 2 H27D H 0.0003 1.0975 0.2210 0.062 Uiso 0.50 1 calc PR A 2 H27E H -0.0501 1.1360 0.2301 0.062 Uiso 0.50 1 calc PR A 2 H27F H -0.0183 1.2189 0.2109 0.062 Uiso 0.50 1 calc PR A 2 Mn2 Mn 0.056638(13) 0.89792(3) 0.153087(13) 0.01703(8) Uani 1 1 d . . . O12 O 0.06674(6) 0.96233(12) 0.09573(6) 0.0159(3) Uani 1 1 d . . . C26A C -0.0687(4) 1.1203(8) 0.1475(3) 0.021(2) Uani 0.50 1 d PDU A 2 H26C H -0.0779 1.0439 0.1439 0.025 Uiso 0.50 1 calc PR A 2 H26D H -0.1025 1.1609 0.1360 0.025 Uiso 0.50 1 calc PR A 2 H9S H 0.1746 1.0328 0.1485 0.025 Uiso 1 1 d RD . . H10S H 0.1333 1.0513 0.2014 0.025 Uiso 1 1 d RD . . H11S H 0.0002 0.7786 0.0514 0.025 Uiso 1 1 d RD . . 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 0.01235(17) 0.02250(18) 0.01353(15) 0.00102(13) 0.00546(13) 0.00177(13) P1 0.0137(3) 0.0215(3) 0.0143(3) -0.0023(2) 0.0050(2) -0.0013(2) O1 0.0161(8) 0.0259(9) 0.0196(8) -0.0014(7) 0.0080(7) 0.0017(7) N1 0.0105(9) 0.0257(10) 0.0146(9) -0.0009(7) 0.0051(7) 0.0015(8) C1 0.0141(11) 0.0352(13) 0.0140(10) -0.0056(9) 0.0060(9) 0.0002(10) O2 0.0116(7) 0.0235(8) 0.0138(7) 0.0000(6) 0.0043(6) 0.0020(6) N2 0.0168(10) 0.0228(10) 0.0146(9) 0.0004(7) 0.0073(8) 0.0002(8) C2 0.0160(11) 0.0360(14) 0.0144(10) -0.0020(9) 0.0077(9) -0.0009(10) Mn3 0.01153(16) 0.02043(17) 0.01095(15) -0.00006(12) 0.00385(13) 0.00101(13) O3 0.0205(8) 0.0310(9) 0.0183(8) 0.0060(7) 0.0100(7) 0.0018(7) N3 0.0138(9) 0.0237(10) 0.0119(8) 0.0007(7) 0.0043(7) -0.0001(8) C3 0.0208(12) 0.0439(15) 0.0175(11) -0.0017(10) 0.0097(10) -0.0041(11) O4 0.0255(9) 0.0260(9) 0.0168(8) 0.0019(7) 0.0115(7) 0.0049(7) C4 0.0173(12) 0.0577(18) 0.0219(12) -0.0039(12) 0.0104(10) -0.0041(12) O5 0.0151(8) 0.0208(8) 0.0140(7) -0.0007(6) 0.0035(6) 0.0023(6) C5 0.0177(12) 0.0550(18) 0.0255(13) -0.0038(12) 0.0110(11) 0.0047(12) O6 0.0221(9) 0.0247(8) 0.0192(8) 0.0048(6) 0.0123(7) 0.0035(7) C6 0.0211(13) 0.0399(15) 0.0208(12) -0.0034(11) 0.0100(10) 0.0050(11) O7 0.0170(8) 0.0224(8) 0.0166(7) -0.0025(6) 0.0048(6) 0.0002(7) C7 0.0162(11) 0.0257(12) 0.0128(10) -0.0034(9) 0.0057(9) -0.0028(9) O8 0.0148(8) 0.0233(8) 0.0162(7) -0.0020(6) 0.0034(6) -0.0012(6) C8 0.0219(12) 0.0280(13) 0.0158(10) -0.0001(9) 0.0093(9) -0.0029(10) O9 0.0142(8) 0.0282(9) 0.0187(8) -0.0039(7) 0.0029(7) 0.0025(7) C9 0.0348(15) 0.0299(14) 0.0211(12) -0.0024(10) 0.0136(11) -0.0060(11) O10 0.0378(11) 0.0456(11) 0.0140(8) -0.0041(8) 0.0094(8) -0.0197(9) C10 0.0219(12) 0.0234(12) 0.0163(11) 0.0012(9) 0.0061(9) -0.0049(10) O11 0.0274(10) 0.0295(9) 0.0253(9) 0.0026(7) 0.0087(8) -0.0011(8) C11 0.0212(12) 0.0192(11) 0.0158(10) -0.0004(9) 0.0047(9) -0.0043(9) C12 0.0263(13) 0.0229(12) 0.0209(11) 0.0024(10) 0.0059(10) -0.0010(10) C13 0.0366(15) 0.0253(13) 0.0196(12) 0.0046(10) 0.0064(11) -0.0034(11) C14 0.0377(15) 0.0278(13) 0.0177(11) 0.0008(10) 0.0124(11) -0.0060(11) C15 0.0266(13) 0.0287(13) 0.0210(11) -0.0005(10) 0.0119(10) -0.0025(11) C16 0.0140(11) 0.0191(11) 0.0195(11) 0.0000(9) 0.0041(9) -0.0026(9) C17 0.0254(13) 0.0209(12) 0.0211(11) 0.0009(9) 0.0091(10) 0.0007(10) C18 0.0232(13) 0.0347(14) 0.0273(13) 0.0018(11) 0.0070(11) 0.0052(11) C19 0.0108(10) 0.0238(12) 0.0176(10) -0.0038(9) 0.0016(9) 0.0023(9) C20 0.0096(10) 0.0298(13) 0.0159(10) -0.0012(9) 0.0018(9) 0.0023(9) C21 0.0166(12) 0.0351(14) 0.0233(12) -0.0043(10) 0.0076(10) 0.0049(10) C22 0.0232(13) 0.0296(14) 0.0325(14) -0.0061(11) 0.0096(11) 0.0070(11) C23 0.0327(15) 0.0257(13) 0.0300(13) 0.0018(11) 0.0087(12) 0.0072(11) C24 0.0262(13) 0.0269(13) 0.0204(11) 0.0018(10) 0.0083(10) 0.0054(10) C25 0.0117(11) 0.0301(13) 0.0136(10) -0.0018(9) 0.0025(9) 0.0013(9) C26 0.024(4) 0.025(4) 0.022(3) 0.006(2) 0.011(3) 0.010(3) C27 0.021(2) 0.041(3) 0.019(2) 0.000(2) 0.010(2) -0.001(2) C28 0.0170(11) 0.0265(12) 0.0148(10) -0.0037(9) 0.0060(9) -0.0021(9) C29 0.0192(12) 0.0280(13) 0.0222(11) -0.0024(10) 0.0084(10) -0.0004(10) C30 0.0282(14) 0.0273(13) 0.0246(12) -0.0001(10) 0.0132(11) -0.0027(11) C31 0.0272(14) 0.0373(15) 0.0279(13) -0.0022(11) 0.0144(11) -0.0090(12) C32 0.0196(13) 0.0495(18) 0.0455(16) 0.0116(14) 0.0159(12) 0.0017(12) C33 0.0201(13) 0.0405(16) 0.0353(14) 0.0105(12) 0.0114(11) 0.0030(12) C34 0.0157(11) 0.0208(11) 0.0190(11) -0.0028(9) 0.0082(9) -0.0052(9) C35 0.0202(12) 0.0248(12) 0.0215(11) -0.0024(9) 0.0087(10) -0.0010(10) C36 0.0252(13) 0.0326(14) 0.0201(11) -0.0070(10) 0.0098(10) -0.0080(11) C37 0.0268(13) 0.0331(14) 0.0302(13) -0.0126(11) 0.0179(11) -0.0084(11) C38 0.0202(13) 0.0300(13) 0.0343(14) -0.0063(11) 0.0127(11) 0.0008(11) C39 0.0171(12) 0.0289(13) 0.0224(11) -0.0031(10) 0.0079(10) -0.0024(10) C40 0.0202(13) 0.0354(15) 0.0380(15) -0.0098(12) -0.0079(12) 0.0078(12) C41 0.137(4) 0.075(3) 0.0276(16) -0.0204(17) 0.040(2) -0.067(3) C42 0.0413(17) 0.0342(16) 0.0405(16) -0.0004(13) 0.0156(14) -0.0076(13) C27A 0.045(3) 0.057(4) 0.024(3) -0.001(3) 0.017(3) 0.021(3) Mn2 0.01421(17) 0.02365(18) 0.01283(15) 0.00245(13) 0.00568(13) 0.00096(14) O12 0.0130(7) 0.0225(8) 0.0123(7) 0.0012(6) 0.0056(6) 0.0014(6) C26A 0.019(3) 0.028(5) 0.021(3) 0.001(3) 0.013(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.8633(16) . ? Mn1 O12 1.8896(15) . ? Mn1 O4 1.9054(16) . ? Mn1 N1 1.9845(19) . ? Mn1 O9 2.2068(16) . ? Mn1 O5 2.4977(15) 5_575 ? Mn1 Mn2 3.2202(8) . ? P1 O8 1.5089(16) . ? P1 O7 1.5125(16) . ? P1 C34 1.805(2) . ? P1 C28 1.808(2) . ? O1 C1 1.329(3) . ? N1 C7 1.297(3) . ? N1 O2 1.396(2) . ? C1 C6 1.408(3) . ? C1 C2 1.417(3) . ? O2 Mn3 1.9570(16) . ? O2 Mn3 2.5280(15) 5_575 ? N2 C16 1.302(3) . ? N2 O4 1.377(2) . ? N2 Mn2 2.0251(19) . ? C2 C3 1.409(3) . ? C2 C7 1.471(3) . ? Mn3 O12 1.8790(15) . ? Mn3 O5 1.9101(15) . ? Mn3 N3 2.0201(19) . ? Mn3 O8 2.1148(16) . ? Mn3 O2 2.5280(15) 5_575 ? O3 C10 1.334(3) . ? O3 Mn2 1.8568(16) . ? N3 C25 1.299(3) . ? N3 O6 1.366(2) . ? C3 C4 1.379(4) . ? C4 C5 1.388(4) . ? O5 C19 1.350(3) . ? O5 Mn1 2.4977(15) 5_575 ? C5 C6 1.382(4) . ? O6 Mn2 1.9149(16) . ? C7 C8 1.499(3) . ? C8 C9 1.536(3) . ? O9 C40 1.411(3) . ? O10 C41 1.342(3) . ? O10 Mn2 2.1877(17) . ? C10 C15 1.405(3) . ? C10 C11 1.413(3) . ? O11 C42 1.422(3) . ? O11 Mn2 2.3181(18) . ? C11 C12 1.409(3) . ? C11 C16 1.467(3) . ? C12 C13 1.378(3) . ? C13 C14 1.386(4) . ? C14 C15 1.378(3) . ? C16 C17 1.501(3) . ? C17 C18 1.527(3) . ? C19 C24 1.394(3) . ? C19 C20 1.420(3) . ? C20 C21 1.401(3) . ? C20 C25 1.467(3) . ? C21 C22 1.370(4) . ? C22 C23 1.391(4) . ? C23 C24 1.377(3) . ? C25 C26 1.507(10) . ? C25 C26A 1.523(9) . ? C26 C27 1.530(11) . ? C28 C33 1.388(3) . ? C28 C29 1.391(3) . ? C29 C30 1.385(3) . ? C30 C31 1.381(4) . ? C31 C32 1.372(4) . ? C32 C33 1.389(4) . ? C34 C39 1.394(3) . ? C34 C35 1.400(3) . ? C35 C36 1.384(3) . ? C36 C37 1.379(4) . ? C37 C38 1.386(4) . ? C38 C39 1.387(3) . ? C27A C26A 1.536(10) . ? Mn2 O12 1.8892(15) . ? 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 O12 175.99(7) . . ? O1 Mn1 O4 90.12(7) . . ? O12 Mn1 O4 93.77(7) . . ? O1 Mn1 N1 88.42(7) . . ? O12 Mn1 N1 87.63(7) . . ? O4 Mn1 N1 175.09(7) . . ? O1 Mn1 O9 90.59(7) . . ? O12 Mn1 O9 90.10(6) . . ? O4 Mn1 O9 94.32(7) . . ? N1 Mn1 O9 90.38(7) . . ? O1 Mn1 O5 89.74(6) . 5_575 ? O12 Mn1 O5 88.91(6) . 5_575 ? O4 Mn1 O5 95.52(6) . 5_575 ? N1 Mn1 O5 79.80(6) . 5_575 ? O9 Mn1 O5 170.16(6) . 5_575 ? O1 Mn1 Mn2 152.41(5) . . ? O12 Mn1 Mn2 31.55(5) . . ? O4 Mn1 Mn2 62.39(5) . . ? N1 Mn1 Mn2 119.17(6) . . ? O9 Mn1 Mn2 89.35(5) . . ? O5 Mn1 Mn2 94.89(4) 5_575 . ? O8 P1 O7 117.11(9) . . ? O8 P1 C34 108.86(10) . . ? O7 P1 C34 107.91(10) . . ? O8 P1 C28 109.23(10) . . ? O7 P1 C28 107.61(10) . . ? C34 P1 C28 105.52(10) . . ? C1 O1 Mn1 119.73(14) . . ? C7 N1 O2 117.94(18) . . ? C7 N1 Mn1 127.18(15) . . ? O2 N1 Mn1 114.76(13) . . ? O1 C1 C6 117.5(2) . . ? O1 C1 C2 123.5(2) . . ? C6 C1 C2 119.0(2) . . ? N1 O2 Mn3 112.82(11) . . ? N1 O2 Mn3 110.58(11) . 5_575 ? Mn3 O2 Mn3 96.34(6) . 5_575 ? C16 N2 O4 114.84(18) . . ? C16 N2 Mn2 128.65(16) . . ? O4 N2 Mn2 114.55(13) . . ? C3 C2 C1 118.6(2) . . ? C3 C2 C7 119.6(2) . . ? C1 C2 C7 121.8(2) . . ? O12 Mn3 O5 169.02(7) . . ? O12 Mn3 O2 90.15(6) . . ? O5 Mn3 O2 89.92(7) . . ? O12 Mn3 N3 88.19(7) . . ? O5 Mn3 N3 89.43(7) . . ? O2 Mn3 N3 167.88(7) . . ? O12 Mn3 O8 101.05(6) . . ? O5 Mn3 O8 89.87(6) . . ? O2 Mn3 O8 95.70(6) . . ? N3 Mn3 O8 96.40(7) . . ? O12 Mn3 O2 87.19(6) . 