Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_1 _database_code_CSD 166256 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Blay, Gonzalo' 'Fernandez, Isabel' 'Gimenez, Tomas' 'Lloret, F.' 'Munoz, M. C.' 'Pardo, Emilio' 'Pedro, Jose R.' 'Ruiz, Rafael' _publ_contact_author_name 'Prof Jose R Pedro' _publ_contact_author_address ; Prof Jose R Pedro Departament de Quimica Organic Universitat de Valencia Facultat de Quimica Burjassot Valencia 46100 ; _publ_contact_author_email 'JOSE.R.PEDRO@UV.ES' _publ_section_title 'Alkane oxidation by a carboxylate-bridged dimanganese(III) complex' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H31.50 Mn N2.50 O9 P' _chemical_formula_weight 717.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.099(3) _cell_length_b 15.446(3) _cell_length_c 17.687(4) _cell_angle_alpha 73.04(3) _cell_angle_beta 79.94(3) _cell_angle_gamma 80.84(3) _cell_volume 3348.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 18 _exptl_crystal_description prismatic _exptl_crystal_colour red-brick _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf CAD-4' _diffrn_measurement_method '? - 2?' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11665 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.97 _reflns_number_total 11665 _reflns_number_gt 7556 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ZORTEP _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^)+(0.1969P)^2^+15.0032P] 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 0.0016(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11665 _refine_ls_number_parameters 875 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1440 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.3134 _refine_ls_wR_factor_gt 0.2511 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn2 Mn 0.43342(9) 0.11978(8) 0.31773(6) 0.0505(3) Uani 1 1 d . . . O12 O 0.3962(6) 0.0692(6) 0.4366(4) 0.095(3) Uani 1 1 d . . . N3 N 0.4551(5) 0.1315(6) 0.2073(4) 0.0627(19) Uani 1 1 d . . . C11 C 0.4776(7) 0.2205(10) 0.1622(6) 0.103(5) Uani 1 1 d . . . O7 O 0.4947(8) 0.2443(8) 0.0898(5) 0.147(4) Uani 1 1 d . . . C12 C 0.4749(8) 0.2758(8) 0.2195(8) 0.082(3) Uani 1 1 d . . . N4 N 0.4039(5) 0.0001(5) 0.3232(5) 0.071(2) Uani 1 1 d . . . C13 C 0.3792(8) -0.0597(8) 0.3891(7) 0.080(3) Uani 1 1 d . . . C14 C 0.3739(7) -0.0189(6) 0.4489(7) 0.074(3) Uani 1 1 d . . . O10 O 0.3617(7) -0.1392(6) 0.4016(6) 0.132(4) Uani 1 1 d . . . O15 O 0.6036(5) 0.0707(5) 0.3324(4) 0.0795(19) Uani 1 1 d . . . O9 O 0.4606(6) 0.2440(5) 0.2894(6) 0.088(2) Uani 1 1 d . . . O2 O 0.2614(4) 0.1850(3) 0.3144(4) 0.0637(15) Uani 1 1 d . . . C20 C 0.4125(7) -0.0133(7) 0.2417(8) 0.076(3) Uani 1 1 d . . . C15 C 0.4388(7) 0.0601(8) 0.1820(6) 0.071(3) Uani 1 1 d . . . C19 C 0.3908(8) -0.0991(11) 0.2294(10) 0.123(5) Uani 1 1 d . . . C16 C 0.4429(9) 0.0600(12) 0.1024(8) 0.115(5) Uani 1 1 d . . . C18 C 0.3987(8) -0.0970(10) 0.1503(8) 0.089(3) Uani 1 1 d . . . C17 C 0.4218(11) -0.0190(14) 0.0871(9) 0.128(6) Uani 1 1 d . . . O8 O 0.4854(6) 0.3618(5) 0.1832(8) 0.153(5) Uani 1 1 d . . . O11 O 0.3477(8) -0.0589(7) 0.5251(5) 0.123(3) Uani 1 1 d . . . Mn1 Mn 0.15216(8) 0.41883(6) 0.17346(5) 0.0390(3) Uani 1 1 d . . . O3 O 0.2319(4) 0.2979(3) 0.2056(3) 0.0452(11) Uani 1 1 d . . . C2 C 0.2229(5) 0.2609(5) 0.2808(4) 0.0465(16) Uani 1 1 d . . . C1 C 0.1534(5) 0.3191(5) 0.3335(4) 0.0443(16) Uani 1 1 d . . . O1 O 0.1373(5) 0.2905(4) 0.4049(3) 0.0741(18) Uani 1 1 d . . . N1 N 0.1196(4) 0.4009(4) 0.2867(3) 0.0364(12) Uani 1 1 d . . . O6 O 0.1530(4) 0.4630(4) 0.0591(3) 0.0530(13) Uani 1 1 d . . . C4 C 0.0967(6) 0.5391(5) 0.0354(4) 0.0489(17) Uani 1 1 d . . . O5 O 0.0877(5) 0.5795(4) -0.0342(3) 0.0717(17) Uani 1 1 d . . . O4 O -0.0200(5) 0.6522(4) 0.0877(3) 0.0647(15) Uani 1 1 d . . . C3 C 0.0398(5) 0.5825(5) 0.1013(4) 0.0434(16) Uani 1 1 d . . . N2 N 0.0654(4) 0.5312(4) 0.1723(3) 0.0391(12) Uani 1 1 d . . . O14 O 0.3117(4) 0.4767(3) 0.1469(3) 0.0564(13) Uani 1 1 d . . . O13 O 0.0023(5) 0.3553(4) 0.1760(3) 0.0633(15) Uani 1 1 d . . . C10 C 0.0189(5) 0.5421(4) 0.2478(4) 0.0393(14) Uani 1 1 d . . . C9 C -0.0511(6) 0.6161(5) 0.2625(4) 0.0469(16) Uani 1 1 d . . . C5 C 0.0478(5) 0.4693(5) 0.3122(4) 0.0396(14) Uani 1 1 d . . . C6 C 0.0079(5) 0.4683(5) 0.3896(4) 0.0460(16) Uani 1 1 d . . . C8 C -0.0897(6) 0.6141(5) 0.3422(5) 0.0522(18) Uani 1 1 d . . . C7 C -0.0597(6) 0.5411(6) 0.4042(5) 0.058(2) Uani 1 1 d . . . P1 P 0.02767(13) -0.07764(11) 0.18307(10) 0.0359(4) Uani 1 1 d . . . C21 C 0.0558(5) 0.0384(4) 0.1457(4) 0.0378(14) Uani 1 1 d . . . C22 C -0.0164(6) 0.1059(5) 0.1067(4) 0.0487(17) Uani 1 1 d . . . C23 C 0.0103(7) 0.1927(5) 0.0734(5) 0.0564(19) Uani 1 1 d . . . C24 C 0.1060(7) 0.2149(5) 0.0798(5) 0.058(2) Uani 1 1 d . . . C25 C 0.1764(7) 0.1496(6) 0.1202(6) 0.066(2) Uani 1 1 d . . . C26 C 0.1507(7) 0.0608(5) 0.1522(6) 0.061(2) Uani 1 1 d . . . C27 C 0.0311(5) -0.1218(5) 0.2882(4) 0.0427(15) Uani 1 1 d . . . C28 C -0.0507(8) -0.1636(7) 0.3361(5) 0.069(2) Uani 1 1 d . . . C29 C -0.0465(9) -0.2014(8) 0.4172(5) 0.086(3) Uani 1 1 d . . . C31 C 0.1202(7) -0.1548(7) 0.4035(5) 0.070(2) Uani 1 1 d . . . C30 C 0.0380(7) -0.1953(6) 0.4501(5) 0.067(2) Uani 1 1 d . . . C32 C 0.1156(6) -0.1178(7) 0.3220(5) 0.068(2) Uani 1 1 d . . . C33 C 0.1258(5) -0.1438(4) 0.1331(4) 0.0405(15) Uani 1 1 d . . . C34 C 0.1686(6) -0.1050(5) 0.0550(4) 0.0515(18) Uani 1 1 d . . . C35 C 0.2420(7) -0.1566(7) 0.0135(5) 0.066(2) Uani 1 1 d . . . C36 C 0.2699(7) -0.2472(6) 0.0509(6) 0.065(2) Uani 1 1 d . . . C37 C 0.2272(7) -0.2866(6) 0.1276(6) 0.065(2) Uani 1 1 d . . . C38 C 0.1539(6) -0.2347(5) 0.1704(5) 0.0526(18) Uani 1 1 d . . . C39 C -0.0986(5) -0.0870(4) 0.1619(4) 0.0369(14) Uani 1 1 d . . . C40 C -0.1866(6) -0.0369(5) 0.1930(5) 0.0502(17) Uani 1 1 d . . . C41 C -0.2839(6) -0.0441(6) 0.1765(6) 0.063(2) Uani 1 1 d . . . C42 C -0.2968(7) -0.1023(6) 0.1336(6) 0.065(2) Uani 1 1 d . . . C43 C -0.2085(7) -0.1524(6) 0.1040(5) 0.063(2) Uani 1 1 d . . . C44 C -0.1103(6) -0.1449(5) 0.1177(4) 0.0457(16) Uani 1 1 d . . . P2 P 0.58442(13) 0.57137(12) 0.32341(10) 0.0381(4) Uani 1 1 d . . . C45 C 0.6161(5) 0.6092(5) 0.2165(4) 0.0400(14) Uani 1 1 d . . . C46 C 0.7116(6) 0.5829(6) 0.1791(4) 0.0540(18) Uani 1 1 d . . . C47 C 0.7331(7) 0.6095(7) 0.0965(5) 0.067(2) Uani 1 1 d . . . C48 C 0.6578(7) 0.6636(6) 0.0518(4) 0.061(2) Uani 1 1 d . . . C49 C 0.5643(7) 0.6924(8) 0.0886(5) 0.078(3) Uani 1 1 d . . . C50 C 0.5424(7) 0.6668(7) 0.1719(5) 0.073(3) Uani 1 1 d . . . C51 C 0.6408(5) 0.4551(5) 0.3596(4) 0.0419(15) Uani 1 1 d . . . C52 C 0.7489(6) 0.4358(5) 0.3573(4) 0.0527(18) Uani 1 1 d . . . C53 C 0.7934(7) 0.3461(6) 0.3794(5) 0.060(2) Uani 1 1 d . . . C54 C 0.7318(7) 0.2760(5) 0.4075(5) 0.062(2) Uani 1 1 d . . . C55 C 0.6225(8) 0.2957(6) 0.4122(5) 0.067(2) Uani 1 1 d . . . C56 C 0.5783(7) 0.3843(5) 0.3873(5) 0.0557(19) Uani 1 1 d . . . C57 C 0.6293(5) 0.6433(5) 0.3709(4) 0.0445(16) Uani 1 1 d . . . C58 C 0.6238(7) 0.7368(6) 0.3349(5) 0.059(2) Uani 1 1 d . . . C59 C 0.6451(7) 0.7950(6) 0.3765(6) 0.067(2) Uani 1 1 d . . . C60 C 0.6705(8) 0.7595(7) 0.4529(6) 0.073(3) Uani 1 1 d . . . C61 C 0.6780(7) 0.6670(7) 0.4880(5) 0.066(2) Uani 1 1 d . . . C62 C 0.6560(6) 0.6066(6) 0.4479(4) 0.0533(18) Uani 1 1 d . . . C63 C 0.4454(5) 0.5796(5) 0.3460(4) 0.0402(15) Uani 1 1 d . . . C64 C 0.3898(6) 0.5364(6) 0.3100(5) 0.0564(19) Uani 1 1 d . . . C65 C 0.2824(7) 0.5422(7) 0.3237(6) 0.066(2) Uani 1 1 d . . . C67 C 0.2848(7) 0.6355(7) 0.4125(5) 0.069(2) Uani 1 1 d . . . C66 C 0.2287(7) 0.5919(7) 0.3751(6) 0.071(2) Uani 1 1 d . . . C68 C 0.3923(6) 0.6291(6) 0.3963(5) 0.0539(18) Uani 1 1 d . . . C69 C 0.7320(9) 0.2514(11) 0.1892(8) 0.101(4) Uani 1 1 d . . . N5 N 0.7333(11) 0.1791(8) 0.2040(11) 0.167(7) Uani 1 1 d . . . C70 C 0.7288(11) 0.3587(10) 0.1715(10) 0.123(5) Uani 1 1 d . . . O16 O 0.4100(9) 0.5693(6) -0.0079(6) 0.139(4) Uani 1 1 d . . . O17 O 0.0177(19) 0.138(2) 0.343(2) 0.60(4) Uani 1 1 d . . . O18 O 0.1038(13) -0.0431(17) 0.5937(18) 0.381(19) 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 Mn2 0.0623(7) 0.0471(6) 0.0385(6) -0.0057(5) -0.0148(5) 0.0017(5) O12 0.080(5) 0.145(7) 0.070(4) -0.055(5) -0.036(4) 0.040(5) N3 0.050(4) 0.104(6) 0.030(3) -0.012(3) -0.006(3) -0.005(4) C11 0.043(5) 0.165(12) 0.045(5) 0.054(7) -0.010(4) -0.001(6) O7 0.118(7) 0.214(11) 0.057(5) 0.049(6) -0.014(4) -0.028(7) C12 0.050(5) 0.095(8) 0.095(8) -0.006(7) -0.022(5) -0.011(5) N4 0.045(4) 0.055(4) 0.088(5) 0.016(4) -0.003(4) -0.003(3) C13 0.071(6) 0.077(7) 0.084(7) 0.008(6) -0.026(5) -0.023(5) C14 0.058(5) 0.039(4) 0.103(8) 0.017(5) -0.008(5) -0.016(4) O10 0.114(7) 0.090(6) 0.167(9) 0.035(6) -0.042(6) -0.049(5) O15 0.058(4) 0.109(5) 0.065(4) -0.017(4) -0.022(3) 0.007(3) O9 0.083(5) 0.062(4) 0.119(7) -0.016(4) -0.027(5) -0.008(3) O2 0.055(3) 0.041(3) 0.074(4) 0.012(3) -0.012(3) 0.006(2) C20 0.047(5) 0.080(6) 0.129(9) -0.074(7) -0.036(5) 0.021(4) C15 0.044(5) 0.101(8) 0.070(6) -0.033(6) -0.010(4) 0.010(5) C19 0.048(6) 0.171(14) 0.170(14) -0.084(12) -0.038(7) 0.030(7) C16 0.072(7) 0.202(15) 0.103(9) -0.102(10) -0.024(6) 0.020(8) C18 0.062(6) 0.134(10) 0.084(8) -0.059(8) -0.024(6) 0.026(6) C17 0.092(9) 0.222(19) 0.096(10) -0.099(12) -0.028(8) 0.028(10) O8 0.071(5) 0.063(5) 0.269(13) 0.053(6) -0.035(6) -0.018(4) O11 0.135(8) 0.148(8) 0.075(5) 0.019(5) -0.026(5) -0.062(6) Mn1 0.0507(6) 0.0359(5) 0.0265(5) -0.0060(4) -0.0088(4) 0.0055(4) O3 0.050(3) 0.040(2) 0.040(3) -0.007(2) -0.006(2) 0.006(2) C2 0.037(4) 0.044(4) 0.053(4) -0.003(3) -0.005(3) -0.006(3) C1 0.046(4) 0.050(4) 0.032(3) -0.002(3) -0.008(3) -0.004(3) O1 0.089(4) 0.078(4) 0.034(3) 0.010(3) -0.006(3) 0.002(3) N1 0.041(3) 0.040(3) 0.027(3) -0.006(2) -0.009(2) -0.003(2) O6 0.064(3) 0.058(3) 0.029(2) -0.007(2) -0.009(2) 0.007(3) C4 0.044(4) 0.062(5) 0.032(3) 0.004(3) -0.010(3) -0.007(3) O5 0.091(4) 0.081(4) 0.030(3) 0.006(3) -0.016(3) -0.001(3) O4 0.072(4) 0.049(3) 0.056(3) 0.002(2) -0.014(3) 0.018(3) C3 0.039(4) 0.043(4) 0.038(4) 0.004(3) -0.010(3) 0.000(3) N2 0.041(3) 0.035(3) 0.037(3) -0.006(2) -0.004(2) 0.001(2) O14 0.055(3) 0.052(3) 0.052(3) -0.005(2) 0.002(2) -0.006(2) O13 0.073(4) 0.068(4) 0.053(3) -0.013(3) -0.024(3) -0.008(3) C10 0.042(4) 0.038(3) 0.038(3) -0.011(3) 0.000(3) -0.010(3) C9 0.044(4) 0.040(4) 0.056(4) -0.014(3) 0.001(3) -0.011(3) C5 0.037(3) 0.046(4) 0.038(3) -0.014(3) -0.003(3) -0.007(3) C6 0.039(4) 0.071(5) 0.034(3) -0.021(3) -0.003(3) -0.014(3) C8 0.040(4) 0.062(5) 0.061(5) -0.031(4) 0.006(3) -0.014(3) C7 0.053(5) 0.077(6) 