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 'Spyros Perlepes' 'Albert Escuer' 'Panayotis Kyritsis' 'Constantinos J. Milios' 'Catherine Raptopoulou' 'Aris Terzis' 'Ramon Vicente' _publ_contact_author_name 'ProfD Spyros Perlepes' _publ_contact_author_address ; Department of Chemistry University of Patras Patras GR-26504 GREECE ; _publ_contact_author_email PERLEPES@PATREAS.UPATRAS.GR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Di-2-pyridyl ketone oxime [(py)2CNOH] in manganese carboxylate chemistry: mononuclear, dinuclear and tetranuclear complexes, and partial transformation of (py)2CNOH to the gem-diolate(-2) form of di-2-pyridyl ketone leading to the formation of NO3- ; data_pekm593 _database_code_depnum_ccdc_archive 'CCDC 187284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H45 Br2 Mn4 N11 O10' _chemical_formula_weight 1459.65 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.735(7) _cell_length_b 12.824(6) _cell_length_c 19.091(9) _cell_angle_alpha 102.08(2) _cell_angle_beta 99.75(2) _cell_angle_gamma 105.42(2) _cell_volume 3078(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.1 _cell_measurement_theta_max 11.6 _exptl_crystal_description parallelipiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.56 _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 2.166 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.9 _diffrn_reflns_number 9997 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 24.00 _reflns_number_total 9664 _reflns_number_gt 7420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Program COLLECT (UCLA Crystal.package, C.E.Strouse 1994)' _computing_cell_refinement 'Program LEAST (UCLA Crystal.package, C.E.Strouse 1994)' _computing_data_reduction 'Program REDUCE (UCLA Crystal.package, C.E.Strouse 1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+6.8180P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9664 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.36805(5) 0.46431(5) 0.00121(4) 0.03138(17) Uani 1 1 d . . . Mn2 Mn 0.24966(5) 0.60240(6) -0.10446(4) 0.03813(18) Uani 1 1 d . . . Br1 Br 0.25439(6) 0.65945(7) -0.22356(4) 0.0786(2) Uani 1 1 d . . . O1 O 0.2933(2) 0.5464(3) 0.05326(17) 0.0414(8) Uani 1 1 d . . . N1 N 0.1177(3) 0.6703(3) -0.0756(2) 0.0432(10) Uani 1 1 d . . . N2 N 0.2260(3) 0.5813(3) 0.0090(2) 0.0383(9) Uani 1 1 d . . . O11 O 0.6103(2) 0.4378(2) 0.06277(16) 0.0328(7) Uani 1 1 d . . . O12 O 0.4603(2) 0.3843(3) -0.02700(16) 0.0351(7) Uani 1 1 d . . . N11 N 0.3802(3) 0.3902(3) 0.0857(2) 0.0348(8) Uani 1 1 d . . . N12 N 0.6254(3) 0.2308(3) 0.0242(2) 0.0415(9) Uani 1 1 d . . . O21 O 0.2368(3) 0.3462(3) -0.07095(19) 0.0469(8) Uani 1 1 d . . . O22 O 0.1725(3) 0.4283(3) -0.1515(2) 0.0525(9) Uani 1 1 d . . . C1 C 0.0564(4) 0.7055(4) -0.1216(3) 0.0515(13) Uani 1 1 d . . . H1 H 0.0679 0.7044 -0.1684 0.058(8) Uiso 1 1 calc R . . C2 C -0.0229(4) 0.7431(5) -0.1020(4) 0.0612(15) Uani 1 1 d . . . H2 H -0.0630 0.7685 -0.1348 0.058(8) Uiso 1 1 calc R . . C3 C -0.0422(4) 0.7430(5) -0.0344(4) 0.0640(16) Uani 1 1 d . . . H3 H -0.0960 0.7671 -0.0205 0.058(8) Uiso 1 1 calc R . . C4 C 0.0206(4) 0.7059(5) 0.0134(3) 0.0554(14) Uani 1 1 d . . . H4 H 0.0094 0.7051 0.0600 0.058(8) Uiso 1 1 calc R . . C5 C 0.0991(4) 0.6706(4) -0.0086(3) 0.0399(11) Uani 1 1 d . . . C6 C 0.1681(3) 0.6304(4) 0.0404(3) 0.0387(11) Uani 1 1 d . . . C7 C 0.1706(4) 0.6500(4) 0.1202(3) 0.0394(11) Uani 1 1 d . . . C8 C 0.1386(5) 0.5636(5) 0.1509(3) 0.0632(16) Uani 1 1 d . . . H8 H 0.1115 0.4901 0.1215 0.110(13) Uiso 1 1 calc R . . C9 C 0.1465(6) 0.5860(6) 0.2256(4) 0.085(2) Uani 1 1 d . . . H9 H 0.1273 0.5281 0.2478 0.110(13) Uiso 1 1 calc R . . C10 C 0.1828(6) 0.6938(7) 0.2659(4) 0.080(2) Uani 1 1 d . . . H10 H 0.1874 0.7118 0.3163 0.110(13) Uiso 1 1 calc R . . C11 C 0.2128(6) 0.7764(6) 0.2319(4) 0.084(2) Uani 1 1 d . . . H11 H 0.2393 0.8504 0.2605 0.110(13) Uiso 1 1 calc R . . N3 N 0.2061(4) 0.7561(4) 0.1590(3) 0.0648(13) Uani 1 1 d . . . C21 C 0.3245(4) 0.3888(4) 0.1376(3) 0.0478(12) Uani 1 1 d . . . H21 H 0.2735 0.4240 0.1359 0.049(7) Uiso 1 1 calc R . . C22 C 0.3403(4) 0.3377(5) 0.1923(3) 0.0539(14) Uani 1 1 d . . . H22 H 0.3002 0.3371 0.2270 0.049(7) Uiso 1 1 calc R . . C23 C 0.4168(4) 0.2872(5) 0.1953(3) 0.0541(14) Uani 1 1 d . . . H23 H 0.4299 0.2534 0.2329 0.049(7) Uiso 1 1 calc R . . C24 C 0.4740(4) 0.2863(4) 0.1427(3) 0.0461(12) Uani 1 1 d . . . H24 H 0.5252 0.2512 0.1438 0.049(7) Uiso 1 1 calc R . . C25 C 0.4538(3) 0.3388(4) 0.0879(2) 0.0351(10) Uani 1 1 d . . . C26 C 0.5153(3) 0.3520(4) 0.0284(2) 0.0323(9) Uani 1 1 d . . . C27 C 0.5347(4) 0.2414(4) -0.0050(2) 0.0368(10) Uani 1 1 d . . . C28 C 0.4598(4) 0.1588(4) -0.0608(3) 0.0480(12) Uani 1 1 d . . . H28 H 0.3965 0.1683 -0.0791 0.064(8) Uiso 1 1 calc R . . C29 C 0.4814(5) 0.0602(5) -0.0890(3) 0.0603(15) Uani 1 1 d . . . H29 H 0.4332 0.0030 -0.1272 0.064(8) Uiso 1 1 calc R . . C30 C 0.5753(5) 0.0493(5) -0.0594(3) 0.0582(15) Uani 1 1 d . . . H30 H 0.5914 -0.0158 -0.0772 0.064(8) Uiso 1 1 calc R . . C31 C 0.6446(4) 0.1348(4) -0.0037(3) 0.0514(13) Uani 1 1 d . . . H31 H 0.7079 0.1266 0.0160 0.064(8) Uiso 1 1 calc R . . C41 C 0.1779(4) 0.3438(4) -0.1303(3) 0.0424(11) Uani 1 1 d . . . C42 C 0.1114(4) 0.2300(4) -0.1787(3) 0.0449(12) Uani 1 1 d . . . C43 C 0.1093(5) 0.1350(5) -0.1544(3) 0.0585(14) Uani 1 1 d . . . H43 H 0.1491 0.1412 -0.1083 0.083(9) Uiso 1 1 calc R . . C44 C 0.0473(6) 0.0303(5) -0.1997(4) 0.0750(19) Uani 1 1 d . . . H44 H 0.0456 -0.0335 -0.1834 0.083(9) Uiso 1 1 calc R . . C45 C -0.0114(5) 0.0198(6) -0.2680(4) 0.0736(19) Uani 1 1 d . . . H45 H -0.0537 -0.0505 -0.2974 0.083(9) Uiso 1 1 calc R . . C46 C -0.0071(5) 0.1142(6) -0.2926(3) 0.0713(18) Uani 1 1 d . . . H46 H -0.0447 0.1075 -0.3395 0.083(9) Uiso 1 1 calc R . . C47 C 0.0531(4) 0.2188(5) -0.2474(3) 0.0598(15) Uani 1 1 d . . . H47 H 0.0543 0.2824 -0.2638 0.083(9) Uiso 1 1 calc R . . Mn3 Mn 0.13078(6) 1.06674(6) -0.47869(4) 0.03810(18) Uani 1 1 d . . . Mn4 Mn 0.18200(6) 1.28286(6) -0.56230(4) 0.0437(2) Uani 1 1 d . . . Br2 Br 0.12674(5) 1.32370(6) -0.68682(3) 0.06614(19) Uani 1 1 d . . . O31 O 0.2207(3) 1.2035(3) -0.41436(19) 0.0548(9) Uani 1 1 d . . . N31 N 0.3166(4) 1.4474(4) -0.5098(3) 0.0574(12) Uani 1 1 d . . . N32 N 0.2559(3) 1.2877(3) -0.4454(2) 0.0476(10) Uani 1 1 d . . . O41 O -0.0704(2) 0.8618(2) -0.45226(17) 0.0371(7) Uani 1 1 d . . . O42 O 0.0425(3) 0.9164(2) -0.52260(17) 0.0407(7) Uani 1 1 d . . . N41 N 0.1644(3) 1.0013(3) -0.3923(2) 0.0452(10) Uani 1 1 d . . . N42 N -0.0745(3) 0.6498(3) -0.5033(2) 0.0509(11) Uani 1 1 d . . . O51 O 0.2431(3) 1.0419(3) -0.5370(2) 0.0578(10) Uani 1 1 d . . . O52 O 0.2674(3) 1.1732(3) -0.5990(2) 0.0585(10) Uani 1 1 d . . . C51 C 0.3442(6) 1.5292(5) -0.5425(4) 0.0749(19) Uani 1 1 d . . . H51 H 0.3070 1.5201 -0.5900 0.092(12) Uiso 1 1 calc R . . C52 C 0.4263(7) 1.6276(6) -0.5086(5) 0.098(3) Uani 1 1 d . . . H52 H 0.4434 1.6835 -0.5327 0.092(12) Uiso 1 1 calc R . . C53 C 0.4808(7) 1.6398(6) -0.4395(5) 0.108(3) Uani 1 1 d . . . H53 H 0.5368 1.7041 -0.4159 0.092(12) Uiso 1 1 calc R . . C54 C 0.4531(6) 1.5566(5) -0.4044(4) 0.082(2) Uani 1 1 d . . . H54 H 0.4894 1.5648 -0.3567 0.092(12) Uiso 1 1 calc R . . C55 C 0.3708(4) 1.4609(4) -0.4410(3) 0.0565(14) Uani 1 1 d . . . C56 C 0.3366(4) 1.3691(4) -0.4055(3) 0.0496(13) Uani 1 1 d . . . C57 C 0.3936(4) 1.3677(4) -0.3325(3) 0.0473(12) Uani 1 1 d . . . C58 C 0.3505(5) 1.3776(6) -0.2723(3) 0.0686(17) Uani 1 1 d . . . H58 H 0.2870 1.3914 -0.2749 0.097(12) Uiso 1 1 calc R . . C59 C 0.4046(6) 1.3663(6) -0.2082(3) 0.0755(19) Uani 1 1 d . . . H59 H 0.3773 1.3720 -0.1667 0.097(12) Uiso 1 1 calc R . . C60 C 0.4966(6) 1.3471(5) -0.2050(4) 0.0701(17) Uani 1 1 d . . . H60 H 0.5332 1.3379 -0.1623 0.097(12) Uiso 1 1 calc R . . C61 C 0.5342(6) 1.3417(7) -0.2669(4) 0.0771(19) Uani 1 1 d . . . H61 H 0.5986 1.3302 -0.2645 0.097(12) Uiso 1 1 calc R . . N33 N 0.4853(4) 1.3516(5) -0.3305(3) 0.0685(14) Uani 1 1 d . . . C71 C 0.2356(4) 1.0543(5) -0.3282(3) 0.0596(15) Uani 1 1 d . . . H71 H 0.2732 1.1295 -0.3198 0.079(10) Uiso 1 1 calc R . . C72 C 0.2541(5) 1.0001(6) -0.2748(4) 0.0730(18) Uani 1 1 d . . . H72 H 0.3038 1.0380 -0.2309 0.079(10) Uiso 1 1 calc R . . C73 C 0.1982(5) 0.8896(6) -0.2874(4) 0.0703(18) Uani 1 1 d . . . H73 H 0.2108 0.8514 -0.2522 0.079(10) Uiso 1 1 calc R . . C74 C 0.1239(5) 0.8351(5) -0.3517(3) 0.0564(14) Uani 1 1 d . . . H74 H 0.0853 0.7603 -0.3600 0.079(10) Uiso 1 1 calc R . . C75 C 0.1066(4) 0.8922(4) -0.4043(3) 0.0418(11) Uani 1 1 d . . . C76 C 0.0208(4) 0.8495(4) -0.4739(3) 0.0404(11) Uani 1 1 d . . . C77 C 0.0023(4) 0.7269(4) -0.5155(3) 0.0479(12) Uani 1 1 d . . . C78 C 0.0626(7) 0.7007(5) -0.5624(4) 0.093(3) Uani 1 1 d . . . H78 H 0.1193 0.7557 -0.5668 0.099(12) Uiso 1 1 calc R . . C79 C 0.0375(9) 0.5917(6) -0.6026(5) 0.125(4) Uani 1 1 d . . . H79 H 0.0771 0.5720 -0.6350 0.099(12) Uiso 1 1 calc R . . C80 C -0.0452(7) 0.5117(6) -0.5953(4) 0.089(2) Uani 1 1 d . . . H80 H -0.0655 0.4383 -0.6246 0.099(12) Uiso 1 1 calc R . . C81 C -0.0979(5) 0.5424(4) -0.5437(4) 0.0690(18) Uani 1 1 d . . . H81 H -0.1517 0.4874 -0.5362 0.099(12) Uiso 1 1 calc R . . C91 C 0.2829(4) 1.0895(4) -0.5814(3) 0.0465(12) Uani 1 1 d . . . C92 C 0.3570(4) 1.0410(4) -0.6151(3) 0.0565(14) Uani 1 1 d . . . C93 C 0.3866(7) 1.0724(6) -0.6753(5) 0.098(3) Uani 1 1 d . . . H93 H 0.3617 1.1244 -0.6938 0.155(18) Uiso 1 1 calc R . . C94 C 0.4541(9) 1.0258(8) -0.7082(7) 0.135(4) Uani 1 1 d . . . H94 H 0.4733 1.0453 -0.7493 0.155(18) Uiso 1 1 calc R . . C95 C 0.4920(9) 0.9512(10) -0.6796(8) 0.147(5) Uani 1 1 d . . . H95 H 0.5385 0.9220 -0.7009 0.155(18) Uiso 1 1 calc R . . C96 C 0.4630(7) 0.9182(8) -0.6202(6) 0.112(3) Uani 1 1 d . . . H96 H 0.4889 0.8666 -0.6020 0.155(18) Uiso 1 1 calc R . . C97 C 0.3949(5) 0.9625(6) -0.5874(4) 0.0778(19) Uani 1 1 d . . . H97 H 0.3745 0.9405 -0.5474 0.155(18) Uiso 1 1 calc R . . N51 N 0.2032(12) 0.0632(12) 0.0159(8) 0.195(6) Uani 1 1 d . . . C101 C 0.1895(9) 0.0380(10) 0.0689(8) 0.120(4) Uani 1 1 d . . . C102 C 0.1791(11) 0.0084(10) 0.1332(8) 0.152(5) 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 0.0337(4) 0.0335(4) 0.0343(4) 0.0151(3) 0.0116(3) 0.0156(3) Mn2 0.0405(4) 0.0398(4) 0.0427(4) 0.0189(3) 0.0116(3) 0.0194(3) Br1 0.0912(5) 0.1016(5) 0.0687(4) 0.0523(4) 0.0239(4) 0.0464(4) O1 0.0463(19) 0.052(2) 0.0386(17) 0.0187(15) 0.0130(14) 0.0296(16) N1 0.039(2) 0.044(2) 0.054(3) 0.022(2) 0.0110(19) 0.0167(18) N2 0.041(2) 0.043(2) 0.043(2) 0.0186(18) 0.0146(18) 0.0228(18) O11 0.0339(16) 0.0303(15) 0.0402(17) 0.0157(13) 0.0120(13) 0.0129(13) O12 0.0415(17) 0.0396(17) 0.0338(16) 0.0183(13) 0.0126(13) 0.0194(14) N11 0.037(2) 0.033(2) 0.042(2) 0.0154(17) 0.0157(17) 0.0141(16) N12 0.044(2) 0.036(2) 0.054(2) 0.0191(19) 0.0190(19) 0.0183(18) O21 0.0420(19) 0.045(2) 0.052(2) 0.0195(16) 0.0055(16) 0.0098(16) O22 0.059(2) 0.044(2) 0.051(2) 0.0149(17) 0.0029(17) 0.0146(17) C1 0.048(3) 0.055(3) 0.057(3) 0.022(3) 0.009(2) 0.023(3) C2 0.053(3) 0.065(4) 0.076(4) 0.029(3) 0.010(3) 0.033(3) C3 0.048(3) 0.074(4) 0.081(4) 0.019(3) 0.017(3) 0.038(3) C4 0.053(3) 