5_575 ? O5 Mn3 O2 81.90(6) . 5_575 ? O2 Mn3 O2 83.66(6) . 5_575 ? N3 Mn3 O2 84.27(6) . 5_575 ? O8 Mn3 O2 171.75(5) . 5_575 ? C10 O3 Mn2 127.63(15) . . ? C25 N3 O6 115.81(18) . . ? C25 N3 Mn3 126.96(16) . . ? O6 N3 Mn3 116.91(13) . . ? C4 C3 C2 121.4(3) . . ? N2 O4 Mn1 116.96(13) . . ? C3 C4 C5 119.7(2) . . ? C19 O5 Mn3 118.93(13) . . ? C19 O5 Mn1 109.00(12) . 5_575 ? Mn3 O5 Mn1 120.29(7) . 5_575 ? C6 C5 C4 120.5(2) . . ? N3 O6 Mn2 118.90(12) . . ? C5 C6 C1 120.7(3) . . ? N1 C7 C2 118.3(2) . . ? N1 C7 C8 121.4(2) . . ? C2 C7 C8 120.3(2) . . ? P1 O8 Mn3 141.09(10) . . ? C7 C8 C9 110.74(18) . . ? C40 O9 Mn1 126.07(15) . . ? C41 O10 Mn2 132.05(19) . . ? O3 C10 C15 118.0(2) . . ? O3 C10 C11 122.8(2) . . ? C15 C10 C11 119.1(2) . . ? C42 O11 Mn2 120.16(15) . . ? C12 C11 C10 118.3(2) . . ? C12 C11 C16 119.0(2) . . ? C10 C11 C16 122.7(2) . . ? C13 C12 C11 121.8(2) . . ? C12 C13 C14 119.2(2) . . ? C15 C14 C13 120.8(2) . . ? C14 C15 C10 120.7(2) . . ? N2 C16 C11 119.6(2) . . ? N2 C16 C17 120.2(2) . . ? C11 C16 C17 120.1(2) . . ? C16 C17 C18 114.2(2) . . ? O5 C19 C24 118.1(2) . . ? O5 C19 C20 122.8(2) . . ? C24 C19 C20 119.1(2) . . ? C21 C20 C19 117.8(2) . . ? C21 C20 C25 119.0(2) . . ? C19 C20 C25 123.2(2) . . ? C22 C21 C20 122.5(2) . . ? C21 C22 C23 119.1(2) . . ? C24 C23 C22 120.2(2) . . ? C23 C24 C19 121.3(2) . . ? N3 C25 C20 119.7(2) . . ? N3 C25 C26 124.9(5) . . ? C20 C25 C26 115.3(5) . . ? N3 C25 C26A 115.5(4) . . ? C20 C25 C26A 124.8(4) . . ? C26 C25 C26A 10.2(8) . . ? C25 C26 C27 111.2(7) . . ? C33 C28 C29 118.5(2) . . ? C33 C28 P1 120.19(19) . . ? C29 C28 P1 121.34(18) . . ? C30 C29 C28 120.9(2) . . ? C31 C30 C29 119.8(2) . . ? C32 C31 C30 120.1(2) . . ? C31 C32 C33 120.3(3) . . ? C28 C33 C32 120.5(2) . . ? C39 C34 C35 118.7(2) . . ? C39 C34 P1 120.97(17) . . ? C35 C34 P1 120.37(18) . . ? C36 C35 C34 120.5(2) . . ? C37 C36 C35 120.2(2) . . ? C36 C37 C38 120.0(2) . . ? C37 C38 C39 120.1(2) . . ? C38 C39 C34 120.5(2) . . ? O3 Mn2 O12 177.23(7) . . ? O3 Mn2 O6 89.13(7) . . ? O12 Mn2 O6 90.31(7) . . ? O3 Mn2 N2 88.92(7) . . ? O12 Mn2 N2 91.15(7) . . ? O6 Mn2 N2 169.60(7) . . ? O3 Mn2 O10 90.82(7) . . ? O12 Mn2 O10 91.94(7) . . ? O6 Mn2 O10 96.91(7) . . ? N2 Mn2 O10 93.33(8) . . ? O3 Mn2 O11 90.60(7) . . ? O12 Mn2 O11 86.70(7) . . ? O6 Mn2 O11 90.72(7) . . ? N2 Mn2 O11 79.09(7) . . ? O10 Mn2 O11 172.26(7) . . ? O3 Mn2 Mn1 148.13(5) . . ? O12 Mn2 Mn1 31.56(5) . . ? O6 Mn2 Mn1 120.49(5) . . ? N2 Mn2 Mn1 59.77(5) . . ? O10 Mn2 Mn1 96.44(5) . . ? O11 Mn2 Mn1 78.46(5) . . ? Mn3 O12 Mn2 121.64(8) . . ? Mn3 O12 Mn1 120.47(8) . . ? Mn2 O12 Mn1 116.90(8) . . ? C25 C26A C27A 111.4(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.618 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.076 # Attachment 'Complex 4.CIF' data_RI2363 _database_code_depnum_ccdc_archive 'CCDC 760680' #TrackingRef 'Complex 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common RI2363 _chemical_melting_point ? _chemical_formula_moiety 'C106 H90 Mn6 N6 O22 P2' _chemical_formula_sum 'C106 H90 Mn6 N6 O22 P2' _chemical_formula_weight 2191.42 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.79(3) _cell_length_b 14.70(3) _cell_length_c 14.74(3) _cell_angle_alpha 66.78(5) _cell_angle_beta 71.84(6) _cell_angle_gamma 75.77(5) _cell_volume 2581(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7363 _exptl_absorpt_correction_T_max 0.8039 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex 2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23495 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 22.48 _reflns_number_total 6519 _reflns_number_gt 5104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. Due to the presence of a badly disordered diethyl ether molecule, the routine squeeze was applied. This was due to the inability to adequately model this disorder. The application of this technique dramatically improved the agreement indices. Numerous restraints were applied due to disorder in one of the Mn ligands. A phenyl ring is disordered over two positions but was modelled success- fully. The crystals were weakly diffracting. ; _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^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6519 _refine_ls_number_parameters 696 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.020 _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 0.16428(4) 0.61852(4) 0.47214(4) 0.01741(19) Uani 1 1 d . . . P1 P -0.32651(8) 0.70850(8) 0.45153(8) 0.0207(3) Uani 1 1 d . . . O1 O -0.21244(19) 0.68893(19) 0.44520(19) 0.0182(6) Uani 1 1 d . . . C1 C -0.3435(3) 0.7581(3) 0.3224(3) 0.0235(10) Uani 1 1 d . . . C49 C 0.2717(11) 1.0492(12) 0.1737(10) 0.030(3) Uani 0.50 1 d PDU A 2 H49 H 0.2647 1.1151 0.1739 0.036 Uiso 0.50 1 calc PR A 2 Mn2 Mn -0.10080(4) 0.58575(4) 0.51853(4) 0.01494(19) Uani 1 1 d . . . O2 O -0.3851(2) 0.6199(2) 0.5108(2) 0.0258(7) Uani 1 1 d . . . C2 C -0.3561(3) 0.6926(4) 0.2806(3) 0.0304(11) Uani 1 1 d . . . H2 H -0.3600 0.6242 0.3212 0.036 Uiso 1 1 calc R . . Mn3 Mn 0.23680(5) 0.55337(5) 0.27067(4) 0.0199(2) Uani 1 1 d . . . O3 O -0.00567(19) 0.67889(19) 0.46184(19) 0.0164(6) Uani 1 1 d . . . C3 C -0.3630(4) 0.7268(4) 0.1803(4) 0.0368(12) Uani 1 1 d . . . H3 H -0.3708 0.6818 0.1520 0.044 Uiso 1 1 calc R . . O4 O -0.1803(2) 0.5496(2) 0.73312(19) 0.0226(7) Uani 1 1 d . . . C4 C -0.3584(4) 0.8258(4) 0.1219(4) 0.0431(13) Uani 1 1 d . . . H4 H -0.3648 0.8494 0.0537 0.052 Uiso 1 1 calc R . . O5 O 0.1541(2) 0.7004(2) 0.5470(2) 0.0230(7) Uani 1 1 d . . . C5 C -0.3446(4) 0.8912(4) 0.1615(4) 0.0441(14) Uani 1 1 d . . . H5 H -0.3398 0.9593 0.1204 0.053 Uiso 1 1 calc R . . O6 O 0.03483(19) 0.47063(19) 0.58971(19) 0.0171(6) Uani 1 1 d . . . C6 C -0.3376(4) 0.8568(3) 0.2625(3) 0.0341(12) Uani 1 1 d . . . H6 H -0.3287 0.9019 0.2900 0.041 Uiso 1 1 calc R . . O7 O 0.2867(2) 0.5879(2) 0.1307(2) 0.0350(8) Uani 1 1 d . . . C7 C -0.3861(3) 0.8022(3) 0.5109(3) 0.0254(10) Uani 1 1 d . . . O8 O 0.2138(2) 0.7166(2) 0.3443(2) 0.0254(7) Uani 1 1 d . . . C8 C -0.4868(4) 0.7990(3) 0.5700(4) 0.0411(13) Uani 1 1 d . . . H8 H -0.5253 0.7512 0.5746 0.049 Uiso 1 1 calc R . . O9 O 0.3195(2) 0.5578(2) 0.5004(2) 0.0258(7) Uani 1 1 d D . . N9 N -0.1478(2) 0.6244(2) 0.6444(2) 0.0184(8) Uani 1 1 d . . . C9 C -0.5311(4) 0.8655(4) 0.6222(4) 0.0516(15) Uani 1 1 d . . . H9 H -0.6001 0.8636 0.6621 0.062 Uiso 1 1 calc R . . O10 O 0.3836(2) 0.4735(2) 0.2982(2) 0.0285(7) Uani 1 1 d D . . C10 C -0.4751(4) 0.9338(4) 0.6159(4) 0.0498(15) Uani 1 1 d . . . H10 H -0.5050 0.9789 0.6522 0.060 Uiso 1 1 calc R . . O11 O 0.17569(19) 0.52429(19) 0.40945(18) 0.0158(6) Uani 1 1 d . . . C11 C -0.3758(4) 0.9374(4) 0.5572(4) 0.0406(13) Uani 1 1 d . . . H11 H -0.3376 0.9850 0.5534 0.049 Uiso 1 1 calc R . . C12 C -0.3306(3) 0.8727(3) 0.5037(3) 0.0266(11) Uani 1 1 d . . . H12 H -0.2623 0.8764 0.4625 0.032 Uiso 1 1 calc R . . C13 C -0.0374(3) 0.7720(3) 0.4668(3) 0.0179(10) Uani 1 1 d . . . C14 C -0.0073(3) 0.8543(3) 0.3802(3) 0.0221(10) Uani 1 1 d . . . H14 H 0.0314 0.8445 0.3182 0.026 Uiso 1 1 calc R . . C15 C -0.0336(3) 0.9488(3) 0.3847(3) 0.0272(11) Uani 1 1 d . . . H15 H -0.0128 1.0040 0.3254 0.033 Uiso 1 1 calc R . . C16 C -0.0899(3) 0.9657(3) 0.4739(3) 0.0286(11) Uani 1 1 d . . . H16 H -0.1080 1.0318 0.4755 0.034 Uiso 1 1 calc R . . N17 N 0.1009(2) 0.5194(2) 0.6025(2) 0.0165(8) Uani 1 1 d . . . C17 C -0.1198(3) 0.8851(3) 0.5609(3) 0.0201(10) Uani 1 1 d . . . H17 H -0.1575 0.8965 0.6224 0.024 Uiso 1 1 calc R . . C18 C -0.0952(3) 0.7869(3) 0.5595(3) 0.0174(9) Uani 1 1 d . . . C19 C -0.1302(3) 0.7042(3) 0.6523(3) 0.0174(9) Uani 1 1 d . . . C20 C -0.1422(3) 0.7099(3) 0.7537(3) 0.0242(10) Uani 1 1 d . . . C21 C -0.2264(3) 0.6821(3) 0.8352(3) 0.0268(11) Uani 1 1 d . . . H21 H -0.2828 0.6627 0.8264 0.032 Uiso 1 1 calc R . . C22 C -0.2277(4) 0.6828(3) 0.9298(3) 0.0320(12) Uani 1 1 d . . . H22 H -0.2860 0.6652 0.9849 0.038 Uiso 1 1 calc R . . C23 C -0.1457(4) 0.7087(3) 0.9448(3) 0.0332(12) Uani 1 1 d . . . H23 H -0.1461 0.7063 1.0103 0.040 Uiso 1 1 calc R . . C24 C -0.0635(4) 0.7381(3) 0.8636(4) 0.0322(12) Uani 1 1 d . . . H24 H -0.0073 0.7572 0.8730 0.039 Uiso 1 1 calc R . . C25 C -0.0617(3) 0.7403(3) 0.7686(3) 0.0236(10) Uani 