Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Neil Connelly' 'Christopher J. Adams' 'Kirsty Anderson' 'Manuel Bardaji' 'Nicholas J. Goodwin' 'Estefania Llamas-Rey' 'A. Guy Orpen' 'Philip H. Reiger' _publ_contact_author_name 'Prof Neil Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol Bristol BS8 4QQ UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Bi- and poly-metallic cyanide-bridged complexes of the redox-active cyanomanganese nitrosyl unit [Mn(CN)(PR3)(NO)(h-C5H4Me)] ; data_30 _database_code_depnum_ccdc_archive 'CCDC 223106' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 F6 Mn2 N5 O2 P' _chemical_formula_weight 761.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9264(14) _cell_length_b 16.5505(17) _cell_length_c 16.5090(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.172(2) _cell_angle_gamma 90.00 _cell_volume 3408.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 178 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594787 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21775 _diffrn_reflns_av_R_equivalents 0.1097 _diffrn_reflns_av_sigmaI/netI 0.1801 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7813 _reflns_number_gt 3176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^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 7813 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1691 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.810 _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 0.26291(5) 0.03800(3) 0.58228(4) 0.02925(18) Uani 1 1 d . . . Mn2 Mn 0.18354(5) 0.01744(4) 0.86476(4) 0.03179(18) Uani 1 1 d . . . C1 C 0.2033(3) 0.0225(2) 0.7532(2) 0.0276(9) Uani 1 1 d . . . N2 N 0.1447(3) 0.05178(19) 0.5174(2) 0.0355(9) Uani 1 1 d . . . N3 N 0.3096(3) 0.0276(2) 0.9164(2) 0.0423(9) Uani 1 1 d . . . N4 N 0.2777(3) -0.1461(2) 0.5782(2) 0.0351(9) Uani 1 1 d . . . N5 N 0.1784(3) -0.1668(2) 0.8581(2) 0.0396(9) Uani 1 1 d . . . O1 O 0.0640(3) 0.06615(19) 0.4650(2) 0.0597(10) Uani 1 1 d . . . O2 O 0.3968(3) 0.0401(2) 0.9599(2) 0.0719(11) Uani 1 1 d . . . N1 N 0.2205(3) 0.0289(2) 0.6882(2) 0.0406(9) Uani 1 1 d . . . C2 C 0.4059(4) 0.1021(3) 0.6580(3) 0.0378(11) Uani 1 1 d . . . C3 C 0.4355(3) 0.0360(3) 0.6156(3) 0.0380(11) Uani 1 1 d . . . H3A H 0.4817 -0.0103 0.6424 0.046 Uiso 1 1 calc R . . C4 C 0.3917(3) 0.0473(3) 0.5277(3) 0.0379(11) Uani 1 1 d . . . H4A H 0.4047 0.0123 0.4820 0.045 Uiso 1 1 calc R . . C5 C 0.3343(3) 0.1202(2) 0.5170(3) 0.0380(11) Uani 1 1 d . . . H5A H 0.2988 0.1461 0.4620 0.046 Uiso 1 1 calc R . . C6 C 0.3423(3) 0.1534(2) 0.5973(3) 0.0371(11) Uani 1 1 d . . . H6A H 0.3104 0.2058 0.6088 0.044 Uiso 1 1 calc R . . C7 C 0.4373(4) 0.1161(3) 0.7510(3) 0.0601(15) Uani 1 1 d . . . H7A H 0.5052 0.1458 0.7667 0.090 Uiso 1 1 calc R . . H7B H 0.4458 0.0640 0.7802 0.090 Uiso 1 1 calc R . . H7C H 0.3814 0.1476 0.7668 0.090 Uiso 1 1 calc R . . C8 C 0.2694(3) -0.0769(3) 0.5793(2) 0.0327(10) Uani 1 1 d . . . C9 C 0.2837(3) -0.2311(2) 0.5794(2) 0.0304(10) Uani 1 1 d . . . C10 C 0.2025(3) -0.2730(3) 0.6028(2) 0.0356(11) Uani 1 1 d . . . C11 C 0.2108(4) -0.3564(3) 0.6041(3) 0.0463(12) Uani 1 1 d . . . H11A H 0.1573 -0.3878 0.6194 0.056 Uiso 1 1 calc R . . C12 C 0.2955(4) -0.3950(3) 0.5836(3) 0.0466(13) Uani 1 1 d . . . H12A H 0.3003 -0.4522 0.5855 0.056 Uiso 1 1 calc R . . C13 C 0.3729(4) -0.3501(3) 0.5604(2) 0.0414(12) Uani 1 1 d . . . H13A H 0.4294 -0.3774 0.5448 0.050 Uiso 1 1 calc R . . C14 C 0.3706(3) -0.2669(2) 0.5593(2) 0.0322(10) Uani 1 1 d . . . C15 C 0.4595(3) -0.2181(3) 0.5402(3) 0.0486(13) Uani 1 1 d . . . H15A H 0.4290 -0.1787 0.4961 0.073 Uiso 1 1 calc R . . H15B H 0.5083 -0.2542 0.5210 0.073 Uiso 1 1 calc R . . H15C H 0.4989 -0.1898 0.5910 0.073 Uiso 1 1 calc R . . C16 C 0.1124(4) -0.2282(3) 0.6255(3) 0.0533(13) Uani 1 1 d . . . H16A H 0.1422 -0.1877 0.6686 0.080 Uiso 1 1 calc R . . H16B H 0.0684 -0.2665 0.6472 0.080 Uiso 1 1 calc R . . H16C H 0.0680 -0.2014 0.5755 0.080 Uiso 1 1 calc R . . C17 C 0.1178(4) 0.0664(3) 0.9602(3) 0.0420(12) Uani 1 1 d . . . H17A H 0.1515 0.0635 1.0219 0.050 Uiso 1 1 calc R . . C18 C 0.0470(3) 0.0095(3) 0.9130(3) 0.0428(12) Uani 1 1 d . . . H18A H 0.0205 -0.0404 0.9353 0.051 Uiso 1 1 calc R . . C19 C 0.0159(3) 0.0366(3) 0.8297(3) 0.0442(12) Uani 1 1 d . . . H19A H -0.0370 0.0098 0.7822 0.053 Uiso 1 1 calc R . . C20 C 0.0675(4) 0.1108(3) 0.8262(3) 0.0398(11) Uani 1 1 d . . . H20A H 0.0586 0.1449 0.7749 0.048 Uiso 1 1 calc R . . C21 C 0.1303(3) 0.1306(2) 0.9061(3) 0.0371(11) Uani 1 1 d . . . C22 C 0.1967(4) 0.2046(3) 0.9311(3) 0.0600(15) Uani 1 1 d . . . H22A H 0.1556 0.2449 0.9532 0.090 Uiso 1 1 calc R . . H22B H 0.2162 0.2268 0.8821 0.090 Uiso 1 1 calc R . . H22C H 0.2619 0.1907 0.9745 0.090 Uiso 1 1 calc R . . C23 C 0.1803(3) -0.0964(3) 0.8593(3) 0.0366(11) Uani 1 1 d . . . C24 C 0.1829(4) -0.2512(2) 0.8569(3) 0.0377(11) Uani 1 1 d . . . C25 C 0.0982(4) -0.2947(3) 0.8753(3) 0.0437(12) Uani 1 1 d . . . C26 C 0.1067(4) -0.3776(3) 0.8749(3) 0.0526(14) Uani 1 1 d . . . H26A H 0.0523 -0.4093 0.8883 0.063 Uiso 1 1 calc R . . C27 C 0.1923(5) -0.4162(3) 0.8554(3) 0.0590(15) Uani 1 1 d . . . H27A H 0.1954 -0.4735 0.8549 0.071 Uiso 1 1 calc R . . C28 C 0.2730(5) -0.3712(3) 0.8368(3) 0.0598(15) Uani 1 1 d . . . H28A H 0.3313 -0.3980 0.8232 0.072 Uiso 1 1 calc R . . C29 C 0.2701(4) -0.2876(3) 0.8375(3) 0.0471(13) Uani 1 1 d . . . C30 C 0.3589(4) -0.2367(3) 0.8193(3) 0.0624(15) Uani 1 1 d . . . H30A H 0.4192 -0.2716 0.8166 0.094 Uiso 1 1 calc R . . H30B H 0.3830 -0.1966 0.8640 0.094 Uiso 1 1 calc R . . H30C H 0.3321 -0.2090 0.7654 0.094 Uiso 1 1 calc R . . C31 C 0.0041(4) -0.2520(3) 0.8928(3) 0.0559(14) Uani 1 1 d . . . H31A H -0.0484 -0.2919 0.9007 0.084 Uiso 1 1 calc R . . H31B H -0.0290 -0.2169 0.8453 0.084 Uiso 1 1 calc R . . H31C H 0.0283 -0.2193 0.9437 0.084 Uiso 1 1 calc R . . P1 P 0.29256(13) -0.62252(8) 0.73010(8) 0.0547(4) Uani 1 1 d . . . F5 F 0.2651(8) -0.6518(4) 0.6399(3) 0.257(4) Uani 1 1 d . A . F6 F 0.3223(4) -0.5936(3) 0.8213(2) 0.160(2) Uani 1 1 d . A . F1 F 0.3472(10) -0.5382(4) 0.7255(5) 0.129(4) Uani 0.569(10) 1 d P A 1 F2 F 0.2489(7) -0.7062(5) 0.7299(9) 0.121(5) Uani 0.569(10) 1 d P A 1 F3 F 0.4110(6) -0.6621(7) 0.7532(5) 0.092(3) Uani 0.569(10) 1 d P A 1 F4 F 0.1840(7) -0.5864(6) 0.6980(8) 0.140(6) Uani 0.569(10) 1 d P A 1 F1' F 0.2328(13) -0.5427(6) 0.6932(6) 0.093(6) Uani 0.431(10) 1 d P A 2 F2' F 0.3288(19) -0.7035(8) 0.7718(8) 0.152(8) Uani 0.431(10) 1 d P A 2 F3' F 0.3771(13) -0.6095(11) 0.6922(14) 0.173(8) Uani 0.431(10) 1 d P A 2 F4' F 0.1869(9) -0.6337(7) 0.7708(7) 0.118(5) Uani 0.431(10) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0311(4) 0.0314(4) 0.0287(4) 0.0014(3) 0.0140(3) 0.0004(3) Mn2 0.0310(4) 0.0382(4) 0.0300(4) 0.0017(3) 0.0148(3) 0.0012(3) C1 0.029(2) 0.032(3) 0.028(2) 0.0047(19) 0.019(2) -0.0016(19) N2 0.037(2) 0.036(2) 0.037(2) -0.0029(17) 0.016(2) 0.0000(18) N3 0.039(2) 0.047(2) 0.044(2) 0.0090(19) 0.016(2) 0.000(2) N4 0.039(2) 0.033(2) 0.032(2) -0.0011(18) 0.0073(19) 0.0010(19) N5 0.046(3) 0.042(3) 0.031(2) 0.0007(19) 0.0091(19) 0.005(2) O1 0.045(2) 0.067(2) 0.060(2) 0.0086(18) 0.002(2) 0.0117(18) O2 0.034(2) 0.098(3) 0.078(3) 0.024(2) 0.004(2) -0.012(2) N1 0.040(2) 0.040(2) 0.045(2) -0.0014(19) 0.016(2) -0.0018(18) C2 0.037(3) 0.044(3) 0.035(3) 0.001(2) 0.014(2) -0.014(2) C3 0.026(2) 0.036(3) 0.056(3) 0.008(2) 0.016(2) -0.002(2) C4 0.033(3) 0.046(3) 0.042(3) -0.001(2) 0.023(2) -0.004(2) C5 0.047(3) 0.039(3) 0.033(3) 0.006(2) 0.021(2) -0.002(2) C6 0.046(3) 0.028(2) 0.043(3) 0.002(2) 0.021(3) -0.004(2) C7 0.063(4) 0.074(4) 0.043(3) -0.002(3) 0.013(3) -0.023(3) C8 0.039(3) 0.038(3) 0.023(2) 0.001(2) 0.011(2) -0.002(2) C9 0.037(3) 0.032(3) 0.019(2) -0.0010(19) 0.002(2) -0.003(2) C10 0.035(3) 0.037(3) 0.033(3) 0.001(2) 0.006(2) -0.005(2) C11 0.043(3) 0.047(3) 0.048(3) 0.005(2) 0.010(3) -0.016(3) C12 0.066(4) 0.024(3) 0.041(3) 0.001(2) -0.001(3) -0.003(3) C13 0.051(3) 0.039(3) 0.030(3) -0.008(2) 0.003(2) 0.011(2) C14 0.035(3) 0.033(3) 0.027(2) 0.0006(19) 0.005(2) 0.001(2) C15 0.047(3) 0.055(3) 0.050(3) -0.005(2) 0.023(3) -0.005(3) C16 0.048(3) 0.060(3) 0.059(3) -0.003(3) 0.027(3) -0.003(3) C17 0.049(3) 0.048(3) 0.036(3) -0.003(2) 0.024(3) 0.009(2) C18 0.043(3) 0.041(3) 0.057(3) -0.006(2) 0.036(3) -0.002(2) C19 0.027(3) 0.053(3) 0.050(3) -0.019(3) 0.007(2) 0.002(2) C20 0.043(3) 0.043(3) 0.036(3) 0.004(2) 0.015(2) 0.013(2) C21 0.037(3) 0.035(3) 0.040(3) -0.005(2) 0.013(2) 0.001(2) C22 0.065(4) 0.052(3) 0.068(4) -0.013(3) 0.026(3) -0.007(3) C23 0.039(3) 0.044(3) 0.032(3) 0.003(2) 0.018(2) 0.001(2) C24 0.050(3) 0.031(3) 0.027(3) 0.001(2) 0.001(2) 0.008(2) C25 0.056(3) 0.042(3) 0.028(3) 0.000(2) 0.002(3) 0.003(3) C26 0.068(4) 0.051(3) 0.030(3) 0.004(2) -0.001(3) -0.007(3) C27 0.091(5) 0.038(3) 0.036(3) -0.004(2) -0.005(3) 0.008(3) C28 0.080(4) 0.051(4) 0.043(3) -0.009(3) 0.008(3) 0.024(3) C29 0.057(4) 0.048(3) 0.032(3) 0.000(2) 0.004(3) 0.011(3) C30 0.057(4) 0.073(4) 0.057(4) -0.008(3) 0.017(3) 0.017(3) C31 0.055(4) 0.064(3) 0.050(3) 0.005(3) 0.015(3) 0.001(3) P1 0.0742(12) 0.0422(9) 0.0400(8) -0.0024(7) 0.0010(8) 0.0049(8) F5 0.427(11) 0.207(6) 0.064(3) -0.062(4) -0.065(5) 0.179(7) F6 0.206(5) 0.199(5) 0.058(3) -0.024(3) 0.007(3) 0.082(4) F1 0.169(10) 0.063(5) 0.124(7) 0.030(4) -0.013(7) -0.033(6) F2 0.080(6) 0.061(5) 0.221(15) 0.001(7) 0.034(7) -0.020(5) F3 0.069(5) 0.115(8) 0.095(6) 0.015(5) 0.026(4) 0.018(5) F4 0.062(6) 0.108(9) 0.218(14) -0.032(9) -0.019(7) 0.054(6) F1' 0.160(16) 0.058(7) 0.056(6) 0.024(5) 0.018(8) 0.030(7) F2' 0.25(2) 0.079(9) 0.108(9) 0.027(7) 0.005(14) 0.089(13) F3' 0.136(13) 0.188(17) 0.27(2) -0.031(15) 0.183(16) -0.027(12) F4' 0.142(10) 0.145(11) 0.095(8) 0.006(6) 0.080(8) -0.061(8) _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 N2 1.637(4) . ? Mn1 C8 1.905(4) . ? Mn1 N1 1.970(4) . ? Mn1 C5 2.094(4) . ? Mn1 C4 2.096(4) . ? Mn1 C6 2.152(4) . ? Mn1 C3 2.153(4) . ? Mn1 C2 2.213(4) . ? Mn2 N3 1.638(4) . ? Mn2 C23 1.886(5) . ? Mn2 C1 1.926(4) . ? Mn2 C19 2.115(4) . ? Mn2 C18 2.123(4) . ? Mn2 C20 2.132(4) . ? Mn2 C17 2.135(4) . ? Mn2 C21 2.167(4) . ? C1 N1 1.156(4) . ? N2 O1 1.191(4) . ? N3 O2 1.186(4) . ? N4 C8 1.150(4) . ? N4 C9 1.409(5) . ? N5 C23 1.165(5) . ? N5 C24 1.399(5) . ? C2 C6 1.404(6) . ? C2 C3 1.406(5) . ? C2 C7 1.499(6) . ? C3 C4 1.425(6) . ? C4 C5 1.402(5) . ? C5 C6 1.415(5) . ? C9 C14 1.385(5) . ? C9 C10 1.394(5) . ? C10 C11 1.386(5) . ? C10 C16 1.507(5) . ? C11 C12 1.383(6) . ? C12 C13 1.378(6) . ? C13 C14 1.377(5) . ? C14 C15 1.504(5) . ? C17 C18 1.399(6) . ? C17 C21 1.424(5) . ? C18 C19 1.402(6) . ? C19 C20 1.405(5) . ? C20 C21 1.395(6) . ? C21 C22 1.489(6) . ? C24 C29 1.387(6) . ? C24 C25 1.408(6) . ? C25 C26 1.376(6) . ? C25 C31 1.499(6) . ? C26 C27 1.386(6) . ? C27 C28 1.380(7) . ? C28 C29 1.386(6) . ? C29 C30 