0.053(5) -0.030(4) 0.005(4) -0.021(4) P1 0.0367(9) 0.0313(8) 0.0369(8) -0.0063(6) -0.0046(7) -0.0014(6) C21 0.037(3) 0.035(3) 0.036(3) -0.006(3) -0.002(3) -0.002(3) C22 0.053(4) 0.041(4) 0.044(4) -0.003(3) -0.005(3) -0.001(3) C23 0.062(5) 0.039(4) 0.057(5) 0.001(3) -0.001(4) -0.008(3) C24 0.078(6) 0.035(4) 0.056(5) -0.010(3) 0.005(4) -0.011(4) C25 0.064(5) 0.053(5) 0.084(6) -0.019(4) -0.011(5) -0.012(4) C26 0.061(5) 0.041(4) 0.083(6) -0.016(4) -0.020(4) -0.005(3) C27 0.044(4) 0.040(3) 0.040(4) -0.005(3) -0.008(3) -0.001(3) C28 0.083(6) 0.079(6) 0.042(4) 0.005(4) -0.013(4) -0.040(5) C29 0.091(7) 0.110(8) 0.048(5) 0.012(5) -0.012(5) -0.051(6) C31 0.060(5) 0.094(7) 0.046(4) -0.002(4) -0.013(4) -0.009(5) C30 0.075(6) 0.077(6) 0.043(4) -0.007(4) -0.014(4) -0.005(5) C32 0.050(5) 0.105(7) 0.047(4) -0.007(4) -0.011(4) -0.021(5) C33 0.037(3) 0.037(3) 0.046(4) -0.011(3) -0.010(3) 0.003(3) C34 0.052(4) 0.057(4) 0.041(4) -0.013(3) 0.001(3) -0.001(3) C35 0.056(5) 0.089(6) 0.055(5) -0.032(5) -0.003(4) 0.003(4) C36 0.055(5) 0.070(6) 0.079(6) -0.042(5) -0.010(4) 0.010(4) C37 0.058(5) 0.049(4) 0.090(7) -0.028(4) -0.016(5) 0.008(4) C38 0.045(4) 0.041(4) 0.066(5) -0.013(3) -0.001(3) 0.001(3) C39 0.037(3) 0.032(3) 0.036(3) -0.002(3) -0.003(3) -0.003(3) C40 0.044(4) 0.041(4) 0.063(5) -0.015(3) -0.003(3) 0.000(3) C41 0.046(4) 0.068(5) 0.073(6) -0.020(4) -0.007(4) -0.004(4) C42 0.049(5) 0.070(5) 0.071(6) -0.005(4) -0.014(4) -0.011(4) C43 0.059(5) 0.069(5) 0.070(5) -0.024(4) -0.016(4) -0.017(4) C44 0.047(4) 0.047(4) 0.044(4) -0.010(3) -0.012(3) -0.005(3) P2 0.0373(9) 0.0439(9) 0.0320(8) -0.0061(7) -0.0049(7) -0.0092(7) C45 0.043(4) 0.044(4) 0.029(3) -0.003(3) -0.005(3) -0.010(3) C46 0.051(4) 0.069(5) 0.038(4) -0.012(3) 0.000(3) -0.006(4) C47 0.062(5) 0.085(6) 0.048(5) -0.017(4) 0.000(4) -0.006(4) C48 0.065(5) 0.077(6) 0.035(4) 0.000(4) -0.004(4) -0.020(4) C49 0.065(6) 0.109(8) 0.037(4) 0.011(4) -0.010(4) -0.001(5) C50 0.054(5) 0.099(7) 0.044(4) 0.003(4) -0.008(4) 0.013(5) C51 0.051(4) 0.046(4) 0.025(3) -0.004(3) -0.006(3) -0.005(3) C52 0.059(5) 0.056(4) 0.044(4) -0.007(3) -0.019(3) -0.007(4) C53 0.071(5) 0.051(4) 0.061(5) -0.014(4) -0.023(4) 0.000(4) C54 0.078(6) 0.046(4) 0.057(5) -0.001(4) -0.022(4) -0.003(4) C55 0.095(7) 0.047(5) 0.056(5) -0.004(4) -0.003(5) -0.024(4) C56 0.066(5) 0.049(4) 0.047(4) 0.001(3) -0.007(4) -0.018(4) C57 0.035(3) 0.056(4) 0.045(4) -0.012(3) -0.006(3) -0.012(3) C58 0.058(5) 0.055(5) 0.059(5) -0.007(4) -0.006(4) -0.014(4) C59 0.074(6) 0.060(5) 0.075(6) -0.029(4) 0.000(5) -0.022(4) C60 0.075(6) 0.082(7) 0.071(6) -0.035(5) 0.015(5) -0.036(5) C61 0.064(5) 0.100(7) 