1 1 d . . . H25 H -0.0052 0.7626 0.7128 0.028 Uiso 1 1 calc R . . C26 C 0.1815(3) 0.6625(3) 0.6359(3) 0.0234(11) Uani 1 1 d . . . C27 C 0.2288(3) 0.7226(4) 0.6584(4) 0.0310(11) Uani 1 1 d . . . H27 H 0.2394 0.7880 0.6118 0.037 Uiso 1 1 calc R . . C28 C 0.2603(3) 0.6867(4) 0.7492(4) 0.0393(13) Uani 1 1 d . . . H28 H 0.2921 0.7282 0.7636 0.047 Uiso 1 1 calc R . . C29 C 0.2461(3) 0.5915(4) 0.8186(4) 0.0362(13) Uani 1 1 d . . . H29 H 0.2702 0.5670 0.8789 0.043 Uiso 1 1 calc R . . C30 C 0.1961(3) 0.5326(4) 0.7990(3) 0.0297(11) Uani 1 1 d . . . H30 H 0.1840 0.4683 0.8475 0.036 Uiso 1 1 calc R . . C31 C 0.1629(3) 0.5666(3) 0.7081(3) 0.0219(10) Uani 1 1 d . . . C32 C 0.1043(3) 0.5032(3) 0.6948(3) 0.0185(10) Uani 1 1 d . . . C33 C 0.0483(3) 0.4275(3) 0.7835(3) 0.0256(11) Uani 1 1 d . . . C34 C -0.0162(3) 0.4555(4) 0.8652(3) 0.0406(13) Uani 1 1 d . . . H34 H -0.0204 0.5206 0.8663 0.049 Uiso 1 1 calc R . . C35 C -0.0740(4) 0.3858(6) 0.9450(4) 0.0618(19) Uani 1 1 d . . . H35 H -0.1182 0.4044 1.0007 0.074 Uiso 1 1 calc R . . C36 C -0.0692(5) 0.2925(7) 0.9461(4) 0.074(2) Uani 1 1 d . . . H36 H -0.1116 0.2473 1.0004 0.088 Uiso 1 1 calc R . . C37 C -0.0015(5) 0.2633(5) 0.8666(4) 0.0644(19) Uani 1 1 d . . . H37 H 0.0054 0.1966 0.8688 0.077 Uiso 1 1 calc R . . C38 C 0.0554(4) 0.3308(4) 0.7847(3) 0.0411(13) Uani 1 1 d . . . H38 H 0.0994 0.3115 0.7294 0.049 Uiso 1 1 calc R . . C39 C 0.3439(3) 0.6574(4) 0.0651(3) 0.0347(12) Uani 1 1 d . . . C40 C 0.3975(4) 0.6461(5) -0.0292(3) 0.0553(17) Uani 1 1 d . . . H40 H 0.3915 0.5897 -0.0424 0.066 Uiso 1 1 calc R . . C41 C 0.4581(4) 0.7152(5) -0.1023(4) 0.0645(19) Uani 1 1 d . . . H41 H 0.4928 0.7067 -0.1657 0.077 Uiso 1 1 calc R . . C42 C 0.4690(4) 0.7966(5) -0.0841(4) 0.0586(17) Uani 1 1 d . . . H42 H 0.5118 0.8437 -0.1346 0.070 Uiso 1 1 calc R . . C43 C 0.4177(4) 0.8098(4) 0.0071(4) 0.0451(13) Uani 1 1 d . . . H43 H 0.4247 0.8668 0.0187 0.054 Uiso 1 1 calc R . . N44 N 0.2579(3) 0.6880(3) 0.2599(3) 0.0242(8) Uani 1 1 d . . . C44 C 0.3548(3) 0.7399(4) 0.0841(3) 0.0315(12) Uani 1 1 d . . . C45 C 0.3028(3) 0.7573(3) 0.1803(3) 0.0271(11) Uani 1 1 d D . . C46 C 0.2925(10) 0.8609(10) 0.1740(8) 0.028(3) Uani 0.50 1 d PDU A 2 C47 C 0.2215(7) 0.9303(7) 0.1259(6) 0.025(2) Uani 0.50 1 d PDU A 2 H47 H 0.1816 0.9132 0.0943 0.030 Uiso 0.50 1 calc PR A 2 C48 C 0.2105(7) 1.0266(7) 0.1255(6) 0.0294(19) Uani 0.50 1 d PDU A 2 H48 H 0.1621 1.0774 0.0931 0.035 Uiso 0.50 1 calc PR A 2 C50 C 0.3411(8) 0.9744(8) 0.2200(7) 0.034(2) Uani 0.50 1 d PDU A 2 H50 H 0.3829 0.9878 0.2525 0.041 Uiso 0.50 1 calc PR A 2 C51 C 0.3492(9) 0.8781(10) 0.2185(8) 0.031(3) Uani 0.50 1 d PDU A 2 H51 H 0.3966 0.8255 0.2503 0.037 Uiso 0.50 1 calc PR A 2 C52 C 0.3088(10) 0.8498(10) 0.2013(8) 0.030(3) Uani 0.50 1 d PDU A 1 C53 C 0.2471(7) 0.9407(8) 0.1674(7) 0.030(2) Uani 0.50 1 d PDU A 1 H53 H 0.1987 0.9437 0.1320 0.036 Uiso 0.50 1 calc PR A 1 C54 C 0.2516(12) 1.0279(12) 0.1818(10) 0.036(3) Uani 0.50 1 d PDU A 1 H54 H 0.2076 1.0881 0.1572 0.044 Uiso 0.50 1 calc PR A 1 C55 C 0.3224(8) 1.0236(9) 0.2332(7) 0.038(2) Uani 0.50 1 d PDU A 1 H55 H 0.3267 1.0823 0.2433 0.046 Uiso 0.50 1 calc PR A 1 C56 C 0.3872(8) 0.9365(7) 0.2704(7) 0.037(2) Uani 0.50 1 d PDU A 1 H56 H 0.4349 0.9350 0.3058 0.044 Uiso 0.50 1 calc PR A 1 C57 C 0.3802(8) 0.8526(9) 0.2544(7) 0.027(2) Uani 0.50 1 d PDU A 1 H57 H 0.4247 0.7930 0.2795 0.032 Uiso 0.50 1 calc PR A 1 C58 C 0.3999(4) 0.6162(4) 0.4682(6) 0.066(2) Uani 1 1 d . . . H58A H 0.4390 0.6192 0.3992 0.099 Uiso 1 1 calc R . . H58B H 0.4458 0.5858 0.5146 0.099 Uiso 1 1 calc R . . H58C H 0.3703 0.6840 0.4683 0.099 Uiso 1 1 calc R . . C59 C 0.4836(4) 0.4891(5) 0.2393(4) 0.072(2) Uani 1 1 d . . . H59A H 0.4929 0.4811 0.1741 0.108 Uiso 1 1 calc R . . H59B H 0.5337 0.4404 0.2755 0.108 Uiso 1 1 calc R . . H59C H 0.4941 0.5570 0.2272 0.108 Uiso 1 1 calc R . . H9O H 0.3384 0.4979 0.4962 0.086 Uiso 1 1 d RD . . H10O H 0.3803 0.4313 0.3586 0.086 Uiso 1 1 d RD . . 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 0.0164(4) 0.0216(4) 0.0156(4) -0.0097(3) 0.0002(3) -0.0051(3) P1 0.0182(6) 0.0228(7) 0.0192(6) -0.0062(5) -0.0041(5) -0.0021(5) O1 0.0193(15) 0.0192(16) 0.0166(15) -0.0061(12) -0.0055(12) -0.0021(12) C1 0.018(2) 0.029(3) 0.025(2) -0.011(2) -0.009(2) 0.001(2) C49 0.043(5) 0.022(5) 0.031(4) -0.014(4) 0.000(4) -0.016(4) Mn2 0.0149(3) 0.0204(4) 0.0107(3) -0.0082(3) 0.0008(3) -0.0047(3) O2 0.0180(15) 0.0261(17) 0.0321(17) -0.0091(14) -0.0073(14) -0.0011(13) C2 0.027(3) 0.038(3) 0.030(3) -0.014(2) -0.008(2) -0.004(2) Mn3 0.0208(4) 0.0284(4) 0.0108(4) -0.0072(3) 0.0014(3) -0.0097(3) O3 0.0143(14) 0.0201(17) 0.0155(15) -0.0089(12) -0.0003(12) -0.0032(12) C3 0.035(3) 0.051(4) 0.032(3) -0.023(3) -0.005(2) -0.009(2) O4 0.0273(16) 0.0288(17) 0.0126(15) -0.0088(13) -0.0001(13) -0.0086(13) C4 0.050(3) 0.059(4) 0.026(3) -0.018(3) -0.017(3) -0.001(3) O5 0.0200(16) 0.0293(17) 0.0239(17) -0.0169(14) -0.0006(13) -0.0043(13) C5 0.065(4) 0.036(3) 0.024(3) 0.005(2) -0.020(3) -0.008(3) O6 0.0177(14) 0.0248(16) 0.0125(15) -0.0113(12) -0.0010(12) -0.0046(12) C6 0.048(3) 0.026(3) 0.031(3) -0.008(2) -0.015(2) -0.007(2) O7 0.0407(19) 0.058(2) 0.0095(16) -0.0097(15) 0.0053(15) -0.0309(17) C7 0.023(2) 0.029(3) 0.015(2) -0.004(2) -0.002(2) 0.003(2) O8 0.0228(16) 0.0251(17) 0.0237(17) -0.0107(14) 0.0071(14) -0.0081(13) C8 0.035(3) 0.021(3) 0.046(3) -0.005(2) 0.008(3) 0.000(2) O9 0.0191(16) 0.0346(18) 0.0309(17) -0.0208(15) -0.0041(14) -0.0029(14) N9 0.0173(18) 0.025(2) 0.0114(19) -0.0064(17) 0.0015(15) -0.0069(16) C9 0.044(3) 0.039(3) 0.033(3) -0.001(3) 0.017(3) 0.010(3) O10 0.0190(16) 0.0373(19) 0.0206(16) -0.0072(14) 0.0041(13) -0.0052(14) C10 0.059(4) 0.052(4) 0.029(3) -0.023(3) -0.014(3) 0.029(3) O11 0.0145(14) 0.0250(16) 0.0087(14) -0.0085(12) 0.0017(11) -0.0053(12) C11 0.040(3) 0.052(3) 0.040(3) -0.030(3) -0.021(3) 0.013(3) C12 0.029(3) 0.029(3) 0.027(3) -0.017(2) -0.012(2) 0.008(2) C13 0.012(2) 0.022(3) 0.023(2) -0.009(2) -0.0043(19) -0.0054(19) C14 0.023(2) 0.022(3) 0.019(2) -0.007(2) -0.002(2) -0.004(2) C15 0.028(3) 0.023(3) 0.027(3) -0.004(2) -0.006(2) -0.008(2) C16 0.028(3) 0.020(3) 0.043(3) -0.012(2) -0.012(2) -0.004(2) N17 0.0137(18) 0.021(2) 0.018(2) -0.0132(16) -0.0023(15) -0.0003(15) C17 0.014(2) 0.028(3) 0.023(2) -0.014(2) -0.0041(19) -0.0028(19) C18 0.013(2) 0.024(3) 0.018(2) -0.0113(19) -0.0037(18) -0.0012(18) C19 0.011(2) 0.025(3) 0.017(2) -0.012(2) -0.0004(18) -0.0001(19) C20 0.027(3) 0.031(3) 0.021(2) -0.019(2) -0.006(2) 0.001(2) C21 0.027(3) 0.032(3) 0.022(3) -0.014(2) -0.003(2) -0.001(2) C22 0.043(3) 0.034(3) 0.016(3) -0.016(2) 0.006(2) -0.004(2) C23 0.052(3) 0.029(3) 0.025(3) -0.016(2) -0.014(3) 0.002(2) C24 0.045(3) 0.027(3) 0.036(3) -0.017(2) -0.023(3) 0.003(2) C25 0.024(2) 0.024(3) 0.023(3) -0.014(2) -0.004(2) 0.004(2) C26 0.014(2) 0.035(3) 0.029(3) -0.026(2) -0.002(2) 0.003(2) C27 0.024(2) 0.038(3) 0.042(3) -0.029(2) -0.005(2) -0.002(2) C28 0.024(3) 0.060(4) 0.058(4) -0.046(3) -0.009(3) -0.004(3) C29 0.023(3) 0.069(4) 0.036(3) -0.042(3) -0.010(2) 0.004(3) C30 0.020(2) 0.047(3) 0.028(3) -0.024(2) -0.006(2) 0.002(2) C31 0.015(2) 0.037(3) 0.021(2) -0.023(2) -0.002(2) 0.001(2) C32 0.017(2) 0.022(2) 0.016(2) -0.0111(19) -0.0014(19) 0.0029(19) C33 0.021(2) 0.048(3) 0.011(2) -0.010(2) -0.006(2) -0.008(2) C34 0.026(3) 0.077(4) 0.010(2) -0.012(2) -0.002(2) 0.001(3) C35 0.022(3) 0.131(6) 0.012(3) -0.010(4) 0.000(2) -0.005(4) C36 0.066(4) 0.133(7) 0.018(3) 0.011(4) -0.009(3) -0.070(5) C37 0.109(5) 0.074(4) 0.023(3) 0.008(3) -0.027(4) -0.061(4) C38 0.062(4) 0.054(4) 0.013(3) -0.007(2) -0.006(2) -0.030(3) C39 0.029(3) 0.058(4) 0.014(3) 0.000(2) -0.005(2) -0.022(3) C40 0.058(4) 0.105(5) 0.014(3) -0.017(3) 0.007(3) -0.055(3) C41 0.065(4) 0.121(6) 0.014(3) -0.014(3) 0.011(3) -0.066(4) C42 0.058(4) 0.090(5) 0.021(3) 0.001(3) 0.006(3) -0.054(3) C43 0.046(3) 0.050(3) 0.028(3) 0.003(2) -0.004(3) -0.022(3) N44 0.0194(19) 0.027(2) 0.022(2) -0.0072(18) -0.0021(17) -0.0021(17) C44 0.025(3) 0.048(3) 0.012(2) 0.003(2) -0.002(2) -0.013(2) C45 0.017(2) 0.021(3) 0.032(3) 0.000(2) -0.001(2) -0.004(2) C46 0.028(5) 0.019(4) 0.020(5) 0.003(4) 0.004(4) -0.005(4) C47 0.032(4) 0.023(4) 0.021(4) -0.005(4) -0.008(4) -0.007(3) C48 0.038(4) 