1.517(6) . ? P1 F3' 1.410(9) . ? P1 F4 1.489(8) . ? P1 F2 1.496(8) . ? P1 F5 1.518(4) . ? P1 F2' 1.523(10) . ? P1 F6 1.530(4) . ? P1 F1' 1.571(10) . ? P1 F1 1.574(7) . ? P1 F3 1.617(7) . ? P1 F4' 1.683(9) . ? F5 F3' 1.637(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 N2 Mn1 C8 99.33(17) . . ? N2 Mn1 N1 99.38(15) . . ? C8 Mn1 N1 88.34(15) . . ? N2 Mn1 C5 91.96(17) . . ? C8 Mn1 C5 127.35(17) . . ? N1 Mn1 C5 140.27(15) . . ? N2 Mn1 C4 114.76(16) . . ? C8 Mn1 C4 90.98(17) . . ? N1 Mn1 C4 145.47(16) . . ? C5 Mn1 C4 39.10(14) . . ? N2 Mn1 C6 106.70(16) . . ? C8 Mn1 C6 150.03(18) . . ? N1 Mn1 C6 101.56(15) . . ? C5 Mn1 C6 38.90(14) . . ? C4 Mn1 C6 64.89(16) . . ? N2 Mn1 C3 153.73(16) . . ? C8 Mn1 C3 86.63(17) . . ? N1 Mn1 C3 106.39(15) . . ? C5 Mn1 C3 64.84(16) . . ? C4 Mn1 C3 39.17(15) . . ? C6 Mn1 C3 63.48(16) . . ? N2 Mn1 C2 143.32(16) . . ? C8 Mn1 C2 117.22(18) . . ? N1 Mn1 C2 85.42(14) . . ? C5 Mn1 C2 64.16(16) . . ? C4 Mn1 C2 64.39(16) . . ? C6 Mn1 C2 37.48(15) . . ? C3 Mn1 C2 37.53(14) . . ? N3 Mn2 C23 97.72(18) . . ? N3 Mn2 C1 97.47(17) . . ? C23 Mn2 C1 90.29(17) . . ? N3 Mn2 C19 159.27(17) . . ? C23 Mn2 C19 97.38(18) . . ? C1 Mn2 C19 96.58(17) . . ? N3 Mn2 C18 128.54(18) . . ? C23 Mn2 C18 86.89(18) . . ? C1 Mn2 C18 133.88(18) . . ? C19 Mn2 C18 38.64(16) . . ? N3 Mn2 C20 127.40(18) . . ? C23 Mn2 C20 134.80(19) . . ? C1 Mn2 C20 86.67(16) . . ? C19 Mn2 C20 38.64(15) . . ? C18 Mn2 C20 64.36(17) . . ? N3 Mn2 C17 96.38(18) . . ? C23 Mn2 C17 113.94(17) . . ? C1 Mn2 C17 150.06(17) . . ? C19 Mn2 C17 64.39(17) . . ? C18 Mn2 C17 38.35(15) . . ? C20 Mn2 C17 63.91(16) . . ? N3 Mn2 C21 95.85(17) . . ? C23 Mn2 C21 150.88(17) . . ? C1 Mn2 C21 113.33(17) . . ? C19 Mn2 C21 64.49(16) . . ? C18 Mn2 C21 64.60(16) . . ? C20 Mn2 C21 37.87(15) . . ? C17 Mn2 C21 38.65(15) . . ? N1 C1 Mn2 175.7(4) . . ? O1 N2 Mn1 173.2(3) . . ? O2 N3 Mn2 172.6(4) . . ? C8 N4 C9 177.0(4) . . ? C23 N5 C24 176.5(5) . . ? C1 N1 Mn1 175.1(3) . . ? C6 C2 C3 107.5(4) . . ? C6 C2 C7 126.1(4) . . ? C3 C2 C7 126.5(4) . . ? C6 C2 Mn1 68.9(2) . . ? C3 C2 Mn1 68.9(2) . . ? C7 C2 Mn1 128.0(3) . . ? C2 C3 C4 108.5(4) . . ? C2 C3 Mn1 73.5(2) . . ? C4 C3 Mn1 68.2(2) . . ? C5 C4 C3 107.3(4) . . ? C5 C4 Mn1 70.4(2) . . ? C3 C4 Mn1 72.6(2) . . ? C4 C5 C6 108.0(4) . . ? C4 C5 Mn1 70.5(2) . . ? C6 C5 Mn1 72.8(2) . . ? C2 C6 C5 108.6(4) . . ? C2 C6 Mn1 73.6(2) . . ? C5 C6 Mn1 68.3(2) . . ? N4 C8 Mn1 177.3(4) . . ? C14 C9 C10 124.8(4) . . ? C14 C9 N4 118.0(4) . . ? C10 C9 N4 117.2(4) . . ? C11 C10 C9 116.0(4) . . ? C11 C10 C16 123.2(4) . . ? C9 C10 C16 120.8(4) . . ? C12 C11 C10 121.3(4) . . ? C13 C12 C11 119.9(4) . . ? C14 C13 C12 121.9(4) . . ? C13 C14 C9 116.1(4) . . ? C13 C14 C15 121.7(4) . . ? C9 C14 C15 122.2(4) . . ? C18 C17 C21 108.6(4) . . ? C18 C17 Mn2 70.3(2) . . ? C21 C17 Mn2 71.9(2) . . ? C17 C18 C19 107.9(4) . . ? C17 C18 Mn2 71.3(2) . . ? C19 C18 Mn2 70.4(2) . . ? C18 C19 C20 107.6(4) . . ? C18 C19 Mn2 71.0(3) . . ? C20 C19 Mn2 71.3(2) . . ? C21 C20 C19 109.4(4) . . ? C21 C20 Mn2 72.4(3) . . ? C19 C20 Mn2 70.0(2) . . ? C20 C21 C17 106.4(4) . . ? C20 C21 C22 127.3(4) . . ? C17 C21 C22 126.3(4) . . ? C20 C21 Mn2 69.7(2) . . ? C17 C21 Mn2 69.5(2) . . ? C22 C21 Mn2 126.2(3) . . ? N5 C23 Mn2 178.3(4) . . ? C29 C24 N5 118.4(4) . . ? C29 C24 C25 123.5(4) . . ? N5 C24 C25 118.1(4) . . ? C26 C25 C24 116.2(5) . . ? C26 C25 C31 122.8(5) . . ? C24 C25 C31 121.1(4) . . ? C25 C26 C27 122.0(5) . . ? C28 C27 C26 119.9(5) . . ? C27 C28 C29 120.9(5) . . ? C28 C29 C24 117.5(5) . . ? C28 C29 C30 122.0(5) . . ? C24 C29 C30 120.6(4) . . ? F3' P1 F4 123.2(11) . . ? F3' P1 F2 118.5(7) . . ? F4 P1 F2 92.9(6) . . ? F3' P1 F5 67.9(7) . . ? F4 P1 F5 79.8(5) . . ? F2 P1 F5 73.2(6) . . ? F3' P1 F2' 98.8(9) . . ? F4 P1 F2' 131.6(10) . . ? F2 P1 F2' 42.1(7) . . ? F5 P1 F2' 97.3(5) . . ? F3' P1 F6 111.3(9) . . ? F4 P1 F6 101.3(5) . . ? F2 P1 F6 106.8(6) . . ? F5 P1 F6 179.0(4) . . ? F2' P1 F6 82.1(5) . . ? F3' P1 F1' 93.3(9) . . ? F4 P1 F1' 37.1(5) . . ? F2 P1 F1' 129.2(7) . . ? F5 P1 F1' 85.6(4) . . ? F2' P1 F1' 167.8(10) . . ? F6 P1 F1' 95.2(4) . . ? F3' P1 F1 55.5(6) . . ? F4 P1 F1 91.1(5) . . ? F2 P1 F1 174.0(6) . . ? F5 P1 F1 103.2(5) . . ? F2' P1 F1 135.4(9) . . ? F6 P1 F1 76.7(4) . . ? F1' P1 F1 54.3(5) . . ? F3' P1 F3 51.0(8) . . ? F4 P1 F3 173.0(6) . . ? F2 P1 F3 87.7(4) . . ? F5 P1 F3 93.8(4) . . ? F2' P1 F3 51.4(7) . . ? F6 P1 F3 85.2(3) . . ? F1' P1 F3 140.5(7) . . ? F1 P1 F3 87.8(5) . . ? F3' P1 F4' 176.2(10) . . ? F4 P1 F4' 53.0(5) . . ? F2 P1 F4' 63.5(5) . . ? F5 P1 F4' 110.5(6) . . ? F2' P1 F4' 84.8(9) . . ? F6 P1 F4' 70.3(4) . . ? F1' P1 F4' 83.1(5) . . ? F1 P1 F4' 122.5(6) . . ? F3 P1 F4' 132.8(6) . . ? P1 F5 F3' 52.9(4) . . ? P1 F3' F5 59.2(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.424 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.070 #===END data_31 _database_code_depnum_ccdc_archive 'CCDC 223107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H74 F12 Mn5 N12 O5 P2' _chemical_formula_weight 1511.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.4219(4) _cell_length_b 14.5958(6) _cell_length_c 25.8306(11) _cell_angle_alpha 86.9700(10) _cell_angle_beta 82.8850(10) _cell_angle_gamma 76.2980(10) _cell_volume 3423.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 156 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1546 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.772953 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29916 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12028 _reflns_number_gt 7133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+1.5733P] 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 12028 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 0.35105(9) -1.28898(6) 0.25402(3) 0.0395(2) Uani 1 1 d . . . Mn2 Mn 0.13543(12) -1.33785(9) 0.44543(4) 0.0643(3) Uani 1 1 d . . . Mn3 Mn 0.29965(10) -1.50650(6) 0.10997(4) 0.0511(3) Uani 1 1 d . . . Mn4 Mn 0.82370(10) -1.51351(6) 0.31405(4) 0.0459(3) Uani 1 1 d . . . Mn5 Mn 0.52353(10) -1.00577(5) 0.16302(3) 0.0408(2) Uani 1 1 d . . . O1 O 0.1209(5) -1.1914(3) 0.2455(2) 0.0744(14) Uani 1 1 d . . . O201 O 0.0565(6) -1.5124(4) 0.4409(2) 0.0862(17) Uani 1 1 d . . . O301 O 0.4016(6) -1.4040(4) 0.0231(2) 0.0804(15) Uani 1 1 d . . . O401 O 0.7846(10) -1.4049(5) 0.4034(3) 0.148(3) Uani 1 1 d . . . O501 O 0.8116(5) -1.0901(3) 0.1210(2) 0.0702(14) Uani 1 1 d . . . N2 N 0.2557(6) -1.3160(4) 0.3300(2) 0.0585(14) Uani 1 1 d . . . N3 N 0.3071(6) -1.3690(4) 0.1949(2) 0.0540(13) Uani 1 1 d . . . N4 N 0.5623(6) -1.3806(4) 0.2671(2) 0.0515(13) Uani 1 1 d . . . N5 N 0.4381(5) -1.1735(3) 0.22667(19) 0.0482(12) Uani 1 1 d . . . N201 N 0.0860(6) -1.4386(5) 0.4414(2) 0.0676(17) Uani 1 1 d . . . N202 N -0.1581(7) -1.2027(5) 0.4297(2) 0.0690(16) Uani 1 1 d . . . N301 N 0.3573(6) -1.4446(4) 0.0595(2) 0.0546(13) Uani 1 1 d . . . N302 N -0.0256(6) -1.4233(3) 0.0982(2) 0.0513(13) Uani 1 1 d . . . N401 N 0.7999(7) -1.4505(4) 0.3660(3) 0.0768(18) Uani 1 1 d . . . N402 N 0.6112(6) -1.6368(4) 0.3537(2) 0.0569(14) Uani 1 1 d . . . N501 N 0.6916(6) -1.0590(3) 0.13826(19) 0.0455(12) Uani 1 1 d . . . N502 N 0.3635(6) -1.0564(4) 0.07654(19) 0.0498(13) Uani 1 1 d . . . C2 C 0.2076(7) -1.3238(5) 0.3722(3) 0.0561(16) Uani 1 1 d . . . C3 C 0.3003(6) -1.4190(4) 0.1634(3) 0.0467(15) Uani 1 1 d . . . C4 C 0.6624(7) -1.4315(4) 0.2824(2) 0.0437(14) Uani 1 1 d . . . C5 C 0.4726(7) -1.1117(4) 0.2031(2) 0.0444(14) Uani 1 1 d . . . C6 C -0.1195(12) -1.2223(7) 0.2408(6) 0.140(5) Uani 1 1 d . . . H6A H -0.1293 -1.2585 0.2111 0.210 Uiso 1 1 calc R . . H6B H -0.1732 -1.1566 0.2365 0.210 Uiso 1 1 calc R . . H6C H -0.1601 -1.2494 0.2732 0.210 Uiso 1 1 calc R . . C7 C 0.0005(12) -1.2249(11) 0.2426(11) 0.354(19) Uani 1 1 d . . . H7A H 0.0396 -1.2638 0.2114 0.424 Uiso 1 1 calc R . . H7B H 0.0148 -1.2712 0.2720 0.424 Uiso 1 1 calc R . . C8 C 0.0836(11) -1.0947(7) 0.2673(5) 0.118(4) Uani 1 1 d . . . H8A H -0.0006 -1.0890 0.2949 0.142 Uiso 1 1 calc R . . H8B H 0.1686 -1.0842 0.2832 0.142 Uiso 1 1 calc R . . C9 C 0.0479(14) -1.0267(10) 0.2281(8) 0.216(9) Uani 1 1 d . . . H9A H -0.0102 -0.9679 0.2438 0.324 Uiso 1 1 calc R . . H9B H -0.0095 -1.0490 0.2044 0.324 Uiso 1 1 calc R . . H9C H 0.1384 -1.0153 0.2085 0.324 Uiso 1 1 calc R . . C201 C 0.470(2) -1.3940(9) 0.4461(6) 0.229(10) Uani 1 1 d . . . H20A H 0.5512 -1.3836 0.4637 0.344 Uiso 1 1 calc R . . H20B H 0.4849 -1.3756 0.4091 0.344 Uiso 1 1 calc R . . H20C H 0.4681 -1.4608 0.4492 0.344 Uiso 1 1 calc R . . C202 C 0.3419(6) -1.3416(6) 0.4683(2) 0.094(3) Uani 1 1 d G . . C203 C 0.2769(9) -1.2440(5) 0.4622(2) 0.117(4) Uani 1 1 d G . . H20D H 0.3151 -1.1988 0.4369 0.140 Uiso 1 1 calc R . . C204 C 0.1484(8) -1.2216(4) 0.4986(3) 0.171(7) Uani 1 1 d G . . H20E H 0.0779 -1.1586 0.5023 0.206 Uiso 1 1 calc R . . C205 C 0.1339(7) -1.3054(6) 0.5271(2) 0.093(3) Uani 1 1 d G . . H20F H 0.0552 -1.3108 0.5560 0.112 Uiso 1 1 calc R . . C206 C 0.2536(9) -1.3796(4) 0.5084(3) 0.107(3) Uani 1 1 d G . . H20G H 0.2782 -1.4449 0.5238 0.129 Uiso 1 1 calc R . . C207 C -0.0480(9) -1.2529(5) 0.4347(3) 0.0635(18) Uani 1 1 d . . . C208 C -0.2995(9) -1.1343(5) 0.4258(3) 0.074(2) Uani 1 1 d . . . C209 C -0.3644(9) -1.1625(7) 0.3796(3) 0.096(3) Uani 1 1 d . . . H20H H -0.2989 -1.1577 0.3476 0.144 Uiso 1 1 calc R . . H20I H -0.4610 -1.1204 0.3767 0.144 Uiso 1 1 calc R . . H20J H -0.3750 -1.2277 0.3850 0.144 Uiso 1 1 calc R . . C210 C -0.3981(9) -1.1446(6) 0.4760(3) 0.081(2) Uani 1 1 d . . . H21D H -0.3472 -1.1385 0.5060 0.121 Uiso 1 1 calc R . . H21E H -0.4215 -1.2067 0.4775 0.121 Uiso 1 1 calc R . . H21F H -0.4892 -1.0953 0.4768 0.121 Uiso 1 1 calc R . . C211 C -0.2683(11) -1.0390(6) 0.4196(4) 0.118(4) Uani 1 1 d . . . H21A H -0.2136 -1.0291 0.4479 0.176 Uiso 1 1 calc R . . H21B H -0.3611 -0.9911 0.4209 0.176 Uiso 1 1 calc R . . H21C H -0.2095 -1.0339 0.3860 0.176 Uiso 1 1 calc R . . C301 C 0.5419(12) -1.5948(6) 0.1925(3) 0.120(4) Uani 1 1 d . . . H30C H 0.6005 -1.6556 0.2039 0.180 Uiso 1 1 calc R . . H30D H 0.4842 -1.5613 0.2229 0.180 Uiso 1 1 calc R . . H30E H 0.6075 -1.5569 0.1749 0.180 Uiso 1 1 calc R . . C302 C 0.4396(7) -1.6110(4) 0.1552(2) 0.0522(16) Uani 1 1 d . . . C304 C 0.2510(16) -1.6398(8) 0.1192(11) 0.208(13) Uani 1 1 d . . . H30F H 0.1532 -1.6525 0.1152 0.249 Uiso 1 1 calc R . . C305 C 0.2932(11) -1.6198(6) 0.1658(6) 0.134(6) Uani 1 1 d . . . H30A H 0.2332 -1.6158 0.2007 0.161 Uiso 1 1 calc R . . C303 C 0.3620(17) -1.6444(6) 0.0801(5) 0.144(7) Uani 1 1 d . . . H30J H 0.3613 -1.6619 0.0432 0.172 Uiso 1 1 calc R . . C306 C 0.4805(8) -1.6267(4) 0.1016(2) 0.0557(17) Uani 1 1 d . . . H30B H 0.5797 -1.6275 0.0824 0.067 Uiso 1 1 calc R . . C307 C 0.0951(7) -1.4546(4) 0.1044(3) 0.0507(16) Uani 1 1 d . . . C308 C -0.1751(6) -1.3862(5) 0.0845(2) 0.0516(16) Uani 1 1 d . . . C309 