0.061(3) 0.065(4) 0.018(3) 0.020(3) 0.034(3) C5 0.035(2) 0.037(3) 0.052(3) 0.016(2) 0.012(2) 0.016(2) C6 0.035(2) 0.037(2) 0.050(3) 0.015(2) 0.016(2) 0.014(2) C7 0.039(3) 0.039(3) 0.049(3) 0.018(2) 0.017(2) 0.019(2) C8 0.084(4) 0.049(3) 0.065(4) 0.018(3) 0.041(3) 0.018(3) C9 0.127(6) 0.074(5) 0.075(5) 0.035(4) 0.061(5) 0.031(4) C10 0.096(5) 0.101(6) 0.054(4) 0.021(4) 0.035(4) 0.034(4) C11 0.109(6) 0.063(4) 0.068(4) 0.002(3) 0.036(4) 0.012(4) N3 0.084(4) 0.052(3) 0.055(3) 0.011(2) 0.025(3) 0.013(3) C21 0.051(3) 0.054(3) 0.054(3) 0.026(3) 0.026(2) 0.023(3) C22 0.064(4) 0.062(3) 0.051(3) 0.030(3) 0.034(3) 0.021(3) C23 0.067(4) 0.060(3) 0.054(3) 0.042(3) 0.027(3) 0.024(3) C24 0.058(3) 0.043(3) 0.055(3) 0.031(2) 0.022(2) 0.024(2) C25 0.038(2) 0.031(2) 0.038(2) 0.0137(19) 0.011(2) 0.0089(19) C26 0.036(2) 0.033(2) 0.036(2) 0.0172(19) 0.0124(19) 0.0148(19) C27 0.045(3) 0.035(2) 0.039(3) 0.017(2) 0.019(2) 0.016(2) C28 0.053(3) 0.042(3) 0.050(3) 0.013(2) 0.008(2) 0.020(2) C29 0.077(4) 0.039(3) 0.058(3) 0.004(3) 0.010(3) 0.018(3) C30 0.073(4) 0.041(3) 0.073(4) 0.013(3) 0.029(3) 0.032(3) C31 0.050(3) 0.041(3) 0.074(4) 0.019(3) 0.022(3) 0.025(2) C41 0.035(3) 0.046(3) 0.047(3) 0.013(2) 0.015(2) 0.010(2) C42 0.041(3) 0.049(3) 0.045(3) 0.009(2) 0.017(2) 0.013(2) C43 0.066(4) 0.050(3) 0.059(4) 0.018(3) 0.015(3) 0.017(3) C44 0.088(5) 0.046(4) 0.085(5) 0.014(3) 0.029(4) 0.010(3) C45 0.065(4) 0.058(4) 0.071(4) -0.011(3) 0.013(3) 0.000(3) C46 0.065(4) 0.079(5) 0.051(3) -0.002(3) 0.000(3) 0.014(3) C47 0.059(3) 0.058(4) 0.056(3) 0.012(3) 0.006(3) 0.017(3) Mn3 0.0425(4) 0.0313(4) 0.0422(4) 0.0183(3) 0.0108(3) 0.0073(3) Mn4 0.0487(4) 0.0361(4) 0.0468(4) 0.0202(3) 0.0116(3) 0.0066(3) Br2 0.0788(4) 0.0709(4) 0.0574(4) 0.0361(3) 0.0181(3) 0.0217(3) O31 0.065(2) 0.0391(19) 0.049(2) 0.0231(16) 0.0012(17) -0.0032(17) N31 0.065(3) 0.041(2) 0.063(3) 0.025(2) 0.018(2) 0.001(2) N32 0.054(3) 0.037(2) 0.048(2) 0.0205(19) 0.009(2) 0.003(2) O41 0.0386(17) 0.0295(16) 0.0434(18) 0.0129(14) 0.0118(14) 0.0072(13) O42 0.0505(19) 0.0312(16) 0.0435(18) 0.0185(14) 0.0148(15) 0.0090(14) N41 0.041(2) 0.043(2) 0.054(3) 0.026(2) 0.009(2) 0.0101(19) N42 0.057(3) 0.033(2) 0.062(3) 0.015(2) 0.012(2) 0.012(2) O51 0.055(2) 0.061(2) 0.073(3) 0.032(2) 0.029(2) 0.0242(19) O52 0.059(2) 0.052(2) 0.076(3) 0.032(2) 0.025(2) 0.0178(19) C51 0.089(5) 0.053(4) 0.081(5) 0.036(3) 0.022(4) 0.004(3) C52 0.125(7) 0.055(4) 0.098(6) 0.035(4) 0.029(5) -0.013(4) C53 0.116(7) 0.062(5) 0.107(6) 0.036(4) 0.012(5) -0.038(4) C54 0.083(5) 0.060(4) 0.070(4) 0.016(3) -0.001(4) -0.019(3) C55 0.058(3) 0.039(3) 0.061(4) 0.016(3) 0.008(3) -0.002(2) C56 0.054(3) 0.040(3) 0.049(3) 0.013(2) 0.012(2) 0.006(2) C57 0.049(3) 0.037(3) 0.047(3) 0.007(2) 0.005(2) 0.007(2) C58 0.060(4) 0.087(5) 0.054(4) 0.006(3) 0.014(3) 0.024(3) C59 0.080(5) 0.089(5) 0.044(3) 0.004(3) 0.018(3) 0.015(4) C60 0.078(5) 0.066(4) 0.054(4) 0.012(3) -0.003(3) 0.016(3) C61 0.072(4) 0.108(6) 0.058(4) 0.020(4) 0.011(3) 0.043(4) N33 0.059(3) 0.093(4) 0.062(3) 0.026(3) 0.020(3) 0.030(3) C71 0.055(3) 0.061(4) 0.057(3) 0.030(3) -0.001(3) 0.006(3) C72 0.064(4) 0.086(5) 0.068(4) 0.042(4) -0.003(3) 0.014(3) C73 0.070(4) 0.076(4) 0.076(4) 0.052(4) 0.007(3) 0.023(3) C74 0.067(4) 0.048(3) 0.068(4) 0.037(3) 0.018(3) 0.024(3) C75 0.044(3) 0.038(3) 0.053(3) 0.021(2) 0.018(2) 0.016(2) C76 0.050(3) 0.030(2) 0.050(3) 0.018(2) 0.021(2) 0.015(2) C77 0.067(3) 0.033(3) 0.053(3) 0.020(2) 0.025(3) 0.018(2) C78 0.157(7) 0.047(4) 0.112(6) 0.036(4) 0.096(6) 0.042(4) C79 0.246(12) 0.056(4) 0.126(7) 0.041(5) 0.136(8) 0.065(6) C80 0.156(8) 0.045(4) 0.071(4) 0.007(3) 0.031(5) 0.044(5) C81 0.083(4) 0.028(3) 0.092(5) 0.014(3) 0.011(4) 0.017(3) C91 0.044(3) 0.043(3) 0.050(3) 0.015(2) 0.012(2) 0.006(2) C92 0.056(3) 0.041(3) 0.068(4) 0.008(3) 0.021(3) 0.009(3) C93 0.133(7) 0.063(4) 0.118(6) 0.029(4) 0.087(6) 0.024(4) C94 0.185(11) 0.088(6) 0.182(10) 0.046(7) 0.147(10) 0.053(7) C95 0.135(9) 0.120(8) 0.229(14) 0.038(9) 0.130(10) 0.059(7) C96 0.111(7) 0.113(7) 0.147(8) 0.034(6) 0.060(6) 0.072(6) C97 0.075(4) 0.076(5) 0.094(5) 0.020(4) 0.028(4) 0.041(4) N51 0.241(14) 0.207(13) 0.201(13) 0.093(11) 0.036(11) 0.155(12) C101 0.115(8) 0.109(8) 0.159(11) 0.040(8) 0.022(8) 0.074(7) C102 0.192(12) 0.114(8) 0.182(12) 0.071(8) 0.108(10) 0.038(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 O1 1.906(3) . ? Mn1 O12 1.908(3) . ? Mn1 O11 1.930(3) 2_665 ? Mn1 N11 2.041(4) . ? Mn1 O21 2.068(3) . ? Mn1 O12 2.518(3) 2_665 ? Mn2 O22 2.120(4) . ? Mn2 O11 2.186(3) 2_665 ? Mn2 N2 2.304(4) . ? Mn2 N1 2.307(4) . ? Mn2 N12 2.378(4) 2_665 ? Mn2 Br1 2.5360(14) . ? O1 N2 1.372(5) . ? N1 C1 1.343(6) . ? N1 C5 1.345(6) . ? N2 C6 1.288(6) . ? O11 C26 1.410(5) . ? O11 Mn1 1.930(3) 2_665 ? O11 Mn2 2.186(3) 2_665 ? O12 C26 1.393(5) . ? O12 Mn1 2.518(3) 2_665 ? N11 C25 1.345(6) . ? N11 C21 1.352(6) . ? N12 C27 1.329(6) . ? N12 C31 1.347(6) . ? N12 Mn2 2.378(4) 2_665 ? O21 C41 1.266(6) . ? O22 C41 1.249(6) . ? C1 C2 1.379(8) . ? C2 C3 1.362(9) . ? C3 C4 1.390(8) . ? C4 C5 1.369(7) . ? C5 C6 1.484(7) . ? C6 C7 1.484(7) . ? C7 N3 1.320(7) . ? C7 C8 1.366(7) . ? C8 C9 1.374(9) . ? C9 C10 1.345(10) . ? C10 C11 1.363(10) . ? C11 N3 1.342(8) . ? C21 C22 1.361(7) . ? C22 C23 1.372(8) . ? C23 C24 1.376(7) . ? C24 C25 1.385(6) . ? C25 C26 1.537(6) . ? C26 C27 1.540(6) . ? C27 C28 1.375(7) . ? C28 C29 1.394(7) . ? C29 C30 1.372(8) . ? C30 C31 1.362(8) . ? C41 C42 1.503(7) . ? C42 C47 1.375(8) . ? C42 C43 1.386(8) . ? C43 C44 1.389(8) . ? C44 C45 1.371(10) . ? C45 C46 1.378(10) . ? C46 C47 1.383(8) . ? Mn3 O31 1.882(3) . ? Mn3 O42 1.904(3) . ? Mn3 O41 1.951(3) 2_574 ? Mn3 N41 2.041(4) . ? Mn3 O51 2.101(4) . ? Mn3 O42 2.451(4) 2_574 ? Mn4 O52 2.142(4) . ? Mn4 O41 2.172(3) 2_574 ? Mn4 N32 2.271(4) . ? Mn4 N31 2.300(5) . ? Mn4 N42 2.312(5) 2_574 ? Mn4 Br2 2.5736(15) . ? O31 N32 1.356(5) . ? N31 C51 1.333(7) . ? N31 C55 1.346(7) . ? N32 C56 1.289(6) . ? O41 C76 1.420(6) . ? O41 Mn3 1.951(3) 2_574 ? O41 Mn4 2.172(3) 2_574 ? O42 C76 1.408(5) . ? O42 Mn3 2.451(4) 2_574 ? N41 C71 1.344(7) . ? N41 C75 1.361(6) . ? N42 C77 1.330(7) . ? N42 C81 1.354(7) . ? N42 Mn4 2.312(5) 2_574 ? O51 C91 1.259(6) . ? O52 C91 1.250(6) . ? C51 C52 1.392(10) . ? C52 C53 1.356(11) . ? C53 C54 1.380(10) . ? C54 C55 1.382(8) . ? C55 C56 1.488(7) . ? C56 C57 1.485(7) . ? C57 N33 1.324(7) . ? C57 C58 1.377(8) . ? C58 C59 1.376(9) . ? C59 C60 1.345(10) . ? C60 C61 1.362(9) . ? C61 N33 1.332(8) . ? C71 C72 1.374(8) . ? C72 C73 1.368(9) . ? C73 C74 1.368(9) . ? C74 C75 1.386(7) . ? C75 C76 1.508(7) . ? C76 C77 1.537(7) . ? C77 C78 1.370(8) . ? C78 C79 1.366(10) . ? C79 C80 1.363(12) . ? C80 C81 1.370(10) . ? C91 C92 1.492(8) . ? C92 C93 1.383(9) . ? C92 C97 1.404(9) . ? C93 C94 1.395(11) . ? C94 C95 1.367(15) . ? C95 C96 1.375(14) . ? C96 C97 1.386(10) . ? N51 C101 1.153(16) . ? C101 C102 1.379(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O12 165.86(13) . . ? O1 Mn1 O11 93.00(13) . 2_665 ? O12 Mn1 O11 96.65(12) . 2_665 ? O1 Mn1 N11 86.77(14) . . ? O12 Mn1 N11 81.26(13) . . ? O11 Mn1 N11 165.16(14) 2_665 . ? O1 Mn1 O21 94.95(15) . . ? O12 Mn1 O21 94.44(14) . . ? O11 Mn1 O21 95.21(13) 2_665 . ? N11 Mn1 O21 99.59(14) . . ? O1 Mn1 O12 100.09(13) . 2_665 ? O12 Mn1 O12 76.10(13) . 2_665 ? O11 Mn1 O12 60.04(11) 2_665 2_665 ? N11 Mn1 O12 105.37(13) . 2_665 ? O21 Mn1 O12 151.42(12) . 2_665 ? O22 Mn2 O11 88.70(13) . 2_665 ? O22 Mn2 N2 89.61(14) . . ? O11 Mn2 N2 79.14(12) 2_665 . ? O22 Mn2 N1 103.06(15) . . ? O11 Mn2 N1 146.59(13) 2_665 . ? N2 Mn2 N1 69.92(14) . . ? O22 Mn2 N12 158.65(14) . 2_665 ? O11 Mn2 N12 71.63(12) 2_665 2_665 ? N2 Mn2 N12 78.84(14) . 2_665 ? N1 Mn2 N12 89.87(14) . 2_665 ? O22 Mn2 Br1 97.88(11) . . ? O11 Mn2 Br1 111.83(8) 2_665 . ? N2 Mn2 Br1 166.71(10) . . ? N1 Mn2 Br1 97.58(10) . . ? N12 Mn2 Br1 97.14(10) 2_665 . ? N2 O1 Mn1 114.0(2) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Mn2 124.7(4) . . ? C5 N1 Mn2 117.2(3) . . ? C6 N2 O1 116.8(4) . . ? C6 N2 Mn2 119.4(3) . . ? O1 N2 Mn2 121.2(3) . . ? C26 O11 Mn1 106.9(2) . 2_665 ? C26 O11 Mn2 120.8(2) . 2_665 ? Mn1 O11 Mn2 112.75(14) 2_665 2_665 ? C26 O12 Mn1 116.4(2) . . ? C26 O12 Mn1 81.9(2) . 2_665 ? Mn1 O12 Mn1 103.90(13) . 2_665 ? C25 N11 C21 118.7(4) . . ? C25 N11 Mn1 113.7(3) . . ? C21 N11 Mn1 127.6(3) . . ? C27 N12 C31 117.7(4) . . ? C27 N12 Mn2 115.6(3) . 2_665 ? C31 N12 Mn2 125.6(3) . 2_665 ? C41 O21 Mn1 134.2(3) . . ? C41 O22 Mn2 132.4(3) . . ? N1 C1 C2 122.2(5) . . ? C3 C2 C1 119.7(5) . . ? C2 C3 C4 118.3(5) . . ? C5 C4 C3 119.7(6) . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 116.4(4) . . ? C4 C5 C6 121.6(5) . . ? N2 C6 C5 115.2(4) . . ? N2 C6 C7 123.7(4) . . ? C5 C6 C7 121.0(4) . . ? N3 C7 C8 122.7(5) . . ? N3 C7 C6 115.4(4) . . ? C8 C7 C6 121.9(5) . . ? C7 C8 C9 119.6(6) . . ? C10 C9 C8 118.3(6) . . ? C9 C10 C11 119.3(6) . . ? N3 C11 C10 123.3(6) . . ? C7 N3 C11 116.8(5) . . ? N11 C21 C22 122.5(5) . . ? C21 C22 C23 118.6(5) . . ? C22 C23 C24 120.2(5) . . ? C23 C24 C25 118.6(5) . . ? N11 C25 C24 121.3(4) . . ? N11 C25 C26 113.5(4) . . ? C24 C25 C26 125.0(4) . . ? O12 C26 O11 109.1(3) . . ? O12 C26 C25 109.6(3) . . ? O11 C26 C25 107.0(3) . . ? O12 C26 C27 109.7(4) . . ? O11 C26 C27 110.6(3) . . ? C25 C26 C27 110.9(3) . . ? N12 C27 C28 123.3(4) . . ? N12 C27 C26 116.2(4) . . ? C28 C27 C26 120.5(4) . . ? C27 C28 C29 118.1(5) . . ? C30 C29 C28 118.8(5) . . ? C31 C30 C29 119.2(5) . . ? N12 C31 C30 122.9(5) . . ? O22 C41 O21 124.8(5) . . ? O22 C41 C42 118.5(5) . . ? O21 C41 C42 116.7(4) . . ? C47 C42 C43 119.4(5) . . ? C47 C42 C41 120.5(5) . . ? C43 C42 C41 120.1(5) . . ? C42 C43 C44 119.4(6) . . ? C45 C44 C43 120.9(6) . . ? C44 C45 C46 119.4(6) . . ? C45 C46 C47 120.0(6) . . ? C42 C47 C46 120.8(6) . . ? O31 Mn3 O42 166.09(14) . . ? O31 Mn3 O41 93.96(14) . 2_574 ? O42 Mn3 O41 98.47(14) . 2_574 ? O31 Mn3 N41 84.70(16) . . ? O42 Mn3 N41 81.65(15) . . ? O41 Mn3 N41 164.50(16) 2_574 . ? O31 Mn3 O51 93.39(17) . . ? O42 Mn3 O51 92.13(15) . . ? O41 Mn3 O51 93.32(14) 2_574 . ? N41 Mn3 O51 102.17(16) . . ? O31 Mn3 O42 103.36(15) . 2_574 ? O42 Mn3 O42 77.48(14) . 2_574 ? O41 Mn3 O42 61.30(12) 2_574 2_574 ? N41 Mn3 O42 103.92(14) . 2_574 ? O51 Mn3 O42 150.06(14) . 2_574 ? O52 Mn4 O41 87.64(13) . 2_574 ? O52 Mn4 N32 87.17(16) . . ? O41 Mn4 N32 79.86(13) 2_574 . ? O52 Mn4 N31 99.85(17) . . ? O41 Mn4 N31 148.49(15) 2_574 . ? N32 Mn4 N31 70.09(16) . . ? O52 Mn4 N42 157.49(15) . 2_574 ? O41 Mn4 N42 73.05(13) 2_574 2_574 ? N32 Mn4 N42 78.30(17) . 2_574 ? N31 Mn4 N42 91.33(17) . 2_574 ? O52 Mn4 Br2 96.73(11) . . ? O41 Mn4 Br2 112.78(9) 2_574 . ? N32 Mn4 Br2 166.83(11) . . ? N31 Mn4 Br2 96.81(12) . . ? N42 Mn4 Br2 101.30(12) 2_574 . ? N32 O31 Mn3 116.7(3) . . ? C51 N31 C55 118.4(5) . . ? C51 N31 Mn4 124.7(4) . . ? C55 N31 Mn4 116.9(3) . . ? C56 N32 O31 116.0(4) . . ? C56 N32 Mn4 121.8(3) . . ? O31 N32 Mn4 122.2(3) . . ? C76 O41 Mn3 105.1(3) . 2_574 ? C76 O41 Mn4 119.2(2) . 2_574 ? Mn3 O41 Mn4 113.64(15) 2_574 2_574 ? C76 O42 Mn3 116.1(3) . . ? C76 O42 Mn3 84.0(2) . 2_574 ? Mn3 O42 Mn3 102.52(14) . 