0.026(4) 0.024(4) -0.007(3) -0.002(4) -0.013(3) C50 0.043(4) 0.022(4) 0.033(4) -0.009(4) -0.004(3) -0.008(4) C51 0.035(5) 0.020(4) 0.023(4) 0.003(4) -0.003(4) -0.001(4) C52 0.029(5) 0.014(4) 0.025(5) 0.009(4) 0.003(4) -0.005(4) C53 0.037(4) 0.022(4) 0.023(4) 0.001(3) -0.006(3) -0.006(3) C54 0.043(5) 0.024(5) 0.032(4) -0.006(4) 0.001(4) -0.005(4) C55 0.040(4) 0.027(5) 0.037(4) -0.015(4) 0.011(4) -0.008(4) C56 0.040(4) 0.032(4) 0.041(4) -0.017(4) -0.007(4) -0.006(4) C57 0.030(4) 0.020(5) 0.035(5) -0.012(4) -0.005(4) -0.008(4) C58 0.021(3) 0.067(4) 0.140(6) -0.076(4) -0.008(3) -0.006(3) C59 0.027(3) 0.130(6) 0.032(3) -0.009(4) 0.002(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 1.885(4) . ? Mn1 O11 1.899(4) . ? Mn1 O8 1.906(4) . ? Mn1 N17 1.986(5) . ? Mn1 O9 2.208(5) . ? Mn1 O3 2.323(5) . ? P1 O1 1.508(4) . ? P1 O2 1.513(4) . ? P1 C7 1.812(5) . ? P1 C1 1.819(6) . ? O1 Mn2 2.106(4) . ? C1 C6 1.376(7) . ? C1 C2 1.397(6) . ? C49 C50 1.37(2) . ? C49 C48 1.42(2) . ? Mn2 O3 1.895(4) . ? Mn2 O11 1.895(4) 2_566 ? Mn2 O6 1.956(4) 2_566 ? Mn2 N9 2.020(5) . ? Mn2 O6 2.393(4) . ? C2 C3 1.388(7) . ? Mn3 O7 1.856(5) . ? Mn3 O11 1.868(5) . ? Mn3 O4 1.890(4) 2_566 ? Mn3 N44 2.008(5) . ? Mn3 O10 2.147(5) . ? O3 C13 1.354(5) . ? C3 C4 1.372(7) . ? O4 N9 1.365(5) . ? O4 Mn3 1.890(4) 2_566 ? C4 C5 1.380(7) . ? O5 C26 1.341(6) . ? C5 C6 1.396(7) . ? O6 N17 1.384(4) . ? O6 Mn2 1.956(4) 2_566 ? O7 C39 1.319(5) . ? C7 C12 1.385(6) . ? C7 C8 1.392(7) . ? O8 N44 1.380(5) . ? C8 C9 1.387(7) . ? O9 C58 1.417(6) . ? N9 C19 1.308(5) . ? C9 C10 1.371(8) . ? O10 C59 1.399(6) . ? C10 C11 1.373(8) . ? O11 Mn2 1.895(4) 2_566 ? C11 C12 1.381(6) . ? C13 C14 1.401(6) . ? C13 C18 1.421(6) . ? C14 C15 1.370(6) . ? C15 C16 1.384(7) . ? C16 C17 1.389(6) . ? N17 C32 1.299(6) . ? C17 C18 1.406(6) . ? C18 C19 1.465(6) . ? C19 C20 1.485(6) . ? C20 C21 1.391(6) . ? C20 C25 1.398(6) . ? C21 C22 1.393(7) . ? C22 C23 1.380(7) . ? C23 C24 1.375(7) . ? C24 C25 1.381(7) . ? C26 C27 1.402(6) . ? C26 C31 1.416(7) . ? C27 C28 1.397(7) . ? C28 C29 1.386(7) . ? C29 C30 1.386(6) . ? C30 C31 1.412(6) . ? C31 C32 1.476(6) . ? C32 C33 1.480(6) . ? C33 C38 1.392(7) . ? C33 C34 1.398(6) . ? C34 C35 1.391(8) . ? C35 C36 1.350(9) . ? C36 C37 1.395(9) . ? C37 C38 1.381(7) . ? C39 C44 1.398(7) . ? C39 C40 1.410(7) . ? C40 C41 1.372(7) . ? C41 C42 1.375(8) . ? C42 C43 1.375(8) . ? C43 C44 1.414(7) . ? N44 C45 1.308(6) . ? C44 C45 1.467(7) . ? C45 C46 1.461(14) . ? C45 C52 1.534(15) . ? C46 C51 1.285(19) . ? C46 C47 1.369(17) . ? C47 C48 1.382(13) . ? C50 C51 1.401(18) . ? C52 C53 1.392(17) . ? C52 C57 1.453(18) . ? C53 C54 1.40(2) . ? C54 C55 1.39(2) . ? C55 C56 1.388(15) . ? C56 C57 1.374(14) . ? 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 O5 Mn1 O11 173.95(12) . . ? O5 Mn1 O8 93.8(2) . . ? O11 Mn1 O8 91.7(2) . . ? O5 Mn1 N17 87.3(2) . . ? O11 Mn1 N17 87.4(2) . . ? O8 Mn1 N17 175.03(12) . . ? O5 Mn1 O9 86.16(13) . . ? O11 Mn1 O9 91.04(13) . . ? O8 Mn1 O9 93.69(16) . . ? N17 Mn1 O9 91.21(17) . . ? O5 Mn1 O3 89.75(13) . . ? O11 Mn1 O3 92.57(12) . . ? O8 Mn1 O3 91.52(15) . . ? N17 Mn1 O3 83.65(15) . . ? O9 Mn1 O3 173.58(10) . . ? O1 P1 O2 116.65(18) . . ? O1 P1 C7 108.69(18) . . ? O2 P1 C7 106.9(2) . . ? O1 P1 C1 107.82(19) . . ? O2 P1 C1 107.95(19) . . ? C7 P1 C1 108.7(2) . . ? P1 O1 Mn2 141.36(18) . . ? C6 C1 C2 119.1(4) . . ? C6 C1 P1 121.9(3) . . ? C2 C1 P1 118.9(4) . . ? C50 C49 C48 119.0(13) . . ? O3 Mn2 O11 168.20(11) . 2_566 ? O3 Mn2 O6 90.72(16) . 2_566 ? O11 Mn2 O6 89.37(17) 2_566 2_566 ? O3 Mn2 N9 88.73(16) . . ? O11 Mn2 N9 88.87(17) 2_566 . ? O6 Mn2 N9 168.65(12) 2_566 . ? O3 Mn2 O1 92.78(18) . . ? O11 Mn2 O1 98.94(18) 2_566 . ? O6 Mn2 O1 95.89(17) 2_566 . ? N9 Mn2 O1 95.47(17) . . ? O3 Mn2 O6 84.80(18) . . ? O11 Mn2 O6 83.57(18) 2_566 . ? O6 Mn2 O6 80.66(17) 2_566 . ? N9 Mn2 O6 88.00(16) . . ? O1 Mn2 O6 175.74(10) . . ? C3 C2 C1 120.4(5) . . ? O7 Mn3 O11 175.15(13) . . ? O7 Mn3 O4 87.32(15) . 2_566 ? O11 Mn3 O4 91.76(14) . 2_566 ? O7 Mn3 N44 89.36(15) . . ? O11 Mn3 N44 90.08(14) . . ? O4 Mn3 N44 162.24(13) 2_566 . ? O7 Mn3 O10 92.34(16) . . ? O11 Mn3 O10 92.51(15) . . ? O4 Mn3 O10 99.97(18) 2_566 . ? N44 Mn3 O10 97.60(16) . . ? C13 O3 Mn2 119.5(2) . . ? C13 O3 Mn1 113.5(2) . . ? Mn2 O3 Mn1 117.93(18) . . ? C4 C3 C2 119.9(4) . . ? N9 O4 Mn3 119.0(2) . 2_566 ? C3 C4 C5 120.5(5) . . ? C26 O5 Mn1 121.1(3) . . ? C4 C5 C6 119.6(5) . . ? N17 O6 Mn2 111.7(2) . 2_566 ? N17 O6 Mn2 111.6(2) . . ? Mn2 O6 Mn2 99.34(17) 2_566 . ? C1 C6 C5 120.6(4) . . ? C39 O7 Mn3 130.4(3) . . ? C12 C7 C8 119.7(4) . . ? C12 C7 P1 120.9(3) . . ? C8 C7 P1 119.2(4) . . ? N44 O8 Mn1 119.2(3) . . ? C9 C8 C7 120.1(5) . . ? C58 O9 Mn1 124.1(3) . . ? C19 N9 O4 116.8(3) . . ? C19 N9 Mn2 126.5(3) . . ? O4 N9 Mn2 115.1(3) . . ? C10 C9 C8 119.7(5) . . ? C59 O10 Mn3 130.5(3) . . ? C9 C10 C11 120.2(5) . . ? Mn3 O11 Mn2 119.72(14) . 2_566 ? Mn3 O11 Mn1 120.08(18) . . ? Mn2 O11 Mn1 118.99(19) 2_566 . ? C10 C11 C12 121.0(5) . . ? C11 C12 C7 119.3(5) . . ? O3 C13 C14 119.0(4) . . ? O3 C13 C18 121.2(4) . . ? C14 C13 C18 119.7(4) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 121.4(4) . . ? C15 C16 C17 119.4(4) . . ? C32 N17 O6 117.8(3) . . ? C32 N17 Mn1 129.7(3) . . ? O6 N17 Mn1 112.0(3) . . ? C16 C17 C18 121.1(4) . . ? C17 C18 C13 118.2(4) . . ? C17 C18 C19 119.4(4) . . ? C13 C18 C19 122.4(4) . . ? N9 C19 C18 119.1(4) . . ? N9 C19 C20 120.7(4) . . ? C18 C19 C20 120.2(4) . . ? C21 C20 C25 118.8(4) . . ? C21 C20 C19 123.5(4) . . ? C25 C20 C19 117.6(4) . . ? C20 C21 C22 119.6(4) . . ? C23 C22 C21 121.2(4) . . ? C24 C23 C22 119.0(4) . . ? C23 C24 C25 120.8(4) . . ? C24 C25 C20 120.5(4) . . ? O5 C26 C27 117.5(4) . . ? O5 C26 C31 123.4(4) . . ? C27 C26 C31 119.0(4) . . ? C28 C27 C26 120.2(5) . . ? C29 C28 C27 121.2(4) . . ? C30 C29 C28 119.2(4) . . ? C29 C30 C31 121.1(5) . . ? C30 C31 C26 119.2(4) . . ? C30 C31 C32 118.4(4) . . ? C26 C31 C32 122.2(4) . . ? N17 C32 C31 117.1(4) . . ? N17 C32 C33 121.8(4) . . ? C31 C32 C33 121.1(4) . . ? C38 C33 C34 119.9(4) . . ? C38 C33 C32 121.2(4) . . ? C34 C33 C32 118.9(4) . . ? C35 C34 C33 118.4(6) . . ? C36 C35 C34 122.2(6) . . ? C35 C36 C37 119.3(5) . . ? C38 C37 C36 120.4(6) . . ? C37 C38 C33 119.7(5) . . ? O7 C39 C44 124.1(4) . . ? O7 C39 C40 117.2(5) . . ? C44 C39 C40 118.7(4) . . ? C41 C40 C39 121.1(5) . . ? C40 C41 C42 120.3(5) . . ? C43 C42 C41 120.0(5) . . ? C42 C43 C44 121.1(5) . . ? C45 N44 O8 113.8(4) . . ? C45 N44 Mn3 128.6(3) . . ? O8 N44 Mn3 117.4(3) . . ? C39 C44 C43 118.7(4) . . ? C39 C44 C45 122.5(4) . . ? C43 C44 C45 118.7(4) . . ? N44 C45 C46 123.7(5) . . ? N44 C45 C44 121.4(4) . . ? C46 C45 C44 114.3(5) . . ? N44 C45 C52 114.3(5) . . ? C46 C45 C52 18.0(8) . . ? C44 C45 C52 123.8(5) . . ? C51 C46 C47 125.3(12) . . ? C51 C46 C45 116.2(11) . . ? C47 C46 C45 118.5(11) . . ? C46 C47 C48 116.9(10) . . ? C47 C48 C49 119.8(11) . . ? C49 C50 C51 118.9(13) . . ? C46 C51 C50 120.1(11) . . ? C53 C52 C57 113.8(12) . . ? C53 C52 C45 122.1(11) . . ? C57 C52 C45 124.1(9) . . ? C52 C53 C54 124.4(13) . . ? C55 C54 C53 117.8(15) . . ? C54 C55 C56 122.3(12) . . ? C57 C56 C55 117.9(11) . . ? C56 C57 C52 123.8(11) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.643 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.079 # Attachment 'Complex 5.CIF' data_RI2316 _database_code_depnum_ccdc_archive 'CCDC 760681' #TrackingRef 'Complex 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common RI2316 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H82 Mn6 N6 O25 P2' _chemical_formula_weight 1762.97 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.954(3) _cell_length_b 12.962(3) _cell_length_c 14.264(3) _cell_angle_alpha 65.467(13) _cell_angle_beta 80.272(14) _cell_angle_gamma 60.186(13) _cell_volume 1888.