C -0.1728(11) -1.2965(6) 0.0532(5) 0.119(4) Uani 1 1 d . . . H30G H -0.1313 -1.2551 0.0725 0.179 Uiso 1 1 calc R . . H30H H -0.2733 -1.2646 0.0470 0.179 Uiso 1 1 calc R . . H30I H -0.1123 -1.3115 0.0197 0.179 Uiso 1 1 calc R . . C310 C -0.2118(11) -1.4554(7) 0.0514(5) 0.141(5) Uani 1 1 d . . . H31D H -0.1911 -1.5179 0.0685 0.212 Uiso 1 1 calc R . . H31E H -0.1523 -1.4576 0.0174 0.212 Uiso 1 1 calc R . . H31F H -0.3163 -1.4364 0.0465 0.212 Uiso 1 1 calc R . . C311 C -0.2745(10) -1.3661(13) 0.1329(4) 0.205(9) Uani 1 1 d . . . H31A H -0.2804 -1.4255 0.1517 0.308 Uiso 1 1 calc R . . H31B H -0.3726 -1.3330 0.1247 0.308 Uiso 1 1 calc R . . H31C H -0.2370 -1.3265 0.1548 0.308 Uiso 1 1 calc R . . C401 C 0.9371(10) -1.7396(5) 0.2779(4) 0.094(3) Uani 1 1 d . . . H40H H 1.0199 -1.7817 0.2578 0.141 Uiso 1 1 calc R . . H40I H 0.8467 -1.7367 0.2621 0.141 Uiso 1 1 calc R . . H40J H 0.9262 -1.7638 0.3139 0.141 Uiso 1 1 calc R . . C402 C 0.9656(7) -1.6422(5) 0.2776(3) 0.0614(18) Uani 1 1 d . . . C403 C 1.0383(7) -1.6070(5) 0.3129(3) 0.070(2) Uani 1 1 d . . . H40B H 1.0815 -1.6422 0.3437 0.084 Uiso 1 1 calc R . . C404 C 1.0487(8) -1.5148(6) 0.2957(3) 0.081(2) Uani 1 1 d . . . H40A H 1.1031 -1.4745 0.3116 0.097 Uiso 1 1 calc R . . C405 C 0.9755(8) -1.4917(6) 0.2503(3) 0.071(2) Uani 1 1 d . . . H40C H 0.9700 -1.4327 0.2284 0.085 Uiso 1 1 calc R . . C406 C 0.9238(7) -1.5711(5) 0.2393(3) 0.0638(19) Uani 1 1 d . . . H40G H 0.8706 -1.5770 0.2089 0.077 Uiso 1 1 calc R . . C407 C 0.6911(7) -1.5904(4) 0.3393(2) 0.0490(15) Uani 1 1 d . . . C408 C 0.5086(8) -1.6971(5) 0.3706(3) 0.0624(18) Uani 1 1 d . . . C409 C 0.4400(9) -1.7124(6) 0.3217(3) 0.091(3) Uani 1 1 d . . . H40D H 0.3894 -1.6513 0.3077 0.137 Uiso 1 1 calc R . . H40E H 0.3693 -1.7518 0.3310 0.137 Uiso 1 1 calc R . . H40F H 0.5175 -1.7439 0.2953 0.137 Uiso 1 1 calc R . . C410 C 0.5961(9) -1.7894(5) 0.3919(3) 0.077(2) Uani 1 1 d . . . H41D H 0.6380 -1.7773 0.4231 0.115 Uiso 1 1 calc R . . H41E H 0.6757 -1.8178 0.3653 0.115 Uiso 1 1 calc R . . H41F H 0.5312 -1.8326 0.4011 0.115 Uiso 1 1 calc R . . C411 C 0.3948(10) -1.6448(6) 0.4121(4) 0.098(3) Uani 1 1 d . . . H41A H 0.4433 -1.6347 0.4420 0.147 Uiso 1 1 calc R . . H41B H 0.3222 -1.6822 0.4233 0.147 Uiso 1 1 calc R . . H41C H 0.3453 -1.5837 0.3978 0.147 Uiso 1 1 calc R . . C501 C 0.5932(19) -0.9679(10) 0.2778(5) 0.242(11) Uani 1 1 d . . . H50H H 0.5244 -0.9455 0.3086 0.363 Uiso 1 1 calc R . . H50I H 0.6847 -0.9476 0.2790 0.363 Uiso 1 1 calc R . . H50J H 0.6145 -1.0369 0.2774 0.363 Uiso 1 1 calc R . . C502 C 0.5258(12) -0.9276(6) 0.2293(3) 0.081(3) Uani 1 1 d . . . C503 C 0.6013(12) -0.8941(5) 0.1924(5) 0.092(3) Uani 1 1 d . . . H50B H 0.7075 -0.8938 0.1921 0.110 Uiso 1 1 calc R . . C504 C 0.5210(10) -0.8601(4) 0.1535(3) 0.066(2) Uani 1 1 d . . . H50C H 0.5582 -0.8298 0.1206 0.080 Uiso 1 1 calc R . . C505 C 0.3752(10) -0.8694(4) 0.1660(4) 0.085(3) Uani 1 1 d . . . H50A H 0.2883 -0.8447 0.1465 0.103 Uiso 1 1 calc R . . C506 C 0.3805(10) -0.9149(5) 0.2193(4) 0.085(3) Uani 1 1 d . . . H50D H 0.2964 -0.9290 0.2434 0.102 Uiso 1 1 calc R . . C507 C 0.4214(6) -1.0351(4) 0.1090(2) 0.0426(14) Uani 1 1 d . . . C508 C 0.2892(7) -1.0888(4) 0.0372(2) 0.0535(16) Uani 1 1 d . . . C509 C 0.2407(9) -1.0061(6) -0.0007(3) 0.083(2) Uani 1 1 d . . . H50E H 0.1670 -0.9561 0.0179 0.124 Uiso 1 1 calc R . . H50F H 0.1982 -1.0278 -0.0292 0.124 Uiso 1 1 calc R . . H50G H 0.3260 -0.9816 -0.0150 0.124 Uiso 1 1 calc R . . C510 C 0.1578(10) -1.1194(9) 0.0654(4) 0.129(4) Uani 1 1 d . . . H51A H 0.1900 -1.1672 0.0923 0.194 Uiso 1 1 calc R . . H51B H 0.1090 -1.1460 0.0405 0.194 Uiso 1 1 calc R . . H51C H 0.0888 -1.0648 0.0819 0.194 Uiso 1 1 calc R . . C511 C 0.3988(9) -1.1669(5) 0.0080(3) 0.085(3) Uani 1 1 d . . . H51D H 0.4393 -1.2165 0.0328 0.128 Uiso 1 1 calc R . . H51E H 0.4785 -1.1416 -0.0109 0.128 Uiso 1 1 calc R . . H51F H 0.3497 -1.1933 -0.0169 0.128 Uiso 1 1 calc R . . P1 P 1.1831(3) -1.9228(2) 0.39160(10) 0.0946(8) Uani 1 1 d . . . P2 P 0.0631(2) -1.22442(13) -0.10233(10) 0.0743(6) Uani 1 1 d . . . F1 F 1.2104(11) -2.0282(5) 0.3770(4) 0.205(4) Uani 1 1 d . . . F2 F 1.1508(8) -1.9439(6) 0.4518(2) 0.160(3) Uani 1 1 d . . . F3 F 1.0148(6) -1.9030(6) 0.3876(3) 0.158(3) Uani 1 1 d . . . F4 F 1.2118(7) -1.8934(7) 0.3336(2) 0.174(3) Uani 1 1 d . . . F5 F 1.1654(7) -1.8159(5) 0.4071(3) 0.148(2) Uani 1 1 d . . . F6 F 1.3514(6) -1.9390(5) 0.3969(3) 0.149(2) Uani 1 1 d . . . F7 F 0.127(2) -1.2321(14) -0.0551(6) 0.434(12) Uani 1 1 d . . . F8 F 0.2164(7) -1.2448(5) -0.1306(6) 0.284(8) Uani 1 1 d . . . F9 F -0.0101(10) -1.2206(9) -0.1503(3) 0.242(5) Uani 1 1 d . . . F10 F 0.0660(9) -1.1220(4) -0.1077(6) 0.255(6) Uani 1 1 d . . . F11 F 0.0672(8) -1.3282(4) -0.0987(5) 0.214(5) Uani 1 1 d . . . F12 F -0.0951(7) -1.2009(5) -0.0761(3) 0.150(3) Uani 1 1 d . . . 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 0.0392(5) 0.0380(5) 0.0393(5) 0.0075(4) -0.0020(4) -0.0082(4) Mn2 0.0559(7) 0.0952(8) 0.0407(5) 0.0120(5) -0.0021(5) -0.0199(6) Mn3 0.0393(5) 0.0317(5) 0.0837(7) -0.0046(5) -0.0194(5) -0.0038(4) Mn4 0.0444(6) 0.0417(5) 0.0511(5) 0.0066(4) -0.0127(4) -0.0070(4) Mn5 0.0535(6) 0.0293(4) 0.0400(5) 0.0040(4) -0.0084(4) -0.0103(4) O1 0.046(3) 0.060(3) 0.112(4) -0.006(3) -0.013(3) 0.002(2) O201 0.085(4) 0.078(4) 0.088(4) 0.020(3) 0.003(3) -0.016(3) O301 0.087(4) 0.064(3) 0.084(4) 0.005(3) -0.006(3) -0.010(3) O401 0.201(8) 0.106(5) 0.136(6) -0.063(5) -0.094(6) 0.016(5) O501 0.045(3) 0.078(3) 0.083(3) 0.013(3) -0.007(3) -0.008(3) N2 0.056(3) 0.069(4) 0.046(3) 0.010(3) 0.002(3) -0.013(3) N3 0.050(3) 0.043(3) 0.067(4) 0.000(3) -0.019(3) -0.001(2) N4 0.048(3) 0.050(3) 0.053(3) 0.010(3) -0.007(3) -0.006(3) N5 0.052(3) 0.037(3) 0.054(3) 0.009(2) -0.004(2) -0.010(2) N201 0.059(4) 0.085(4) 0.053(3) 0.023(3) 0.000(3) -0.013(3) N202 0.060(4) 0.073(4) 0.070(4) -0.005(3) 0.004(3) -0.013(3) N301 0.048(3) 0.042(3) 0.072(4) -0.005(3) -0.015(3) -0.003(2) N302 0.040(3) 0.050(3) 0.065(3) 0.008(3) -0.018(3) -0.008(2) N401 0.080(5) 0.059(4) 0.091(5) -0.014(4) -0.042(4) 0.004(3) N402 0.050(3) 0.041(3) 0.074(4) 0.016(3) -0.001(3) -0.006(3) N501 0.047(3) 0.039(3) 0.051(3) 0.003(2) -0.011(2) -0.009(2) N502 0.046(3) 0.055(3) 0.046(3) -0.001(3) -0.007(3) -0.006(2) C2 0.047(4) 0.066(4) 0.056(4) 0.009(3) -0.007(3) -0.016(3) C3 0.034(3) 0.033(3) 0.070(4) 0.003(3) -0.011(3) -0.001(3) C4 0.042(4) 0.041(3) 0.049(3) 0.006(3) -0.005(3) -0.013(3) C5 0.051(4) 0.035(3) 0.045(3) 0.001(3) -0.008(3) -0.003(3) C6 0.082(8) 0.090(7) 0.234(15) -0.004(8) -0.008(8) 0.004(6) C7 0.040(7) 0.179(14) 0.86(6) -0.26(2) -0.090(15) 0.024(8) C8 0.073(6) 0.103(8) 0.167(11) -0.006(8) -0.015(7) 0.004(6) C9 0.113(11) 0.164(13) 0.39(3) 0.079(16) -0.124(14) -0.050(9) C201 0.33(2) 0.146(12) 0.176(14) -0.085(11) -0.140(16) 0.082(14) C202 0.043(5) 0.158(9) 0.068(5) -0.050(6) -0.005(4) 0.009(5) C203 0.140(10) 0.100(7) 0.132(9) -0.008(7) -0.089(8) -0.032(7) C204 0.094(9) 0.35(2) 0.073(7) -0.069(11) -0.025(6) -0.046(11) C205 0.115(8) 0.118(8) 0.049(5) 0.022(5) -0.005(5) -0.038(6) C206 0.107(8) 0.154(9) 0.054(5) 0.009(6) -0.038(5) -0.003(7) C207 0.061(5) 0.077(5) 0.054(4) 0.002(4) 0.007(4) -0.026(4) C208 0.065(5) 0.067(5) 0.078(5) 0.006(4) 0.014(4) -0.003(4) C209 0.075(6) 0.112(7) 0.081(6) 0.010(5) -0.004(5) 0.010(5) C210 0.069(5) 0.095(6) 0.074(5) -0.012(4) 0.018(4) -0.020(4) C211 0.106(8) 0.069(6) 0.163(10) 0.016(6) 0.024(7) -0.016(5) C301 0.200(11) 0.064(5) 0.084(6) 0.002(5) -0.086(7) 0.027(6) C302 0.060(4) 0.030(3) 0.055(4) 0.007(3) 0.000(3) 0.006(3) C304 0.105(10) 0.031(5) 0.52(4) 0.020(12) -0.149(17) -0.022(6) C305 0.082(7) 0.040(5) 0.235(14) 0.055(7) 0.079(8) 0.012(5) C303 0.210(14) 0.038(5) 0.190(13) -0.046(7) -0.155(12) 0.034(8) C306 0.068(4) 0.035(3) 0.053(4) 0.001(3) -0.010(3) 0.009(3) C307 0.043(4) 0.037(3) 0.075(4) 0.000(3) -0.016(3) -0.010(3) C308 0.029(3) 0.065(4) 0.058(4) 0.016(3) -0.010(3) -0.006(3) C309 0.114(8) 0.077(6) 0.184(11) 0.052(7) -0.089(8) -0.030(5) C310 0.097(8) 0.101(7) 0.241(14) -0.037(8) -0.109(9) -0.001(6) C311 0.040(5) 0.46(3) 0.073(6) 0.048(11) 0.007(5) 0.002(9) C401 0.097(7) 0.057(5) 0.109(7) -0.008(5) 0.017(5) 0.005(4) C402 0.045(4) 0.059(4) 0.068(4) 0.002(4) 0.004(3) 0.006(3) C403 0.043(4) 0.078(5) 0.081(5) 0.021(4) -0.017(4) 0.004(4) C404 0.046(4) 0.098(6) 0.107(6) 0.004(5) -0.025(4) -0.025(4) C405 0.052(4) 0.084(5) 0.072(5) 0.027(4) -0.001(4) -0.016(4) C406 0.045(4) 0.086(5) 0.051(4) 0.007(4) -0.003(3) 0.001(4) C407 0.054(4) 0.035(3) 0.048(3) 0.000(3) 0.000(3) 0.007(3) C408 0.055(4) 0.056(4) 0.075(5) 0.012(4) 0.000(4) -0.016(3) C409 0.083(6) 0.097(6) 0.102(7) 0.025(5) -0.029(5) -0.036(5) C410 0.084(6) 0.054(4) 0.094(6) 0.026(4) -0.019(5) -0.022(4) C411 0.090(6) 0.084(6) 0.110(7) -0.005(5) 0.040(5) -0.028(5) C501 0.31(2) 0.190(14) 0.181(13) -0.118(11) -0.172(15) 0.125(14) C502 0.109(8) 0.054(5) 0.071(5) -0.028(4) -0.020(5) 0.008(5) C503 0.116(8) 0.039(4) 0.129(8) -0.015(5) -0.038(7) -0.022(5) C504 0.095(6) 0.028(3) 0.076(5) 0.005(3) -0.009(5) -0.016(4) C505 0.092(6) 0.030(3) 0.130(8) -0.029(4) -0.063(6) 0.026(4) C506 0.095(7) 0.032(4) 0.110(7) -0.025(4) 0.061(6) -0.013(4) C507 0.040(3) 0.040(3) 0.045(3) 0.004(3) -0.003(3) -0.008(3) C508 0.051(4) 0.058(4) 0.051(4) -0.010(3) -0.013(3) -0.006(3) C509 0.091(6) 0.089(6) 0.067(5) -0.006(4) -0.034(4) -0.005(5) C510 0.087(7) 0.251(14) 0.083(6) -0.008(8) -0.001(5) -0.108(8) C511 0.073(5) 0.077(5) 0.103(6) -0.042(5) -0.022(5) 0.001(4) P1 0.0789(17) 0.126(2) 0.0790(16) -0.0242(15) 0.0136(13) -0.0300(15) P2 0.0464(11) 0.0531(11) 0.1283(19) -0.0075(12) -0.0253(12) -0.0126(9) F1 0.268(10) 0.132(6) 0.230(9) -0.075(6) -0.071(8) -0.040(6) F2 0.169(6) 0.203(7) 0.099(4) 0.015(5) 0.010(4) -0.044(5) F3 0.084(4) 0.272(9) 0.128(5) 0.019(5) 0.003(3) -0.076(5) F4 0.118(5) 0.313(10) 0.078(4) -0.001(5) 0.028(3) -0.043(6) F5 0.135(5) 0.127(5) 0.164(6) -0.029(4) 0.035(4) -0.020(4) F6 0.084(4) 0.181(6) 0.172(6) -0.065(5) -0.011(4) -0.003(4) F7 0.50(3) 0.61(3) 0.354(18) 0.069(19) -0.34(2) -0.31(2) F8 0.055(4) 0.124(6) 0.63(2) 0.050(9) 0.058(8) -0.006(4) F9 0.182(8) 0.431(17) 0.103(5) 0.028(8) -0.026(5) -0.054(9) F10 0.161(7) 0.069(4) 0.511(19) -0.038(7) 0.094(9) -0.043(4) F11 0.129(6) 0.062(3) 0.451(15) 0.021(6) -0.060(7) -0.014(3) F12 0.116(5) 0.142(5) 0.182(6) -0.065(5) 0.062(4) -0.036(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 N5 2.098(5) . ? Mn1 N3 2.106(6) . ? Mn1 N2 2.112(5) . ? Mn1 N4 2.173(5) . ? Mn1 O1 2.324(4) . ? Mn2 N201 1.656(7) . ? Mn2 C207 1.915(8) . ? Mn2 C2 1.946(7) . ? Mn2 C206 2.068(6) . ? Mn2 C202 2.090(6) . ? Mn2 C205 2.183(6) . ? Mn2 C203 2.217(6) . ? Mn2 C204 2.272(6) . ? Mn3 N301 1.656(6) . ? Mn3 C307 1.917(6) . ? Mn3 C3 1.931(7) . ? Mn3 C304 2.098(11) . ? Mn3 C303 2.117(9) . ? Mn3 C306 2.135(6) . ? Mn3 C305 2.143(9) . ? Mn3 C302 2.162(6) . ? Mn4 