2_574 ? C71 N41 C75 119.8(4) . . ? C71 N41 Mn3 126.8(3) . . ? C75 N41 Mn3 113.4(3) . . ? C77 N42 C81 117.6(5) . . ? C77 N42 Mn4 116.0(3) . 2_574 ? C81 N42 Mn4 124.5(4) . 2_574 ? C91 O51 Mn3 132.9(4) . . ? C91 O52 Mn4 133.4(4) . . ? N31 C51 C52 122.8(7) . . ? C53 C52 C51 118.2(6) . . ? C52 C53 C54 119.9(7) . . ? C53 C54 C55 119.0(7) . . ? N31 C55 C54 121.6(5) . . ? N31 C55 C56 117.0(5) . . ? C54 C55 C56 121.4(5) . . ? N32 C56 C57 122.7(5) . . ? N32 C56 C55 114.1(5) . . ? C57 C56 C55 123.1(5) . . ? N33 C57 C58 123.1(5) . . ? N33 C57 C56 115.6(5) . . ? C58 C57 C56 121.2(5) . . ? C59 C58 C57 117.7(6) . . ? C60 C59 C58 120.6(6) . . ? C59 C60 C61 117.4(6) . . ? N33 C61 C60 124.8(6) . . ? C57 N33 C61 116.5(5) . . ? N41 C71 C72 121.6(6) . . ? C73 C72 C71 118.9(6) . . ? C72 C73 C74 120.2(5) . . ? C73 C74 C75 119.6(5) . . ? N41 C75 C74 119.9(5) . . ? N41 C75 C76 113.4(4) . . ? C74 C75 C76 126.4(5) . . ? O42 C76 O41 107.8(4) . . ? O42 C76 C75 110.3(4) . . ? O41 C76 C75 106.3(4) . . ? O42 C76 C77 107.9(4) . . ? O41 C76 C77 110.3(4) . . ? C75 C76 C77 114.0(4) . . ? N42 C77 C78 122.8(5) . . ? N42 C77 C76 116.4(4) . . ? C78 C77 C76 120.7(5) . . ? C79 C78 C77 118.4(7) . . ? C80 C79 C78 120.3(7) . . ? C79 C80 C81 118.3(6) . . ? N42 C81 C80 122.4(6) . . ? O52 C91 O51 126.5(5) . . ? O52 C91 C92 117.4(5) . . ? O51 C91 C92 116.1(5) . . ? C93 C92 C97 120.0(6) . . ? C93 C92 C91 119.3(6) . . ? C97 C92 C91 120.7(6) . . ? C92 C93 C94 119.7(8) . . ? C95 C94 C93 119.6(9) . . ? C94 C95 C96 121.6(8) . . ? C95 C96 C97 119.5(9) . . ? C96 C97 C92 119.5(8) . . ? N51 C101 C102 176.8(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.660 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.081 #===END #COMPOUND 3 data_pekm622 _database_code_depnum_ccdc_archive 'CCDC 187285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H44 Br2 Mn4 N12 O10' _chemical_formula_weight 1376.57 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.147(6) _cell_length_b 19.939(8) _cell_length_c 10.272(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.27(1) _cell_angle_gamma 90.00 _cell_volume 2885(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 11.5 _exptl_crystal_description parallelipiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.56 _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.3 _diffrn_reflns_number 5051 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 24.50 _reflns_number_total 4764 _reflns_number_gt 3127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Program COLLECT (UCLA Crystal.package C.E.Strouse 1994)' _computing_cell_refinement 'Program LEAST (UCLA Crystal.package C.E.Strouse 1994)' _computing_data_reduction 'Program REDUCE (UCLA Crystal.package C.E.Strouse 1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+4.3104P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4764 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.40985(6) 0.03871(4) -0.09894(8) 0.0366(2) Uani 1 1 d . . . Mn2 Mn 0.43809(6) 0.20861(4) -0.07267(10) 0.0485(3) Uani 1 1 d . . . Br1 Br 0.46653(6) 0.29343(4) 0.11084(10) 0.0919(3) Uani 1 1 d . . . O1 O 0.4103(3) 0.08110(18) -0.2634(4) 0.0508(10) Uani 1 1 d . . . N1 N 0.4135(4) 0.2801(3) -0.2474(6) 0.0615(15) Uani 1 1 d . . . N2 N 0.4104(3) 0.1492(2) -0.2621(5) 0.0478(12) Uani 1 1 d . . . O11 O 0.4826(2) 0.10915(17) -0.0081(3) 0.0381(8) Uani 1 1 d . . . O12 O 0.5850(2) 0.02310(16) -0.0427(3) 0.0374(8) Uani 1 1 d . . . N11 N 0.6339(3) 0.0455(2) 0.2011(4) 0.0411(10) Uani 1 1 d . . . N12 N 0.5940(3) 0.1953(2) -0.1295(5) 0.0470(12) Uani 1 1 d . . . O21 O 0.2761(3) 0.0761(2) -0.0663(4) 0.0536(11) Uani 1 1 d . . . O22 O 0.2931(3) 0.1871(2) -0.0451(5) 0.0590(12) Uani 1 1 d . . . C1 C 0.4209(5) 0.3466(4) -0.2384(10) 0.082(2) Uani 1 1 d . . . H1 H 0.4290 0.3658 -0.1555 0.095(14) Uiso 1 1 calc R . . C2 C 0.4174(6) 0.3885(4) -0.3454(12) 0.095(3) Uani 1 1 d . . . H2 H 0.4241 0.4347 -0.3351 0.095(14) Uiso 1 1 calc R . . C3 C 0.4039(6) 0.3607(5) -0.4662(11) 0.097(3) Uani 1 1 d . . . H3 H 0.4004 0.3881 -0.5398 0.095(14) Uiso 1 1 calc R . . C4 C 0.3951(5) 0.2920(4) -0.4810(9) 0.085(3) Uani 1 1 d . . . H4 H 0.3859 0.2724 -0.5633 0.095(14) Uiso 1 1 calc R . . C5 C 0.4006(4) 0.2536(3) -0.3683(7) 0.0572(17) Uani 1 1 d . . . C6 C 0.3959(4) 0.1784(3) -0.3745(6) 0.0522(15) Uani 1 1 d . . . C7 C 0.3762(6) 0.1425(4) -0.5002(7) 0.069(2) Uani 1 1 d . . . N3 N 0.3038(13) 0.1531(7) -0.5770(15) 0.107(5) Uani 0.60 1 d P . . C8 C 0.4461(11) 0.0876(8) -0.5389(16) 0.093(5) Uani 0.60 1 d P . . C9 C 0.4212(13) 0.0542(9) -0.6585(16) 0.098(5) Uani 0.60 1 d P . . C10 C 0.3296(15) 0.0757(7) -0.7304(13) 0.132(6) Uani 1 1 d . . . C11 C 0.2825(19) 0.1178(11) -0.690(2) 0.126(10) Uani 0.60 1 d P . . N3A N 0.2806(15) 0.1211(10) -0.5090(17) 0.083(5) Uani 0.40 1 d P . . C8A C 0.4318(14) 0.1500(14) -0.588(2) 0.095(8) Uani 0.40 1 d P . . C9A C 0.398(3) 0.116(2) -0.709(2) 0.132(14) Uani 0.40 1 d P . . C11A C 0.254(3) 0.0892(15) -0.620(2) 0.119(13) Uani 0.40 1 d P . . C21 C 0.6688(5) 0.0487(3) 0.3270(6) 0.0598(17) Uani 1 1 d . . . H21 H 0.6741 0.0097 0.3767 0.076(11) Uiso 1 1 calc R . . C22 C 0.6969(5) 0.1086(4) 0.3834(7) 0.070(2) Uani 1 1 d . . . H22 H 0.7213 0.1099 0.4706 0.076(11) Uiso 1 1 calc R . . C23 C 0.6891(5) 0.1668(3) 0.3113(7) 0.0615(18) Uani 1 1 d . . . H23 H 0.7075 0.2077 0.3492 0.076(11) Uiso 1 1 calc R . . C24 C 0.6540(4) 0.1635(3) 0.1833(6) 0.0528(16) Uani 1 1 d . . . H24 H 0.6491 0.2021 0.1323 0.076(11) Uiso 1 1 calc R . . C25 C 0.6256(4) 0.1015(3) 0.1297(6) 0.0394(13) Uani 1 1 d . . . C26 C 0.5796(3) 0.0911(3) -0.0089(5) 0.0356(12) Uani 1 1 d . . . C27 C 0.6280(4) 0.1333(3) -0.1076(5) 0.0394(13) Uani 1 1 d . . . C28 C 0.7041(4) 0.1085(3) -0.1687(6) 0.0445(13) Uani 1 1 d . . . H28 H 0.7257 0.0651 -0.1520 0.067(10) Uiso 1 1 calc R . . C29 C 0.7474(4) 0.1487(3) -0.2542(6) 0.0535(16) Uani 1 1 d . . . H29 H 0.7978 0.1327 -0.2973 0.067(10) Uiso 1 1 calc R . . C30 C 0.7147(4) 0.2131(3) -0.2748(7) 0.0564(16) Uani 1 1 d . . . H30 H 0.7438 0.2420 -0.3298 0.067(10) Uiso 1 1 calc R . . C31 C 0.6382(4) 0.2337(3) -0.2125(7) 0.0599(18) Uani 1 1 d . . . H31 H 0.6155 0.2770 -0.2286 0.067(10) Uiso 1 1 calc R . . C41 C 0.2454(4) 0.1349(4) -0.0520(7) 0.0567(16) Uani 1 1 d . . . C42 C 0.1394(5) 0.1411(4) -0.0397(9) 0.087(3) Uani 1 1 d . . . H42A H 0.1242 0.1193 0.0390 0.18(3) Uiso 1 1 calc R . . H42B H 0.1049 0.1203 -0.1137 0.18(3) Uiso 1 1 calc R . . H42C H 0.1224 0.1877 -0.0366 0.18(3) Uiso 1 1 calc R . . N31 N -0.0667(16) 0.0219(11) 0.743(2) 0.175(8) Uiso 0.60 1 d P A 1 C51 C 0.0029(18) 0.0326(11) 0.686(2) 0.138(7) Uiso 0.60 1 d P A 1 C52 C 0.1013(18) 0.0492(13) 0.644(2) 0.149(8) Uiso 0.60 1 d P A 1 N41 N -0.111(2) -0.0031(17) 0.601(4) 0.181(12) Uiso 0.40 1 d P B 2 C61 C -0.120(2) -0.036(2) 0.496(4) 0.154(12) Uiso 0.40 1 d P B 2 C62 C -0.143(3) -0.0801(18) 0.399(4) 0.138(11) Uiso 0.40 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0388(4) 0.0313(4) 0.0391(4) -0.0010(4) 0.0006(3) -0.0004(4) Mn2 0.0449(5) 0.0348(5) 0.0657(6) -0.0040(4) 0.0040(4) 0.0046(4) Br1 0.0753(5) 0.0752(6) 0.1261(8) -0.0523(5) 0.0146(5) -0.0001(4) O1 0.075(3) 0.033(2) 0.044(2) 0.0031(17) 0.000(2) 0.0030(19) N1 0.048(3) 0.040(3) 0.096(5) 0.011(3) 0.002(3) 0.004(2) N2 0.051(3) 0.038(3) 0.053(3) 0.007(2) 0.000(2) -0.001(2) O11 0.035(2) 0.037(2) 0.043(2) -0.0021(16) 0.0028(16) -0.0004(16) O12 0.0384(19) 0.0284(19) 0.045(2) -0.0053(16) 0.0021(16) 0.0001(15) N11 0.040(2) 0.043(3) 0.039(3) 0.000(2) -0.005(2) -0.005(2) N12 0.043(3) 0.037(3) 0.061(3) 0.002(2) 0.007(2) 0.000(2) O21 0.040(2) 0.046(2) 0.074(3) 0.000(2) 0.003(2) 0.0041(18) O22 0.046(2) 0.048(3) 0.083(3) -0.002(2) 0.006(2) 0.005(2) C1 0.066(5) 0.050(4) 0.129(8) 0.009(5) -0.001(5) -0.001(4) C2 0.075(6) 0.044(5) 0.162(10) 0.031(6) -0.008(6) -0.003(4) C3 0.066(5) 0.075(6) 0.145(9) 0.060(6) -0.023(6) -0.014(4) C4 0.080(5) 0.063(5) 0.107(7) 0.041(5) -0.018(5) -0.014(4) C5 0.041(3) 0.055(4) 0.074(5) 0.018(4) -0.003(3) -0.002(3) C6 0.051(4) 0.047(3) 0.057(4) 0.017(3) -0.003(3) -0.005(3) C7 0.086(5) 0.069(5) 0.050(4) 0.026(4) 0.000(4) -0.003(4) N3 0.160(14) 0.064(8) 0.085(10) -0.010(7) -0.043(11) 0.040(9) C8 0.089(10) 0.098(11) 0.100(12) -0.004(10) 0.053(9) 0.005(9) C9 0.125(13) 0.100(12) 0.075(10) -0.016(9) 0.043(10) 0.006(10) C10 0.212(17) 0.094(9) 0.086(9) 0.025(7) -0.015(10) -0.013(10) C11 0.19(3) 0.096(14) 0.074(13) -0.019(12) -0.061(15) 0.065(15) N3A 0.110(15) 0.089(14) 0.048(11) 0.000(10) 0.005(10) -0.021(12) C8A 0.067(13) 0.15(2) 0.069(15) 0.052(15) 0.032(11) 0.026(14) C9A 0.17(3) 0.20(4) 0.031(13) 0.017(18) 0.025(15) 0.10(3) C11A 0.21(3) 0.096(19) 0.042(14) 0.006(13) -0.023(17) -0.05(2) C21 0.068(4) 0.060(4) 0.047(4) 0.001(3) -0.018(3) -0.008(3) C22 0.088(5) 0.066(5) 0.053(4) -0.013(4) -0.014(4) -0.009(4) C23 0.068(4) 0.053(4) 0.062(4) -0.020(3) 0.000(3) -0.015(3) C24 0.045(3) 0.049(4) 0.064(4) -0.016(3) -0.002(3) -0.007(3) C25 0.031(3) 0.038(3) 0.049(3) -0.007(3) 0.002(2) 0.000(2) C26 0.032(3) 0.034(3) 0.040(3) -0.002(2) 0.001(2) -0.002(2) C27 0.034(3) 0.038(3) 0.045(3) -0.001(2) -0.003(2) -0.004(2) C28 0.042(3) 0.043(3) 0.048(3) -0.003(3) 0.006(3) 0.000(3) C29 0.047(3) 0.058(4) 0.056(4) -0.002(3) 0.013(3) -0.005(3) C30 0.048(4) 0.059(4) 0.063(4) 0.012(3) 0.009(3) -0.008(3) C31 0.051(4) 0.045(4) 0.083(5) 0.021(3) 0.007(3) 0.000(3) C41 0.042(3) 0.065(5) 0.062(4) -0.003(3) -0.002(3) 0.007(3) C42 0.045(4) 0.075(5) 0.140(8) -0.017(5) 0.013(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.890(4) . ? Mn1 O12 1.903(4) 3_655 ? Mn1 O11 1.930(3) . ? Mn1 N11 2.045(4) 3_655 ? Mn1 O21 2.090(4) . ? Mn1 O12 2.512(4) . ? Mn2 O22 2.140(4) . ? Mn2 O11 2.166(4) . ? Mn2 N2 2.281(5) . ? Mn2 N1 2.293(6) . ? Mn2 N12 2.348(5) . ? Mn2 Br1 2.5371(14) . ? O1 N2 1.358(6) . ? N1 C1 1.334(9) . ? N1 C5 1.346(9) . ? N2 C6 1.293(7) . ? O11 C26 1.419(6) . ? O12 C26 1.404(6) . ? O12 Mn1 1.903(4) 3_655 ? N11 C25 1.337(7) . ? N11 C21 1.343(7) . ? N11 Mn1 2.045(4) 3_655 ? N12 C27 1.338(7) . ? N12 C31 1.343(8) . ? O21 C41 1.264(7) . ? O22 C41 1.238(7) . ? C1 C2 1.378(12) . ? C2 C3 1.357(13) . ? C3 C4 1.382(12) . ? C4 C5 1.384(10) . ? C5 C6 1.501(9) . ? C6 C7 1.480(10) . ? C7 N3 1.251(14) . ? C7 C8A 1.263(19) . ? C7 N3A 1.41(2) . ? C7 C8 1.552(16) . ? N3 N3A 1.021(19) . ? N3 C11 1.36(2) . ? N3 C11A 1.50(3) . ? N3 C8A 1.83(3) . ? C8 C8A 1.35(3) . ? C8 C9 1.41(2) . ? C8 C9A 1.90(3) . ? C9 C9A 1.36(4) . ? C9 C10 1.50(2) . ? C10 C11 1.17(2) . ? C10 C9A 1.26(4) . ? C10 C11A 1.65(4) . ? C11 C11A 1.02(3) . ? C11 C9A 1.66(4) . ? C11 N3A 1.86(3) . ? N3A C11A 1.33(3) . ? C8A C9A 1.45(4) . ? C21 C22 1.370(9) . ? C22 C23 1.376(9) . ? C23 C24 1.363(9) . ? C24 C25 1.397(8) . ? C25 C26 1.524(7) . ? C26 C27 1.527(7) . ? C27 C28 1.386(8) . ? C28 C29 1.374(8) . ? C29 C30 1.374(9) . ? C30 C31 1.370(9) . ? C41 C42 1.521(9) . ? N31 C51 1.21(3) . ? C51 C52 1.53(3) . ? N41 C61 1.27(4) . ? C61 C62 1.34(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O12 165.97(16) . 3_655 ? O1 Mn1 O11 93.51(16) . . ? O12 Mn1 O11 96.93(15) 3_655 . ? O1 Mn1 N11 86.19(17) . 3_655 ? O12 Mn1 N11 81.35(16) 3_655 3_655 ? O11 Mn1 N11 165.45(16) . 