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6696 _exptl_absorpt_correction_T_max 0.7449 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex 2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24364 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 23.33 _reflns_number_total 5317 _reflns_number_gt 4135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+6.5127P] 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 5317 _refine_ls_number_parameters 485 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.25466(6) 0.94180(6) 0.15283(5) 0.01329(18) Uani 1 1 d . . . P1 P 0.01984(11) 0.73407(12) 0.35372(9) 0.0183(3) Uani 1 1 d . . . O1 O 0.3544(3) 0.9932(3) 0.1783(2) 0.0166(7) Uani 1 1 d . . . N1 N 0.4009(3) 0.7810(4) 0.1531(3) 0.0161(9) Uani 1 1 d . . . C1 C 0.4429(4) 0.9126(5) 0.2499(3) 0.0173(11) Uani 1 1 d . . . Mn2 Mn -0.00350(6) 0.97354(6) 0.12173(5) 0.01146(18) Uani 1 1 d . . . O2 O 0.3946(3) 0.7311(3) 0.0878(2) 0.0162(7) Uani 1 1 d . . . N2 N 0.0124(3) 1.0914(3) 0.1690(3) 0.0146(9) Uani 1 1 d . . . C2 C 0.4678(4) 0.9637(5) 0.3076(4) 0.0207(11) Uani 1 1 d . . . H2 H 0.4196 1.0524 0.2960 0.025 Uiso 1 1 calc R . . Mn3 Mn 0.24265(6) 0.74473(6) 0.07772(5) 0.01295(18) Uani 1 1 d . . . O3 O -0.1722(2) 1.0881(3) 0.0983(2) 0.0125(7) Uani 1 1 d . . . N3 N 0.0854(3) 0.7573(3) 0.0667(3) 0.0145(9) Uani 1 1 d . . . C3 C 0.5611(4) 0.8874(5) 0.3810(4) 0.0270(12) Uani 1 1 d . . . H3 H 0.5762 0.9242 0.4191 0.032 Uiso 1 1 calc R . . O4 O 0.1155(3) 1.0984(3) 0.1502(2) 0.0180(7) Uani 1 1 d . . . C4 C 0.6319(5) 0.7590(5) 0.3993(4) 0.0302(13) Uani 1 1 d . . . H4 H 0.6949 0.7063 0.4508 0.036 Uiso 1 1 calc R . . O5 O 0.3109(3) 0.6190(3) 0.0238(2) 0.0170(7) Uani 1 1 d . . . C5 C 0.6105(4) 0.7077(5) 0.3422(4) 0.0238(12) Uani 1 1 d . . . H5 H 0.6612 0.6192 0.3542 0.029 Uiso 1 1 calc R . . O6 O -0.0113(2) 0.8792(3) 0.0494(2) 0.0133(7) Uani 1 1 d . . . C6 C 0.5168(4) 0.7809(4) 0.2669(3) 0.0159(10) Uani 1 1 d . . . O7 O -0.0343(3) 0.8646(3) 0.2677(2) 0.0220(8) Uani 1 1 d . . . C7 C 0.5037(4) 0.7229(4) 0.2041(3) 0.0152(10) Uani 1 1 d . . . O8 O 0.1496(3) 0.6751(3) 0.3840(2) 0.0229(8) Uani 1 1 d . . . C8 C 0.6041(4) 0.6011(5) 0.1974(4) 0.0256(12) Uani 1 1 d . . . H8A H 0.5768 0.5722 0.1576 0.038 Uiso 1 1 calc R . . H8B H 0.6312 0.5343 0.2670 0.038 Uiso 1 1 calc R . . H8C H 0.6701 0.6168 0.1630 0.038 Uiso 1 1 calc R . . O9 O 0.2707(3) 0.5949(3) 0.2366(2) 0.0204(8) Uani 1 1 d D . . C9 C -0.2317(4) 1.1294(4) 0.1740(3) 0.0131(10) Uani 1 1 d . . . O10 O 0.2373(3) 0.8465(3) 0.3230(2) 0.0240(8) Uani 1 1 d D . . C10 C -0.3425(4) 1.1351(4) 0.1976(4) 0.0182(11) Uani 1 1 d . . . H10 H -0.3747 1.1109 0.1601 0.022 Uiso 1 1 calc R . . O11 O 0.2715(3) 1.0228(3) -0.0184(2) 0.0157(7) Uani 1 1 d D . . C11 C -0.4069(4) 1.1753(4) 0.2748(4) 0.0197(11) Uani 1 1 d . . . H11 H -0.4819 1.1773 0.2907 0.024 Uiso 1 1 calc R . . O12 O 0.2749(6) 0.6139(7) 0.5578(5) 0.0331(18) Uiso 0.50 1 d P A 1 H12S H 0.2306 0.6157 0.5198 0.040 Uiso 0.50 1 calc PR A 1 C12 C -0.3620(4) 1.2126(4) 0.3288(4) 0.0199(11) Uani 1 1 d . . . H12 H -0.4050 1.2380 0.3831 0.024 Uiso 1 1 calc R . . O13 O 0.1630(2) 0.8800(3) 0.1261(2) 0.0124(7) Uani 1 1 d . . . C13 C -0.2551(4) 1.2129(4) 0.3039(3) 0.0170(11) Uani 1 1 d . . . H13 H -0.2262 1.2415 0.3400 0.020 Uiso 1 1 calc R . . C14 C -0.1873(4) 1.1718(4) 0.2264(3) 0.0132(10) Uani 1 1 d . . . C15 C -0.0734(4) 1.1742(4) 0.2040(3) 0.0160(10) Uani 1 1 d . . . C16 C -0.0529(4) 1.2682(5) 0.2228(4) 0.0286(13) Uani 1 1 d . . . H16A H -0.0046 1.2242 0.2870 0.043 Uiso 1 1 calc R . . H16B H -0.1297 1.3386 0.2285 0.043 Uiso 1 1 calc R . . H16C H -0.0111 1.3033 0.1652 0.043 Uiso 1 1 calc R . . C17 C 0.2809(4) 0.5267(4) 0.0492(3) 0.0159(11) Uani 1 1 d . . . C18 C 0.3713(4) 0.4068(4) 0.0488(4) 0.0209(11) Uani 1 1 d . . . H18 H 0.4494 0.3950 0.0314 0.025 Uiso 1 1 calc R . . C19 C 0.3472(4) 0.3065(5) 0.0735(4) 0.0242(12) Uani 1 1 d . . . H19 H 0.4094 0.2260 0.0733 0.029 Uiso 1 1 calc R . . C20 C 0.2337(4) 0.3209(5) 0.0985(4) 0.0220(11) Uani 1 1 d . . . H20 H 0.2178 0.2513 0.1157 0.026 Uiso 1 1 calc R . . C21 C 0.1449(4) 0.4384(4) 0.0979(3) 0.0178(11) Uani 1 1 d . . . H21 H 0.0667 0.4491 0.1134 0.021 Uiso 1 1 calc R . . C22 C 0.1649(4) 0.5433(4) 0.0754(3) 0.0148(10) Uani 1 1 d . . . C23 C 0.0637(4) 0.6659(4) 0.0736(3) 0.0135(10) Uani 1 1 d . . . C24 C -0.0601(4) 0.6858(4) 0.0818(4) 0.0207(11) Uani 1 1 d . . . H24A H -0.0740 0.6430 0.1540 0.031 Uiso 1 1 calc R . . H24B H -0.0720 0.6491 0.0393 0.031 Uiso 1 1 calc R . . H24C H -0.1162 0.7783 0.0577 0.031 Uiso 1 1 calc R . . C25 C -0.0687(4) 0.7404(4) 0.4637(3) 0.0191(11) Uani 1 1 d . . . C26 C -0.0425(5) 0.6291(5) 0.5531(4) 0.0286(13) Uani 1 1 d . . . H26 H 0.0258 0.5502 0.5568 0.034 Uiso 1 1 calc R . . C27 C -0.1146(5) 0.6327(5) 0.6360(4) 0.0339(14) Uani 1 1 d . . . H27 H -0.0978 0.5561 0.6956 0.041 Uiso 1 1 calc R . . C28 C -0.2115(5) 0.7486(5) 0.6316(4) 0.0288(13) Uani 1 1 d . . . H28 H -0.2610 0.7513 0.6887 0.035 Uiso 1 1 calc R . . C29 C -0.2369(4) 0.8594(5) 0.5459(4) 0.0252(12) Uani 1 1 d . . . H29 H -0.3026 0.9390 0.5443 0.030 Uiso 1 1 calc R . . C30 C -0.1658(4) 0.8548(5) 0.4611(4) 0.0214(11) Uani 1 1 d . . . H30 H -0.1845 0.9313 0.4010 0.026 Uiso 1 1 calc R . . C31 C 0.3782(4) 0.4779(4) 0.2762(4) 0.0244(12) Uani 1 1 d . . . H31A H 0.4180 0.4491 0.2201 0.037 Uiso 1 1 calc R . . H31B H 0.3603 0.4119 0.3294 0.037 Uiso 1 1 calc R . . H31C H 0.4305 0.4918 0.3062 0.037 Uiso 1 1 calc R . . C32 C 0.1915(5) 0.9162(6) 0.3892(4) 0.0412(15) Uani 1 1 d . . . H32A H 0.2074 0.9897 0.3611 0.062 Uiso 1 1 calc R . . H32B H 0.2302 0.8592 0.4582 0.062 Uiso 1 1 calc R . . H32C H 0.1053 0.9476 0.3937 0.062 Uiso 1 1 calc R . . C33 C 0.3557(4) 1.0613(5) -0.0765(4) 0.0232(12) Uani 1 1 d . . . H33A H 0.3647 1.1154 -0.0502 0.035 Uiso 1 1 calc R . . H33B H 0.3279 1.1105 -0.1492 0.035 Uiso 1 1 calc R . . H33C H 0.4327 0.9847 -0.0703 0.035 Uiso 1 1 calc R . . C34 C 0.3894(9) 0.5824(11) 0.5161(8) 0.043(3) Uiso 0.50 1 d P A 1 H34A H 0.3866 0.6588 0.4580 0.064 Uiso 0.50 1 calc PR A 1 H34B H 0.4132 0.5133 0.4921 0.064 Uiso 0.50 1 calc PR A 1 H34C H 0.4474 0.5536 0.5695 0.064 Uiso 0.50 1 calc PR A 1 H1S H 0.0123 0.6550 0.3285 0.051 Uiso 1 1 d R . . H11S H 0.2419 1.0091 -0.0539 0.051 Uiso 1 1 d RD . . H9S H 0.2443 0.6162 0.2849 0.051 Uiso 1 1 d RD . . H10S H 0.2165 0.7908 0.3416 0.051 Uiso 1 1 d RD . . 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 0.0121(4) 0.0150(4) 0.0188(4) -0.0103(3) 0.0032(3) -0.0084(3) P1 0.0209(7) 0.0188(7) 0.0172(7) -0.0077(6) 0.0052(5) -0.0115(6) O1 0.0163(17) 0.0147(17) 0.0228(18) -0.0081(15) -0.0007(14) -0.0090(14) N1 0.027(2) 0.018(2) 0.015(2) -0.0103(18) 0.0056(18) -0.0172(19) C1 0.017(3) 0.027(3) 0.018(3) -0.011(2) 0.005(2) -0.017(2) Mn2 0.0109(4) 0.0125(4) 0.0149(4) -0.0080(3) 0.0025(3) -0.0068(3) O2 0.0139(16) 0.0198(18) 0.0200(17) -0.0140(15) 0.0026(14) -0.0072(14) N2 0.022(2) 0.017(2) 0.017(2) -0.0095(18) 0.0060(17) -0.0168(19) C2 0.023(3) 0.025(3) 0.027(3) -0.017(2) 0.007(2) -0.016(2) Mn3 0.0116(4) 0.0134(4) 0.0176(4) -0.0092(3) 0.0025(3) -0.0067(3) O3 0.0111(16) 0.0140(17) 0.0154(16) -0.0071(14) 0.0031(13) -0.0078(14) N3 0.015(2) 0.012(2) 0.018(2) -0.0091(17) 0.0036(17) -0.0054(18) C3 0.026(3) 0.036(3) 0.031(3) -0.018(3) 0.000(2) -0.019(3) O4 0.0100(16) 0.0216(18) 0.0304(19) -0.0172(16) 0.0063(14) -0.0091(14) C4 0.030(3) 0.036(3) 0.028(3) -0.010(3) -0.007(2) -0.018(3) O5 0.0159(17) 0.0177(18) 0.0237(18) -0.0125(15) 0.0042(14) -0.0098(15) C5 0.020(3) 0.025(3) 0.028(3) -0.010(2) -0.004(2) -0.010(2) O6 0.0104(16) 0.0096(16) 0.0190(17) -0.0077(14) 0.0023(13) -0.0030(13) C6 0.014(2) 0.021(3) 0.019(3) -0.010(2) 0.005(2) -0.012(2) O7 0.0221(18) 0.0199(18) 0.0173(18) -0.0039(15) 0.0055(14) -0.0094(15) C7 0.015(3) 0.019(3) 0.017(2) -0.009(2) 0.004(2) -0.012(2) O8 0.0201(18) 0.0260(19) 0.0198(18) -0.0084(16) 0.0030(15) -0.0101(16) C8 0.016(3) 0.026(3) 0.036(3) -0.017(3) -0.003(2) -0.006(2) O9 0.0184(18) 0.0187(18) 0.0200(18) -0.0100(15) 0.0022(14) -0.0045(15) C9 0.015(2) 0.007(2) 0.013(2) -0.005(2) 0.003(2) -0.002(2) O10 0.030(2) 0.035(2) 0.0216(18) -0.0146(17) 0.0086(16) -0.0248(17) C10 0.014(3) 0.020(3) 0.024(3) -0.010(2) 0.002(2) -0.010(2) O11 0.0159(17) 0.0212(18) 0.0174(17) -0.0098(15) 0.0042(14) -0.0131(15) C11 0.013(2) 0.020(3) 0.027(3) -0.012(2) 0.006(2) -0.008(2) C12 0.017(3) 0.020(3) 0.017(3) -0.010(2) 0.005(2) -0.004(2) O13 0.0116(16) 0.0131(16) 0.0168(16) -0.0083(14) 0.0020(13) -0.0074(14) C13 0.014(2) 0.017(3) 0.021(3) -0.012(2) -0.001(2) -0.004(2) C14 0.012(2) 0.009(2) 0.015(2) -0.003(2) 0.0006(19) -0.0034(19) C15 0.017(3) 0.014(3) 0.017(3) -0.007(2) 0.000(2) -0.006(2) C16 0.022(3) 0.029(3) 0.050(4) -0.029(3) 