N401 1.629(7) . ? Mn4 C407 1.906(7) . ? Mn4 C4 1.937(6) . ? Mn4 C405 2.106(7) . ? Mn4 C404 2.110(7) . ? Mn4 C403 2.153(6) . ? Mn4 C406 2.162(7) . ? Mn4 C402 2.211(7) . ? Mn5 N501 1.655(5) . ? Mn5 C507 1.910(6) . ? Mn5 C5 1.937(6) . ? Mn5 C502 2.113(7) . ? Mn5 C504 2.123(6) . ? Mn5 C506 2.136(7) . ? Mn5 C505 2.142(6) . ? Mn5 C503 2.146(8) . ? O1 C7 1.349(13) . ? O1 C8 1.494(11) . ? O201 N201 1.176(8) . ? O301 N301 1.172(7) . ? O401 N401 1.178(8) . ? O501 N501 1.156(6) . ? N2 C2 1.140(8) . ? N3 C3 1.140(7) . ? N4 C4 1.153(7) . ? N5 C5 1.149(7) . ? N202 C207 1.137(9) . ? N202 C208 1.474(10) . ? N302 C307 1.149(7) . ? N302 C308 1.465(7) . ? N402 C407 1.144(7) . ? N402 C408 1.469(8) . ? N502 C507 1.148(7) . ? N502 C508 1.461(8) . ? C6 C7 1.128(13) . ? C8 C9 1.394(16) . ? C201 C202 1.347(16) . ? C202 C203 1.4200 . ? C202 C206 1.4200 . ? C203 C204 1.4200 . ? C204 C205 1.4200 . ? C205 C206 1.4200 . ? C208 C211 1.486(11) . ? C208 C210 1.521(10) . ? C208 C209 1.523(11) . ? C301 C302 1.507(11) . ? C302 C306 1.407(9) . ? C302 C305 1.408(12) . ? C304 C303 1.35(2) . ? C304 C305 1.38(2) . ? C303 C306 1.388(13) . ? C308 C311 1.466(11) . ? C308 C310 1.482(11) . ? C308 C309 1.505(9) . ? C401 C402 1.507(10) . ? C402 C403 1.392(10) . ? C402 C406 1.417(9) . ? C403 C404 1.417(10) . ? C404 C405 1.418(10) . ? C405 C406 1.415(10) . ? C408 C411 1.516(10) . ? C408 C410 1.519(9) . ? C408 C409 1.537(11) . ? C501 C502 1.503(14) . ? C502 C503 1.267(12) . ? C502 C506 1.392(12) . ? C503 C504 1.336(11) . ? C504 C505 1.408(11) . ? C505 C506 1.497(12) . ? C508 C510 1.506(10) . ? C508 C511 1.508(9) . ? C508 C509 1.532(9) . ? P1 F4 1.546(6) . ? P1 F1 1.556(7) . ? P1 F3 1.558(6) . ? P1 F6 1.569(6) . ? P1 F2 1.574(6) . ? P1 F5 1.596(7) . ? P2 F7 1.417(10) . ? P2 F9 1.483(8) . ? P2 F10 1.501(6) . ? P2 F11 1.504(6) . ? P2 F8 1.505(7) . ? P2 F12 1.527(6) . ? 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 N5 Mn1 N3 114.5(2) . . ? N5 Mn1 N2 128.5(2) . . ? N3 Mn1 N2 115.2(2) . . ? N5 Mn1 N4 94.86(19) . . ? N3 Mn1 N4 96.31(19) . . ? N2 Mn1 N4 92.5(2) . . ? N5 Mn1 O1 86.66(18) . . ? N3 Mn1 O1 85.89(19) . . ? N2 Mn1 O1 84.1(2) . . ? N4 Mn1 O1 176.52(19) . . ? N201 Mn2 C207 98.6(3) . . ? N201 Mn2 C2 97.7(3) . . ? C207 Mn2 C2 90.4(3) . . ? N201 Mn2 C206 95.8(3) . . ? C207 Mn2 C206 135.4(3) . . ? C2 Mn2 C206 129.0(3) . . ? N201 Mn2 C202 118.8(3) . . ? C207 Mn2 C202 141.9(3) . . ? C2 Mn2 C202 91.6(3) . . ? C206 Mn2 C202 39.93(10) . . ? N201 Mn2 C205 110.2(3) . . ? C207 Mn2 C205 96.7(3) . . ? C2 Mn2 C205 149.7(3) . . ? C206 Mn2 C205 38.90(10) . . ? C202 Mn2 C205 65.00(12) . . ? N201 Mn2 C203 157.0(3) . . ? C207 Mn2 C203 103.9(3) . . ? C2 Mn2 C203 86.8(3) . . ? C206 Mn2 C203 64.73(12) . . ? C202 Mn2 C203 38.35(10) . . ? C205 Mn2 C203 62.94(12) . . ? N201 Mn2 C204 146.1(3) . . ? C207 Mn2 C204 81.8(3) . . ? C2 Mn2 C204 116.2(3) . . ? C206 Mn2 C204 63.73(12) . . ? C202 Mn2 C204 63.41(12) . . ? C205 Mn2 C204 37.10(9) . . ? C203 Mn2 C204 36.86(9) . . ? N301 Mn3 C307 94.4(3) . . ? N301 Mn3 C3 97.3(3) . . ? C307 Mn3 C3 91.7(3) . . ? N301 Mn3 C304 134.4(8) . . ? C307 Mn3 C304 87.8(4) . . ? C3 Mn3 C304 128.2(8) . . ? N301 Mn3 C303 101.1(5) . . ? C307 Mn3 C303 109.6(4) . . ? C3 Mn3 C303 150.4(3) . . ? C304 Mn3 C303 37.4(6) . . ? N301 Mn3 C306 96.8(3) . . ? C307 Mn3 C306 147.4(3) . . ? C3 Mn3 C306 116.9(2) . . ? C304 Mn3 C306 62.8(5) . . ? C303 Mn3 C306 38.1(4) . . ? N301 Mn3 C305 160.4(3) . . ? C307 Mn3 C305 102.3(3) . . ? C3 Mn3 C305 92.4(5) . . ? C304 Mn3 C305 38.0(6) . . ? C303 Mn3 C305 63.8(6) . . ? C306 Mn3 C305 63.6(3) . . ? N301 Mn3 C302 125.4(2) . . ? C307 Mn3 C302 140.1(3) . . ? C3 Mn3 C302 86.4(2) . . ? C304 Mn3 C302 63.4(5) . . ? C303 Mn3 C302 64.1(3) . . ? C306 Mn3 C302 38.2(2) . . ? C305 Mn3 C302 38.2(3) . . ? N401 Mn4 C407 96.7(3) . . ? N401 Mn4 C4 94.2(3) . . ? C407 Mn4 C4 87.4(2) . . ? N401 Mn4 C405 120.0(3) . . ? C407 Mn4 C405 143.3(3) . . ? C4 Mn4 C405 91.6(3) . . ? N401 Mn4 C404 95.4(3) . . ? C407 Mn4 C404 143.3(3) . . ? C4 Mn4 C404 126.0(3) . . ? C405 Mn4 C404 39.3(3) . . ? N401 Mn4 C403 106.5(3) . . ? C407 Mn4 C403 104.5(3) . . ? C4 Mn4 C403 154.4(3) . . ? C405 Mn4 C403 65.3(3) . . ? C404 Mn4 C403 38.8(3) . . ? N401 Mn4 C406 158.2(3) . . ? C407 Mn4 C406 104.6(3) . . ? C4 Mn4 C406 91.5(2) . . ? C405 Mn4 C406 38.7(3) . . ? C404 Mn4 C406 64.5(3) . . ? C403 Mn4 C406 63.8(3) . . ? N401 Mn4 C402 141.8(3) . . ? C407 Mn4 C402 86.4(3) . . ? C4 Mn4 C402 124.0(3) . . ? C405 Mn4 C402 64.1(3) . . ? C404 Mn4 C402 63.4(3) . . ? C403 Mn4 C402 37.2(3) . . ? C406 Mn4 C402 37.8(2) . . ? N501 Mn5 C507 97.4(2) . . ? N501 Mn5 C5 98.3(2) . . ? C507 Mn5 C5 88.0(2) . . ? N501 Mn5 C502 111.8(3) . . ? C507 Mn5 C502 149.9(3) . . ? C5 Mn5 C502 94.4(3) . . ? N501 Mn5 C504 103.8(3) . . ? C507 Mn5 C504 106.4(3) . . ? C5 Mn5 C504 151.6(3) . . ? C502 Mn5 C504 60.9(3) . . ? N501 Mn5 C506 150.0(4) . . ? C507 Mn5 C506 112.1(4) . . ? C5 Mn5 C506 88.1(3) . . ? C502 Mn5 C506 38.3(3) . . ? C504 Mn5 C506 63.9(3) . . ? N501 Mn5 C505 140.9(3) . . ? C507 Mn5 C505 87.8(3) . . ? C5 Mn5 C505 120.7(3) . . ? C502 Mn5 C505 65.3(3) . . ? C504 Mn5 C505 38.6(3) . . ? C506 Mn5 C505 41.0(3) . . ? N501 Mn5 C503 91.8(3) . . ? C507 Mn5 C503 142.7(3) . . ? C5 Mn5 C503 126.4(4) . . ? C502 Mn5 C503 34.6(3) . . ? C504 Mn5 C503 36.5(3) . . ? C506 Mn5 C503 61.7(4) . . ? C505 Mn5 C503 63.6(3) . . ? C7 O1 C8 112.4(7) . . ? C7 O1 Mn1 122.8(7) . . ? C8 O1 Mn1 119.1(5) . . ? C2 N2 Mn1 174.0(6) . . ? C3 N3 Mn1 171.5(5) . . ? C4 N4 Mn1 168.2(5) . . ? C5 N5 Mn1 166.4(5) . . ? O201 N201 Mn2 175.7(6) . . ? C207 N202 C208 176.4(8) . . ? O301 N301 Mn3 177.3(5) . . ? C307 N302 C308 173.9(6) . . ? O401 N401 Mn4 179.2(7) . . ? C407 N402 C408 178.3(7) . . ? O501 N501 Mn5 175.1(5) . . ? C507 N502 C508 176.4(6) . . ? N2 C2 Mn2 177.1(6) . . ? N3 C3 Mn3 177.0(5) . . ? N4 C4 Mn4 175.2(5) . . ? N5 C5 Mn5 178.0(5) . . ? C6 C7 O1 157.4(14) . . ? C9 C8 O1 110.5(12) . . ? C201 C202 C203 130.3(10) . . ? C201 C202 C206 121.4(10) . . ? C203 C202 C206 108.0 . . ? C201 C202 Mn2 125.0(8) . . ? C203 C202 Mn2 75.7(2) . . ? C206 C202 Mn2 69.2(2) . . ? C202 C203 C204 108.0 . . ? C202 C203 Mn2 66.0(2) . . ? C204 C203 Mn2 73.7(2) . . ? C205 C204 C203 108.0 . . ? C205 C204 Mn2 68.1(2) . . ? C203 C204 Mn2 69.5(2) . . ? C204 C205 C206 108.0 . . ? C204 C205 Mn2 74.8(2) . . ? C206 C205 Mn2 66.2(2) . . ? C205 C206 C202 108.0 . . ? C205 C206 Mn2 74.9(2) . . ? C202 C206 Mn2 70.9(2) . . ? N202 C207 Mn2 178.3(6) . . ? N202 C208 C211 107.3(7) . . ? N202 C208 C210 107.0(6) . . ? C211 C208 C210 112.0(7) . . ? N202 C208 C209 106.9(6) . . ? C211 C208 C209 113.7(8) . . ? C210 C208 C209 109.8(7) . . ? C306 C302 C305 106.5(9) . . ? C306 C302 C301 124.3(7) . . ? C305 C302 C301 129.1(10) . . ? C306 C302 Mn3 69.9(3) . . ? C305 C302 Mn3 70.2(5) . . ? C301 C302 Mn3 127.7(4) . . ? C303 C304 C305 110.9(11) . . ? C303 C304 Mn3 72.0(8) . . ? C305 C304 Mn3 72.8(6) . . ? C304 C305 C302 106.8(11) . . ? C304 C305 Mn3 69.2(8) . . ? C302 C305 Mn3 71.7(4) . . ? C304 C303 C306 107.1(12) . . ? C304 C303 Mn3 70.5(7) . . ? C306 C303 Mn3 71.7(4) . . ? C303 C306 C302 108.7(9) . . ? C303 C306 Mn3 70.2(5) . . ? C302 C306 Mn3 71.9(3) . . ? N302 C307 Mn3 176.4(6) . . ? N302 C308 C311 108.2(6) . . ? N302 C308 C310 108.6(6) . . ? C311 C308 C310 113.8(9) . . ? N302 C308 C309 106.4(5) . . ? C311 C308 C309 110.3(9) . . ? C310 C308 C309 109.3(7) . . ? C403 C402 C406 108.5(7) . . ? C403 C402 C401 127.2(7) . . ? C406 C402 C401 124.3(8) . . ? C403 C402 Mn4 69.1(4) . . ? C406 C402 Mn4 69.2(4) . . ? C401 C402 Mn4 128.5(5) . . ? C402 C403 C404 108.0(6) . . ? C402 C403 Mn4 73.7(4) . . ? C404 C403 Mn4 69.0(4) . . ? C403 C404 C405 108.2(7) . . ? C403 C404 Mn4 72.2(4) . . ? C405 C404 Mn4 70.2(4) . . ? C406 C405 C404 107.1(7) . . ? C406 C405 Mn4 72.8(4) . . ? C404 C405 Mn4 70.5(4) . . ? C405 C406 C402 108.1(7) . . ? C405 C406 Mn4 68.5(4) . . ? C402 C406 Mn4 73.0(4) . . ? N402 C407 Mn4 178.9(6) . . ? N402 C408 C411 107.3(6) . . ? N402 C408 C410 107.9(6) . . ? C411 C408 C410 111.6(6) . . ? N402 C408 C409 106.2(6) . . ? C411 C408 C409 112.0(7) . . ? C410 C408 C409 111.5(7) . . ? C503 C502 C506 111.3(9) . . ? C503 C502 C501 120.3(13) . . ? C506 C502 C501 128.3(13) . . ? C503 C502 Mn5 74.1(5) . . ? C506 C502 Mn5 71.7(5) . . ? C501 C502 Mn5 124.9(6) . . ? C502 C503 C504 111.1(10) . . ? C502 C503 Mn5 71.3(5) . . ? C504 C503 Mn5 70.8(5) . . ? C503 C504 C505 110.7(8) . . ? C503 C504 Mn5 72.7(4) . . ? C505 C504 Mn5 71.5(4) . . ? C504 C505 C506 101.7(6) . . ? C504 C505 Mn5 70.0(4) . . ? C506 C505 Mn5 69.3(3) . . ? C502 C506 C505 105.1(7) . . ? C502 C506 Mn5 70.0(4) . . ? C505 C506 Mn5 69.8(4) . . ? N502 C507 Mn5 177.2(5) . . ? N502 C508 C510 107.1(6) . . ? N502 C508 C511 107.7(5) . . ? C510 C508 C511 113.7(7) . . ? N502 C508 C509 108.1(5) . . ? C510 C508 C509 110.7(7) . . ? C511 C508 C509 109.3(6) . . ? F4 P1 F1 91.1(5) . . ? F4 P1 F3 90.6(4) . . ? F1 P1 F3 93.5(5) . . ? F4 P1 F6 89.9(4) . . ? F1 P1 F6 88.8(5) . . ? F3 P1 F6 177.7(4) . . ? F4 P1 F2 175.3(5) . . ? F1 P1 F2 93.6(5) . . ? F3 P1 F2 88.9(4) . . ? F6 P1 F2 90.4(4) . . ? F4 P1 F5 89.0(5) . . ? F1 P1 F5 176.5(5) . . ? F3 P1 F5 90.0(4) . . ? F6 P1 F5 87.7(4) . . ? F2 P1 F5 86.2(4) . . ? F7 P2 F9 176.3(8) . . ? F7 P2 F10 90.4(8) . . ? F9 P2 F10 92.6(7) . . ? F7 P2 F11 89.9(9) . . ? F9 P2 F11 87.2(6) . . ? F10 P2 F11 177.2(5) . . ? F7 P2 F8 87.7(9) . . ? F9 P2 F8 94.7(7) . . ? F10 P2 F8 86.9(4) . . ? F11 P2 F8 90.3(4) . . ? F7 P2 F12 94.8(9) . . ? F9 P2 F12 82.8(5) . . ? F10 P2 F12 91.7(4) . . ? F11 P2 F12 91.1(4) . . ? F8 P2 F12 177.1(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.878 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.083 #===END data_32.2acetone _database_code_depnum_ccdc_archive 'CCDC 223108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H76 F6 Mn5 N13 O9 P' _chemical_formula_weight 1663.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 26.525(2) _cell_length_b 12.1585(10) _cell_length_c 24.814(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.690(2) _cell_angle_gamma 90.00 _cell_volume 7580.