3_655 ? O1 Mn1 O21 93.52(18) . . ? O12 Mn1 O21 94.57(16) 3_655 . ? O11 Mn1 O21 96.53(16) . . ? N11 Mn1 O21 98.01(17) 3_655 . ? O1 Mn1 O12 100.18(16) . . ? O12 Mn1 O12 77.09(15) 3_655 . ? O11 Mn1 O12 60.53(13) . . ? N11 Mn1 O12 105.18(15) 3_655 . ? O21 Mn1 O12 153.69(14) . . ? O22 Mn2 O11 91.79(15) . . ? O22 Mn2 N2 85.24(17) . . ? O11 Mn2 N2 78.94(15) . . ? O22 Mn2 N1 98.61(18) . . ? O11 Mn2 N1 145.83(18) . . ? N2 Mn2 N1 69.7(2) . . ? O22 Mn2 N12 160.76(16) . . ? O11 Mn2 N12 73.70(14) . . ? N2 Mn2 N12 79.70(17) . . ? N1 Mn2 N12 87.38(18) . . ? O22 Mn2 Br1 97.12(13) . . ? O11 Mn2 Br1 111.16(10) . . ? N2 Mn2 Br1 169.46(13) . . ? N1 Mn2 Br1 99.78(16) . . ? N12 Mn2 Br1 99.87(12) . . ? N2 O1 Mn1 116.0(3) . . ? C1 N1 C5 117.2(7) . . ? C1 N1 Mn2 123.9(6) . . ? C5 N1 Mn2 118.5(4) . . ? C6 N2 O1 116.2(5) . . ? C6 N2 Mn2 121.9(4) . . ? O1 N2 Mn2 121.9(3) . . ? C26 O11 Mn1 106.6(3) . . ? C26 O11 Mn2 119.0(3) . . ? Mn1 O11 Mn2 113.02(16) . . ? C26 O12 Mn1 115.8(3) . 3_655 ? C26 O12 Mn1 82.0(3) . . ? Mn1 O12 Mn1 102.91(15) 3_655 . ? C25 N11 C21 119.6(5) . . ? C25 N11 Mn1 113.4(3) . 3_655 ? C21 N11 Mn1 127.0(4) . 3_655 ? C27 N12 C31 116.9(5) . . ? C27 N12 Mn2 113.2(4) . . ? C31 N12 Mn2 126.6(4) . . ? C41 O21 Mn1 132.5(4) . . ? C41 O22 Mn2 133.2(4) . . ? N1 C1 C2 123.4(9) . . ? C3 C2 C1 118.3(8) . . ? C2 C3 C4 120.6(8) . . ? C3 C4 C5 117.4(9) . . ? N1 C5 C4 123.1(7) . . ? N1 C5 C6 115.6(6) . . ? C4 C5 C6 121.3(7) . . ? N2 C6 C7 124.2(6) . . ? N2 C6 C5 114.2(6) . . ? C7 C6 C5 121.6(6) . . ? N3 C7 C8A 93.1(14) . . ? N3 C7 N3A 44.6(9) . . ? C8A C7 N3A 130.2(15) . . ? N3 C7 C6 123.1(9) . . ? C8A C7 C6 119.3(15) . . ? N3A C7 C6 107.8(9) . . ? N3 C7 C8 117.4(11) . . ? C8A C7 C8 56.3(12) . . ? N3A C7 C8 113.6(12) . . ? C6 C7 C8 119.4(8) . . ? N3A N3 C7 76.1(15) . . ? N3A N3 C11 101(2) . . ? C7 N3 C11 123.5(14) . . ? N3A N3 C11A 60.2(17) . . ? C7 N3 C11A 112.0(16) . . ? C11 N3 C11A 41.5(13) . . ? N3A N3 C8A 113.9(19) . . ? C7 N3 C8A 43.7(9) . . ? C11 N3 C8A 94.1(18) . . ? C11A N3 C8A 113.0(19) . . ? C8A C8 C9 95.2(17) . . ? C8A C8 C7 51.0(10) . . ? C9 C8 C7 116.2(14) . . ? C8A C8 C9A 49.7(18) . . ? C9 C8 C9A 45.7(15) . . ? C7 C8 C9A 81.0(12) . . ? C9A C9 C8 86.4(18) . . ? C9A C9 C10 51.9(19) . . ? C8 C9 C10 115.4(13) . . ? C11 C10 C9A 86(2) . . ? C11 C10 C9 121.7(16) . . ? C9A C10 C9 58.6(18) . . ? C11 C10 C11A 38.1(16) . . ? C9A C10 C11A 108.0(19) . . ? C9 C10 C11A 107.0(15) . . ? C11A C11 C10 97(3) . . ? C11A C11 N3 76(2) . . ? C10 C11 N3 125.6(19) . . ? C11A C11 C9A 121(3) . . ? C10 C11 C9A 49.0(17) . . ? N3 C11 C9A 88(2) . . ? C11A C11 N3A 44.0(18) . . ? C10 C11 N3A 116.2(15) . . ? N3 C11 N3A 32.5(10) . . ? C9A C11 N3A 102.9(14) . . ? N3 N3A C11A 78.1(18) . . ? N3 N3A C7 59.4(14) . . ? C11A N3A C7 113(2) . . ? N3 N3A C11 46.0(14) . . ? C11A N3A C11 32.3(14) . . ? C7 N3A C11 88.5(13) . . ? C7 C8A C8 72.7(13) . . ? C7 C8A C9A 112(2) . . ? C8 C8A C9A 85(2) . . ? C7 C8A N3 43.2(8) . . ? C8 C8A N3 97.0(15) . . ? C9A C8A N3 79.5(17) . . ? C10 C9A C9 70(3) . . ? C10 C9A C8A 130(2) . . ? C9 C9A C8A 92.9(19) . . ? C10 C9A C11 44.8(15) . . ? C9 C9A C11 101(3) . . ? C8A C9A C11 98.1(17) . . ? C10 C9A C8 100(2) . . ? C9 C9A C8 47.9(11) . . ? C8A C9A C8 45.2(12) . . ? C11 C9A C8 100.0(15) . . ? C11 C11A N3A 104(3) . . ? C11 C11A N3 62(2) . . ? N3A C11A N3 41.8(11) . . ? C11 C11A C10 45(2) . . ? N3A C11A C10 121(3) . . ? N3 C11A C10 91.7(19) . . ? N11 C21 C22 121.1(6) . . ? C21 C22 C23 120.1(6) . . ? C24 C23 C22 118.9(6) . . ? C23 C24 C25 119.3(6) . . ? N11 C25 C24 121.1(5) . . ? N11 C25 C26 114.0(4) . . ? C24 C25 C26 124.9(5) . . ? O12 C26 O11 108.7(4) . . ? O12 C26 C25 109.5(4) . . ? O11 C26 C25 106.9(4) . . ? O12 C26 C27 109.2(4) . . ? O11 C26 C27 110.9(4) . . ? C25 C26 C27 111.5(4) . . ? N12 C27 C28 122.4(5) . . ? N12 C27 C26 116.3(5) . . ? C28 C27 C26 121.3(5) . . ? C29 C28 C27 119.5(6) . . ? C28 C29 C30 118.6(6) . . ? C31 C30 C29 118.6(6) . . ? N12 C31 C30 124.0(6) . . ? O22 C41 O21 126.6(6) . . ? O22 C41 C42 117.6(6) . . ? O21 C41 C42 115.9(6) . . ? N31 C51 C52 167(2) . . ? N41 C61 C62 166(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.602 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.078 #===END data_pekm587 _database_code_depnum_ccdc_archive 'CCDC 247219' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28.50 Mn N6 O6.25' _chemical_formula_weight 700.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.870(4) _cell_length_b 11.566(4) _cell_length_c 15.768(6) _cell_angle_alpha 70.03(1) _cell_angle_beta 76.99(1) _cell_angle_gamma 64.79(1) _cell_volume 1678(1) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 11.6 _exptl_crystal_description parallelipiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.37 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 723 _exptl_absorpt_coefficient_mu 0.450 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.2 _diffrn_reflns_number 5108 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4808 _reflns_number_gt 3828 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.7726P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4808 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.006 _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 Mn Mn 0.27711(4) 0.55720(4) 0.74825(3) 0.04482(15) Uani 1 1 d . . . N1 N 0.2093(2) 0.4545(2) 0.67704(16) 0.0518(6) Uani 1 1 d . . . N2 N 0.0562(2) 0.5744(2) 0.80198(15) 0.0446(5) Uani 1 1 d . . . N11 N 0.3426(2) 0.3783(2) 0.87540(15) 0.0462(5) Uani 1 1 d . . . N12 N 0.5007(2) 0.4225(2) 0.72356(16) 0.0515(6) Uani 1 1 d . . . O21 O 0.2782(2) 0.6941(2) 0.80731(17) 0.0703(6) Uani 1 1 d . . . O31 O 0.2666(2) 0.7025(2) 0.62332(16) 0.0751(7) Uani 1 1 d . . . C1 C 0.2832(4) 0.4039(4) 0.6087(2) 0.0670(9) Uani 1 1 d . . . C2 C 0.2342(4) 0.3570(4) 0.5600(3) 0.0842(12) Uani 1 1 d . . . C3 C 0.1033(5) 0.3627(5) 0.5819(3) 0.0935(14) Uani 1 1 d . . . C4 C 0.0236(4) 0.4162(4) 0.6516(2) 0.0720(10) Uani 1 1 d . . . C5 C 0.0797(3) 0.4602(3) 0.69768(19) 0.0485(7) Uani 1 1 d . . . C6 C -0.0001(3) 0.5194(3) 0.77248(18) 0.0437(6) Uani 1 1 d . . . O1 O -0.0206(2) 0.6264(2) 0.87218(14) 0.0564(5) Uani 1 1 d . . . C7 C -0.1374(3) 0.5152(3) 0.80903(18) 0.0452(6) Uani 1 1 d . . . C8 C -0.1576(3) 0.4276(3) 0.8894(2) 0.0583(8) Uani 1 1 d . . . C9 C -0.2878(4) 0.4297(4) 0.9197(2) 0.0670(9) Uani 1 1 d . . . C10 C -0.3921(4) 0.5186(4) 0.8692(2) 0.0657(9) Uani 1 1 d . . . C11 C -0.3627(4) 0.6000(4) 0.7892(3) 0.0813(12) Uani 1 1 d . . . N3 N -0.2379(3) 0.6005(3) 0.7576(2) 0.0759(9) Uani 1 1 d . . . C21 C 0.2697(3) 0.3634(3) 0.9564(2) 0.0546(8) Uani 1 1 d . . . C22 C 0.3180(4) 0.2596(3) 1.0308(2) 0.0647(9) Uani 1 1 d . . . C23 C 0.4470(4) 0.1666(4) 1.0236(2) 0.0684(9) Uani 1 1 d . . . C24 C 0.5246(3) 0.1788(3) 0.9414(2) 0.0583(8) Uani 1 1 d . . . C25 C 0.4699(3) 0.2855(3) 0.86876(19) 0.0457(6) Uani 1 1 d . . . C26 C 0.5496(3) 0.3067(3) 0.77931(19) 0.0471(7) Uani 1 1 d . . . O11 O 0.5773(2) 0.4407(3) 0.64128(15) 0.0712(7) Uani 1 1 d . . . C27 C 0.6784(3) 0.1963(3) 0.7606(2) 0.0547(7) Uani 1 1 d . . . C28 C 0.8014(4) 0.2058(5) 0.7471(4) 0.0955(15) Uani 1 1 d . . . C29 C 0.9174(5) 0.0977(7) 0.7327(4) 0.121(2) Uani 1 1 d . . . C30 C 0.9041(5) -0.0116(6) 0.7325(3) 0.1071(19) Uani 1 1 d . . . C31 C 0.7769(6) -0.0174(4) 0.7485(3) 0.0976(15) Uani 1 1 d . . . N13 N 0.6618(3) 0.0858(3) 0.7637(2) 0.0801(9) Uani 1 1 d . . . O22 O 0.0964(2) 0.7509(2) 0.90489(15) 0.0663(6) Uani 1 1 d . . . C41 C 0.1975(3) 0.7677(3) 0.8555(2) 0.0529(7) Uani 1 1 d . . . C42 C 0.2256(3) 0.8864(3) 0.8520(2) 0.0538(7) Uani 1 1 d . . . C43 C 0.3074(4) 0.9340(4) 0.7820(3) 0.0707(9) Uani 1 1 d . . . C44 C 0.3261(5) 1.0474(4) 0.7775(4) 0.0925(13) Uani 1 1 d . . . C45 C 0.2626(5) 1.1116(4) 0.8432(4) 0.0998(16) Uani 1 1 d . . . C46 C 0.1839(5) 1.0634(4) 0.9144(4) 0.0909(13) Uani 1 1 d . . . C47 C 0.1635(4) 0.9512(4) 0.9193(3) 0.0724(10) Uani 1 1 d . . . O32 O 0.4775(3) 0.6872(3) 0.5696(2) 0.0966(9) Uani 1 1 d . . . C51 C 0.3521(4) 0.7508(3) 0.5755(2) 0.0632(8) Uani 1 1 d . . . C52 C 0.2984(3) 0.8945(3) 0.5236(2) 0.0569(8) Uani 1 1 d . . . C53 C 0.3851(5) 0.9527(4) 0.4655(3) 0.0838(12) Uani 1 1 d . . . C54 C 0.3347(6) 1.0863(5) 0.4183(3) 0.0944(14) Uani 1 1 d . . . C55 C 0.2005(6) 1.1623(4) 0.4283(3) 0.0829(12) Uani 1 1 d . . . C56 C 0.1139(5) 1.1068(4) 0.4848(3) 0.0904(13) Uani 1 1 d . . . C57 C 0.1628(4) 0.9738(4) 0.5326(3) 0.0783(11) Uani 1 1 d . . . HO1 H 0.028(4) 0.666(4) 0.885(3) 0.111(15) Uiso 1 1 d . . . H1 H 0.377(4) 0.400(3) 0.597(2) 0.073(10) Uiso 1 1 d . . . H2 H 0.295(4) 0.319(4) 0.515(3) 0.091(12) Uiso 1 1 d . . . H3 H 0.064(4) 0.331(4) 0.550(3) 0.107(14) Uiso 1 1 d . . . H4 H -0.073(4) 0.429(3) 0.666(2) 0.077(10) Uiso 1 1 d . . . H8 H -0.082(3) 0.371(3) 0.924(2) 0.069(10) Uiso 1 1 d . . . H9 H -0.313(4) 0.378(4) 0.973(3) 0.095(12) Uiso 1 1 d . . . H10 H -0.483(4) 0.521(3) 0.889(2) 0.077(10) Uiso 1 1 d . . . H11 H -0.433(4) 0.661(4) 0.752(3) 0.092(12) Uiso 1 1 d . . . HO11 H 0.529(5) 0.538(5) 0.611(3) 0.128(17) Uiso 1 1 d . . . H21 H 0.178(3) 0.432(3) 0.957(2) 0.067(9) Uiso 1 1 d . . . H22 H 0.266(3) 0.255(3) 1.084(2) 0.058(9) Uiso 1 1 d . . . H23 H 0.480(3) 0.094(3) 1.071(2) 0.068(10) Uiso 1 1 d . . . H24 H 0.616(3) 0.114(3) 0.936(2) 0.064(9) Uiso 1 1 d . . . H28 H 0.803(5) 0.275(4) 0.750(3) 0.109(17) Uiso 1 1 d . . . H29 H 0.988(6) 0.101(6) 0.722(4) 0.15(2) Uiso 1 1 d . . . H30 H 0.986(5) -0.090(5) 0.720(3) 0.125(16) Uiso 1 1 d . . . H31 H 0.766(5) -0.104(5) 0.748(3) 0.147(19) Uiso 1 1 d . . . H43 H 0.354(3) 0.886(3) 0.738(2) 0.073(11) Uiso 1 1 d . . . H44 H 0.382(4) 1.083(4) 0.724(3) 0.113(15) Uiso 1 1 d . . . H45 H 0.273(4) 1.186(5) 0.844(3) 0.114(15) Uiso 1 1 d . . . H46 H 0.136(5) 1.110(5) 0.957(3) 0.115(16) Uiso 1 1 d . . . H47 H 0.103(4) 0.918(3) 0.968(2) 0.083(12) Uiso 1 1 d . . . H53 H 0.477(5) 0.903(5) 0.465(3) 0.122(17) Uiso 1 1 d . . . H54 H 0.401(4) 1.121(4) 0.384(3) 0.112(15) Uiso 1 1 d . . . H55 H 0.165(4) 1.260(4) 0.397(3) 0.108(14) Uiso 1 1 d . . . H56 H 0.022(4) 1.164(4) 0.492(3) 0.108(15) Uiso 1 1 d . . . H57 H 0.109(4) 0.932(3) 0.568(2) 0.074(11) Uiso 1 1 d . . . W1 O 0.1672(16) 0.6663(15) 0.4710(10) 0.135(5) Uiso 0.25 1 d P . . 