0.010(3) -0.014(2) C17 0.019(3) 0.017(3) 0.016(2) -0.011(2) 0.002(2) -0.009(2) C18 0.021(3) 0.023(3) 0.024(3) -0.015(2) 0.003(2) -0.010(2) C19 0.027(3) 0.019(3) 0.029(3) -0.016(2) 0.000(2) -0.007(2) C20 0.026(3) 0.019(3) 0.026(3) -0.010(2) -0.001(2) -0.013(2) C21 0.016(3) 0.016(3) 0.021(3) -0.008(2) -0.003(2) -0.006(2) C22 0.017(3) 0.019(3) 0.014(2) -0.008(2) 0.001(2) -0.012(2) C23 0.017(3) 0.014(2) 0.013(2) -0.006(2) 0.0009(19) -0.009(2) C24 0.021(3) 0.013(3) 0.029(3) -0.007(2) -0.002(2) -0.009(2) C25 0.021(3) 0.020(3) 0.016(3) -0.007(2) 0.003(2) -0.011(2) C26 0.029(3) 0.017(3) 0.028(3) -0.007(2) 0.009(2) -0.006(2) C27 0.046(4) 0.025(3) 0.021(3) -0.006(2) 0.011(3) -0.015(3) C28 0.035(3) 0.033(3) 0.020(3) -0.014(3) 0.014(2) -0.018(3) C29 0.020(3) 0.029(3) 0.028(3) -0.018(3) 0.003(2) -0.008(2) C30 0.025(3) 0.021(3) 0.019(3) -0.009(2) 0.004(2) -0.012(2) C31 0.023(3) 0.016(3) 0.026(3) -0.005(2) -0.005(2) -0.003(2) C32 0.054(4) 0.067(4) 0.032(3) -0.035(3) 0.016(3) -0.041(4) C33 0.022(3) 0.033(3) 0.028(3) -0.016(2) 0.012(2) -0.022(2) _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 1.860(3) . ? Mn1 O13 1.884(3) . ? Mn1 O4 1.922(3) . ? Mn1 N1 2.000(4) . ? Mn1 O11 2.244(3) . ? Mn1 O10 2.251(3) . ? Mn1 Mn3 3.2281(11) . ? P1 O7 1.499(3) . ? P1 O8 1.513(3) . ? P1 C25 1.786(5) . ? O1 C1 1.330(5) . ? N1 C7 1.320(6) . ? N1 O2 1.368(4) . ? C1 C2 1.406(6) . ? C1 C6 1.414(6) . ? Mn2 O13 1.873(3) . ? Mn2 O3 1.923(3) . ? Mn2 O6 1.943(3) . ? Mn2 N2 2.012(3) . ? Mn2 O7 2.080(3) . ? Mn2 O6 2.445(3) 2_575 ? O2 Mn3 1.912(3) . ? N2 C15 1.306(6) . ? N2 O4 1.357(5) . ? C2 C3 1.384(7) . ? Mn3 O5 1.846(3) . ? Mn3 O13 1.892(3) . ? Mn3 N3 1.990(4) . ? Mn3 O9 2.228(3) . ? Mn3 O3 2.474(3) 2_575 ? O3 C9 1.356(5) . ? O3 Mn3 2.474(3) 2_575 ? N3 C23 1.310(6) . ? N3 O6 1.392(4) . ? C3 C4 1.371(7) . ? C4 C5 1.376(7) . ? O5 C17 1.331(5) . ? C5 C6 1.407(6) . ? O6 Mn2 2.445(3) 2_575 ? C6 C7 1.461(6) . ? C7 C8 1.495(6) . ? O9 C31 1.419(5) . ? C9 C10 1.390(6) . ? C9 C14 1.411(6) . ? O10 C32 1.431(6) . ? C10 C11 1.384(6) . ? O11 C33 1.421(5) . ? C11 C12 1.379(7) . ? O12 C34 1.422(12) . ? C12 C13 1.371(6) . ? C13 C14 1.404(6) . ? C14 C15 1.469(6) . ? C15 C16 1.497(6) . ? C17 C18 1.408(6) . ? C17 C22 1.413(6) . ? C18 C19 1.377(7) . ? C19 C20 1.389(7) . ? C20 C21 1.376(6) . ? C21 C22 1.407(6) . ? C22 C23 1.466(6) . ? C23 C24 1.485(6) . ? C25 C30 1.377(6) . ? C25 C26 1.398(7) . ? C26 C27 1.379(7) . ? C27 C28 1.382(7) . ? C28 C29 1.368(7) . ? C29 C30 1.394(7) . ? 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 O13 176.09(13) . . ? O1 Mn1 O4 91.71(13) . . ? O13 Mn1 O4 92.17(13) . . ? O1 Mn1 N1 87.62(14) . . ? O13 Mn1 N1 88.49(14) . . ? O4 Mn1 N1 178.77(15) . . ? O1 Mn1 O11 92.71(12) . . ? O13 Mn1 O11 86.63(12) . . ? O4 Mn1 O11 92.98(12) . . ? N1 Mn1 O11 86.02(13) . . ? O1 Mn1 O10 91.33(13) . . ? O13 Mn1 O10 89.14(12) . . ? O4 Mn1 O10 89.80(13) . . ? N1 Mn1 O10 91.25(14) . . ? O11 Mn1 O10 175.02(11) . . ? O1 Mn1 Mn3 144.84(10) . . ? O13 Mn1 Mn3 31.32(8) . . ? O4 Mn1 Mn3 121.79(9) . . ? N1 Mn1 Mn3 58.67(11) . . ? O11 Mn1 Mn3 76.49(8) . . ? O10 Mn1 Mn3 98.53(8) . . ? O7 P1 O8 116.92(19) . . ? O7 P1 C25 108.8(2) . . ? O8 P1 C25 110.2(2) . . ? C1 O1 Mn1 121.3(3) . . ? C7 N1 O2 117.0(3) . . ? C7 N1 Mn1 127.5(3) . . ? O2 N1 Mn1 115.3(3) . . ? O1 C1 C2 117.7(4) . . ? O1 C1 C6 123.6(4) . . ? C2 C1 C6 118.6(4) . . ? O13 Mn2 O3 171.44(13) . . ? O13 Mn2 O6 89.06(12) . . ? O3 Mn2 O6 91.15(12) . . ? O13 Mn2 N2 88.54(14) . . ? O3 Mn2 N2 89.57(14) . . ? O6 Mn2 N2 168.54(14) . . ? O13 Mn2 O7 99.21(13) . . ? O3 Mn2 O7 89.26(12) . . ? O6 Mn2 O7 96.91(13) . . ? N2 Mn2 O7 94.53(14) . . ? O13 Mn2 O6 86.60(11) . 2_575 ? O3 Mn2 O6 84.89(11) . 2_575 ? O6 Mn2 O6 85.39(12) . 2_575 ? N2 Mn2 O6 83.29(12) . 2_575 ? O7 Mn2 O6 173.76(11) . 2_575 ? N1 O2 Mn3 114.6(2) . . ? C15 N2 O4 116.7(3) . . ? C15 N2 Mn2 125.3(3) . . ? O4 N2 Mn2 117.3(3) . . ? C3 C2 C1 121.3(5) . . ? O5 Mn3 O13 175.78(13) . . ? O5 Mn3 O2 90.51(13) . . ? O13 Mn3 O2 92.77(12) . . ? O5 Mn3 N3 88.88(13) . . ? O13 Mn3 N3 87.84(13) . . ? O2 Mn3 N3 179.39(14) . . ? O5 Mn3 O9 90.40(12) . . ? O13 Mn3 O9 92.20(12) . . ? O2 Mn3 O9 90.92(12) . . ? N3 Mn3 O9 89.05(13) . . ? O5 Mn3 O3 89.56(12) . 2_575 ? O13 Mn3 O3 87.22(11) . 2_575 ? O2 Mn3 O3 100.77(11) . 2_575 ? N3 Mn3 O3 79.27(12) . 2_575 ? O9 Mn3 O3 168.31(11) . 2_575 ? O5 Mn3 Mn1 151.84(10) . . ? O13 Mn3 Mn1 31.17(9) . . ? O2 Mn3 Mn1 61.65(9) . . ? N3 Mn3 Mn1 118.96(10) . . ? O9 Mn3 Mn1 93.97(8) . . ? O3 Mn3 Mn1 91.57(7) 2_575 . ? C9 O3 Mn2 117.5(3) . . ? C9 O3 Mn3 113.7(2) . 2_575 ? Mn2 O3 Mn3 116.91(13) . 2_575 ? C23 N3 O6 117.8(3) . . ? C23 N3 Mn3 127.8(3) . . ? O6 N3 Mn3 114.4(2) . . ? C4 C3 C2 120.4(5) . . ? N2 O4 Mn1 115.0(2) . . ? C3 C4 C5 119.1(5) . . ? C17 O5 Mn3 123.6(3) . . ? C4 C5 C6 122.7(5) . . ? N3 O6 Mn2 116.3(2) . . ? N3 O6 Mn2 108.0(2) . 2_575 ? Mn2 O6 Mn2 94.61(12) . 2_575 ? C5 C6 C1 117.8(4) . . ? C5 C6 C7 120.0(4) . . ? C1 C6 C7 122.1(4) . . ? P1 O7 Mn2 142.98(19) . . ? N1 C7 C6 118.3(4) . . ? N1 C7 C8 120.8(4) . . ? C6 C7 C8 120.9(4) . . ? C31 O9 Mn3 124.6(3) . . ? O3 C9 C10 118.6(4) . . ? O3 C9 C14 122.2(4) . . ? C10 C9 C14 119.1(4) . . ? C32 O10 Mn1 122.3(3) . . ? C11 C10 C9 121.1(4) . . ? C33 O11 Mn1 130.3(3) . . ? C12 C11 C10 119.9(4) . . ? C13 C12 C11 119.9(4) . . ? Mn2 O13 Mn1 119.49(15) . . ? Mn2 O13 Mn3 121.79(15) . . ? Mn1 O13 Mn3 117.52(15) . . ? C12 C13 C14 121.5(4) . . ? C13 C14 C9 118.3(4) . . ? C13 C14 C15 118.6(4) . . ? C9 C14 C15 123.1(4) . . ? N2 C15 C14 119.6(4) . . ? N2 C15 C16 119.3(4) . . ? C14 C15 C16 121.1(4) . . ? O5 C17 C18 116.9(4) . . ? O5 C17 C22 123.7(4) . . ? C18 C17 C22 119.4(4) . . ? C19 C18 C17 120.4(4) . . ? C18 C19 C20 121.2(4) . . ? C21 C20 C19 118.5(4) . . ? C20 C21 C22 122.7(4) . . ? C21 C22 C17 117.7(4) . . ? C21 C22 C23 118.7(4) . . ? C17 C22 C23 123.5(4) . . ? N3 C23 C22 118.3(4) . . ? N3 C23 C24 120.4(4) . . ? C22 C23 C24 121.3(4) . . ? C30 C25 C26 118.8(4) . . ? C30 C25 P1 120.5(4) . . ? C26 C25 P1 120.7(4) . . ? C27 C26 C25 120.7(5) . . ? C26 C27 C28 119.4(5) . . ? C29 C28 C27 120.8(5) . . ? C28 C29 C30 119.6(5) . . ? C25 C30 C29 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.098 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.083 # Attachment 'Complex 6.CIF' data_RI2317.CIF _database_code_depnum_ccdc_archive 'CCDC 760682' #TrackingRef 'Complex 6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common RI2317 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H98 Mn6 N6 O26 P2' _chemical_formula_weight 1879.16 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.258(17) _cell_length_b 13.083(18) _cell_length_c 13.767(19) _cell_angle_alpha 98.28(4) _cell_angle_beta 97.92(5) _cell_angle_gamma 109.20(3) _cell_volume 2022(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6820 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex 2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48036 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.92 _reflns_number_total 9544 _reflns_number_gt 7562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.5393P] 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 9544 _refine_ls_number_parameters 522 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 -0.11006(3) 0.39456(3) 0.17099(2) 0.01099(9) Uani 1 1 d . . . P1 P 0.28444(5) 0.58157(5) 0.31241(5) 0.01639(14) Uani 1 1 d . . . O1 O -0.19884(13) 0.24566(13) 0.16260(12) 0.0142(3) Uani 1 1 d . . . N1 N -0.00273(16) 0.34731(15) 0.09565(13) 0.0112(4) Uani 1 1 d . . . C1 C -0.1506(2) 0.16884(19) 0.17283(17) 0.0142(5) Uani 1 1 d . . . Mn2 Mn -0.06496(3) 0.65542(3) 0.23468(2) 0.01143(9) Uani 1 1 d . . . O2 O 0.05054(13) 0.41983(12) 0.03696(11) 0.0120(3) Uani 1 1 d . . . N2 N -0.18101(16) 0.54107(15) 0.28892(14) 0.0123(4) Uani 1 1 d . . . C2 C -0.0442(2) 0.17187(19) 0.14287(17) 0.0144(5) Uani 1 1 d . . . Mn3 Mn 0.10215(3) 0.57559(3) 0.09848(2) 0.01024(8) Uani 1 1 d . . . O3 O -0.12169(14) 0.76012(13) 0.29383(12) 0.0155(3) Uani 1 1 d . . . N3 N 0.12608(16) 0.73748(16) 0.13709(14) 0.0125(4) Uani 1 1 d . . . C3 C -0.0043(2) 0.0846(2) 0.15574(18) 0.0182(5) Uani 1 1 d . . . H3 H 0.0671 0.0856 0.1356 0.022 Uiso 1 1 calc R . . O4 O -0.22460(13) 0.43662(13) 0.22977(12) 0.0142(3) Uani 1 