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 77 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3412 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.814295 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19944 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6669 _reflns_number_gt 4491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+27.2869P] 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 6669 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.0000 0.82145(8) 0.2500 0.0233(2) Uani 1 2 d S . . Mn2 Mn 0.13351(3) 0.75686(6) 0.13890(3) 0.0334(2) Uani 1 1 d . . . Mn3 Mn 0.09676(3) 0.49530(6) 0.37815(3) 0.0305(2) Uani 1 1 d . . . N1 N 0.04858(16) 0.7043(3) 0.31012(16) 0.0351(10) Uani 1 1 d . . . N2 N 0.05491(17) 0.8274(4) 0.20116(18) 0.0398(10) Uani 1 1 d . . . N3 N 0.15161(17) 0.6554(3) 0.47359(18) 0.0384(10) Uani 1 1 d . . . N4 N 0.14538(18) 0.4796(3) 0.3508(2) 0.0419(11) Uani 1 1 d . . . N5 N 0.09331(16) 0.9550(3) 0.06122(17) 0.0337(9) Uani 1 1 d . . . N6 N 0.09581(17) 0.6653(3) 0.09527(18) 0.0365(10) Uani 1 1 d . . . O1 O 0.17954(17) 0.4622(3) 0.3307(2) 0.0665(13) Uani 1 1 d . . . O2 O 0.07039(16) 0.5963(3) 0.06403(17) 0.0512(10) Uani 1 1 d . . . O3 O 0.03291(14) 0.9901(3) 0.28892(15) 0.0413(9) Uani 1 1 d . . . O4 O 0.0000 1.1449(5) 0.2500 0.086(2) Uani 1 2 d S . . C1 C 0.06591(19) 0.6258(4) 0.3347(2) 0.0311(11) Uani 1 1 d . . . C2 C 0.0836(2) 0.8017(4) 0.1775(2) 0.0346(11) Uani 1 1 d . . . C3 C -0.0358(2) 0.4869(5) 0.3219(3) 0.0500(15) Uani 1 1 d . . . H3A H -0.0666 0.4467 0.3255 0.075 Uiso 1 1 calc R . . H3B H -0.0360 0.4836 0.2823 0.075 Uiso 1 1 calc R . . H3C H -0.0376 0.5638 0.3329 0.075 Uiso 1 1 calc R . . C4 C 0.0143(2) 0.4358(4) 0.3600(2) 0.0380(12) Uani 1 1 d . . . C5 C 0.0387(2) 0.4549(4) 0.4181(2) 0.0421(13) Uani 1 1 d . . . H5A H 0.0252 0.5058 0.4421 0.050 Uiso 1 1 calc R . . C6 C 0.0852(2) 0.3838(4) 0.4388(2) 0.0440(13) Uani 1 1 d . . . H6A H 0.1084 0.3744 0.4791 0.053 Uiso 1 1 calc R . . C7 C 0.0881(2) 0.3259(4) 0.3922(2) 0.0438(13) Uani 1 1 d . . . H7A H 0.1152 0.2681 0.3931 0.053 Uiso 1 1 calc R . . C8 C 0.0457(2) 0.3575(4) 0.3430(2) 0.0405(13) Uani 1 1 d . . . H8A H 0.0382 0.3267 0.3038 0.049 Uiso 1 1 calc R . . C9 C 0.1316(2) 0.5936(4) 0.4381(2) 0.0366(12) Uani 1 1 d . . . C10 C 0.17297(18) 0.7369(4) 0.5136(2) 0.0313(11) Uani 1 1 d . . . C11 C 0.19254(19) 0.8324(4) 0.4961(2) 0.0359(12) Uani 1 1 d . . . C12 C 0.2131(2) 0.9120(4) 0.5377(3) 0.0505(16) Uani 1 1 d . . . H12A H 0.2276 0.9778 0.5281 0.061 Uiso 1 1 calc R . . C13 C 0.2129(2) 0.8966(5) 0.5928(3) 0.0541(16) Uani 1 1 d . . . H13A H 0.2267 0.9523 0.6204 0.065 Uiso 1 1 calc R . . C14 C 0.1930(2) 0.8027(5) 0.6078(2) 0.0495(15) Uani 1 1 d . . . H14A H 0.1930 0.7940 0.6459 0.059 Uiso 1 1 calc R . . C15 C 0.1730(2) 0.7203(4) 0.5692(2) 0.0390(12) Uani 1 1 d . . . C16 C 0.1515(3) 0.6152(5) 0.5857(3) 0.0684(19) Uani 1 1 d . . . H16A H 0.1568 0.6158 0.6266 0.103 Uiso 1 1 calc R . . H16B H 0.1702 0.5521 0.5764 0.103 Uiso 1 1 calc R . . H16C H 0.1134 0.6093 0.5647 0.103 Uiso 1 1 calc R . . C17 C 0.1900(2) 0.8479(5) 0.4357(3) 0.0574(16) Uani 1 1 d . . . H17A H 0.2085 0.7869 0.4241 0.086 Uiso 1 1 calc R . . H17B H 0.2072 0.9175 0.4319 0.086 Uiso 1 1 calc R . . H17C H 0.1527 0.8493 0.4113 0.086 Uiso 1 1 calc R . . C18 C 0.1766(3) 0.7393(8) 0.2791(3) 0.104(3) Uani 1 1 d . . . H18A H 0.2095 0.7378 0.3116 0.156 Uiso 1 1 calc R . . H18B H 0.1554 0.6735 0.2798 0.156 Uiso 1 1 calc R . . H18C H 0.1560 0.8051 0.2813 0.156 Uiso 1 1 calc R . . C19 C 0.1902(2) 0.7414(6) 0.2246(2) 0.0579(17) Uani 1 1 d . . . C20 C 0.1927(2) 0.6477(5) 0.1926(3) 0.0559(17) Uani 1 1 d . . . H20A H 0.1866 0.5702 0.2025 0.067 Uiso 1 1 calc R . . C21 C 0.2079(2) 0.6816(5) 0.1452(3) 0.0471(14) Uani 1 1 d . . . H21A H 0.2148 0.6316 0.1163 0.057 Uiso 1 1 calc R . . C22 C 0.2142(2) 0.7952(5) 0.1473(2) 0.0430(13) Uani 1 1 d . . . H22A H 0.2264 0.8407 0.1203 0.052 Uiso 1 1 calc R . . C23 C 0.2022(2) 0.8351(5) 0.1961(2) 0.0431(13) Uani 1 1 d . . . H23A H 0.2046 0.9131 0.2095 0.052 Uiso 1 1 calc R . . C24 C 0.11023(19) 0.8820(4) 0.0911(2) 0.0333(11) Uani 1 1 d . . . C25 C 0.07064(18) 1.0426(4) 0.0253(2) 0.0290(10) Uani 1 1 d . . . C26 C 0.06827(18) 1.0356(4) -0.0317(2) 0.0288(10) Uani 1 1 d . . . C27 C 0.04598(19) 1.1234(4) -0.0668(2) 0.0331(11) Uani 1 1 d . . . H27A H 0.0437 1.1213 -0.1057 0.040 Uiso 1 1 calc R . . C28 C 0.0272(2) 1.2133(4) -0.0460(2) 0.0397(13) Uani 1 1 d . . . H28A H 0.0125 1.2731 -0.0707 0.048 Uiso 1 1 calc R . . C29 C 0.0291(2) 1.2186(4) 0.0106(2) 0.0400(13) Uani 1 1 d . . . H29A H 0.0152 1.2812 0.0239 0.048 Uiso 1 1 calc R . . C30 C 0.05132(19) 1.1322(4) 0.0480(2) 0.0344(11) Uani 1 1 d . . . C31 C 0.0543(2) 1.1345(5) 0.1096(2) 0.0515(15) Uani 1 1 d . . . H31A H 0.0368 1.0689 0.1182 0.077 Uiso 1 1 calc R . . H31B H 0.0363 1.2005 0.1169 0.077 Uiso 1 1 calc R . . H31C H 0.0916 1.1356 0.1337 0.077 Uiso 1 1 calc R . . C32 C 0.0890(2) 0.9355(4) -0.0538(2) 0.0404(12) Uani 1 1 d . . . H32A H 0.0811 0.9420 -0.0951 0.061 Uiso 1 1 calc R . . H32B H 0.0717 0.8694 -0.0453 0.061 Uiso 1 1 calc R . . H32C H 0.1275 0.9299 -0.0354 0.061 Uiso 1 1 calc R . . N7 N 0.0000 1.0437(5) 0.2500 0.0437(16) Uani 1 2 d S . . O99 O 0.31484(17) 0.5948(4) 0.26748(17) 0.0605(11) Uani 1 1 d . . . C97 C 0.3326(3) 0.5516(8) 0.1829(3) 0.092(3) Uani 1 1 d . . . H97A H 0.3068 0.4925 0.1804 0.138 Uiso 1 1 calc R . . H97B H 0.3675 0.5196 0.1870 0.138 Uiso 1 1 calc R . . H97C H 0.3209 0.5965 0.1483 0.138 Uiso 1 1 calc R . . C98 C 0.3365(2) 0.6218(6) 0.2333(2) 0.0552(16) Uani 1 1 d . . . C99 C 0.3671(3) 0.7257(7) 0.2405(4) 0.099(3) Uani 1 1 d . . . H99A H 0.3642 0.7653 0.2738 0.149 Uiso 1 1 calc R . . H99B H 0.3528 0.7714 0.2065 0.149 Uiso 1 1 calc R . . H99C H 0.4046 0.7090 0.2461 0.149 Uiso 1 1 calc R . . P1 P 0.2500 0.7500 0.0000 0.0393(5) Uani 1 2 d S . . F1 F 0.27779(18) 0.8162(6) 0.0552(2) 0.136(2) Uani 1 1 d . . . F2 F 0.19605(15) 0.7721(4) 0.01200(16) 0.0932(15) Uani 1 1 d . . . F3 F 0.2577(3) 0.6459(4) 0.0364(3) 0.167(3) Uani 1 1 d . . . 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 0.0267(5) 0.0222(5) 0.0234(5) 0.000 0.0112(4) 0.000 Mn2 0.0321(4) 0.0363(4) 0.0370(4) 0.0112(3) 0.0185(3) 0.0091(3) Mn3 0.0326(4) 0.0232(4) 0.0336(4) -0.0008(3) 0.0076(3) 0.0005(3) N1 0.038(2) 0.036(2) 0.030(2) 0.0067(19) 0.0093(19) 0.0039(19) N2 0.039(3) 0.048(3) 0.043(3) 0.008(2) 0.027(2) 0.008(2) N3 0.037(2) 0.029(2) 0.043(3) -0.006(2) 0.004(2) -0.0001(19) N4 0.035(2) 0.032(2) 0.059(3) -0.008(2) 0.016(2) 0.0012(19) N5 0.031(2) 0.038(2) 0.034(2) 0.008(2) 0.0128(19) 0.0028(19) N6 0.042(3) 0.033(2) 0.042(3) 0.007(2) 0.024(2) 0.012(2) O1 0.050(3) 0.057(3) 0.105(4) -0.025(3) 0.041(3) -0.008(2) O2 0.055(3) 0.042(2) 0.056(2) -0.008(2) 0.017(2) 0.0057(19) O3 0.042(2) 0.038(2) 0.039(2) -0.0020(17) 0.0056(17) -0.0051(17) O4 0.115(6) 0.027(3) 0.109(6) 0.000 0.025(5) 0.000 C1 0.029(3) 0.034(3) 0.031(3) -0.001(2) 0.010(2) -0.001(2) C2 0.036(3) 0.036(3) 0.032(3) 0.013(2) 0.012(2) 0.008(2) C3 0.034(3) 0.051(4) 0.064(4) -0.007(3) 0.013(3) -0.004(3) C4 0.040(3) 0.030(3) 0.046(3) -0.004(2) 0.018(3) -0.008(2) C5 0.050(3) 0.036(3) 0.044(3) -0.007(2) 0.022(3) -0.008(3) C6 0.055(4) 0.034(3) 0.043(3) 0.011(2) 0.015(3) 0.000(3) C7 0.058(4) 0.021(3) 0.056(3) 0.008(2) 0.024(3) 0.000(2) C8 0.051(3) 0.028(3) 0.045(3) -0.011(2) 0.018(3) -0.009(2) C9 0.037(3) 0.027(3) 0.041(3) 0.005(2) 0.005(2) 0.005(2) C10 0.028(3) 0.026(3) 0.035(3) -0.003(2) 0.004(2) 0.001(2) C11 0.027(3) 0.031(3) 0.049(3) 0.006(2) 0.011(2) 0.007(2) C12 0.025(3) 0.026(3) 0.091(5) 0.002(3) 0.007(3) -0.002(2) C13 0.037(3) 0.046(4) 0.068(4) -0.029(3) 0.001(3) -0.001(3) C14 0.036(3) 0.064(4) 0.045(3) -0.015(3) 0.007(3) 0.005(3) C15 0.031(3) 0.044(3) 0.040(3) 0.004(2) 0.009(2) 0.000(2) C16 0.073(5) 0.061(4) 0.073(5) 0.020(4) 0.025(4) -0.010(4) C17 0.046(4) 0.060(4) 0.068(4) 0.022(3) 0.020(3) 0.012(3) C18 0.071(5) 0.181(10) 0.048(4) 0.041(5) 0.002(4) 0.018(6) C19 0.035(3) 0.093(5) 0.045(3) 0.026(4) 0.011(3) 0.018(3) C20 0.035(3) 0.051(4) 0.080(4) 0.031(3) 0.016(3) 0.019(3) C21 0.028(3) 0.044(3) 0.074(4) 0.003(3) 0.022(3) 0.011(2) C22 0.030(3) 0.051(3) 0.051(3) 0.003(3) 0.017(3) -0.004(2) C23 0.031(3) 0.056(4) 0.041(3) 0.002(3) 0.010(2) 0.007(3) C24 0.026(3) 0.043(3) 0.037(3) 0.006(2) 0.019(2) 0.003(2) C25 0.023(2) 0.026(2) 0.038(3) 0.008(2) 0.010(2) 0.0029(19) C26 0.022(2) 0.028(2) 0.033(3) -0.001(2) 0.006(2) -0.0020(19) C27 0.030(3) 0.036(3) 0.032(3) 0.009(2) 0.007(2) 0.003(2) C28 0.035(3) 0.031(3) 0.047(3) 0.012(2) 0.004(2) 0.003(2) C29 0.032(3) 0.027(3) 0.059(4) -0.006(2) 0.013(3) 0.007(2) C30 0.025(3) 0.039(3) 0.037(3) -0.009(2) 0.006(2) -0.006(2) C31 0.044(3) 0.068(4) 0.045(3) -0.010(3) 0.018(3) 0.004(3) C32 0.046(3) 0.034(3) 0.044(3) -0.001(2) 0.018(3) 0.004(2) N7 0.053(4) 0.027(3) 0.050(4) 0.000 0.015(4) 0.000 O99 0.066(3) 0.072(3) 0.046(2) 0.003(2) 0.022(2) 0.000(2) C97 0.063(5) 0.155(8) 0.053(4) -0.020(5) 0.012(4) 0.037(5) C98 0.043(3) 0.081(5) 0.037(3) 0.021(3) 0.007(3) 0.019(3) C99 0.093(6) 0.100(7) 0.097(6) 0.051(5) 0.019(5) -0.020(5) P1 0.0391(11) 0.0399(11) 0.0387(10) -0.0072(9) 0.0120(9) 0.0100(9) F1 0.072(3) 0.253(7) 0.089(3) -0.104(4) 0.034(3) -0.054(4) F2 0.053(2) 0.166(5) 0.065(2) -0.008(3) 0.025(2) 0.042(3) F3 0.311(9) 0.082(3) 0.190(6) 0.062(4) 0.196(7) 0.092(5) _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 N1 2.164(4) 2 ? Mn1 N1 2.164(4) . ? Mn1 N2 2.174(4) 2 ? Mn1 N2 2.174(4) . ? Mn1 O3 2.315(3) 2 ? Mn1 O3 2.315(3) . ? Mn2 N6 1.649(5) . ? Mn2 C24 1.906(5) . ? Mn2 C2 1.945(5) . ? Mn2 C22 2.134(5) . ? Mn2 C21 2.136(5) . ? Mn2 C23 2.140(6) . ? Mn2 C20 2.159(5) . ? Mn2 C19 2.184(6) . ? Mn3 N4 1.650(5) . ? Mn3 C9 1.901(5) . ? Mn3 C1 1.945(5) . ? Mn3 C7 2.113(5) . ? Mn3 C6 2.119(5) . ? Mn3 C5 2.139(5) . ? Mn3 C8 2.155(5) . ? Mn3 C4 2.208(5) . ? N1 C1 1.147(6) . ? N2 C2 1.143(6) . ? N3 C9 1.150(6) . ? N3 C10 1.389(6) . ? N4 O1 1.185(5) . ? N5 C24 1.152(6) . ? N5 C25 1.395(6) . ? N6 O2 1.194(5) . ? O3 N7 1.256(4) . ? O4 N7 1.230(8) . ? C3 C4 1.497(7) . ? C4 C5 1.399(7) . ? C4 C8 1.415(7) . ? C5 C6 1.458(8) . ? C6 C7 1.376(7) . ? C7 C8 1.422(8) . ? C10 C15 1.394(7) . ? C10 C11 1.397(7) . ? C11 C12 1.393(8) . ? C11 C17 1.490(7) . ? C12 C13 1.381(9) . ? C13 C14 1.359(8) . ? C14 C15 1.371(7) . ? C15 C16 1.509(8) . ? C18 C19 1.509(9) . ? C19 C20 1.402(9) . ? C19 C23 1.428(8) . ? C20 C21 1.422(8) . ? C21 C22 1.390(8) . ? C22 C23 1.433(7) . ? C25 C30 1.396(7) . ? C25 C26 1.399(6) . ? C26 C27 1.385(6) . ? C26 C32 1.509(7) . ? C27 C28 1.368(7) . ? C28 C29 1.390(7) . ? C29 C30 1.402(7) . ? C30 C31 1.504(7) . ? N7 O3 1.256(4) 2 ? O99 C98 1.211(7) . ? C97 C98 1.490(9) . ? C98 C99 1.481(10) . ? P1 F3 1.530(5) . ? P1 F3 1.530(5) 7_565 ? P1 F1 1.556(4) . ? P1 F1 1.556(4) 7_565 ? P1 F2 1.575(3) . ? P1 F2 1.575(3) 7_565 ? 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 N1 Mn1 N1 97.7(2) 2 . ? N1 Mn1 N2 92.80(15) 2 2 ? N1 Mn1 N2 89.70(16) . 2 ? N1 Mn1 N2 89.71(16) 2 . ? N1 Mn1 N2 92.80(15) . . ? N2 Mn1 N2 176.2(2) 2 . ? N1 Mn1 O3 103.53(14) 2 2 ? N1 Mn1 O3 158.79(14) . 2 ? N2 Mn1 O3 88.44(15) 2 2 ? N2 Mn1 O3 88.19(15) . 