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 Mn 0.0392(2) 0.0436(3) 0.0499(3) -0.01379(19) 0.00271(18) -0.01701(19) N1 0.0507(14) 0.0563(15) 0.0505(14) -0.0205(12) 0.0053(11) -0.0230(12) N2 0.0386(12) 0.0467(13) 0.0492(13) -0.0175(11) 0.0028(10) -0.0171(10) N11 0.0443(13) 0.0451(13) 0.0486(14) -0.0175(11) 0.0024(11) -0.0164(11) N12 0.0436(13) 0.0521(15) 0.0529(14) -0.0148(12) 0.0078(11) -0.0187(11) O21 0.0617(14) 0.0628(14) 0.0999(18) -0.0430(14) -0.0010(13) -0.0237(11) O31 0.0794(16) 0.0719(15) 0.0697(15) 0.0038(12) -0.0054(13) -0.0437(13) C1 0.064(2) 0.080(2) 0.065(2) -0.0360(19) 0.0136(17) -0.0322(19) C2 0.084(3) 0.113(3) 0.078(3) -0.062(3) 0.023(2) -0.044(2) C3 0.097(3) 0.132(4) 0.096(3) -0.074(3) 0.014(2) -0.063(3) C4 0.067(2) 0.097(3) 0.077(2) -0.046(2) 0.0083(19) -0.044(2) C5 0.0534(17) 0.0482(16) 0.0488(16) -0.0144(13) -0.0010(14) -0.0251(14) C6 0.0437(15) 0.0445(15) 0.0421(15) -0.0085(12) -0.0016(12) -0.0199(13) O1 0.0463(11) 0.0694(14) 0.0655(14) -0.0390(11) 0.0127(10) -0.0262(11) C7 0.0440(16) 0.0482(16) 0.0476(16) -0.0141(13) -0.0052(13) -0.0203(13) C8 0.0523(19) 0.067(2) 0.0521(18) -0.0052(16) -0.0069(15) -0.0274(16) C9 0.064(2) 0.084(2) 0.055(2) -0.0073(18) 0.0029(17) -0.044(2) C10 0.0495(19) 0.080(2) 0.078(2) -0.027(2) 0.0040(18) -0.0364(19) C11 0.049(2) 0.080(3) 0.101(3) 0.000(2) -0.023(2) -0.0227(19) N3 0.0534(17) 0.0759(19) 0.080(2) 0.0145(16) -0.0183(15) -0.0296(15) C21 0.0507(18) 0.0517(18) 0.0518(18) -0.0188(15) 0.0039(15) -0.0117(15) C22 0.067(2) 0.061(2) 0.0482(19) -0.0141(16) 0.0059(17) -0.0139(17) C23 0.072(2) 0.057(2) 0.051(2) -0.0088(17) -0.0037(17) -0.0072(18) C24 0.0510(18) 0.0511(18) 0.058(2) -0.0136(15) -0.0040(15) -0.0076(15) C25 0.0415(15) 0.0434(15) 0.0519(16) -0.0177(13) -0.0019(13) -0.0138(13) C26 0.0402(15) 0.0488(17) 0.0538(17) -0.0174(14) 0.0003(13) -0.0183(13) O11 0.0592(14) 0.0684(15) 0.0581(14) -0.0082(11) 0.0181(11) -0.0175(12) C27 0.0452(17) 0.0526(18) 0.0528(18) -0.0132(14) 0.0012(13) -0.0102(14) C28 0.047(2) 0.070(3) 0.143(4) -0.015(3) 0.005(2) -0.016(2) C29 0.048(3) 0.106(4) 0.144(5) 0.005(3) 0.006(3) -0.005(3) C30 0.085(4) 0.092(4) 0.068(3) -0.011(2) 0.018(2) 0.016(3) C31 0.118(4) 0.066(3) 0.079(3) -0.034(2) -0.002(3) -0.001(3) N13 0.081(2) 0.0663(19) 0.088(2) -0.0342(16) -0.0029(17) -0.0165(17) O22 0.0778(15) 0.0727(15) 0.0654(14) -0.0243(12) 0.0018(12) -0.0447(13) C41 0.0548(18) 0.0477(17) 0.0593(18) -0.0129(15) -0.0166(15) -0.0183(15) C42 0.0505(17) 0.0436(16) 0.071(2) -0.0155(15) -0.0157(15) -0.0173(14) C43 0.069(2) 0.066(2) 0.082(3) -0.017(2) -0.010(2) -0.0314(19) C44 0.098(3) 0.070(3) 0.116(4) -0.005(3) -0.017(3) -0.051(2) C45 0.101(3) 0.054(2) 0.163(5) -0.024(3) -0.048(3) -0.034(2) C46 0.086(3) 0.067(3) 0.139(4) -0.051(3) -0.024(3) -0.023(2) C47 0.066(2) 0.063(2) 0.098(3) -0.037(2) -0.008(2) -0.0227(18) O32 0.0714(18) 0.0743(17) 0.105(2) 0.0142(15) -0.0006(15) -0.0255(14) C51 0.071(2) 0.067(2) 0.0523(18) -0.0065(16) -0.0036(17) -0.0354(19) C52 0.070(2) 0.0571(18) 0.0456(17) -0.0070(14) -0.0045(15) -0.0322(17) C53 0.080(3) 0.077(3) 0.082(3) 0.004(2) -0.004(2) -0.041(2) C54 0.114(4) 0.082(3) 0.080(3) 0.011(2) -0.006(3) -0.058(3) C55 0.126(4) 0.062(2) 0.063(2) -0.012(2) -0.010(2) -0.042(3) C56 0.103(3) 0.058(2) 0.089(3) -0.026(2) 0.005(3) -0.014(2) C57 0.088(3) 0.070(2) 0.070(2) -0.022(2) 0.020(2) -0.035(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O31 2.096(2) . ? Mn O21 2.098(2) . ? Mn N1 2.291(2) . ? Mn N12 2.291(2) . ? Mn N2 2.305(2) . ? Mn N11 2.316(2) . ? N1 C1 1.338(4) . ? N1 C5 1.350(4) . ? N2 C6 1.287(3) . ? N2 O1 1.377(3) . ? N11 C21 1.342(4) . ? N11 C25 1.350(3) . ? N12 C26 1.284(4) . ? N12 O11 1.378(3) . ? O21 C41 1.256(4) . ? O31 C51 1.258(4) . ? C1 C2 1.373(5) . ? C1 H1 0.98(3) . ? C2 C3 1.365(6) . ? C2 H2 0.94(4) . ? C3 C4 1.385(5) . ? C3 H3 0.97(4) . ? C4 C5 1.369(4) . ? C4 H4 0.98(3) . ? C5 C6 1.483(4) . ? C6 C7 1.490(4) . ? O1 HO1 0.92(4) . ? C7 N3 1.326(4) . ? C7 C8 1.366(4) . ? C8 C9 1.380(5) . ? C8 H8 0.96(3) . ? C9 C10 1.353(5) . ? C9 H9 0.92(4) . ? C10 C11 1.358(5) . ? C10 H10 0.96(4) . ? C11 N3 1.337(4) . ? C11 H11 0.94(4) . ? C21 C22 1.369(4) . ? C21 H21 0.98(3) . ? C22 C23 1.364(5) . ? C22 H22 0.90(3) . ? C23 C24 1.377(5) . ? C23 H23 0.91(3) . ? C24 C25 1.380(4) . ? C24 H24 0.97(3) . ? C25 C26 1.481(4) . ? C26 C27 1.492(4) . ? O11 HO11 1.00(5) . ? C27 N13 1.349(4) . ? C27 C28 1.351(5) . ? C28 C29 1.388(7) . ? C28 H28 0.82(4) . ? C29 C30 1.335(8) . ? C29 H29 0.76(6) . ? C30 C31 1.374(7) . ? C30 H30 1.00(5) . ? C31 N13 1.355(5) . ? C31 H31 1.06(5) . ? O22 C41 1.243(4) . ? C41 C42 1.509(4) . ? C42 C43 1.368(5) . ? C42 C47 1.390(5) . ? C43 C44 1.387(5) . ? C43 H43 0.96(3) . ? C44 C45 1.367(7) . ? C44 H44 1.00(4) . ? C45 C46 1.359(7) . ? C45 H45 0.91(5) . ? C46 C47 1.382(5) . ? C46 H46 0.92(5) . ? C47 H47 0.98(4) . ? O32 C51 1.242(4) . ? C51 C52 1.495(4) . ? C52 C57 1.369(5) . ? C52 C53 1.382(5) . ? C53 C54 1.385(6) . ? C53 H53 0.92(4) . ? C54 C55 1.350(6) . ? C54 H54 0.95(4) . ? C55 C56 1.356(6) . ? C55 H55 1.00(4) . ? C56 C57 1.382(5) . ? C56 H56 0.94(4) . ? C57 H57 0.89(3) . ? 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 O31 Mn O21 87.43(10) . . ? O31 Mn N1 85.95(10) . . ? O21 Mn N1 162.43(9) . . ? O31 Mn N12 96.64(9) . . ? O21 Mn N12 106.51(9) . . ? N1 Mn N12 90.43(9) . . ? O31 Mn N2 106.77(9) . . ? O21 Mn N2 96.21(8) . . ? N1 Mn N2 70.28(8) . . ? N12 Mn N2 148.01(8) . . ? O31 Mn N11 166.61(9) . . ? O21 Mn N11 94.15(9) . . ? N1 Mn N11 96.05(9) . . ? N12 Mn N11 70.15(8) . . ? N2 Mn N11 86.30(8) . . ? C1 N1 C5 117.6(3) . . ? C1 N1 Mn 124.3(2) . . ? C5 N1 Mn 117.55(18) . . ? C6 N2 O1 113.9(2) . . ? C6 N2 Mn 119.64(18) . . ? O1 N2 Mn 126.08(16) . . ? C21 N11 C25 117.3(2) . . ? C21 N11 Mn 125.97(19) . . ? C25 N11 Mn 116.55(18) . . ? C26 N12 O11 114.8(2) . . ? C26 N12 Mn 119.32(18) . . ? O11 N12 Mn 123.59(18) . . ? C41 O21 Mn 137.9(2) . . ? C51 O31 Mn 131.7(2) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1 115(2) . . ? C2 C1 H1 122(2) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 H2 124(2) . . ? C1 C2 H2 118(2) . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 122(2) . . ? C4 C3 H3 119(2) . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 119(2) . . ? C3 C4 H4 122(2) . . ? N1 C5 C4 122.3(3) . . ? N1 C5 C6 116.1(2) . . ? C4 C5 C6 121.5(3) . . ? N2 C6 C5 115.9(2) . . ? N2 C6 C7 123.4(2) . . ? C5 C6 C7 120.7(2) . . ? N2 O1 HO1 105(3) . . ? N3 C7 C8 122.4(3) . . ? N3 C7 C6 115.4(2) . . ? C8 C7 C6 122.1(3) . . ? C7 C8 C9 119.1(3) . . ? C7 C8 H8 118(2) . . ? C9 C8 H8 122(2) . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 115(2) . . ? C8 C9 H9 126(2) . . ? C9 C10 C11 118.0(3) . . ? C9 C10 H10 120(2) . . ? C11 C10 H10 122(2) . . ? N3 C11 C10 124.5(3) . . ? N3 C11 H11 116(2) . . ? C10 C11 H11 120(2) . . ? C7 N3 C11 116.8(3) . . ? N11 C21 C22 123.2(3) . . ? N11 C21 H21 114.1(18) . . ? C22 C21 H21 122.7(18) . . ? C23 C22 C21 119.2(3) . . ? C23 C22 H22 120.8(19) . . ? C21 C22 H22 120.0(19) . . ? C22 C23 C24 119.1(3) . . ? C22 C23 H23 121(2) . . ? C24 C23 H23 120(2) . . ? C23 C24 C25 119.0(3) . . ? C23 C24 H24 119.6(18) . . ? C25 C24 H24 121.4(18) . . ? N11 C25 C24 122.3(3) . . ? N11 C25 C26 116.1(2) . . ? C24 C25 C26 121.6(3) . . ? N12 C26 C25 115.7(2) . . ? N12 C26 C27 125.0(3) . . ? C25 C26 C27 119.2(2) . . ? N12 O11 HO11 102(3) . . ? N13 C27 C28 123.7(3) . . ? N13 C27 C26 114.5(3) . . ? C28 C27 C26 121.7(3) . . ? C27 C28 C29 118.6(5) . . ? C27 C28 H28 117(3) . . ? C29 C28 H28 124(3) . . ? C30 C29 C28 119.2(5) . . ? C30 C29 H29 119(5) . . ? C28 C29 H29 122(5) . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120(3) . . ? C31 C30 H30 120(3) . . ? N13 C31 C30 122.3(5) . . ? N13 C31 H31 118(3) . . ? C30 C31 H31 120(3) . . ? C27 N13 C31 116.2(4) . . ? O22 C41 O21 125.2(3) . . ? O22 C41 C42 117.9(3) . . ? O21 C41 C42 116.9(3) . . ? C43 C42 C47 119.5(3) . . ? C43 C42 C41 121.1(3) . . ? C47 C42 C41 119.4(3) . . ? C42 C43 C44 120.2(4) . . ? C42 C43 H43 119(2) . . ? C44 C43 H43 121(2) . . ? C45 C44 C43 119.8(5) . . ? C45 C44 H44 122(3) . . ? C43 C44 H44 118(3) . . ? C46 C45 C44 120.6(4) . . ? C46 C45 H45 116(3) . . ? C44 C45 H45 123(3) . . ? C45 C46 C47 120.1(5) . . ? C45 C46 H46 121(3) . . ? C47 C46 H46 119(3) . . ? C46 C47 C42 119.8(4) . . ? C46 C47 H47 121(2) . . ? C42 C47 H47 119(2) . . ? O32 C51 O31 124.3(3) . . ? O32 C51 C52 118.3(3) . . ? O31 C51 C52 117.4(3) . . ? C57 C52 C53 117.6(3) . . ? C57 C52 C51 121.7(3) . . ? C53 C52 C51 120.7(3) . . ? C52 C53 C54 120.4(4) . . ? C52 C53 H53 118(3) . . ? C54 C53 H53 121(3) . . ? C55 C54 C53 120.9(4) . . ? C55 C54 H54 123(3) . . ? C53 C54 H54 116(3) . . ? C54 C55 C56 119.5(4) . . ? C54 C55 H55 121(2) . . ? C56 C55 H55 120(2) . . ? C55 C56 C57 120.2(5) . . ? C55 C56 H56 117(3) . . ? C57 C56 H56 123(3) . . ? C52 C57 C56 121.4(4) . . ? C52 C57 H57 115(2) . . ? C56 C57 H57 123(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.303 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.041 #===END data_pekm523b _database_code_depnum_ccdc_archive 'CCDC 247220' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H48 Cl2 Mn4 N12 O10' _chemical_formula_weight 1411.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.738(5) _cell_length_b 15.170(6) _cell_length_c 18.191(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.72(1) _cell_angle_gamma 90.00 _cell_volume 3147(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 11.6 _exptl_crystal_description parallelipiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.48 _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method "floating method'" _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.7 _diffrn_reflns_number 6052 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5856 _reflns_number_gt 4250 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.6151P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5856 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.006 _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 0.11692(5) 0.03621(4) 0.96117(3) 0.03342(15) Uani 1 1 d . . . Mn2 Mn 0.01342(5) 0.19771(4) 0.83021(3) 0.03611(16) Uani 1 1 d . . . N1 N 0.1114(3) 0.3248(2) 0.81789(19) 0.0425(8) Uani 1 1 d . . . N2 N 0.1792(3) 0.2050(2) 0.92316(18) 0.0397(7) Uani 1 1 d . . . O1 O 0.2111(2) 0.13998(17) 0.97537(15) 0.0441(7) Uani 1 1 d . . . N11 N 0.2461(3) -0.0155(2) 1.04609(19) 0.0417(8) Uani 1 1 d . . . N12 N 0.0670(3) -0.2697(2) 1.08107(18) 0.0406(8) Uani 1 1 d . . . O11 O 0.0223(2) -0.09696(16) 1.09249(14) 0.0339(6) Uani 1 1 d . . . O12 O 0.0460(2) -0.07387(16) 0.97235(14) 0.0354(6) Uani 1 1 d . . . O21 O 0.1700(3) -0.0017(2) 0.86463(17) 0.0528(8) Uani 1 1 d . . . O22 O 0.1118(3) 0.1055(2) 0.77982(17) 0.0540(8) Uani 1 1 d . . . Cl Cl -0.15037(10) 0.21227(8) 0.72579(6) 0.0568(3) Uani 1 1 d . . . C1 C 0.0718(4) 0.3863(3) 0.7653(3) 0.0541(11) Uani 1 1 d . . . H1 H 0.0018 0.3759 0.7298 0.062(7) Uiso 1 1 calc R . . C2 C 0.1309(5) 0.4649(3) 0.7613(3) 0.0701(15) Uani 1 1 d . . . H2 H 0.1017 0.5063 0.7238 0.062(7) Uiso 1 1 calc R . . C3 C 0.2330(5) 0.4795(3) 0.8143(3) 0.0753(17) Uani 1 1 d . . . H3 H 0.2739 0.5319 0.8136 0.062(7) Uiso 1 1 calc R . . C4 C 0.2756(4) 0.4169(3) 0.8687(3) 0.0620(13) Uani 1 1 d . . . H4 H 0.3456 0.4261 0.9045 0.062(7) Uiso 1 1 calc R . . C5 C 0.2123(4) 0.3398(3) 0.8692(2) 0.0435(9) Uani 1 1 d . . . C6 C 0.2522(3) 0.2686(2) 0.9258(2) 0.0386(9) Uani 1 1 d . . . C7 C 0.3703(3) 0.2714(3) 0.9790(2) 0.0419(9) Uani 1 1 d . . . C8 C 0.4570(5) 0.2199(5) 0.9670(4) 0.103(3) Uani 1 1 d . . . H8 H 0.4446 0.1824 0.9254 0.136(14) Uiso 1 1 calc R . . C9 C 0.5656(5) 0.2239(6) 1.0181(5) 0.123(3) Uani 1 1 d . . . H9 H 0.6269 0.1888 1.0107 0.136(14) Uiso 1 1 calc R . . C10 C 0.5820(5) 0.2768(5) 1.0767(4) 0.0832(18) Uani 1 1 d . . . H10 H 0.6547 0.2815 1.1107 0.136(14) Uiso 1 1 calc R . . C11 C 0.4897(6) 0.3235(6) 1.0853(4) 0.115(3) Uani 1 1 d . . . H11 H 0.4998 0.3588 1.1282 0.136(14) Uiso 1 1 calc R . . N3 N 0.3831(4) 0.3237(4) 1.0371(3) 0.0922(17) Uani 1 1 d . . . C21 C 0.3537(4) 0.0177(3) 1.0740(3) 0.0653(15) Uani 1 1 d . . . H21 