1 d . . . C4 C -0.0646(2) -0.0022(2) 0.19642(19) 0.0221(5) Uani 1 1 d . . . H4 H -0.0351 -0.0597 0.2047 0.026 Uiso 1 1 calc R . . O5 O 0.20332(13) 0.60918(12) 0.00352(11) 0.0121(3) Uani 1 1 d . . . C5 C -0.1694(2) -0.0042(2) 0.22518(19) 0.0219(5) Uani 1 1 d . . . H5 H -0.2127 -0.0642 0.2523 0.026 Uiso 1 1 calc R . . O6 O 0.03802(13) 0.76276(13) 0.17494(12) 0.0138(3) Uani 1 1 d . . . C6 C -0.2109(2) 0.0800(2) 0.21479(18) 0.0195(5) Uani 1 1 d . . . H6 H -0.2817 0.0781 0.2364 0.023 Uiso 1 1 calc R . . O7 O -0.01652(13) 0.54280(12) 0.17405(11) 0.0114(3) Uani 1 1 d . . . C7 C 0.02128(19) 0.25741(19) 0.09273(16) 0.0133(5) Uani 1 1 d . . . O8 O 0.24303(14) 0.57683(14) 0.20305(12) 0.0175(4) Uani 1 1 d . . . C8 C 0.1180(2) 0.2436(2) 0.04225(18) 0.0168(5) Uani 1 1 d . . . H8A H 0.1176 0.2751 -0.0190 0.020 Uiso 1 1 calc R . . H8B H 0.1047 0.1640 0.0223 0.020 Uiso 1 1 calc R . . O9 O 0.19430(14) 0.56219(14) 0.37847(12) 0.0176(4) Uani 1 1 d . . . C9 C 0.2367(2) 0.3019(2) 0.1132(2) 0.0251(6) Uani 1 1 d . . . H9A H 0.2508 0.3810 0.1311 0.038 Uiso 1 1 calc R . . H9B H 0.2992 0.2912 0.0802 0.038 Uiso 1 1 calc R . . H9C H 0.2366 0.2710 0.1739 0.038 Uiso 1 1 calc R . . O10 O 0.06977(14) 0.69420(13) 0.37464(12) 0.0178(4) Uani 1 1 d D . . C10 C -0.1446(2) 0.7642(2) 0.38630(17) 0.0164(5) Uani 1 1 d . . . O11 O -0.00954(14) 0.39509(14) 0.31509(12) 0.0174(4) Uani 1 1 d D . . C11 C -0.1943(2) 0.6687(2) 0.42526(17) 0.0162(5) Uani 1 1 d . . . O12 O -0.22096(14) 0.60044(14) 0.10090(12) 0.0163(3) Uani 1 1 d D . . C12 C -0.2134(2) 0.6823(2) 0.52388(18) 0.0224(5) Uani 1 1 d . . . H12 H -0.2469 0.6188 0.5507 0.027 Uiso 1 1 calc R . . O13 O -0.4104(2) 0.1895(2) 0.2507(2) 0.0656(8) Uani 1 1 d . . . H13S H -0.3579 0.2129 0.2177 0.079 Uiso 1 1 calc R . . C13 C -0.1847(3) 0.7857(2) 0.5825(2) 0.0309(7) Uani 1 1 d . . . H13 H -0.1963 0.7931 0.6496 0.037 Uiso 1 1 calc R . . C14 C -0.1390(3) 0.8782(2) 0.5432(2) 0.0320(7) Uani 1 1 d . . . H14 H -0.1208 0.9495 0.5829 0.038 Uiso 1 1 calc R . . C15 C -0.1195(2) 0.8680(2) 0.4465(2) 0.0248(6) Uani 1 1 d . . . H15 H -0.0884 0.9327 0.4204 0.030 Uiso 1 1 calc R . . C16 C -0.22948(19) 0.55695(19) 0.36555(17) 0.0136(5) Uani 1 1 d . . . C17 C -0.3224(2) 0.4634(2) 0.39110(18) 0.0177(5) Uani 1 1 d . . . H17A H -0.3000 0.4605 0.4623 0.021 Uiso 1 1 calc R . . H17B H -0.3277 0.3929 0.3496 0.021 Uiso 1 1 calc R . . C18 C -0.4431(2) 0.4764(3) 0.3733(2) 0.0348(7) Uani 1 1 d . . . H18A H -0.4375 0.5471 0.4128 0.052 Uiso 1 1 calc R . . H18B H -0.5011 0.4158 0.3936 0.052 Uiso 1 1 calc R . . H18C H -0.4678 0.4745 0.3020 0.052 Uiso 1 1 calc R . . C19 C 0.30424(19) 0.69869(19) 0.03042(17) 0.0130(5) Uani 1 1 d . . . C20 C 0.3074(2) 0.8024(2) 0.07927(18) 0.0171(5) Uani 1 1 d . . . C21 C 0.4122(2) 0.8934(2) 0.0944(2) 0.0232(6) Uani 1 1 d . . . H21 H 0.4138 0.9644 0.1238 0.028 Uiso 1 1 calc R . . C22 C 0.5131(2) 0.8828(2) 0.0679(2) 0.0253(6) Uani 1 1 d . . . H22 H 0.5837 0.9454 0.0796 0.030 Uiso 1 1 calc R . . C23 C 0.5098(2) 0.7798(2) 0.0242(2) 0.0260(6) Uani 1 1 d . . . H23 H 0.5794 0.7711 0.0076 0.031 Uiso 1 1 calc R . . C24 C 0.4066(2) 0.6894(2) 0.0043(2) 0.0209(5) Uani 1 1 d . . . H24 H 0.4055 0.6196 -0.0277 0.025 Uiso 1 1 calc R . . C25 C 0.2060(2) 0.81943(19) 0.11521(18) 0.0164(5) Uani 1 1 d . . . C26 C 0.1974(2) 0.9323(2) 0.1297(2) 0.0226(5) Uani 1 1 d . . . H26A H 0.1141 0.9250 0.1093 0.027 Uiso 1 1 calc R . . H26B H 0.2433 0.9756 0.0860 0.027 Uiso 1 1 calc R . . C27 C 0.2432(3) 0.9938(2) 0.2375(2) 0.0297(6) Uani 1 1 d . . . H27A H 0.1928 0.9552 0.2801 0.044 Uiso 1 1 calc R . . H27B H 0.2423 1.0691 0.2429 0.044 Uiso 1 1 calc R . . H27C H 0.3240 0.9970 0.2593 0.044 Uiso 1 1 calc R . . C28 C 0.4018(2) 0.7111(2) 0.36552(19) 0.0229(6) Uani 1 1 d . . . C29 C 0.4241(3) 0.7559(2) 0.4677(2) 0.0323(7) Uani 1 1 d . . . H29 H 0.3771 0.7178 0.5098 0.039 Uiso 1 1 calc R . . C30 C 0.5149(3) 0.8558(3) 0.5077(2) 0.0474(9) Uani 1 1 d . . . H30 H 0.5310 0.8855 0.5775 0.057 Uiso 1 1 calc R . . C31 C 0.5817(3) 0.9121(3) 0.4469(3) 0.0553(10) Uani 1 1 d . . . H31 H 0.6444 0.9802 0.4751 0.066 Uiso 1 1 calc R . . C32 C 0.5585(3) 0.8707(3) 0.3455(3) 0.0533(10) Uani 1 1 d . . . H32 H 0.6034 0.9115 0.3037 0.064 Uiso 1 1 calc R . . C33 C 0.4696(2) 0.7697(3) 0.3044(2) 0.0361(7) Uani 1 1 d . . . H33 H 0.4550 0.7404 0.2347 0.043 Uiso 1 1 calc R . . C34 C 0.1473(2) 0.8041(2) 0.4213(2) 0.0258(6) Uani 1 1 d . . . H34A H 0.2140 0.8258 0.3873 0.039 Uiso 1 1 calc R . . H34B H 0.1765 0.8065 0.4919 0.039 Uiso 1 1 calc R . . H34C H 0.1045 0.8552 0.4168 0.039 Uiso 1 1 calc R . . C35 C -0.0622(2) 0.3569(2) 0.39590(19) 0.0251(6) Uani 1 1 d . . . H35A H -0.1382 0.2970 0.3689 0.038 Uiso 1 1 calc R . . H35B H -0.0746 0.4180 0.4375 0.038 Uiso 1 1 calc R . . H35C H -0.0100 0.3297 0.4367 0.038 Uiso 1 1 calc R . . C36 C -0.3347(2) 0.5988(2) 0.1146(2) 0.0227(6) Uani 1 1 d . . . H36A H -0.3680 0.5415 0.1519 0.034 Uiso 1 1 calc R . . H36B H -0.3865 0.5828 0.0491 0.034 Uiso 1 1 calc R . . H36C H -0.3278 0.6710 0.1521 0.034 Uiso 1 1 calc R . . C37 C -0.5060(3) 0.2221(3) 0.2201(3) 0.0550(10) Uani 1 1 d . . . H37A H -0.5474 0.2280 0.2754 0.083 Uiso 1 1 calc R . . H37B H -0.5602 0.1670 0.1628 0.083 Uiso 1 1 calc R . . H37C H -0.4769 0.2939 0.2007 0.083 Uiso 1 1 calc R . . H1S H 0.3337 0.5024 0.3175 0.066 Uiso 1 1 d R . . H12S H -0.2296 0.5428 0.0651 0.066 Uiso 1 1 d RD . . H11S H 0.0530 0.4419 0.3360 0.066 Uiso 1 1 d RD . . H10S H 0.1070 0.6534 0.3766 0.066 Uiso 1 1 d RD . . 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 0.01263(17) 0.00908(17) 0.01245(18) 0.00310(13) 0.00418(13) 0.00437(14) P1 0.0153(3) 0.0180(3) 0.0154(3) 0.0057(3) -0.0004(2) 0.0056(3) O1 0.0156(8) 0.0106(8) 0.0175(8) 0.0046(7) 0.0036(6) 0.0053(7) N1 0.0135(9) 0.0097(9) 0.0107(9) 0.0043(7) 0.0031(7) 0.0033(8) C1 0.0189(11) 0.0097(11) 0.0123(11) 0.0002(9) 0.0012(9) 0.0045(9) Mn2 0.01448(17) 0.00944(18) 0.01209(18) 0.00296(14) 0.00544(13) 0.00506(14) O2 0.0158(8) 0.0101(8) 0.0117(8) 0.0050(6) 0.0057(6) 0.0044(6) N2 0.0154(9) 0.0108(10) 0.0125(9) 0.0023(8) 0.0030(7) 0.0068(8) C2 0.0206(12) 0.0101(11) 0.0123(11) 0.0026(9) 0.0033(9) 0.0053(10) Mn3 0.01181(16) 0.00882(17) 0.01090(17) 0.00264(13) 0.00366(13) 0.00390(14) O3 0.0216(8) 0.0133(8) 0.0158(8) 0.0044(7) 0.0093(7) 0.0087(7) N3 0.0136(9) 0.0128(10) 0.0124(9) 0.0015(8) 0.0044(7) 0.0063(8) C3 0.0250(13) 0.0162(12) 0.0187(12) 0.0054(10) 0.0087(10) 0.0116(10) O4 0.0163(8) 0.0095(8) 0.0155(8) 0.0009(6) 0.0037(6) 0.0035(7) C4 0.0324(14) 0.0163(13) 0.0242(13) 0.0093(11) 0.0112(11) 0.0129(11) O5 0.0135(8) 0.0106(8) 0.0119(8) 0.0027(6) 0.0037(6) 0.0032(6) C5 0.0283(13) 0.0135(12) 0.0251(14) 0.0082(11) 0.0094(11) 0.0054(11) O6 0.0169(8) 0.0120(8) 0.0166(8) 0.0040(7) 0.0084(7) 0.0078(7) C6 0.0211(12) 0.0152(12) 0.0225(13) 0.0060(10) 0.0081(10) 0.0046(10) O7 0.0128(7) 0.0092(8) 0.0136(8) 0.0025(6) 0.0047(6) 0.0047(6) C7 0.0154(11) 0.0130(11) 0.0107(11) 0.0021(9) 0.0009(9) 0.0051(9) O8 0.0154(8) 0.0217(9) 0.0155(8) 0.0050(7) 0.0011(7) 0.0070(7) C8 0.0239(12) 0.0152(12) 0.0180(12) 0.0074(10) 0.0107(10) 0.0112(10) O9 0.0182(8) 0.0168(9) 0.0156(8) 0.0052(7) 0.0020(7) 0.0029(7) C9 0.0206(13) 0.0314(15) 0.0304(15) 0.0109(12) 0.0098(11) 0.0148(12) O10 0.0202(8) 0.0136(9) 0.0167(8) 0.0011(7) 0.0005(7) 0.0042(7) C10 0.0207(12) 0.0180(13) 0.0155(12) 0.0047(10) 0.0076(10) 0.0114(10) O11 0.0189(8) 0.0186(9) 0.0130(8) 0.0067(7) 0.0032(7) 0.0028(7) C11 0.0190(12) 0.0176(12) 0.0153(12) 0.0041(10) 0.0041(9) 0.0101(10) O12 0.0155(8) 0.0186(9) 0.0161(8) 0.0035(7) 0.0048(7) 0.0070(7) C12 0.0341(14) 0.0215(14) 0.0172(13) 0.0063(11) 0.0113(11) 0.0136(12) O13 0.0606(17) 0.0653(19) 0.098(2) 0.0437(17) 0.0424(16) 0.0349(16) C13 0.0510(18) 0.0287(16) 0.0189(14) 0.0034(12) 0.0169(13) 0.0184(14) C14 0.0563(19) 0.0203(14) 0.0221(14) -0.0015(11) 0.0154(13) 0.0164(14) C15 0.0367(15) 0.0156(13) 0.0261(14) 0.0054(11) 0.0125(12) 0.0114(12) C16 0.0142(11) 0.0186(12) 0.0122(11) 0.0068(9) 0.0037(9) 0.0092(10) C17 0.0193(12) 0.0187(13) 0.0172(12) 0.0065(10) 0.0084(10) 0.0064(10) C18 0.0202(13) 0.0424(18) 0.0480(19) 0.0198(15) 0.0148(13) 0.0115(13) C19 0.0123(10) 0.0121(11) 0.0132(11) 0.0045(9) 0.0013(9) 0.0023(9) C20 0.0152(11) 0.0142(12) 0.0217(13) 0.0028(10) 0.0047(10) 0.0046(10) C21 