2 ? N1 Mn1 O3 158.79(14) 2 . ? N1 Mn1 O3 103.53(14) . . ? N2 Mn1 O3 88.18(15) 2 . ? N2 Mn1 O3 88.44(15) . . ? O3 Mn1 O3 55.30(18) 2 . ? N6 Mn2 C24 97.1(2) . . ? N6 Mn2 C2 98.5(2) . . ? C24 Mn2 C2 86.94(19) . . ? N6 Mn2 C22 126.1(2) . . ? C24 Mn2 C22 90.1(2) . . ? C2 Mn2 C22 135.3(2) . . ? N6 Mn2 C21 96.3(2) . . ? C24 Mn2 C21 119.7(2) . . ? C2 Mn2 C21 147.5(2) . . ? C22 Mn2 C21 38.0(2) . . ? N6 Mn2 C23 160.7(2) . . ? C24 Mn2 C23 95.4(2) . . ? C2 Mn2 C23 96.8(2) . . ? C22 Mn2 C23 39.18(19) . . ? C21 Mn2 C23 64.6(2) . . ? N6 Mn2 C20 99.1(2) . . ? C24 Mn2 C20 154.3(2) . . ? C2 Mn2 C20 110.1(2) . . ? C22 Mn2 C20 64.3(2) . . ? C21 Mn2 C20 38.6(2) . . ? C23 Mn2 C20 64.4(2) . . ? N6 Mn2 C19 131.7(2) . . ? C24 Mn2 C19 131.2(3) . . ? C2 Mn2 C19 84.8(2) . . ? C22 Mn2 C19 64.4(2) . . ? C21 Mn2 C19 63.9(2) . . ? C23 Mn2 C19 38.6(2) . . ? C20 Mn2 C19 37.7(2) . . ? N4 Mn3 C9 98.5(2) . . ? N4 Mn3 C1 96.4(2) . . ? C9 Mn3 C1 86.1(2) . . ? N4 Mn3 C7 95.5(2) . . ? C9 Mn3 C7 122.4(2) . . ? C1 Mn3 C7 146.9(2) . . ? N4 Mn3 C6 121.9(2) . . ? C9 Mn3 C6 89.5(2) . . ? C1 Mn3 C6 141.6(2) . . ? C7 Mn3 C6 38.0(2) . . ? N4 Mn3 C5 159.8(2) . . ? C9 Mn3 C5 91.3(2) . . ? C1 Mn3 C5 101.9(2) . . ? C7 Mn3 C5 64.4(2) . . ? C6 Mn3 C5 40.0(2) . . ? N4 Mn3 C8 102.4(2) . . ? C9 Mn3 C8 152.9(2) . . ? C1 Mn3 C8 108.2(2) . . ? C7 Mn3 C8 38.9(2) . . ? C6 Mn3 C8 64.9(2) . . ? C5 Mn3 C8 63.7(2) . . ? N4 Mn3 C4 137.0(2) . . ? C9 Mn3 C4 124.5(2) . . ? C1 Mn3 C4 86.60(19) . . ? C7 Mn3 C4 64.0(2) . . ? C6 Mn3 C4 64.9(2) . . ? C5 Mn3 C4 37.51(19) . . ? C8 Mn3 C4 37.84(19) . . ? C1 N1 Mn1 164.5(4) . . ? C2 N2 Mn1 162.2(4) . . ? C9 N3 C10 175.0(5) . . ? O1 N4 Mn3 176.3(4) . . ? C24 N5 C25 177.5(5) . . ? O2 N6 Mn2 177.2(4) . . ? N7 O3 Mn1 93.6(3) . . ? N1 C1 Mn3 178.4(5) . . ? N2 C2 Mn2 178.7(4) . . ? C5 C4 C8 107.3(5) . . ? C5 C4 C3 127.3(5) . . ? C8 C4 C3 125.4(5) . . ? C5 C4 Mn3 68.6(3) . . ? C8 C4 Mn3 69.0(3) . . ? C3 C4 Mn3 127.9(4) . . ? C4 C5 C6 108.8(5) . . ? C4 C5 Mn3 73.9(3) . . ? C6 C5 Mn3 69.3(3) . . ? C7 C6 C5 106.1(5) . . ? C7 C6 Mn3 70.8(3) . . ? C5 C6 Mn3 70.7(3) . . ? C6 C7 C8 110.0(5) . . ? C6 C7 Mn3 71.3(3) . . ? C8 C7 Mn3 72.1(3) . . ? C4 C8 C7 107.7(5) . . ? C4 C8 Mn3 73.1(3) . . ? C7 C8 Mn3 69.0(3) . . ? N3 C9 Mn3 178.1(5) . . ? N3 C10 C15 118.3(4) . . ? N3 C10 C11 118.6(4) . . ? C15 C10 C11 123.1(5) . . ? C12 C11 C10 116.3(5) . . ? C12 C11 C17 122.6(5) . . ? C10 C11 C17 121.1(5) . . ? C13 C12 C11 120.9(5) . . ? C14 C13 C12 120.7(5) . . ? C13 C14 C15 121.3(6) . . ? C14 C15 C10 117.6(5) . . ? C14 C15 C16 121.7(5) . . ? C10 C15 C16 120.7(5) . . ? C20 C19 C23 108.1(5) . . ? C20 C19 C18 124.2(7) . . ? C23 C19 C18 127.8(7) . . ? C20 C19 Mn2 70.2(3) . . ? C23 C19 Mn2 69.1(3) . . ? C18 C19 Mn2 125.9(4) . . ? C19 C20 C21 108.1(5) . . ? C19 C20 Mn2 72.1(3) . . ? C21 C20 Mn2 69.8(3) . . ? C22 C21 C20 108.6(5) . . ? C22 C21 Mn2 70.9(3) . . ? C20 C21 Mn2 71.6(3) . . ? C21 C22 C23 108.1(5) . . ? C21 C22 Mn2 71.1(3) . . ? C23 C22 Mn2 70.6(3) . . ? C19 C23 C22 107.1(5) . . ? C19 C23 Mn2 72.4(3) . . ? C22 C23 Mn2 70.2(3) . . ? N5 C24 Mn2 176.1(5) . . ? N5 C25 C30 118.5(4) . . ? N5 C25 C26 118.0(4) . . ? C30 C25 C26 123.5(4) . . ? C27 C26 C25 117.4(4) . . ? C27 C26 C32 121.7(4) . . ? C25 C26 C32 120.9(4) . . ? C28 C27 C26 120.9(5) . . ? C27 C28 C29 121.2(5) . . ? C28 C29 C30 120.4(5) . . ? C25 C30 C29 116.7(4) . . ? C25 C30 C31 121.1(5) . . ? C29 C30 C31 122.2(5) . . ? O4 N7 O3 121.2(3) . 2 ? O4 N7 O3 121.2(3) . . ? O3 N7 O3 117.6(6) 2 . ? O99 C98 C99 120.7(7) . . ? O99 C98 C97 120.8(7) . . ? C99 C98 C97 118.5(7) . . ? F3 P1 F3 179.997(1) . 7_565 ? F3 P1 F1 88.4(4) . . ? F3 P1 F1 91.6(4) 7_565 . ? F3 P1 F1 91.6(4) . 7_565 ? F3 P1 F1 88.4(4) 7_565 7_565 ? F1 P1 F1 180.0(2) . 7_565 ? F3 P1 F2 89.3(3) . . ? F3 P1 F2 90.7(3) 7_565 . ? F1 P1 F2 87.0(2) . . ? F1 P1 F2 93.0(2) 7_565 . ? F3 P1 F2 90.7(3) . 7_565 ? F3 P1 F2 89.3(3) 7_565 7_565 ? F1 P1 F2 93.0(2) . 7_565 ? F1 P1 F2 87.0(2) 7_565 7_565 ? F2 P1 F2 180.0 . 7_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.877 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.082 #===END data_35 _database_code_depnum_ccdc_archive 'CCDC 223109' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H64 F12 Mn5 N12 O5 P2' _chemical_formula_weight 1645.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 15.268(6) _cell_length_b 16.101(7) _cell_length_c 17.677(9) _cell_angle_alpha 65.32(2) _cell_angle_beta 87.48(5) _cell_angle_gamma 67.70(3) _cell_volume 3619(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 65 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1670 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.832955 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SiemensCCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 31606 _diffrn_reflns_av_R_equivalents 0.1434 _diffrn_reflns_av_sigmaI/netI 0.3414 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.54 _reflns_number_total 16259 _reflns_number_gt 5011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1749P)^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 16259 _refine_ls_number_parameters 867 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3093 _refine_ls_R_factor_gt 0.1118 _refine_ls_wR_factor_ref 0.3692 _refine_ls_wR_factor_gt 0.2786 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 5.800 _refine_ls_shift/su_mean 0.035 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 0.31272(11) 0.03910(11) 0.28107(10) 0.0322(4) Uani 1 1 d . . . Mn2 Mn 0.57410(12) 0.14258(12) 0.11861(10) 0.0390(5) Uani 1 1 d . . . Mn3 Mn 0.34276(14) -0.29117(12) 0.53141(11) 0.0460(5) Uani 1 1 d . . . Mn4 Mn 0.04958(13) 0.16495(13) 0.04575(11) 0.0467(5) Uani 1 1 d . . . Mn5 Mn 0.31068(19) 0.1984(2) 0.48212(17) 0.0866(9) Uani 1 1 d . . . O1 O 0.3616(5) -0.0734(5) 0.2245(5) 0.051(2) Uani 1 1 d . . . N2 N 0.4199(7) 0.0849(6) 0.2210(6) 0.042(2) Uani 1 1 d . . . N3 N 0.3280(7) -0.0866(8) 0.3930(6) 0.053(3) Uani 1 1 d . . . N4 N 0.1826(7) 0.1089(7) 0.2022(6) 0.052(3) Uani 1 1 d . . . N6 N 0.2820(8) 0.1326(9) 0.3472(7) 0.065(3) Uani 1 1 d . . . N201 N 0.6361(8) 0.1431(7) 0.1914(7) 0.048(3) Uani 1 1 d . . . N202 N 0.4469(7) 0.3657(7) 0.0423(6) 0.045(2) Uani 1 1 d . . . N301 N 0.3652(9) -0.2801(7) 0.6165(7) 0.068(3) Uani 1 1 d . . . N302 N 0.1258(10) -0.1920(8) 0.5090(7) 0.061(3) Uani 1 1 d . . . N401 N -0.0311(7) 0.1241(7) 0.0934(7) 0.057(3) Uani 1 1 d . . . N402 N -0.0600(7) 0.3819(7) 0.0188(7) 0.056(3) Uani 1 1 d . . . N501 N 0.3154(13) 0.0774(13) 0.5932(12) 0.147(7) Uiso 1 1 d . . . O501 O 0.3296 -0.0369 0.6891 0.177 Uiso 1 1 d . . . N502 N 0.0982(12) 0.3154(11) 0.4818(8) 0.077(4) Uani 1 1 d . . . O201 O 0.6894(7) 0.1405(6) 0.2396(6) 0.067(3) Uani 1 1 d . . . O301 O 0.3887(9) -0.2805(8) 0.6798(6) 0.103(4) Uani 1 1 d . . . O401 O -0.0874(7) 0.0919(7) 0.1258(7) 0.087(3) Uani 1 1 d . . . C2 C 0.4742(8) 0.1074(7) 0.1838(7) 0.038(3) Uani 1 1 d . . . C3 C 0.3347(8) -0.1628(8) 0.4454(7) 0.042(3) Uani 1 1 d . . . C4 C 0.1304(8) 0.1322(8) 0.1437(8) 0.043(3) Uani 1 1 d . . . C5 C 0.2887(10) 0.1606(12) 0.3957(10) 0.071(4) Uani 1 1 d . . . C201 C 0.7645(11) -0.0607(10) 0.1838(9) 0.083(5) Uani 1 1 d . . . H20A H 0.8131 -0.1052 0.1644 0.124 Uiso 1 1 calc R . . H20B H 0.7368 -0.0993 0.2291 0.124 Uiso 1 1 calc R . . H20C H 0.7940 -0.0284 0.2046 0.124 Uiso 1 1 calc R . . C202 C 0.6876(9) 0.0170(8) 0.1123(7) 0.046(3) Uani 1 1 d . . . C203 C 0.5989(11) 0.0176(10) 0.0949(8) 0.059(4) Uani 1 1 d . . . H20D H 0.5772 -0.0370 0.1278 0.071 Uiso 1 1 calc R . . C204 C 0.5466(10) 0.1034(10) 0.0232(8) 0.063(4) Uani 1 1 d . . . H20E H 0.4825 0.1204 -0.0045 0.075 Uiso 1 1 calc R . . C205 C 0.6034(11) 0.1578(10) -0.0052(8) 0.064(4) Uani 1 1 d . . . H20F H 0.5857 0.2223 -0.0567 0.077 Uiso 1 1 calc R . . C206 C 0.6900(8) 0.1067(8) 0.0482(7) 0.041(3) Uani 1 1 d . . . H20G H 0.7447 0.1277 0.0414 0.049 Uiso 1 1 calc R . . C207 C 0.4916(8) 0.2801(9) 0.0717(7) 0.042(3) Uani 1 1 d . . . C208 C 0.3906(8) 0.4675(8) 0.0112(8) 0.047(3) Uani 1 1 d . . . C209 C 0.3798(10) 0.5224(9) -0.0759(9) 0.062(4) Uani 1 1 d . . . C210 C 0.3266(11) 0.6230(11) -0.1072(12) 0.080(5) Uani 1 1 d . . . H21A H 0.3184 0.6642 -0.1657 0.096 Uiso 1 1 calc R . . C211 C 0.2870(11) 0.6620(11) -0.0558(14) 0.083(5) Uani 1 1 d . . . H21B H 0.2489 0.7315 -0.0802 0.100 Uiso 1 1 calc R . . C212 C 0.2956(10) 0.6129(12) 0.0273(12) 0.072(4) Uani 1 1 d . . . H21C H 0.2646 0.6468 0.0601 0.087 Uiso 1 1 calc R . . C213 C 0.3528(9) 0.5071(10) 0.0666(10) 0.060(4) Uani 1 1 d . . . C214 C 0.3711(12) 0.4422(13) 0.1592(11) 0.097(5) Uani 1 1 d . . . H21D H 0.3535 0.3860 0.1707 0.145 Uiso 1 1 calc R . . H21E H 0.3328 0.4811 0.1882 0.145 Uiso 1 1 calc R . . H21F H 0.4391 0.4172 0.1794 0.145 Uiso 1 1 calc R . . C215 C 0.4232(14) 0.4737(11) -0.1317(9) 0.094(6) Uani 1 1 d . . . H21G H 0.4425 0.5192 -0.1794 0.141 Uiso 1 1 calc R . . H21H H 0.3763 0.4574 -0.1524 0.141 Uiso 1 1 calc R . . H21I H 0.4794 0.4124 -0.1000 0.141 Uiso 1 1 calc R . . C301 C 0.5108(10) -0.4979(10) 0.6632(9) 0.075(4) Uani 1 1 d . . . H30A H 0.5177 -0.5674 0.6881 0.112 Uiso 1 1 calc R . . H30B H 0.4796 -0.4668 0.6998 0.112 Uiso 1 1 calc R . . H30C H 0.5741 -0.4957 0.6570 0.112 Uiso 1 1 calc R . . C302 C 0.4522(9) -0.4434(8) 0.5798(8) 0.053(3) Uani 1 1 d . . . C303 C 0.3608(9) -0.4413(8) 0.5617(8) 0.053(3) Uani 1 1 d . . . H30D H 0.3270 -0.4794 0.6025 0.064 Uiso 1 1 calc R . . C304 C 0.3322(10) -0.3845(10) 0.4729(8) 0.061(4) Uani 1 1 d . . . H30E H 0.2728 -0.3736 0.4416 0.073 Uiso 1 1 calc R . . C305 C 0.3994(12) -0.3477(9) 0.4374(9) 0.070(4) Uani 1 1 d . . . H30F H 0.3963 -0.3053 0.3763 0.084 Uiso 1 1 calc R . . C306 C 0.4729(10) -0.3784(8) 0.5005(9) 0.058(4) Uani 1 1 d . . . H30G H 0.5323 -0.3650 0.4918 0.069 Uiso 1 1 calc R . . C307 C 0.2099(12) -0.2332(10) 0.5188(8) 0.057(4) Uani 1 1 d . . . C308 C 0.0274(10) -0.1233(10) 0.4806(9) 0.055(4) Uani 1 1 d . . . C309 C -0.0351(12) -0.1171(11) 0.5386(10) 0.073(5) Uani 1 1 d . . . C310 C -0.1287(10) -0.0434(12) 0.5095(12) 0.070(5) Uani 1 1 d . . . H31A H -0.1735 -0.0363 0.5477 0.084 Uiso 1 1 calc R . . C311 C -0.1540(14) 0.0178(14) 0.4252(13) 0.090(5) Uani 1 1 d . . . H31B H -0.2168 0.0681 0.4045 0.108 Uiso 1 1 calc R . . C312 C -0.0908(12) 0.0069(12) 0.3723(11) 0.075(4) Uani 1 1 d . . . H31C H -0.1104 0.0492 0.3140 0.090 Uiso 1 1 calc R . . C313 C 0.0021(10) -0.0632(12) 0.3986(11) 0.069(4) Uani 1 1 d . . . C314 C 0.0708(11) -0.0699(13) 0.3342(9) 0.092(5) Uani 1 1 d . . . H31D H 0.1145 -0.1396 0.3516 0.137 Uiso 1 1 calc R . . H31E H 0.1077 -0.0303 0.3304 0.137 Uiso 1 1 calc R . . H31F H 0.0345 -0.0441 0.2792 0.137 Uiso 1 1 calc R . . C315 C 0.0014(12) -0.1909(12) 0.6327(11) 0.102(6) Uani 1 1 d . . . H31G H -0.0527 -0.1857 0.6649 0.153 Uiso 1 1 calc R . . H31H H 0.0473 -0.1744 0.6544 0.153 Uiso 1 1 calc R . . H31I H 0.0326 -0.2590 0.6381 0.153 Uiso 1 1 calc R . . C401 C 0.2805(16) 0.0966(19) 0.0252(15) 0.162(9) Uani 1 1 d . . . H40A H 0.3278 0.0551 0.0026 0.243 Uiso 1 1 calc R . . H40B H 0.2955 0.0658 0.0866 0.243 Uiso 1 1 calc R . . H40C H 0.2818 0.1630 0.0017 0.243 Uiso 1 1 calc R . . C402 C 0.1835(6) 0.1055(15) 0.0022(10) 0.177(16) Uani 1 1 d G . . C403 C 0.1328(12) 0.2073(13) -0.0539(11) 0.22(2) Uani 1 1 d G . . H40D H 0.1562 0.2617 -0.0687 