H 0.3753 0.0694 1.0534 0.070(8) Uiso 1 1 calc R . . C22 C 0.4321(4) -0.0222(3) 1.1317(3) 0.0726(16) Uani 1 1 d . . . H22 H 0.5059 0.0022 1.1504 0.070(8) Uiso 1 1 calc R . . C23 C 0.4008(4) -0.0988(3) 1.1617(3) 0.0628(13) Uani 1 1 d . . . H23 H 0.4533 -0.1268 1.2011 0.070(8) Uiso 1 1 calc R . . C24 C 0.2910(4) -0.1339(3) 1.1330(2) 0.0481(10) Uani 1 1 d . . . H24 H 0.2685 -0.1860 1.1526 0.070(8) Uiso 1 1 calc R . . C25 C 0.2151(3) -0.0906(2) 1.0750(2) 0.0352(8) Uani 1 1 d . . . C26 C 0.0895(3) -0.1192(2) 1.0400(2) 0.0327(8) Uani 1 1 d . . . C27 C 0.0852(3) -0.2185(2) 1.0249(2) 0.0352(8) Uani 1 1 d . . . C28 C 0.1046(4) -0.2519(3) 0.9588(3) 0.0495(10) Uani 1 1 d . . . H28 H 0.1159 -0.2145 0.9207 0.064(7) Uiso 1 1 calc R . . C29 C 0.1071(5) -0.3427(3) 0.9500(3) 0.0624(13) Uani 1 1 d . . . H29 H 0.1185 -0.3672 0.9054 0.064(7) Uiso 1 1 calc R . . C30 C 0.0924(5) -0.3957(3) 1.0081(3) 0.0640(14) Uani 1 1 d . . . H30 H 0.0960 -0.4568 1.0042 0.064(7) Uiso 1 1 calc R . . C31 C 0.0722(4) -0.3570(3) 1.0723(3) 0.0545(11) Uani 1 1 d . . . H31 H 0.0617 -0.3932 1.1114 0.064(7) Uiso 1 1 calc R . . C41 C 0.1674(3) 0.0360(3) 0.8027(2) 0.0438(9) Uani 1 1 d . . . C42 C 0.2371(4) -0.0064(3) 0.7530(2) 0.0461(10) Uani 1 1 d . . . C43 C 0.2484(5) 0.0342(4) 0.6870(3) 0.0750(15) Uani 1 1 d . . . H43 H 0.2096 0.0869 0.6716 0.114(11) Uiso 1 1 calc R . . C44 C 0.3189(6) -0.0047(5) 0.6435(4) 0.097(2) Uani 1 1 d . . . H44 H 0.3282 0.0227 0.5996 0.114(11) Uiso 1 1 calc R . . C45 C 0.3737(5) -0.0829(5) 0.6659(4) 0.093(2) Uani 1 1 d . . . H45 H 0.4209 -0.1082 0.6373 0.114(11) Uiso 1 1 calc R . . C46 C 0.3601(5) -0.1242(4) 0.7294(4) 0.0747(16) Uani 1 1 d . . . H46 H 0.3963 -0.1782 0.7432 0.114(11) Uiso 1 1 calc R . . C47 C 0.2927(4) -0.0863(3) 0.7736(3) 0.0561(12) Uani 1 1 d . . . H47 H 0.2845 -0.1145 0.8175 0.114(11) Uiso 1 1 calc R . . N21 N 0.3771(6) 0.2434(6) 0.2496(5) 0.134(3) Uani 1 1 d . . . C51 C 0.2948(7) 0.2343(5) 0.2009(5) 0.099(2) Uani 1 1 d . . . C52 C 0.1880(7) 0.2281(6) 0.1407(4) 0.111(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 0.0317(3) 0.0314(3) 0.0339(3) 0.0053(2) 0.0014(2) -0.0010(2) Mn2 0.0373(3) 0.0359(3) 0.0324(3) 0.0055(2) 0.0029(2) 0.0002(2) N1 0.0385(18) 0.0407(18) 0.048(2) 0.0128(15) 0.0094(15) 0.0004(14) N2 0.0397(17) 0.0326(16) 0.0431(19) 0.0066(14) 0.0024(14) -0.0024(14) O1 0.0404(15) 0.0374(14) 0.0466(16) 0.0139(12) -0.0054(12) -0.0079(12) N11 0.0322(16) 0.0406(18) 0.0466(19) 0.0086(15) -0.0021(14) -0.0005(14) N12 0.0457(19) 0.0337(17) 0.0420(19) 0.0058(14) 0.0098(15) 0.0027(14) O11 0.0340(13) 0.0313(13) 0.0355(14) 0.0059(11) 0.0067(11) 0.0036(10) O12 0.0350(13) 0.0329(13) 0.0340(14) 0.0058(11) -0.0004(11) -0.0030(11) O21 0.0621(19) 0.0505(17) 0.0515(19) 0.0050(15) 0.0247(15) 0.0083(15) O22 0.0586(19) 0.0525(18) 0.0518(18) -0.0018(15) 0.0151(15) 0.0093(15) Cl 0.0575(6) 0.0635(7) 0.0408(6) 0.0035(5) -0.0055(5) 0.0075(5) C1 0.049(3) 0.054(3) 0.058(3) 0.016(2) 0.008(2) 0.007(2) C2 0.068(3) 0.054(3) 0.085(4) 0.034(3) 0.011(3) 0.006(3) C3 0.071(3) 0.044(3) 0.107(5) 0.028(3) 0.011(3) -0.010(2) C4 0.053(3) 0.048(3) 0.078(3) 0.017(2) 0.004(2) -0.012(2) C5 0.043(2) 0.040(2) 0.046(2) 0.0059(19) 0.0092(18) -0.0030(18) C6 0.037(2) 0.036(2) 0.042(2) 0.0040(17) 0.0070(17) -0.0019(16) C7 0.037(2) 0.039(2) 0.047(2) 0.0022(18) 0.0029(18) -0.0057(17) C8 0.046(3) 0.153(7) 0.100(5) -0.058(5) -0.004(3) 0.019(4) C9 0.042(3) 0.180(8) 0.131(6) -0.054(6) -0.012(4) 0.026(4) C10 0.047(3) 0.113(5) 0.076(4) 0.008(4) -0.013(3) -0.009(3) C11 0.076(4) 0.166(8) 0.083(5) -0.055(5) -0.021(4) 0.008(5) N3 0.060(3) 0.125(4) 0.077(3) -0.045(3) -0.013(2) 0.012(3) C21 0.041(2) 0.049(3) 0.091(4) 0.019(3) -0.014(2) -0.011(2) C22 0.044(3) 0.063(3) 0.094(4) 0.014(3) -0.019(3) -0.011(2) C23 0.044(2) 0.070(3) 0.061(3) 0.014(3) -0.013(2) 0.007(2) C24 0.041(2) 0.050(2) 0.048(3) 0.014(2) 0.0005(19) 0.0038(19) C25 0.0354(19) 0.0361(19) 0.0325(19) 0.0028(16) 0.0050(16) 0.0032(16) C26 0.0323(18) 0.0322(18) 0.0321(19) 0.0049(15) 0.0045(15) 0.0021(15) C27 0.0336(19) 0.0344(19) 0.037(2) 0.0027(16) 0.0065(16) 0.0020(15) C28 0.060(3) 0.045(2) 0.045(2) 0.000(2) 0.016(2) 0.000(2) C29 0.087(4) 0.044(2) 0.064(3) -0.012(2) 0.032(3) -0.004(2) C30 0.082(4) 0.031(2) 0.086(4) -0.008(2) 0.034(3) 0.001(2) C31 0.069(3) 0.033(2) 0.066(3) 0.012(2) 0.026(2) 0.005(2) C41 0.040(2) 0.041(2) 0.051(3) -0.005(2) 0.0134(18) -0.0051(18) C42 0.046(2) 0.046(2) 0.050(3) -0.009(2) 0.017(2) -0.0108(19) C43 0.100(4) 0.065(3) 0.070(4) 0.002(3) 0.041(3) -0.004(3) C44 0.125(6) 0.102(5) 0.087(5) -0.010(4) 0.070(4) -0.027(5) C45 0.076(4) 0.102(5) 0.114(6) -0.045(5) 0.052(4) -0.013(4) C46 0.056(3) 0.073(4) 0.100(5) -0.025(3) 0.029(3) 0.002(3) C47 0.046(2) 0.052(3) 0.072(3) -0.009(2) 0.016(2) -0.001(2) N21 0.089(5) 0.152(7) 0.154(7) 0.027(5) 0.013(5) 0.005(5) C51 0.091(5) 0.097(5) 0.119(6) 0.006(5) 0.044(5) 0.002(4) C52 0.110(5) 0.146(7) 0.070(4) -0.019(4) 0.009(4) -0.042(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 O12 1.898(3) . ? Mn1 O1 1.905(3) . ? Mn1 O11 1.928(2) 3_557 ? Mn1 N11 2.047(3) . ? Mn1 O21 2.079(3) . ? Mn2 O22 2.153(3) . ? Mn2 O11 2.184(3) 3_557 ? Mn2 N2 2.257(3) . ? Mn2 N1 2.283(3) . ? Mn2 N12 2.326(3) 3_557 ? Mn2 Cl 2.3708(14) . ? N1 C1 1.339(5) . ? N1 C5 1.342(5) . ? N2 C6 1.284(5) . ? N2 O1 1.359(4) . ? N11 C25 1.340(5) . ? N11 C21 1.343(5) . ? N12 C31 1.337(5) . ? N12 C27 1.340(5) . ? N12 Mn2 2.326(3) 3_557 ? O11 C26 1.417(4) . ? O11 Mn1 1.928(2) 3_557 ? O11 Mn2 2.184(2) 3_557 ? O12 C26 1.396(4) . ? O21 C41 1.258(5) . ? O22 C41 1.257(5) . ? C1 C2 1.390(6) . ? C1 H1 0.9300 . ? C2 C3 1.367(7) . ? C2 H2 0.9300 . ? C3 C4 1.378(6) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.489(5) . ? C6 C7 1.491(5) . ? C7 N3 1.301(6) . ? C7 C8 1.342(7) . ? C8 C9 1.389(8) . ? C8 H8 0.9300 . ? C9 C10 1.312(9) . ? C9 H9 0.9300 . ? C10 C11 1.335(9) . ? C10 H10 0.9300 . ? C11 N3 1.347(7) . ? C11 H11 0.9300 . ? C21 C22 1.362(6) . ? C21 H21 0.9300 . ? C22 C23 1.370(7) . ? C22 H22 0.9300 . ? C23 C24 1.378(6) . ? C23 H23 0.9300 . ? C24 C25 1.376(5) . ? C24 H24 0.9300 . ? C25 C26 1.524(5) . ? C26 C27 1.529(5) . ? C27 C28 1.373(6) . ? C28 C29 1.388(6) . ? C28 H28 0.9300 . ? C29 C30 1.371(7) . ? C29 H29 0.9300 . ? C30 C31 1.378(7) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C41 C42 1.500(6) . ? C42 C47 1.384(6) . ? C42 C43 1.384(7) . ? C43 C44 1.402(8) . ? C43 H43 0.9300 . ? C44 C45 1.365(9) . ? C44 H44 0.9300 . ? C45 C46 1.356(9) . ? C45 H45 0.9300 . ? C46 C47 1.381(7) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? N21 C51 1.154(9) . ? C51 C52 1.459(10) . ? 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 O12 Mn1 O1 165.29(11) . . ? O12 Mn1 O11 97.73(11) . 3_557 ? O1 Mn1 O11 93.92(11) . 3_557 ? O12 Mn1 N11 81.18(12) . . ? O1 Mn1 N11 84.99(12) . . ? O11 Mn1 N11 162.31(13) 3_557 . ? O12 Mn1 O21 94.23(12) . . ? O1 Mn1 O21 93.60(13) . . ? O11 Mn1 O21 95.30(12) 3_557 . ? N11 Mn1 O21 102.40(13) . . ? O22 Mn2 O11 91.35(11) . 3_557 ? O22 Mn2 N2 84.08(12) . . ? O11 Mn2 N2 79.35(10) 3_557 . ? O22 Mn2 N1 100.00(13) . . ? O11 Mn2 N1 146.35(11) 3_557 . ? N2 Mn2 N1 70.57(12) . . ? O22 Mn2 N12 161.35(12) . 3_557 ? O11 Mn2 N12 73.15(11) 3_557 3_557 ? N2 Mn2 N12 82.92(12) . 3_557 ? N1 Mn2 N12 88.20(12) . 3_557 ? O22 Mn2 Cl 97.72(9) . . ? O11 Mn2 Cl 109.76(8) 3_557 . ? N2 Mn2 Cl 170.60(9) . . ? N1 Mn2 Cl 100.04(9) . . ? N12 Mn2 Cl 97.29(9) 3_557 . ? C1 N1 C5 118.6(4) . . ? C1 N1 Mn2 124.2(3) . . ? C5 N1 Mn2 117.2(3) . . ? C6 N2 O1 116.7(3) . . ? C6 N2 Mn2 120.9(3) . . ? O1 N2 Mn2 122.2(2) . . ? N2 O1 Mn1 116.8(2) . . ? C25 N11 C21 119.3(3) . . ? C25 N11 Mn1 113.6(2) . . ? C21 N11 Mn1 127.1(3) . . ? C31 N12 C27 117.6(4) . . ? C31 N12 Mn2 125.8(3) . 3_557 ? C27 N12 Mn2 114.9(2) . 3_557 ? C26 O11 Mn1 108.3(2) . 3_557 ? C26 O11 Mn2 119.3(2) . 3_557 ? Mn1 O11 Mn2 113.05(11) 3_557 3_557 ? C26 O12 Mn1 116.8(2) . . ? C41 O21 Mn1 133.1(3) . . ? C41 O22 Mn2 133.9(3) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 117.9(4) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 122.3(4) . . ? N2 C6 C5 114.9(3) . . ? N2 C6 C7 123.7(3) . . ? C5 C6 C7 121.4(3) . . ? N3 C7 C8 122.8(4) . . ? N3 C7 C6 117.1(4) . . ? C8 C7 C6 120.1(4) . . ? C7 C8 C9 118.5(6) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 120.3(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 116.9(6) . . ? C9 C10 H10 121.5 . . ? C11 C10 H10 121.5 . . ? C10 C11 N3 125.4(6) . . ? C10 C11 H11 117.3 . . ? N3 C11 H11 117.3 . . ? C7 N3 C11 116.0(5) . . ? N11 C21 C22 121.8(4) . . ? N11 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C23 119.2(4) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 118.8(4) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N11 C25 C24 121.4(4) . . ? N11 C25 C26 113.8(3) . . ? C24 C25 C26 124.8(3) . . ? O12 C26 O11 109.4(3) . . ? O12 C26 C25 110.0(3) . . ? O11 C26 C25 106.8(3) . . ? O12 C26 C27 109.7(3) . . ? O11 C26 C27 110.8(3) . . ? C25 C26 C27 110.0(3) . . ? N12 C27 C28 122.9(4) . . ? N12 C27 C26 116.0(3) . . ? C28 C27 C26 121.1(4) . . ? C27 C28 C29 118.8(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C28 118.8(5) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 118.8(4) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N12 C31 C30 123.1(4) . . ? N12 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? O22 C41 O21 125.3(4) . . ? O22 C41 C42 118.4(4) . . ? O21 C41 C42 116.3(4) . . ? C47 C42 C43 119.3(5) . . ? C47 C42 C41 120.1(4) . . ? C43 C42 C41 120.6(4) . . ? C42 C43 C44 119.5(6) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C45 C44 C43 119.8(6) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 120.9(6) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 120.2(6) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C42 120.3(5) . . ? C46 C47 H47 119.9 . . ? C42 C47 H47 119.9 . . ? N21 C51 C52 176.4(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.389 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.066 #===END data_pekm421 _database_code_depnum_ccdc_archive 'CCDC 247221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H43 Mn4 N13 O17' _chemical_formula_weight 1317.