0.0219(13) 0.0155(13) 0.0293(14) 0.0003(11) 0.0107(11) 0.0022(11) C22 0.0164(12) 0.0201(14) 0.0338(15) 0.0009(12) 0.0083(11) -0.0003(11) C23 0.0158(12) 0.0252(15) 0.0378(16) 0.0043(12) 0.0108(11) 0.0067(11) C24 0.0191(12) 0.0164(13) 0.0300(14) 0.0046(11) 0.0110(11) 0.0075(10) C25 0.0174(11) 0.0116(12) 0.0194(12) 0.0015(10) 0.0049(10) 0.0044(10) C26 0.0227(13) 0.0147(13) 0.0325(15) 0.0047(11) 0.0129(11) 0.0064(11) C27 0.0335(15) 0.0214(14) 0.0320(16) 0.0027(12) 0.0073(12) 0.0078(12) C28 0.0161(12) 0.0270(14) 0.0219(13) 0.0065(11) -0.0022(10) 0.0048(11) C29 0.0357(16) 0.0271(16) 0.0238(15) 0.0106(12) -0.0046(12) -0.0006(13) C30 0.053(2) 0.0327(18) 0.0293(17) 0.0032(14) -0.0148(15) -0.0100(16) C31 0.0380(19) 0.042(2) 0.053(2) 0.0070(17) -0.0109(16) -0.0206(16) C32 0.0326(17) 0.054(2) 0.049(2) 0.0155(18) 0.0069(16) -0.0164(16) C33 0.0256(14) 0.0421(19) 0.0312(16) 0.0089(14) 0.0065(12) -0.0012(13) C34 0.0295(14) 0.0163(13) 0.0234(14) 0.0001(11) 0.0015(11) 0.0008(11) C35 0.0270(14) 0.0307(15) 0.0152(12) 0.0105(11) 0.0060(10) 0.0039(12) C36 0.0196(12) 0.0246(14) 0.0265(14) 0.0022(11) 0.0038(11) 0.0125(11) C37 0.049(2) 0.057(2) 0.061(2) 0.014(2) 0.0158(19) 0.0187(19) _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 1.870(3) . ? Mn1 O7 1.892(3) . ? Mn1 O4 1.903(3) . ? Mn1 N1 1.979(3) . ? Mn1 O11 2.184(3) . ? Mn1 O5 2.501(4) 2_565 ? Mn1 Mn2 3.238(5) . ? P1 O8 1.507(3) . ? P1 O9 1.507(2) . ? P1 C28 1.796(3) . ? P1 H1S 1.3646 . ? O1 C1 1.337(3) . ? N1 C7 1.300(3) . ? N1 O2 1.392(3) . ? C1 C6 1.406(3) . ? C1 C2 1.411(4) . ? Mn2 O3 1.867(2) . ? Mn2 O7 1.892(2) . ? Mn2 O6 1.922(2) . ? Mn2 N2 2.008(3) . ? Mn2 O10 2.233(3) . ? Mn2 O12 2.304(3) . ? O2 Mn3 1.944(3) . ? O2 Mn3 2.475(3) 2_565 ? N2 C16 1.304(3) . ? N2 O4 1.377(3) . ? C2 C3 1.406(3) . ? C2 C7 1.469(3) . ? Mn3 O7 1.876(2) . ? Mn3 O5 1.922(3) . ? Mn3 N3 2.020(3) . ? Mn3 O8 2.084(3) . ? Mn3 O2 2.475(3) 2_565 ? O3 C10 1.338(3) . ? N3 C25 1.298(3) . ? N3 O6 1.373(3) . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? O5 C19 1.355(3) . ? O5 Mn1 2.501(4) 2_565 ? C5 C6 1.373(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.501(4) . ? C8 C9 1.522(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 C34 1.432(3) . ? O10 H10S 0.8086 . ? C10 C15 1.399(4) . ? C10 C11 1.415(4) . ? O11 C35 1.432(3) . ? O11 H11S 0.7906 . ? C11 C12 1.405(4) . ? C11 C16 1.464(4) . ? O12 C36 1.426(3) . ? O12 H12S 0.8054 . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? O13 C37 1.406(4) . ? O13 H13S 0.8400 . ? C13 C14 1.378(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.496(3) . ? C17 C18 1.535(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.390(4) . ? C19 C20 1.410(4) . ? C20 C21 1.400(4) . ? C20 C25 1.470(4) . ? C21 C22 1.381(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.379(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.502(4) . ? C26 C27 1.515(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.395(4) . ? C28 C29 1.396(4) . ? C29 C30 1.385(4) . ? C29 H29 0.9500 . ? C30 C31 1.371(5) . ? C30 H30 0.9500 . ? C31 C32 1.376(5) . ? C31 H31 0.9500 . ? C32 C33 1.386(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 O7 177.00(7) . . ? O1 Mn1 O4 90.08(11) . . ? O7 Mn1 O4 92.70(11) . . ? O1 Mn1 N1 88.79(11) . . ? O7 Mn1 N1 88.33(11) . . ? O4 Mn1 N1 173.75(7) . . ? O1 Mn1 O11 88.85(9) . . ? O7 Mn1 O11 92.13(9) . . ? O4 Mn1 O11 93.48(11) . . ? N1 Mn1 O11 92.64(12) . . ? O1 Mn1 O5 92.28(8) . 2_565 ? O7 Mn1 O5 86.39(8) . 2_565 ? O4 Mn1 O5 93.89(11) . 2_565 ? N1 Mn1 O5 80.02(11) . 2_565 ? O11 Mn1 O5 172.54(6) . 2_565 ? O1 Mn1 Mn2 151.69(7) . . ? O7 Mn1 Mn2 31.14(7) . . ? O4 Mn1 Mn2 61.63(6) . . ? N1 Mn1 Mn2 119.43(7) . . ? O11 Mn1 Mn2 91.75(7) . . ? O5 Mn1 Mn2 90.75(7) 2_565 . ? O8 P1 O9 118.11(13) . . ? O8 P1 C28 109.42(13) . . ? O9 P1 C28 109.03(14) . . ? O8 P1 H1S 107.1 . . ? O9 P1 H1S 106.8 . . ? C28 P1 H1S 105.7 . . ? C1 O1 Mn1 123.23(17) . . ? C7 N1 O2 117.14(19) . . ? C7 N1 Mn1 128.33(16) . . ? O2 N1 Mn1 114.50(15) . . ? O1 C1 C6 117.5(2) . . ? O1 C1 C2 123.6(2) . . ? C6 C1 C2 118.8(2) . . ? O3 Mn2 O7 176.56(7) . . ? O3 Mn2 O6 91.51(12) . . ? O7 Mn2 O6 91.40(12) . . ? O3 Mn2 N2 88.38(13) . . ? O7 Mn2 N2 88.60(13) . . ? O6 Mn2 N2 176.16(7) . . ? O3 Mn2 O10 89.35(11) . . ? O7 Mn2 O10 92.33(10) . . ? O6 Mn2 O10 93.18(11) . . ? N2 Mn2 O10 90.66(12) . . ? O3 Mn2 O12 89.64(11) . . ? O7 Mn2 O12 88.30(10) . . ? O6 Mn2 O12 94.36(11) . . ? N2 Mn2 O12 81.80(11) . . ? O10 Mn2 O12 172.42(6) . . ? O3 Mn2 Mn1 145.56(7) . . ? O7 Mn2 Mn1 31.14(6) . . ? O6 Mn2 Mn1 121.30(8) . . ? N2 Mn2 Mn1 58.15(9) . . ? O10 Mn2 Mn1 98.20(6) . . ? O12 Mn2 Mn1 78.54(6) . . ? N1 O2 Mn3 114.98(15) . . ? N1 O2 Mn3 109.21(14) . 2_565 ? Mn3 O2 Mn3 95.71(9) . 2_565 ? C16 N2 O4 116.94(19) . . ? C16 N2 Mn2 127.65(18) . . ? O4 N2 Mn2 114.83(15) . . ? C3 C2 C1 118.0(2) . . ? C3 C2 C7 119.0(2) . . ? C1 C2 C7 122.9(2) . . ? O7 Mn3 O5 170.37(6) . . ? O7 Mn3 O2 89.64(8) . . ? O5 Mn3 O2 89.23(9) . . ? O7 Mn3 N3 89.20(8) . . ? O5 Mn3 N3 89.70(8) . . ? O2 Mn3 N3 166.69(7) . . ? O7 Mn3 O8 99.46(13) . . ? O5 Mn3 O8 90.18(13) . . ? O2 Mn3 O8 96.13(9) . . ? N3 Mn3 O8 97.14(9) . . ? O7 Mn3 O2 86.40(13) . 2_565 ? O5 Mn3 O2 83.97(12) . 2_565 ? O2 Mn3 O2 84.29(9) . 2_565 ? N3 Mn3 O2 82.40(8) . 2_565 ? O8 Mn3 O2 174.13(6) . 2_565 ? C10 O3 Mn2 122.44(15) . . ? C25 N3 O6 115.5(2) . . ? C25 N3 Mn3 126.60(17) . . ? O6 N3 Mn3 116.89(13) . . ? C4 C3 C2 122.5(2) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? N2 O4 Mn1 114.09(14) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C19 O5 Mn3 119.06(16) . . ? C19 O5 Mn1 107.62(14) . 2_565 ? Mn3 O5 Mn1 117.70(12) . 2_565 ? C6 C5 C4 120.5(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? N3 O6 Mn2 118.13(15) . . ? C5 C6 C1 121.3(2) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? Mn3 O7 Mn2 120.58(10) . . ? Mn3 O7 Mn1 120.68(9) . . ? Mn2 O7 Mn1 117.73(12) . . ? N1 C7 C2 119.1(2) . . ? N1 C7 C8 120.2(2) . . ? C2 C7 C8 120.7(2) . . ? P1 O8 Mn3 143.72(11) . . ? C7 C8 C9 110.0(2) . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C34 O10 Mn2 123.25(15) . . ? C34 O10 H10S 108.4 . . ? Mn2 O10 H10S 115.1 . . ? O3 C10 C15 118.2(2) . . ? O3 C10 C11 123.1(2) . . ? C15 C10 C11 118.7(2) . . ? C35 O11 Mn1 123.82(17) . . ? C35 O11 H11S 110.3 . . ? Mn1 O11 H11S 119.0 . . ? C12 C11 C10 118.5(2) . . ? C12 C11 C16 119.1(2) . . ? C10 C11 C16 122.3(2) . . ? C36 O12 Mn2 121.17(17) . . ? C36 O12 H12S 107.6 . . ? Mn2 O12 H12S 113.7 . . ? C13 C12 C11 121.5(2) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C37 O13 H13S 109.5 . . ? C12 C13 C14 119.6(3) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C10 121.1(2) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? N2 C16 C11 119.2(2) . . ? N2 C16 C17 120.9(2) . . ? C11 C16 C17 119.9(2) . . ? C16 C17 C18 111.5(2) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 C24 118.8(2) . . ? O5 C19 C20 122.1(2) . . ? C24 C19 C20 118.9(2) . . ? C21 C20 C19 118.5(2) . . ? C21 C20 C25 118.4(2) . . ? C19 C20 C25 123.1(2) . . ? C22 C21 C20 121.7(3) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C23 C22 C21 118.9(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 120.7(2) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C19 121.1(3) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? N3 C25 C20 119.8(2) . . ? N3 C25 C26 120.3(2) . . ? C20 C25 C26 119.9(2) . . ? C25 C26 C27 111.9(2) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 119.2(3) . . ? C33 C28 P1 120.2(2) . . ? C29 C28 P1 120.5(2) . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.3(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.0(3) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? O10 C34 H34A 109.5 . . ? O10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O11 C35 H35A 109.5 . . ? O11 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O11 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O12 C36 H36A 109.5 . . ? O12 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O12 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O13 C37 H37A 109.5 . . ? O13 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O13 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.979 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.085