0.266 Uiso 1 1 calc R . . C404 C 0.0447(11) 0.2176(7) -0.0878(7) 0.160(12) Uani 1 1 d G . . H40E H -0.0047 0.2803 -0.1310 0.193 Uiso 1 1 calc R . . C405 C 0.0409(7) 0.1221(9) -0.0526(8) 0.070(4) Uani 1 1 d G . . H40F H -0.0116 0.1060 -0.0666 0.084 Uiso 1 1 calc R . . C406 C 0.1267(9) 0.0529(7) 0.0030(7) 0.084(5) Uani 1 1 d G . . H40G H 0.1450 -0.0205 0.0355 0.100 Uiso 1 1 calc R . . C407 C -0.0151(8) 0.3003(10) 0.0297(7) 0.051(3) Uani 1 1 d . . . C408 C -0.1168(8) 0.4779(9) 0.0068(9) 0.050(3) Uani 1 1 d . . . C409 C -0.1441(10) 0.5514(10) -0.0765(11) 0.073(5) Uani 1 1 d . . . C410 C -0.2090(13) 0.6482(12) -0.0814(16) 0.118(9) Uani 1 1 d . . . H41A H -0.2317 0.7044 -0.1345 0.142 Uiso 1 1 calc R . . C411 C -0.236(2) 0.658(3) -0.013(3) 0.17(2) Uani 1 1 d . . . H41B H -0.2758 0.7241 -0.0212 0.210 Uiso 1 1 calc R . . C412 C -0.218(2) 0.596(3) 0.059(2) 0.134(14) Uani 1 1 d . . . H41C H -0.2473 0.6115 0.1030 0.160 Uiso 1 1 calc R . . C413 C -0.1489(13) 0.4942(16) 0.0773(12) 0.085(5) Uani 1 1 d . . . C414 C -0.1172(15) 0.4081(19) 0.1630(12) 0.153(10) Uani 1 1 d . . . H41D H -0.0473 0.3756 0.1729 0.229 Uiso 1 1 calc R . . H41E H -0.1437 0.3600 0.1664 0.229 Uiso 1 1 calc R . . H41F H -0.1401 0.4323 0.2056 0.229 Uiso 1 1 calc R . . C415 C -0.1095(12) 0.5292(14) -0.1481(10) 0.112(7) Uani 1 1 d . . . H41G H -0.0403 0.4904 -0.1359 0.167 Uiso 1 1 calc R . . H41H H -0.1241 0.5917 -0.1988 0.167 Uiso 1 1 calc R . . H41I H -0.1414 0.4908 -0.1571 0.167 Uiso 1 1 calc R . . C506 C 0.3469(18) 0.3039(18) 0.4147(13) 0.154(11) Uani 1 1 d G . . H50A H 0.3178 0.3540 0.3557 0.184 Uiso 1 1 calc R . . C505 C 0.334(2) 0.322(3) 0.487(2) 1.06(16) Uani 1 1 d G . . H50B H 0.2838 0.3820 0.4903 1.271 Uiso 1 1 calc R . . C504 C 0.395(3) 0.235(4) 0.5565(12) 1.16(19) Uani 1 1 d G . . H50C H 0.3925 0.2218 0.6169 1.390 Uiso 1 1 calc R . . C503 C 0.446(2) 0.1628(18) 0.527(3) 0.39(4) Uani 1 1 d G . . H50D H 0.4945 0.0940 0.5616 0.470 Uiso 1 1 calc R . . C502 C 0.416(2) 0.205(2) 0.439(3) 0.66(9) Uiso 1 1 d G . . C501 C 0.4476 0.2204 0.3599 0.796 Uiso 1 1 d . . . H50E H 0.4244 0.1870 0.3352 0.995 Uiso 1 1 calc R . . H50F H 0.5176 0.1929 0.3667 0.995 Uiso 1 1 calc R . . H50G H 0.4226 0.2920 0.3227 0.995 Uiso 1 1 calc R . . C507 C 0.1805(14) 0.2669(13) 0.4786(10) 0.080(5) Uani 1 1 d . . . C508 C 0.0096(11) 0.3696(12) 0.4936(11) 0.069(4) Uani 1 1 d . . . C509 C -0.0533(17) 0.4529(15) 0.4212(11) 0.096(6) Uani 1 1 d . . . C510 C -0.1420(19) 0.506(2) 0.440(2) 0.134(10) Uani 1 1 d . . . H51A H -0.1875 0.5624 0.3955 0.161 Uiso 1 1 calc R . . C511 C -0.163(2) 0.480(3) 0.513(3) 0.163(15) Uani 1 1 d . . . H51B H -0.2242 0.5176 0.5226 0.196 Uiso 1 1 calc R . . C512 C -0.0980(18) 0.3973(19) 0.5833(15) 0.109(7) Uani 1 1 d . . . H51C H -0.1158 0.3812 0.6382 0.131 Uiso 1 1 calc R . . C513 C -0.0127(12) 0.3419(12) 0.5729(11) 0.069(4) Uani 1 1 d . . . C514 C 0.0584(12) 0.2543(12) 0.6436(10) 0.088(5) Uani 1 1 d . . . H51D H 0.0916 0.2016 0.6258 0.131 Uiso 1 1 calc R . . H51E H 0.0255 0.2296 0.6915 0.131 Uiso 1 1 calc R . . H51F H 0.1049 0.2742 0.6602 0.131 Uiso 1 1 calc R . . C515 C -0.0252(18) 0.4781(18) 0.3391(13) 0.160(10) Uani 1 1 d . . . H51G H 0.0321 0.4226 0.3401 0.240 Uiso 1 1 calc R . . H51H H -0.0114 0.5377 0.3215 0.240 Uiso 1 1 calc R . . H51I H -0.0770 0.4913 0.2995 0.240 Uiso 1 1 calc R . . P1 P 0.2208(3) -0.2495(3) 0.1960(2) 0.0612(11) Uani 1 1 d . . . P2 P 0.6255(3) 0.7155(2) 0.2387(2) 0.0516(9) Uani 1 1 d . . . F1 F 0.2475(9) -0.2926(11) 0.2908(6) 0.169(6) Uani 1 1 d . . . F2 F 0.2528(8) -0.1627(9) 0.1837(9) 0.149(5) Uani 1 1 d . . . F3 F 0.1869(7) -0.3326(7) 0.2057(6) 0.112(3) Uani 1 1 d . . . F4 F 0.1169(6) -0.1877(8) 0.2052(6) 0.115(4) Uani 1 1 d . . . F5 F 0.3259(5) -0.3125(6) 0.1846(5) 0.091(3) Uani 1 1 d . . . F6 F 0.1893(5) -0.1990(5) 0.0979(4) 0.068(2) Uani 1 1 d . . . F7 F 0.6442(9) 0.7608(7) 0.1439(6) 0.144(5) Uani 1 1 d . . . F8 F 0.5372(7) 0.7073(7) 0.2113(7) 0.126(4) Uani 1 1 d . . . F9 F 0.7155(6) 0.7263(7) 0.2630(8) 0.130(4) Uani 1 1 d . . . F10 F 0.6089(8) 0.6715(6) 0.3334(5) 0.101(3) Uani 1 1 d . . . F11 F 0.6894(6) 0.6067(5) 0.2509(5) 0.084(3) Uani 1 1 d . . . F12 F 0.5618(5) 0.8266(5) 0.2262(6) 0.096(3) Uani 1 1 d . . . 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 0.0350(10) 0.0289(9) 0.0283(9) -0.0091(7) 0.0103(7) -0.0126(8) Mn2 0.0462(11) 0.0338(10) 0.0362(10) -0.0113(8) 0.0149(8) -0.0206(9) Mn3 0.0686(13) 0.0320(10) 0.0328(10) -0.0079(8) 0.0080(9) -0.0222(10) Mn4 0.0441(11) 0.0368(10) 0.0474(11) -0.0103(8) -0.0010(9) -0.0123(9) Mn5 0.101(2) 0.128(2) 0.105(2) -0.0859(18) 0.0590(16) -0.0850(18) O1 0.048(5) 0.043(5) 0.062(5) -0.030(4) 0.010(4) -0.011(4) N2 0.047(6) 0.031(5) 0.056(6) -0.022(5) 0.032(5) -0.022(5) N3 0.045(6) 0.051(7) 0.044(6) -0.010(5) 0.009(5) -0.013(5) N4 0.043(6) 0.051(7) 0.042(6) -0.006(5) 0.000(5) -0.015(5) N6 0.083(9) 0.083(9) 0.071(8) -0.047(7) 0.046(7) -0.063(7) N201 0.061(7) 0.045(6) 0.046(7) -0.022(5) 0.017(5) -0.028(6) N202 0.046(6) 0.033(6) 0.055(6) -0.015(5) 0.010(5) -0.021(5) N301 0.118(10) 0.050(7) 0.038(7) -0.017(5) 0.015(7) -0.039(7) N302 0.077(9) 0.062(8) 0.074(8) -0.040(6) 0.046(7) -0.051(8) N401 0.048(7) 0.040(6) 0.063(7) -0.003(5) 0.005(6) -0.019(5) N402 0.050(7) 0.024(6) 0.068(7) -0.006(5) -0.018(5) -0.001(5) N502 0.107(12) 0.098(11) 0.084(10) -0.063(8) 0.036(9) -0.076(10) O201 0.079(7) 0.064(6) 0.054(6) -0.021(5) 0.002(5) -0.029(5) O301 0.174(12) 0.083(8) 0.043(6) -0.027(6) 0.003(7) -0.042(8) O401 0.061(7) 0.073(7) 0.106(9) -0.013(6) 0.016(6) -0.035(6) C2 0.050(7) 0.028(6) 0.034(6) -0.010(5) 0.010(6) -0.018(6) C3 0.044(7) 0.031(7) 0.035(7) -0.011(6) 0.010(5) -0.006(6) C4 0.041(7) 0.031(6) 0.045(8) -0.013(6) 0.017(6) -0.008(6) C5 0.075(10) 0.110(13) 0.083(11) -0.071(10) 0.058(9) -0.067(10) C201 0.084(11) 0.068(10) 0.075(11) -0.037(9) 0.011(9) -0.002(9) C202 0.056(8) 0.025(6) 0.041(7) -0.013(5) 0.009(6) -0.003(6) C203 0.092(11) 0.056(9) 0.062(9) -0.041(8) 0.047(8) -0.049(8) C204 0.073(10) 0.068(10) 0.040(8) -0.020(7) 0.010(7) -0.024(8) C205 0.087(11) 0.044(8) 0.041(8) -0.010(6) 0.025(8) -0.018(8) C206 0.040(7) 0.030(6) 0.054(8) -0.023(6) 0.021(6) -0.012(6) C207 0.045(7) 0.045(8) 0.045(7) -0.022(6) 0.017(6) -0.025(6) C208 0.044(7) 0.031(7) 0.073(9) -0.027(7) 0.003(7) -0.017(6) C209 0.065(9) 0.039(8) 0.063(9) 0.005(7) -0.005(7) -0.030(7) C210 0.069(11) 0.045(10) 0.133(16) -0.033(10) 0.034(11) -0.038(9) C211 0.064(11) 0.036(9) 0.122(16) -0.010(10) 0.008(11) -0.018(8) C212 0.051(9) 0.079(12) 0.120(15) -0.076(11) 0.017(9) -0.023(9) C213 0.056(9) 0.057(9) 0.081(11) -0.050(8) -0.001(8) -0.012(7) C214 0.105(14) 0.118(15) 0.096(14) -0.073(12) 0.038(11) -0.047(12) C215 0.178(18) 0.063(10) 0.050(9) -0.027(8) 0.039(11) -0.057(11) C301 0.082(11) 0.060(9) 0.069(10) -0.028(8) -0.019(8) -0.012(8) C302 0.060(9) 0.035(7) 0.057(9) -0.015(6) 0.004(7) -0.019(7) C303 0.065(9) 0.033(7) 0.048(8) -0.004(6) 0.017(7) -0.022(7) C304 0.056(9) 0.070(9) 0.054(9) -0.022(7) -0.003(7) -0.026(8) C305 0.105(13) 0.039(8) 0.043(8) -0.015(6) -0.007(9) -0.006(8) C306 0.057(9) 0.033(7) 0.076(10) -0.023(7) 0.021(8) -0.012(6) C307 0.088(11) 0.052(8) 0.061(9) -0.033(7) 0.048(8) -0.054(9) C308 0.059(9) 0.059(9) 0.068(10) -0.043(8) 0.038(8) -0.030(8) C309 0.092(12) 0.074(10) 0.098(13) -0.053(10) 0.047(10) -0.064(10) C310 0.043(9) 0.093(12) 0.125(15) -0.085(11) 0.059(9) -0.042(9) C311 0.108(15) 0.122(15) 0.096(15) -0.065(13) 0.022(12) -0.084(13) C312 0.073(12) 0.089(12) 0.077(12) -0.037(9) 0.002(9) -0.043(10) C313 0.047(9) 0.084(11) 0.096(13) -0.062(10) 0.012(9) -0.022(8) C314 0.072(11) 0.134(15) 0.057(10) -0.044(10) 0.019(8) -0.027(11) C315 0.114(15) 0.105(13) 0.109(15) -0.056(12) 0.072(12) -0.060(12) C401 0.15(2) 0.24(3) 0.15(2) -0.11(2) 0.015(17) -0.09(2) C402 0.026(9) 0.36(4) 0.21(3) -0.26(3) -0.021(12) 0.012(15) C403 0.23(3) 0.42(5) 0.36(4) -0.36(4) 0.26(3) -0.29(4) C404 0.34(4) 0.043(11) 0.061(12) -0.020(9) 0.030(17) -0.036(15) C405 0.051(9) 0.066(10) 0.096(11) -0.050(9) -0.017(8) -0.006(8) C406 0.102(13) 0.057(9) 0.075(11) -0.039(8) 0.018(10) -0.003(9) C407 0.036(7) 0.050(8) 0.040(7) 0.006(6) -0.015(6) -0.017(6) C408 0.039(7) 0.052(8) 0.068(9) -0.026(7) -0.003(7) -0.026(7) C409 0.057(9) 0.041(9) 0.100(13) -0.002(8) 0.008(9) -0.030(8) C410 0.068(13) 0.040(10) 0.19(2) 0.014(12) -0.026(14) -0.031(10) C411 0.11(2) 0.23(4) 0.34(6) -0.23(5) 0.10(4) -0.11(3) C412 0.13(2) 0.23(4) 0.20(3) -0.19(3) 0.11(3) -0.13(3) C413 0.090(13) 0.133(16) 0.102(15) -0.086(13) 0.031(11) -0.078(12) C414 0.16(2) 0.28(3) 0.063(13) -0.067(17) 0.023(13) -0.14(2) C415 0.076(12) 0.143(17) 0.063(11) -0.008(11) 0.010(9) -0.031(12) C506 0.18(2) 0.25(3) 0.128(19) -0.13(2) 0.016(17) -0.12(3) C505 0.47(16) 0.8(2) 1.9(5) -0.4(3) 0.3(2) -0.40(15) C504 0.39(11) 2.0(5) 0.74(19) -0.4(2) 0.50(13) -0.40(18) C503 0.15(3) 0.25(4) 0.70(10) -0.07(5) -0.17(4) -0.14(3) C507 0.110(14) 0.111(14) 0.076(11) -0.072(11) 0.040(11) -0.069(13) C508 0.054(10) 0.085(11) 0.094(13) -0.050(10) 0.013(9) -0.043(9) C509 0.132(18) 0.105(15) 0.057(11) -0.012(10) -0.030(12) -0.076(14) C510 0.076(18) 0.12(2) 0.21(3) -0.06(2) -0.033(19) -0.043(16) C511 0.11(2) 0.16(3) 0.28(5) -0.12(3) 0.07(3) -0.10(2) C512 0.110(18) 0.137(19) 0.128(19) -0.058(16) 0.043(15) -0.098(17) C513 0.063(11) 0.089(12) 0.084(12) -0.048(10) 0.040(10) -0.050(10) C514 0.118(14) 0.091(12) 0.082(12) -0.048(10) 0.023(11) -0.060(12) C515 0.23(3) 0.21(3) 0.086(16) -0.067(16) -0.007(17) -0.14(2) P1 0.062(3) 0.086(3) 0.043(2) -0.0256(19) 0.0043(18) -0.039(2) P2 0.059(2) 0.0314(18) 0.053(2) -0.0070(15) 0.0061(17) -0.0183(17) F1 0.156(10) 0.270(15) 0.042(6) -0.038(8) -0.027(6) -0.076(11) F2 0.151(10) 0.173(11) 0.212(13) -0.126(10) 0.018(9) -0.105(9) F3 0.132(8) 0.109(7) 0.099(7) -0.012(6) 0.023(6) -0.089(7) F4 0.085(7) 0.186(10) 0.100(7) -0.108(7) 0.024(5) -0.030(7) F5 0.052(5) 0.097(6) 0.098(7) -0.031(5) -0.001(5) -0.015(5) F6 0.057(5) 0.064(5) 0.057(5) -0.011(4) 0.008(4) -0.014(4) F7 0.191(11) 0.081(7) 0.069(7) 0.002(5) 0.049(7) -0.004(7) F8 0.097(7) 0.098(7) 0.177(11) -0.049(7) -0.040(7) -0.039(6) F9 0.076(6) 0.078(6) 0.235(13) -0.057(7) -0.002(7) -0.039(5) F10 0.171(9) 0.058(5) 0.069(6) -0.026(4) 0.048(6) -0.046(6) F11 0.120(7) 0.037(4) 0.074(6) -0.021(4) 0.007(5) -0.014(4) F12 0.068(5) 0.036(4) 0.139(8) -0.009(5) 0.038(5) -0.010(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 N4 2.096(10) . ? Mn1 N3 2.099(10) . ? Mn1 N2 2.111(9) . ? Mn1 N6 2.176(12) . ? Mn1 O1 2.293(8) . ? Mn2 N201 1.634(12) . ? Mn2 C207 1.902(13) . ? Mn2 C2 1.982(12) . ? Mn2 C203 2.116(12) . ? Mn2 C204 2.138(14) . ? Mn2 C205 2.146(13) . ? Mn2 C202 2.148(11) . ? Mn2 C206 2.156(11) . ? Mn3 N301 1.651(12) . ? Mn3 C307 1.861(16) . ? Mn3 C3 1.948(11) . ? Mn3 C303 2.152(11) . ? Mn3 C306 2.155(12) . ? Mn3 C302 2.191(12) . ? Mn3 C304 2.203(14) . ? Mn3 C305 2.208(14) . ? Mn4 