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.25(1) _cell_length_b 19.79(2) _cell_length_c 10.365(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.18(3) _cell_angle_gamma 90.00 _cell_volume 2918(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 11.6 _exptl_crystal_description parallelipiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 1.49 _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2.9 _diffrn_reflns_number 4944 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4664 _reflns_number_gt 3668 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+5.4841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4664 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1969 _refine_ls_wR_factor_gt 0.1797 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.016 _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 0.59108(5) 0.53581(4) 0.09678(7) 0.0373(3) Uani 1 1 d . . . Mn2 Mn 0.57154(6) 0.70707(4) 0.07751(8) 0.0447(3) Uani 1 1 d . . . O1 O 0.5918(3) 0.57695(17) 0.2625(3) 0.0500(9) Uani 1 1 d . . . N1 N 0.5973(3) 0.7777(2) 0.2508(5) 0.0533(12) Uani 1 1 d . . . N2 N 0.5933(3) 0.6458(2) 0.2627(4) 0.0469(11) Uani 1 1 d . . . O11 O 0.5219(2) 0.60873(16) 0.0125(3) 0.0379(8) Uani 1 1 d . . . O12 O 0.4159(2) 0.52478(16) 0.0459(3) 0.0385(8) Uani 1 1 d . . . N11 N 0.3715(3) 0.5514(2) -0.1929(4) 0.0440(10) Uani 1 1 d . . . N12 N 0.4148(3) 0.6966(2) 0.1394(5) 0.0542(12) Uani 1 1 d . . . O21 O 0.7241(3) 0.5714(2) 0.0586(4) 0.0542(10) Uani 1 1 d . . . O22 O 0.7155(3) 0.6839(2) 0.0462(4) 0.0575(10) Uani 1 1 d . . . O31 O 0.5369(9) 0.8001(4) -0.0367(8) 0.158(4) Uani 1 1 d . . . O32 O 0.5679(7) 0.7293(5) -0.1611(10) 0.162(4) Uani 1 1 d . . . C1 C 0.5925(5) 0.8455(3) 0.2449(7) 0.0650(17) Uani 1 1 d . . . H1 H 0.5865 0.8661 0.1642 0.068(10) Uiso 1 1 calc R . . C2 C 0.5960(5) 0.8859(3) 0.3540(8) 0.076(2) Uani 1 1 d . . . H2 H 0.5918 0.9326 0.3460 0.068(10) Uiso 1 1 calc R . . C3 C 0.6056(5) 0.8571(3) 0.4724(8) 0.072(2) Uani 1 1 d . . . H3 H 0.6080 0.8837 0.5465 0.068(10) Uiso 1 1 calc R . . C4 C 0.6116(5) 0.7875(3) 0.4810(7) 0.0635(17) Uani 1 1 d . . . H4 H 0.6184 0.7665 0.5613 0.068(10) Uiso 1 1 calc R . . C5 C 0.6076(4) 0.7496(3) 0.3690(6) 0.0492(13) Uani 1 1 d . . . C6 C 0.6102(4) 0.6739(3) 0.3727(5) 0.0468(12) Uani 1 1 d . . . C7 C 0.6292(5) 0.6372(3) 0.4963(6) 0.0575(15) Uani 1 1 d . . . C8 C 0.5649(7) 0.5905(5) 0.5417(9) 0.102(3) Uani 1 1 d . . . H8 H 0.5080 0.5823 0.4960 0.15(2) Uiso 1 1 calc R . . C9 C 0.5880(9) 0.5572(6) 0.6558(10) 0.117(4) Uani 1 1 d . . . H9 H 0.5480 0.5248 0.6874 0.15(2) Uiso 1 1 calc R . . C10 C 0.6704(10) 0.5726(4) 0.7211(8) 0.108(4) Uani 1 1 d . . . H10 H 0.6855 0.5538 0.8017 0.15(2) Uiso 1 1 calc R . . C11 C 0.7268(10) 0.6136(6) 0.6699(12) 0.158(6) Uani 1 1 d . . . H11 H 0.7855 0.6199 0.7120 0.15(2) Uiso 1 1 calc R . . N3 N 0.7077(7) 0.6489(4) 0.5579(8) 0.129(4) Uani 1 1 d . . . C21 C 0.3390(4) 0.5572(3) -0.3163(6) 0.0554(15) Uani 1 1 d . . . H21 H 0.3325 0.5184 -0.3668 0.060(9) Uiso 1 1 calc R . . C22 C 0.3153(5) 0.6181(3) -0.3697(6) 0.0658(18) Uani 1 1 d . . . H22 H 0.2933 0.6208 -0.4557 0.060(9) Uiso 1 1 calc R . . C23 C 0.3243(5) 0.6756(3) -0.2948(7) 0.0638(17) Uani 1 1 d . . . H23 H 0.3082 0.7176 -0.3298 0.060(9) Uiso 1 1 calc R . . C24 C 0.3573(4) 0.6703(3) -0.1677(6) 0.0520(14) Uani 1 1 d . . . H24 H 0.3634 0.7085 -0.1154 0.060(9) Uiso 1 1 calc R . . C25 C 0.3812(3) 0.6068(3) -0.1193(5) 0.0413(11) Uani 1 1 d . . . C26 C 0.4251(3) 0.5930(2) 0.0152(5) 0.0400(11) Uani 1 1 d . . . C27 C 0.3782(4) 0.6353(3) 0.1162(5) 0.0417(12) Uani 1 1 d . . . C28 C 0.3013(4) 0.6119(3) 0.1782(6) 0.0495(13) Uani 1 1 d . . . H28 H 0.2777 0.5688 0.1614 0.062(9) Uiso 1 1 calc R . . C29 C 0.2597(4) 0.6537(3) 0.2662(6) 0.0588(15) Uani 1 1 d . . . H29 H 0.2079 0.6390 0.3093 0.062(9) Uiso 1 1 calc R . . C30 C 0.2957(5) 0.7168(3) 0.2885(7) 0.0648(17) Uani 1 1 d . . . H30 H 0.2688 0.7459 0.3464 0.062(9) Uiso 1 1 calc R . . C31 C 0.3724(4) 0.7364(3) 0.2236(7) 0.0621(17) Uani 1 1 d . . . H31 H 0.3965 0.7795 0.2387 0.062(9) Uiso 1 1 calc R . . C41 C 0.7597(4) 0.6293(3) 0.0435(5) 0.0514(14) Uani 1 1 d . . . C42 C 0.8630(4) 0.6327(4) 0.0201(8) 0.074(2) Uani 1 1 d . . . H42A H 0.8804 0.5943 -0.0298 0.14(2) Uiso 1 1 calc R . . H42B H 0.8987 0.6328 0.1014 0.14(2) Uiso 1 1 calc R . . H42C H 0.8758 0.6734 -0.0263 0.14(2) Uiso 1 1 calc R . . N51 N 0.5399(5) 0.7890(4) -0.1337(9) 0.088(2) Uani 1 1 d . . . O33 O 0.5177(6) 0.8225(4) -0.2340(7) 0.136(3) Uani 1 1 d . . . N61 N 0.6191(17) 0.0654(13) 0.128(2) 0.159(8) Uiso 0.50 1 d P . . C61 C 0.629(3) 0.025(2) 0.023(4) 0.181(13) Uiso 0.50 1 d P . . C62 C 0.635(3) -0.013(2) -0.060(4) 0.193(14) Uiso 0.50 1 d P . . OW1 O 0.446(2) 0.0168(14) 0.223(3) 0.221(10) Uiso 0.50 1 d P . . 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 0.0441(4) 0.0273(4) 0.0401(5) 0.0001(3) -0.0012(3) 0.0003(3) Mn2 0.0520(5) 0.0308(4) 0.0514(5) 0.0011(3) 0.0020(4) -0.0050(3) O1 0.076(3) 0.0311(19) 0.043(2) -0.0023(15) -0.0020(18) -0.0032(17) N1 0.057(3) 0.035(2) 0.067(3) -0.006(2) 0.000(2) -0.009(2) N2 0.057(3) 0.031(2) 0.052(3) -0.003(2) 0.002(2) -0.0014(19) O11 0.0401(18) 0.0299(17) 0.0433(19) 0.0021(14) -0.0007(14) 0.0011(14) O12 0.0482(19) 0.0273(17) 0.0397(18) 0.0005(14) -0.0006(15) 0.0014(14) N11 0.047(2) 0.040(2) 0.045(2) 0.0016(19) -0.0021(19) 0.0051(19) N12 0.058(3) 0.037(2) 0.067(3) -0.006(2) 0.004(2) 0.003(2) O21 0.045(2) 0.045(2) 0.072(3) -0.0001(19) 0.0038(18) -0.0080(17) O22 0.051(2) 0.052(2) 0.070(3) 0.002(2) 0.0068(19) -0.0060(19) O31 0.298(13) 0.096(5) 0.076(5) 0.026(4) -0.026(6) -0.024(6) O32 0.141(7) 0.141(8) 0.205(10) 0.057(7) 0.019(6) 0.020(6) C1 0.073(4) 0.042(3) 0.079(5) -0.002(3) 0.003(3) -0.005(3) C2 0.084(5) 0.036(3) 0.108(6) -0.015(4) -0.001(4) 0.002(3) C3 0.081(5) 0.046(4) 0.088(5) -0.026(4) -0.010(4) 0.009(3) C4 0.071(4) 0.055(4) 0.063(4) -0.013(3) -0.009(3) 0.006(3) C5 0.049(3) 0.042(3) 0.056(3) -0.007(3) -0.001(2) -0.004(2) C6 0.053(3) 0.042(3) 0.045(3) -0.004(2) 0.006(2) -0.003(2) C7 0.078(4) 0.044(3) 0.049(3) -0.011(3) -0.008(3) -0.003(3) C8 0.089(6) 0.125(8) 0.094(6) 0.038(6) 0.025(5) 0.000(5) C9 0.153(10) 0.113(8) 0.091(7) 0.036(6) 0.045(7) 0.015(7) C10 0.201(12) 0.058(5) 0.061(5) 0.008(4) -0.025(6) -0.015(6) C11 0.208(14) 0.113(9) 0.138(10) 0.053(8) -0.104(10) -0.060(9) N3 0.163(8) 0.092(5) 0.123(6) 0.050(5) -0.074(6) -0.058(5) C21 0.068(4) 0.052(3) 0.045(3) -0.001(3) -0.008(3) 0.010(3) C22 0.081(4) 0.065(4) 0.050(4) 0.011(3) -0.011(3) 0.010(3) C23 0.067(4) 0.044(3) 0.080(5) 0.021(3) -0.003(3) 0.010(3) C24 0.058(3) 0.037(3) 0.060(4) 0.007(3) -0.007(3) 0.005(2) C25 0.039(3) 0.037(3) 0.048(3) 0.003(2) 0.002(2) 0.000(2) C26 0.042(3) 0.028(2) 0.050(3) 0.004(2) -0.001(2) -0.001(2) C27 0.045(3) 0.031(3) 0.049(3) 0.002(2) -0.002(2) 0.008(2) C28 0.050(3) 0.040(3) 0.059(3) -0.001(3) 0.006(3) 0.004(2) C29 0.053(3) 0.059(4) 0.065(4) 0.002(3) 0.011(3) 0.008(3) C30 0.062(4) 0.060(4) 0.073(4) -0.020(3) 0.009(3) 0.012(3) C31 0.059(4) 0.039(3) 0.089(5) -0.025(3) 0.007(3) 0.003(3) C41 0.044(3) 0.065(4) 0.045(3) 0.003(3) -0.002(2) -0.008(3) C42 0.047(3) 0.071(4) 0.105(6) 0.005(4) 0.009(3) -0.008(3) N51 0.068(4) 0.072(5) 0.123(7) 0.048(5) 0.005(4) -0.010(3) O33 0.157(7) 0.140(6) 0.110(5) 0.055(5) 0.010(5) 0.032(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 O1 1.900(4) . ? Mn1 O12 1.902(3) 3_665 ? Mn1 O11 1.929(3) . ? Mn1 N11 2.049(4) 3_665 ? Mn1 O21 2.081(4) . ? Mn2 O22 2.144(4) . ? Mn2 O11 2.165(4) . ? Mn2 O31 2.229(8) . ? Mn2 N2 2.277(5) . ? Mn2 N1 2.290(5) . ? Mn2 N12 2.366(5) . ? Mn2 O32 2.509(10) . ? O1 N2 1.363(6) . ? N1 C1 1.344(8) . ? N1 C5 1.346(8) . ? N2 C6 1.278(7) . ? O11 C26 1.416(6) . ? O12 C26 1.394(6) . ? O12 Mn1 1.902(3) 3_665 ? N11 C25 1.338(7) . ? N11 C21 1.341(7) . ? N11 Mn1 2.049(4) 3_665 ? N12 C27 1.338(7) . ? N12 C31 1.342(8) . ? O21 C41 1.265(7) . ? O22 C41 1.252(7) . ? O31 N51 1.032(10) . ? O32 N51 1.284(12) . ? C1 C2 1.383(10) . ? C1 H1 0.9300 . ? C2 C3 1.352(11) . ? C2 H2 0.9300 . ? C3 C4 1.383(9) . ? C3 H3 0.9300 . ? C4 C5 1.381(8) . ? C4 H4 0.9300 . ? C5 C6 1.499(8) . ? C6 C7 1.484(8) . ? C7 N3 1.279(9) . ? C7 C8 1.401(11) . ? C8 C9 1.378(13) . ? C8 H8 0.9300 . ? C9 C10 1.357(15) . ? C9 H9 0.9300 . ? C10 C11 1.277(15) . ? C10 H10 0.9300 . ? C11 N3 1.369(12) . ? C11 H11 0.9300 . ? C21 C22 1.361(8) . ? C21 H21 0.9300 . ? C22 C23 1.381(9) . ? C22 H22 0.9300 . ? C23 C24 1.379(9) . ? C23 H23 0.9300 . ? C24 C25 1.389(7) . ? C24 H24 0.9300 . ? C25 C26 1.521(7) . ? C26 C27 1.524(7) . ? C27 C28 1.381(8) . ? C28 C29 1.388(8) . ? C28 H28 0.9300 . ? C29 C30 1.365(9) . ? C29 H29 0.9300 . ? C30 C31 1.371(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C41 C42 1.508(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N51 O33 1.258(9) . ? N61 C61 1.37(4) . ? C61 C62 1.14(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O12 165.97(15) . 3_665 ? O1 Mn1 O11 93.77(16) . . ? O12 Mn1 O11 96.67(15) 3_665 . ? O1 Mn1 N11 86.18(17) . 3_665 ? O12 Mn1 N11 81.25(17) 3_665 3_665 ? O11 Mn1 N11 164.36(16) . 3_665 ? O1 Mn1 O21 93.87(17) . . ? O12 Mn1 O21 94.28(16) 3_665 . ? O11 Mn1 O21 96.23(16) . . ? N11 Mn1 O21 99.37(17) 3_665 . ? O22 Mn2 O11 93.42(15) . . ? O22 Mn2 O31 106.4(3) . . ? O11 Mn2 O31 121.2(3) . . ? O22 Mn2 N2 85.81(17) . . ? O11 Mn2 N2 79.10(15) . . ? O31 Mn2 N2 154.6(3) . . ? O22 Mn2 N1 97.82(17) . . ? O11 Mn2 N1 145.91(16) . . ? O31 Mn2 N1 86.2(3) . . ? N2 Mn2 N1 69.83(18) . . ? O22 Mn2 N12 161.36(16) . . ? O11 Mn2 N12 73.09(15) . . ? O31 Mn2 N12 91.8(3) . . ? N2 Mn2 N12 79.12(17) . . ? N1 Mn2 N12 87.30(17) . . ? O22 Mn2 O32 81.7(2) . . ? O11 Mn2 O32 82.1(3) . . ? O31 Mn2 O32 48.7(3) . . ? N2 Mn2 O32 156.7(3) . . ? N1 Mn2 O32 131.3(3) . . ? N12 Mn2 O32 108.3(3) . . ? N2 O1 Mn1 115.4(3) . . ? C1 N1 C5 117.2(5) . . ? C1 N1 Mn2 124.6(5) . . ? C5 N1 Mn2 117.8(4) . . ? C6 N2 O1 116.0(4) . . ? C6 N2 Mn2 122.1(4) . . ? O1 N2 Mn2 121.9(3) . . ? C26 O11 Mn1 107.5(3) . . ? C26 O11 Mn2 119.6(3) . . ? Mn1 O11 Mn2 112.43(16) . . ? C26 O12 Mn1 115.7(3) . 3_665 ? C25 N11 C21 119.6(5) . . ? C25 N11 Mn1 113.4(3) . 3_665 ? C21 N11 Mn1 127.0(4) . 3_665 ? C27 N12 C31 117.6(5) . . ? C27 N12 Mn2 113.2(3) . . ? C31 N12 Mn2 126.2(4) . . ? C41 O21 Mn1 134.8(4) . . ? C41 O22 Mn2 132.4(4) . . ? N51 O31 Mn2 108.8(8) . . ? N51 O32 Mn2 86.2(7) . . ? N1 C1 C2 122.7(7) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 118.7(7) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 122.5(5) . . ? N1 C5 C6 116.0(5) . . ? C4 C5 C6 121.4(5) . . ? N2 C6 C7 125.0(5) . . ? N2 C6 C5 114.1(5) . . ? C7 C6 C5 120.9(5) . . ? N3 C7 C8 121.5(7) . . ? N3 C7 C6 117.1(6) . . ? C8 C7 C6 121.4(6) . . ? C9 C8 C7 118.3(10) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C10 C9 C8 118.7(10) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C11 C10 C9 118.8(9) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 N3 125.2(11) . . ? C10 C11 H11 117.4 . . ? N3 C11 H11 117.4 . . ? C7 N3 C11 117.3(9) . . ? N11 C21 C22 121.9(6) . . ? N11 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C23 119.2(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 119.4(5) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 118.5(5) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N11 C25 C24 121.4(5) . . ? N11 C25 C26 113.5(4) . . ? C24 C25 C26 125.0(5) . . ? O12 C26 O11 108.8(4) . . ? O12 C26 C25 110.1(4) . . ? O11 C26 C25 107.1(4) . . ? O12 C26 C27 109.0(4) . . ? O11 C26 C27 110.9(4) . . ? C25 C26 C27 110.9(4) . . ? N12 C27 C28 122.1(5) . . ? N12 C27 C26 116.2(5) . . ? C28 C27 C26 121.7(5) . . ? C27 C28 C29 119.1(5) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 119.1(6) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 118.5(6) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? N12 C31 C30 123.6(6) . . ? N12 C31 H31 118.2 . . ? C30 C31 H31 118.2 . . ? O22 C41 O21 125.0(5) . . ? O22 C41 C42 117.4(5) . . ? O21 C41 C42 117.5(6) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O31 N51 O33 132.1(11) . . ? O31 N51 O32 116.2(9) . . ? O33 N51 O32 111.6(10) . . ? C62 C61 N61 176(5) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.936 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.098 #===END data_pekm487 _database_code_depnum_ccdc_archive 'CCDC 247222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H20 F18 Mn2 N6 O10' _chemical_formula_weight 1148.