N401 1.649(11) . ? Mn4 C407 1.918(14) . ? Mn4 C4 1.932(14) . ? Mn4 C404 2.144(12) . ? Mn4 C405 2.147(10) . ? Mn4 C403 2.154(12) . ? Mn4 C406 2.159(10) . ? Mn4 C402 2.163(11) . ? Mn5 C502 1.77(5) . ? Mn5 C507 1.86(2) . ? Mn5 C506 1.89(3) . ? Mn5 C5 1.949(16) . ? Mn5 C503 2.023(18) . ? Mn5 N501 2.091(18) . ? Mn5 C505 2.19(4) . ? Mn5 C504 2.26(4) . ? N2 C2 1.110(12) . ? N3 C3 1.158(13) . ? N4 C4 1.169(14) . ? N6 C5 1.146(15) . ? N201 O201 1.181(12) . ? N202 C207 1.164(13) . ? N202 C208 1.395(14) . ? N301 O301 1.188(13) . ? N302 C307 1.182(16) . ? N302 C308 1.441(18) . ? N401 O401 1.177(12) . ? N402 C407 1.163(14) . ? N402 C408 1.382(15) . ? N501 O501 1.852(18) . ? O501 O201 1.742(9) 2_656 ? N502 C507 1.215(19) . ? N502 C508 1.366(19) . ? O201 O501 1.742(9) 2_656 ? C201 C202 1.495(17) . ? C202 C203 1.397(17) . ? C202 C206 1.429(14) . ? C203 C204 1.393(18) . ? C204 C205 1.395(18) . ? C205 C206 1.397(17) . ? C208 C213 1.375(17) . ? C208 C209 1.397(17) . ? C209 C210 1.372(18) . ? C209 C215 1.491(19) . ? C210 C211 1.31(2) . ? C211 C212 1.33(2) . ? C212 C213 1.443(19) . ? C213 C214 1.50(2) . ? C301 C302 1.477(17) . ? C302 C303 1.430(17) . ? C302 C306 1.465(17) . ? C303 C304 1.432(17) . ? C304 C305 1.376(18) . ? C305 C306 1.406(18) . ? C308 C313 1.336(19) . ? C308 C309 1.377(18) . ? C309 C310 1.408(19) . ? C309 C315 1.55(2) . ? C310 C311 1.37(2) . ? C311 C312 1.33(2) . ? C312 C313 1.381(19) . ? C313 C314 1.522(19) . ? C401 C402 1.49(2) . ? C402 C406 1.4200 . ? C402 C403 1.4200 . ? C403 C404 1.4200 . ? C404 C405 1.4200 . ? C405 C406 1.4200 . ? C408 C409 1.402(18) . ? C408 C413 1.41(2) . ? C409 C410 1.46(2) . ? C409 C415 1.48(2) . ? C410 C411 1.32(4) . ? C411 C412 1.21(5) . ? C412 C413 1.48(3) . ? C413 C414 1.50(2) . ? C506 C502 1.4200 . ? C506 C505 1.4200 . ? C505 C504 1.4200 . ? C504 C503 1.4200 . ? C503 C502 1.4200 . ? C502 C501 1.42(5) . ? C508 C513 1.35(2) . ? C508 C509 1.43(2) . ? C509 C510 1.41(3) . ? C509 C515 1.43(3) . ? C510 C511 1.26(4) . ? C511 C512 1.42(4) . ? C512 C513 1.33(2) . ? C513 C514 1.49(2) . ? P1 F1 1.527(9) . ? P1 F3 1.554(9) . ? P1 F4 1.565(9) . ? P1 F2 1.580(10) . ? P1 F6 1.581(8) . ? P1 F5 1.597(9) . ? P2 F8 1.521(9) . ? P2 F9 1.549(9) . ? P2 F11 1.572(8) . ? P2 F10 1.574(8) . ? P2 F7 1.588(9) . ? P2 F12 1.601(8) . ? 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 N4 Mn1 N3 116.4(4) . . ? N4 Mn1 N2 113.1(4) . . ? N3 Mn1 N2 128.6(4) . . ? N4 Mn1 N6 99.4(5) . . ? N3 Mn1 N6 91.5(4) . . ? N2 Mn1 N6 93.7(4) . . ? N4 Mn1 O1 87.8(4) . . ? N3 Mn1 O1 83.7(4) . . ? N2 Mn1 O1 85.0(3) . . ? N6 Mn1 O1 172.6(4) . . ? N201 Mn2 C207 96.8(5) . . ? N201 Mn2 C2 99.1(5) . . ? C207 Mn2 C2 90.7(4) . . ? N201 Mn2 C203 125.2(6) . . ? C207 Mn2 C203 137.9(6) . . ? C2 Mn2 C203 85.3(5) . . ? N201 Mn2 C204 157.9(5) . . ? C207 Mn2 C204 100.7(5) . . ? C2 Mn2 C204 94.1(5) . . ? C203 Mn2 C204 38.2(5) . . ? N201 Mn2 C205 129.8(5) . . ? C207 Mn2 C205 89.3(5) . . ? C2 Mn2 C205 130.7(5) . . ? C203 Mn2 C205 63.3(5) . . ? C204 Mn2 C205 38.0(5) . . ? N201 Mn2 C202 93.8(5) . . ? C207 Mn2 C202 151.9(5) . . ? C2 Mn2 C202 113.2(4) . . ? C203 Mn2 C202 38.2(5) . . ? C204 Mn2 C202 64.6(5) . . ? C205 Mn2 C202 64.1(5) . . ? N201 Mn2 C206 96.5(5) . . ? C207 Mn2 C206 113.9(4) . . ? C2 Mn2 C206 149.0(4) . . ? C203 Mn2 C206 63.8(4) . . ? C204 Mn2 C206 64.1(5) . . ? C205 Mn2 C206 37.9(5) . . ? C202 Mn2 C206 38.8(4) . . ? N301 Mn3 C307 98.3(6) . . ? N301 Mn3 C3 99.8(5) . . ? C307 Mn3 C3 86.3(5) . . ? N301 Mn3 C303 111.0(5) . . ? C307 Mn3 C303 98.5(5) . . ? C3 Mn3 C303 147.6(5) . . ? N301 Mn3 C306 110.4(6) . . ? C307 Mn3 C306 150.4(6) . . ? C3 Mn3 C306 95.5(5) . . ? C303 Mn3 C306 65.0(5) . . ? N301 Mn3 C302 92.1(5) . . ? C307 Mn3 C302 135.7(5) . . ? C3 Mn3 C302 134.1(5) . . ? C303 Mn3 C302 38.4(4) . . ? C306 Mn3 C302 39.4(4) . . ? N301 Mn3 C304 149.4(5) . . ? C307 Mn3 C304 88.8(5) . . ? C3 Mn3 C304 110.3(5) . . ? C303 Mn3 C304 38.4(5) . . ? C306 Mn3 C304 62.8(5) . . ? C302 Mn3 C304 63.3(5) . . ? N301 Mn3 C305 147.9(6) . . ? C307 Mn3 C305 113.7(6) . . ? C3 Mn3 C305 85.3(5) . . ? C303 Mn3 C305 63.3(5) . . ? C306 Mn3 C305 37.6(5) . . ? C302 Mn3 C305 63.5(5) . . ? C304 Mn3 C305 36.4(5) . . ? N401 Mn4 C407 97.4(5) . . ? N401 Mn4 C4 98.8(5) . . ? C407 Mn4 C4 91.4(5) . . ? N401 Mn4 C404 119.8(6) . . ? C407 Mn4 C404 89.1(5) . . ? C4 Mn4 C404 141.0(6) . . ? N401 Mn4 C405 92.7(5) . . ? C407 Mn4 C405 121.5(5) . . ? C4 Mn4 C405 143.4(4) . . ? C404 Mn4 C405 38.65(18) . . ? N401 Mn4 C403 156.8(5) . . ? C407 Mn4 C403 91.4(5) . . ? C4 Mn4 C403 102.4(6) . . ? C404 Mn4 C403 38.58(19) . . ? C405 Mn4 C403 64.6(2) . . ? N401 Mn4 C406 101.2(5) . . ? C407 Mn4 C406 152.9(5) . . ? C4 Mn4 C406 104.9(5) . . ? C404 Mn4 C406 64.5(2) . . ? C405 Mn4 C406 38.51(16) . . ? C403 Mn4 C406 64.4(2) . . ? N401 Mn4 C402 136.9(6) . . ? C407 Mn4 C402 125.6(6) . . ? C4 Mn4 C402 84.1(4) . . ? C404 Mn4 C402 64.5(2) . . ? C405 Mn4 C402 64.4(2) . . ? C403 Mn4 C402 38.40(18) . . ? C406 Mn4 C402 38.36(17) . . ? C502 Mn5 C507 146.0(13) . . ? C502 Mn5 C506 45.5(8) . . ? C507 Mn5 C506 101.4(9) . . ? C502 Mn5 C5 86.8(9) . . ? C507 Mn5 C5 92.3(6) . . ? C506 Mn5 C5 98.4(7) . . ? C502 Mn5 C503 43.3(5) . . ? C507 Mn5 C503 147.9(15) . . ? C506 Mn5 C503 71.8(6) . . ? C5 Mn5 C503 119.5(16) . . ? C502 Mn5 N501 121.4(13) . . ? C507 Mn5 N501 91.9(7) . . ? C506 Mn5 N501 154.5(7) . . ? C5 Mn5 N501 102.7(7) . . ? C503 Mn5 N501 85.3(10) . . ? C502 Mn5 C505 70.0(6) . . ? C507 Mn5 C505 88.5(9) . . ? C506 Mn5 C505 39.9(7) . . ? C5 Mn5 C505 137.1(10) . . ? C503 Mn5 C505 65.9(8) . . ? N501 Mn5 C505 120.2(10) . . ? C502 Mn5 C504 68.2(5) . . ? C507 Mn5 C504 109.9(12) . . ? C506 Mn5 C504 66.5(8) . . ? C5 Mn5 C504 154.8(10) . . ? C503 Mn5 C504 38.2(6) . . ? N501 Mn5 C504 88.6(11) . . ? C505 Mn5 C504 37.1(7) . . ? C2 N2 Mn1 173.8(10) . . ? C3 N3 Mn1 168.0(10) . . ? C4 N4 Mn1 157.2(10) . . ? C5 N6 Mn1 160.9(13) . . ? O201 N201 Mn2 172.6(10) . . ? C207 N202 C208 176.6(12) . . ? O301 N301 Mn3 173.7(12) . . ? C307 N302 C308 166.4(12) . . ? O401 N401 Mn4 177.0(11) . . ? C407 N402 C408 177.4(13) . . ? O501 N501 Mn5 174.8(11) . . ? O201 O501 N501 160.9(7) 2_656 . ? C507 N502 C508 173.4(15) . . ? N201 O201 O501 84.8(7) . 2_656 ? N2 C2 Mn2 178.0(10) . . ? N3 C3 Mn3 178.2(11) . . ? N4 C4 Mn4 176.8(11) . . ? N6 C5 Mn5 175.0(15) . . ? C203 C202 C206 106.0(11) . . ? C203 C202 C201 127.4(12) . . ? C206 C202 C201 126.6(13) . . ? C203 C202 Mn2 69.7(7) . . ? C206 C202 Mn2 70.9(6) . . ? C201 C202 Mn2 123.7(9) . . ? C204 C203 C202 110.4(11) . . ? C204 C203 Mn2 71.7(8) . . ? C202 C203 Mn2 72.1(7) . . ? C203 C204 C205 106.7(13) . . ? C203 C204 Mn2 70.1(8) . . ? C205 C204 Mn2 71.3(8) . . ? C204 C205 C206 109.3(11) . . ? C204 C205 Mn2 70.7(7) . . ? C206 C205 Mn2 71.4(7) . . ? C205 C206 C202 107.6(11) . . ? C205 C206 Mn2 70.7(7) . . ? C202 C206 Mn2 70.3(6) . . ? N202 C207 Mn2 175.1(10) . . ? C213 C208 N202 119.2(12) . . ? C213 C208 C209 124.9(12) . . ? N202 C208 C209 115.9(12) . . ? C210 C209 C208 116.5(15) . . ? C210 C209 C215 121.9(14) . . ? C208 C209 C215 121.6(12) . . ? C211 C210 C209 119.7(17) . . ? C210 C211 C212 125.9(16) . . ? C211 C212 C213 118.7(14) . . ? C208 C213 C212 114.3(13) . . ? C208 C213 C214 120.7(12) . . ? C212 C213 C214 124.9(14) . . ? C303 C302 C306 106.2(11) . . ? C303 C302 C301 125.9(12) . . ? C306 C302 C301 127.9(12) . . ? C303 C302 Mn3 69.3(7) . . ? C306 C302 Mn3 69.0(6) . . ? C301 C302 Mn3 124.6(9) . . ? C302 C303 C304 107.4(11) . . ? C302 C303 Mn3 72.3(7) . . ? C304 C303 Mn3 72.7(7) . . ? C305 C304 C303 109.2(12) . . ? C305 C304 Mn3 72.0(8) . . ? C303 C304 Mn3 68.9(7) . . ? C304 C305 C306 109.4(12) . . ? C304 C305 Mn3 71.6(9) . . ? C306 C305 Mn3 69.2(7) . . ? C305 C306 C302 107.4(12) . . ? C305 C306 Mn3 73.3(8) . . ? C302 C306 Mn3 71.6(7) . . ? N302 C307 Mn3 176.8(11) . . ? C313 C308 C309 122.6(15) . . ? C313 C308 N302 117.7(12) . . ? C309 C308 N302 119.5(14) . . ? C308 C309 C310 118.1(15) . . ? C308 C309 C315 118.6(15) . . ? C310 C309 C315 123.4(14) . . ? C311 C310 C309 118.9(14) . . ? C312 C311 C310 120.0(18) . . ? C311 C312 C313 122.8(17) . . ? C308 C313 C312 117.5(15) . . ? C308 C313 C314 122.8(13) . . ? C312 C313 C314 119.7(16) . . ? C406 C402 C403 108.0 . . ? C406 C402 C401 145.5(17) . . ? C403 C402 C401 105.4(17) . . ? C406 C402 Mn4 70.6(4) . . ? C403 C402 Mn4 70.4(5) . . ? C401 C402 Mn4 130.0(12) . . ? C404 C403 C402 108.0 . . ? C404 C403 Mn4 70.3(4) . . ? C402 C403 Mn4 71.2(4) . . ? C403 C404 C405 108.0 . . ? C403 C404 Mn4 71.1(4) . . ? C405 C404 Mn4 70.8(4) . . ? C406 C405 C404 108.0 . . ? C406 C405 Mn4 71.2(4) . . ? C404 C405 Mn4 70.6(4) . . ? C402 C406 C405 108.0 . . ? C402 C406 Mn4 71.0(4) . . ? C405 C406 Mn4 70.3(4) . . ? N402 C407 Mn4 175.4(11) . . ? N402 C408 C409 116.9(13) . . ? N402 C408 C413 118.5(13) . . ? C409 C408 C413 124.4(15) . . ? C408 C409 C410 111.7(17) . . ? C408 C409 C415 121.9(14) . . ? C410 C409 C415 126.3(16) . . ? C411 C410 C409 121(3) . . ? C412 C411 C410 130(4) . . ? C411 C412 C413 117(3) . . ? C408 C413 C412 116.0(18) . . ? C408 C413 C414 119.2(18) . . ? C412 C413 C414 125(2) . . ? C502 C506 C505 108.0 . . ? C502 C506 Mn5 62.8(17) . . ? C505 C506 Mn5 82(2) . . ? C504 C505 C506 108.0 . . ? C504 C505 Mn5 74.2(8) . . ? C506 C505 Mn5 58.6(18) . . ? C505 C504 C503 108.0 . . ? C505 C504 Mn5 68.7(8) . . ? C503 C504 Mn5 61.7(16) . . ? C502 C503 C504 108.0 . . ? C502 C503 Mn5 58.8(18) . . ? C504 C503 Mn5 80(2) . . ? C501 C502 C503 145(2) . . ? C501 C502 C506 97(3) . . ? C503 C502 C506 108.0 . . ? C501 C502 Mn5 135.1(19) . . ? C503 C502 Mn5 77.8(15) . . ? C506 C502 Mn5 71.7(13) . . ? N502 C507 Mn5 173.0(13) . . ? C513 C508 N502 117.8(15) . . ? C513 C508 C509 124.3(18) . . ? N502 C508 C509 117.8(18) . . ? C510 C509 C515 125(2) . . ? C510 C509 C508 114(2) . . ? C515 C509 C508 121(2) . . ? C511 C510 C509 122(3) . . ? C510 C511 C512 122(3) . . ? C513 C512 C511 121(2) . . ? C512 C513 C508 116.9(18) . . ? C512 C513 C514 123.2(18) . . ? C508 C513 C514 119.9(15) . . ? F1 P1 F3 92.1(7) . . ? F1 P1 F4 89.0(6) . . ? F3 P1 F4 87.8(6) . . ? F1 P1 F2 89.4(7) . . ? F3 P1 F2 178.2(7) . . ? F4 P1 F2 91.2(6) . . ? F1 P1 F6 176.7(7) . . ? F3 P1 F6 89.7(5) . . ? F4 P1 F6 88.3(5) . . ? F2 P1 F6 88.8(6) . . ? F1 P1 F5 92.2(6) . . ? F3 P1 F5 91.6(6) . . ? F4 P1 F5 178.6(5) . . ? F2 P1 F5 89.4(6) . . ? F6 P1 F5 90.4(4) . . ? F8 P2 F9 177.8(7) . . ? F8 P2 F11 90.8(5) . . ? F9 P2 F11 89.7(5) . . ? F8 P2 F10 91.1(6) . . ? F9 P2 F10 91.1(7) . . ? F11 P2 F10 89.1(4) . . ? F8 P2 F7 90.4(7) . . ? F9 P2 F7 87.4(7) . . ? F11 P2 F7 91.3(5) . . ? F10 P2 F7 178.4(7) . . ? F8 P2 F12 90.0(5) . . ? F9 P2 F12 89.5(5) . . ? F11 P2 F12 179.2(5) . . ? F10 P2 F12 91.2(5) . . ? F7 P2 F12 88.4(5) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.271 _refine_diff_density_min -2.473 _refine_diff_density_rms 0.133 #===END