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.317(4) _cell_length_b 16.989(6) _cell_length_c 11.679(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.56(1) _cell_angle_gamma 90.00 _cell_volume 2238(1) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 11.6 _exptl_crystal_description parallelipiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.69 _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2.9 _diffrn_reflns_number 4142 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3942 _reflns_number_gt 2956 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+2.2617P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3942 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.007 _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 Mn Mn 0.00709(5) 0.07932(3) 0.71075(5) 0.0575(2) Uani 1 1 d . . . N1 N 0.1621(3) 0.07522(18) 0.6015(3) 0.0593(8) Uani 1 1 d . . . N2 N -0.0616(3) 0.09192(17) 0.5209(3) 0.0543(8) Uani 1 1 d . . . N3 N -0.0293(3) 0.05365(19) 0.2485(3) 0.0584(8) Uani 1 1 d . . . O11 O 0.0127(3) 0.20784(17) 0.7013(2) 0.0738(8) Uani 1 1 d . . . O12 O 0.1154(3) 0.10204(17) 0.8653(2) 0.0741(8) Uani 1 1 d . . . O21 O -0.1569(3) 0.0796(2) 0.7818(3) 0.0859(9) Uani 1 1 d . . . C1 C 0.2753(4) 0.0659(3) 0.6437(4) 0.0690(11) Uani 1 1 d . . . C2 C 0.3688(4) 0.0701(3) 0.5774(5) 0.0835(14) Uani 1 1 d . . . C3 C 0.3470(5) 0.0835(3) 0.4626(5) 0.0883(15) Uani 1 1 d . . . C4 C 0.2301(4) 0.0929(3) 0.4165(4) 0.0755(12) Uani 1 1 d . . . C5 C 0.1402(3) 0.0883(2) 0.4878(3) 0.0563(9) Uani 1 1 d . . . C6 C 0.0139(3) 0.0969(2) 0.4458(3) 0.0543(9) Uani 1 1 d . . . O1 O -0.1769(3) 0.10220(18) 0.4766(3) 0.0642(7) Uani 1 1 d . . . C7 C -0.0193(3) 0.1146(2) 0.3228(3) 0.0581(9) Uani 1 1 d . . . C8 C -0.0370(5) 0.1911(3) 0.2889(4) 0.0826(14) Uani 1 1 d . . . C9 C -0.0654(6) 0.2073(3) 0.1740(5) 0.0950(17) Uani 1 1 d . . . C10 C -0.0751(5) 0.1460(3) 0.0981(4) 0.0836(14) Uani 1 1 d . . . C11 C -0.0583(4) 0.0717(3) 0.1377(4) 0.0724(12) Uani 1 1 d . . . C21 C 0.0688(5) 0.3396(3) 0.7169(5) 0.0900(16) Uani 1 1 d . . . F1 F -0.0428(4) 0.3663(2) 0.7182(3) 0.1260(13) Uani 1 1 d . . . F2 F 0.0835(4) 0.3441(3) 0.6093(4) 0.1537(17) Uani 1 1 d . . . F3 F 0.1318(5) 0.3876(2) 0.7767(5) 0.219(3) Uani 1 1 d . . . C22 C 0.0749(3) 0.2546(2) 0.7601(3) 0.0624(10) Uani 1 1 d . . . C23 C 0.1486(4) 0.2385(3) 0.8587(4) 0.0737(12) Uani 1 1 d . . . C24 C 0.1629(4) 0.1639(3) 0.9017(3) 0.0649(10) Uani 1 1 d . . . C25 C 0.2528(5) 0.1529(3) 1.0060(4) 0.0878(15) Uani 1 1 d . . . F4 F 0.2159(3) 0.1053(3) 1.0808(3) 0.1259(13) Uani 1 1 d . . . F5 F 0.2844(6) 0.2151(2) 1.0569(4) 0.221(3) Uani 1 1 d . . . F6 F 0.3468(3) 0.1200(4) 0.9751(4) 0.186(2) Uani 1 1 d . . . C31 C -0.2624(4) 0.0909(3) 0.7469(4) 0.0731(12) Uani 1 1 d . . . O22 O -0.3081(3) 0.0967(2) 0.6495(3) 0.0964(11) Uani 1 1 d . . . C32 C -0.3455(5) 0.1015(5) 0.8431(5) 0.107(2) Uani 1 1 d . . . F7 F -0.3225(18) 0.0567(10) 0.9309(14) 0.137(6) Uani 0.598(19) 1 d P . . F8 F -0.4521(8) 0.1105(11) 0.8119(10) 0.123(7) Uani 0.598(19) 1 d P . . F9 F -0.3168(11) 0.1806(7) 0.8887(9) 0.124(4) Uani 0.598(19) 1 d P . . F7A F -0.4334(16) 0.0327(18) 0.8202(10) 0.159(9) Uani 0.402(19) 1 d P . . F8A F -0.403(3) 0.1514(17) 0.846(3) 0.208(18) Uani 0.402(19) 1 d P . . F9A F -0.305(2) 0.0766(16) 0.9387(15) 0.120(9) Uani 0.402(19) 1 d P . . HO1 H -0.214(4) 0.096(3) 0.531(4) 0.066(15) Uiso 1 1 d . . . H1 H 0.282(4) 0.054(3) 0.729(4) 0.080(13) Uiso 1 1 d . . . H2 H 0.449(5) 0.063(3) 0.612(4) 0.086(14) Uiso 1 1 d . . . H3 H 0.406(5) 0.086(3) 0.417(5) 0.098(18) Uiso 1 1 d . . . H4 H 0.213(4) 0.104(3) 0.341(4) 0.080(14) Uiso 1 1 d . . . H8 H -0.034(4) 0.228(3) 0.342(4) 0.085(15) Uiso 1 1 d . . . H9 H -0.071(5) 0.265(4) 0.150(5) 0.13(2) Uiso 1 1 d . . . H10 H -0.090(4) 0.154(2) 0.017(4) 0.071(12) Uiso 1 1 d . . . H11 H -0.063(4) 0.027(3) 0.086(4) 0.084(14) Uiso 1 1 d . . . H23 H 0.186(5) 0.277(3) 0.893(4) 0.098(17) Uiso 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 Mn 0.0568(4) 0.0626(4) 0.0498(3) -0.0075(3) -0.0163(2) 0.0024(3) N1 0.0549(17) 0.0597(18) 0.0599(18) -0.0045(15) -0.0160(14) 0.0015(14) N2 0.0519(17) 0.0561(18) 0.0517(17) -0.0052(14) -0.0159(14) 0.0017(14) N3 0.0618(18) 0.0622(19) 0.0489(16) 0.0010(14) -0.0084(14) 0.0010(15) O11 0.086(2) 0.0638(17) 0.0661(17) -0.0101(14) -0.0291(15) 0.0055(15) O12 0.085(2) 0.0682(18) 0.0638(17) -0.0025(14) -0.0292(15) -0.0057(15) O21 0.0660(19) 0.106(3) 0.084(2) 0.0023(18) -0.0019(16) 0.0135(17) C1 0.061(2) 0.074(3) 0.069(3) -0.006(2) -0.017(2) 0.007(2) C2 0.055(3) 0.099(4) 0.094(4) -0.016(3) -0.015(2) 0.004(2) C3 0.064(3) 0.112(4) 0.089(4) -0.005(3) 0.007(3) -0.004(3) C4 0.071(3) 0.086(3) 0.067(3) -0.001(2) -0.006(2) -0.003(2) C5 0.056(2) 0.054(2) 0.057(2) -0.0051(17) -0.0080(17) -0.0047(16) C6 0.061(2) 0.046(2) 0.053(2) -0.0054(15) -0.0117(18) -0.0016(16) O1 0.0536(15) 0.0797(19) 0.0557(17) -0.0018(14) -0.0176(14) 0.0065(13) C7 0.059(2) 0.059(2) 0.054(2) 0.0036(18) -0.0092(17) -0.0014(17) C8 0.114(4) 0.062(3) 0.069(3) 0.004(2) -0.008(3) 0.003(3) C9 0.130(5) 0.069(3) 0.081(3) 0.018(3) -0.020(3) 0.007(3) C10 0.097(4) 0.092(4) 0.058(3) 0.016(3) -0.014(2) -0.003(3) C11 0.085(3) 0.077(3) 0.053(2) 0.001(2) -0.009(2) 0.000(2) C21 0.102(4) 0.079(3) 0.082(3) 0.007(3) -0.035(3) -0.008(3) F1 0.140(3) 0.099(2) 0.131(3) -0.008(2) -0.036(2) 0.036(2) F2 0.192(4) 0.149(4) 0.123(3) 0.054(3) 0.029(3) -0.010(3) F3 0.254(6) 0.083(2) 0.283(6) 0.051(3) -0.202(5) -0.062(3) C22 0.059(2) 0.067(2) 0.059(2) -0.0068(19) -0.0099(18) -0.0016(19) C23 0.078(3) 0.072(3) 0.065(3) -0.005(2) -0.026(2) -0.015(2) C24 0.066(2) 0.074(3) 0.051(2) -0.0037(19) -0.0196(18) -0.005(2) C25 0.086(3) 0.100(4) 0.070(3) 0.010(3) -0.037(3) -0.019(3) F4 0.118(3) 0.173(3) 0.080(2) 0.040(2) -0.0376(18) -0.019(2) F5 0.337(7) 0.102(3) 0.187(4) 0.006(3) -0.205(5) -0.033(3) F6 0.078(2) 0.366(8) 0.106(3) 0.022(4) -0.031(2) 0.038(4) C31 0.065(3) 0.078(3) 0.076(3) -0.007(2) 0.000(2) 0.010(2) O22 0.073(2) 0.142(3) 0.074(2) -0.012(2) -0.0016(17) 0.007(2) C32 0.078(4) 0.160(7) 0.082(4) 0.001(4) 0.000(3) 0.039(4) F7 0.168(14) 0.118(7) 0.132(12) 0.051(7) 0.055(9) 0.045(7) F8 0.066(4) 0.20(2) 0.106(5) -0.026(8) 0.015(3) 0.003(6) F9 0.133(8) 0.126(6) 0.114(5) -0.041(4) 0.012(5) 0.030(6) F7A 0.137(10) 0.22(2) 0.127(9) -0.006(9) 0.028(7) -0.096(13) F8A 0.23(3) 0.16(2) 0.26(4) 0.07(2) 0.15(3) 0.13(2) F9A 0.091(8) 0.21(2) 0.061(8) -0.034(11) 0.002(6) 0.012(11) _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 Mn O21 2.092(3) . ? Mn O12 2.135(3) . ? Mn O11 2.187(3) . ? Mn N1 2.251(4) . ? Mn N2 2.301(3) . ? Mn N3 2.318(3) 3_556 ? N1 C1 1.344(5) . ? N1 C5 1.350(5) . ? N2 C6 1.275(5) . ? N2 O1 1.376(4) . ? N3 C11 1.345(5) . ? N3 C7 1.350(5) . ? N3 Mn 2.318(3) 3_556 ? O11 C22 1.233(4) . ? O12 C24 1.240(5) . ? O21 C31 1.246(5) . ? C1 C2 1.362(7) . ? C1 H1 1.01(5) . ? C2 C3 1.363(8) . ? C2 H2 0.97(5) . ? C3 C4 1.397(7) . ? C3 H3 0.89(6) . ? C4 C5 1.367(6) . ? C4 H4 0.90(5) . ? C5 C6 1.481(5) . ? C6 C7 1.487(5) . ? O1 HO1 0.80(4) . ? C7 C8 1.369(6) . ? C8 C9 1.382(7) . ? C8 H8 0.88(5) . ? C9 C10 1.367(7) . ? C9 H9 1.02(6) . ? C10 C11 1.353(7) . ? C10 H10 0.96(4) . ? C11 H11 0.97(5) . ? C21 F3 1.259(6) . ? C21 F2 1.282(6) . ? C21 F1 1.344(7) . ? C21 C22 1.529(6) . ? C22 C23 1.394(5) . ? C23 C24 1.368(6) . ? C23 H23 0.86(5) . ? C24 C25 1.535(5) . ? C25 F5 1.252(6) . ? C25 F6 1.278(7) . ? C25 F4 1.284(6) . ? C31 O22 1.215(6) . ? C31 C32 1.532(8) . ? C32 F8A 1.073(14) . ? C32 F8 1.241(11) . ? C32 F9A 1.25(2) . ? C32 F7 1.287(15) . ? C32 F9 1.472(14) . ? C32 F7A 1.543(18) . ? F7 F7A 1.78(2) . ? F8 F8A 0.95(4) . ? F8 F7A 1.34(2) . ? F9 F8A 1.17(4) . ? 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 O21 Mn O12 97.60(14) . . ? O21 Mn O11 92.75(13) . . ? O12 Mn O11 81.08(10) . . ? O21 Mn N1 168.74(12) . . ? O12 Mn N1 93.65(12) . . ? O11 Mn N1 88.58(12) . . ? O21 Mn N2 98.03(13) . . ? O12 Mn N2 157.71(12) . . ? O11 Mn N2 82.40(10) . . ? N1 Mn N2 71.06(11) . . ? O21 Mn N3 90.32(13) . 3_556 ? O12 Mn N3 87.53(11) . 3_556 ? O11 Mn N3 168.50(10) . 3_556 ? N1 Mn N3 90.57(12) . 3_556 ? N2 Mn N3 108.15(11) . 3_556 ? C1 N1 C5 118.4(4) . . ? C1 N1 Mn 124.0(3) . . ? C5 N1 Mn 117.5(2) . . ? C6 N2 O1 113.6(3) . . ? C6 N2 Mn 118.4(2) . . ? O1 N2 Mn 127.7(3) . . ? C11 N3 C7 116.5(4) . . ? C11 N3 Mn 115.7(3) . 3_556 ? C7 N3 Mn 127.8(3) . 3_556 ? C22 O11 Mn 129.2(3) . . ? C24 O12 Mn 130.3(3) . . ? C31 O21 Mn 136.7(3) . . ? N1 C1 C2 123.1(4) . . ? N1 C1 H1 112(3) . . ? C2 C1 H1 125(3) . . ? C1 C2 C3 118.7(5) . . ? C1 C2 H2 120(3) . . ? C3 C2 H2 122(3) . . ? C2 C3 C4 119.3(5) . . ? C2 C3 H3 120(4) . . ? C4 C3 H3 120(4) . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4 119(3) . . ? C3 C4 H4 122(3) . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C6 116.0(4) . . ? C4 C5 C6 122.6(4) . . ? N2 C6 C5 116.6(3) . . ? N2 C6 C7 123.1(3) . . ? C5 C6 C7 120.2(4) . . ? N2 O1 HO1 103(3) . . ? N3 C7 C8 122.6(4) . . ? N3 C7 C6 117.9(3) . . ? C8 C7 C6 119.4(4) . . ? C7 C8 C9 119.2(5) . . ? C7 C8 H8 119(3) . . ? C9 C8 H8 122(3) . . ? C10 C9 C8 118.5(5) . . ? C10 C9 H9 124(3) . . ? C8 C9 H9 117(3) . . ? C11 C10 C9 119.2(4) . . ? C11 C10 H10 119(3) . . ? C9 C10 H10 122(3) . . ? N3 C11 C10 123.9(4) . . ? N3 C11 H11 114(3) . . ? C10 C11 H11 122(3) . . ? F3 C21 F2 113.2(6) . . ? F3 C21 F1 105.4(6) . . ? F2 C21 F1 100.8(4) . . ? F3 C21 C22 114.9(4) . . ? F2 C21 C22 111.9(5) . . ? F1 C21 C22 109.5(5) . . ? O11 C22 C23 127.6(4) . . ? O11 C22 C21 114.6(3) . . ? C23 C22 C21 117.8(4) . . ? C24 C23 C22 122.1(4) . . ? C24 C23 H23 120(3) . . ? C22 C23 H23 118(3) . . ? O12 C24 C23 128.6(3) . . ? O12 C24 C25 114.2(4) . . ? C23 C24 C25 117.1(4) . . ? F5 C25 F6 106.9(6) . . ? F5 C25 F4 107.7(5) . . ? F6 C25 F4 103.9(5) . . ? F5 C25 C24 114.8(5) . . ? F6 C25 C24 110.1(5) . . ? F4 C25 C24 112.7(4) . . ? O22 C31 O21 130.1(5) . . ? O22 C31 C32 115.9(4) . . ? O21 C31 C32 114.0(5) . . ? F8A C32 F8 48(2) . . ? F8A C32 F9A 115(2) . . ? F8 C32 F9A 125.7(14) . . ? F8A C32 F7 121.9(16) . . ? F8 C32 F7 115.9(13) . . ? F9A C32 F7 18.0(17) . . ? F8A C32 F9 52(3) . . ? F8 C32 F9 100.1(9) . . ? F9A C32 F9 86.0(14) . . ? F7 C32 F9 103.1(10) . . ? F8A C32 C31 121.7(12) . . ? F8 C32 C31 116.0(7) . . ? F9A C32 C31 114.5(12) . . ? F7 C32 C31 114.8(10) . . ? F9 C32 C31 104.0(7) . . ? F8A C32 F7A 102.5(19) . . ? F8 C32 F7A 56.3(9) . . ? F9A C32 F7A 94.8(13) . . ? F7 C32 F7A 77.1(12) . . ? F9 C32 F7A 150.9(10) . . ? C31 C32 F7A 102.1(9) . . ? C32 F7 F7A 57.9(10) . . ? F8A F8 C32 56.7(11) . . ? F8A F8 F7A 127.3(19) . . ? C32 F8 F7A 73.3(9) . . ? F8A F9 C32 46.2(8) . . ? F8 F7A C32 50.4(7) . . ? F8 F7A F7 85.7(11) . . ? C32 F7A F7 44.9(7) . . ? F8 F8A C32 75(2) . . ? F8 F8A F9 157(2) . . ? C32 F8A F9 82(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.565 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.056 #===END