0.046(4) -0.027(5) -0.001(4) -0.037(5) C62 0.050(4) 0.072(5) 0.040(4) -0.015(4) -0.001(3) -0.021(4) C63 0.038(3) 0.052(4) 0.030(3) -0.007(3) -0.006(3) -0.008(3) C64 0.052(4) 0.072(5) 0.050(4) -0.018(4) -0.012(3) -0.015(4) C65 0.048(5) 0.088(6) 0.067(5) -0.020(5) -0.013(4) -0.018(4) C67 0.047(5) 0.096(7) 0.063(5) -0.026(5) 0.001(4) -0.006(4) C66 0.047(5) 0.087(6) 0.070(6) 0.000(5) -0.015(4) -0.016(4) C68 0.050(4) 0.064(5) 0.047(4) -0.013(4) -0.006(3) -0.012(4) C69 0.075(7) 0.116(10) 0.109(9) -0.041(8) 0.013(6) -0.006(7) N5 0.133(11) 0.070(7) 0.271(19) -0.060(9) 0.075(11) -0.023(7) C70 0.100(9) 0.116(11) 0.162(14) -0.064(10) 0.021(9) -0.037(8) O16 0.170(9) 0.089(6) 0.112(7) -0.007(5) 0.033(6) 0.023(6) O17 0.35(3) 0.68(5) 1.03(7) -0.80(6) 0.47(4) -0.37(3) O18 0.156(13) 0.46(3) 0.74(5) -0.52(4) -0.15(2) 0.124(17) _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 Mn2 N3 1.883(6) . ? Mn2 O9 1.911(7) . ? Mn2 N4 1.920(8) . ? Mn2 O12 2.019(7) . ? Mn2 O15 2.272(6) . ? Mn2 O2 2.321(5) . ? Mn2 C12 2.601(12) . ? O12 C14 1.384(12) . ? N3 C15 1.363(13) . ? N3 C11 1.421(14) . ? C11 O7 1.215(12) . ? C11 C12 1.497(18) . ? C12 O9 1.182(13) . ? C12 O8 1.314(13) . ? N4 C13 1.286(12) . ? N4 C20 1.498(13) . ? C13 O10 1.234(13) . ? C13 C14 1.368(16) . ? C14 O11 1.317(12) . ? O2 C2 1.221(8) . ? C20 C15 1.348(15) . ? C20 C19 1.481(18) . ? C15 C16 1.400(14) . ? C19 C18 1.376(18) . ? C16 C17 1.40(2) . ? C18 C17 1.42(2) . ? Mn1 N1 1.919(5) . ? Mn1 N2 1.914(5) . ? Mn1 O6 1.935(5) . ? Mn1 O3 1.968(4) . ? Mn1 O13 2.318(6) . ? Mn1 O14 2.323(5) . ? O3 C2 1.278(8) . ? C2 C1 1.561(10) . ? C1 O1 1.203(8) . ? C1 N1 1.348(8) . ? N1 C5 1.421(8) . ? O6 C4 1.283(9) . ? C4 O5 1.224(8) . ? C4 C3 1.535(11) . ? O4 C3 1.215(8) . ? C3 N2 1.342(8) . ? N2 C10 1.413(8) . ? C10 C5 1.404(9) . ? C10 C9 1.404(10) . ? C9 C8 1.405(10) . ? C5 C6 1.374(9) . ? C6 C7 1.374(11) . ? C8 C7 1.385(12) . ? P1 C33 1.787(7) . ? P1 C27 1.791(7) . ? P1 C21 1.795(6) . ? P1 C39 1.795(7) . ? C21 C26 1.373(10) . ? C21 C22 1.397(9) . ? C22 C23 1.373(10) . ? C23 C24 1.382(12) . ? C24 C25 1.375(12) . ? C25 C26 1.393(11) . ? C27 C32 1.363(11) . ? C27 C28 1.367(11) . ? C28 C29 1.389(12) . ? C29 C30 1.365(13) . ? C31 C30 1.354(13) . ? C31 C32 1.396(11) . ? C33 C38 1.386(10) . ? C33 C34 1.390(10) . ? C34 C35 1.396(11) . ? C35 C36 1.382(13) . ? C36 C37 1.373(13) . ? C37 C38 1.411(11) . ? C39 C44 1.389(10) . ? C39 C40 1.405(9) . ? C40 C41 1.384(11) . ? C41 C42 1.380(13) . ? C42 C43 1.395(13) . ? C43 C44 1.378(11) . ? P2 C63 1.787(7) . ? P2 C57 1.792(7) . ? P2 C51 1.804(7) . ? P2 C45 1.803(6) . ? C45 C46 1.369(10) . ? C45 C50 1.389(10) . ? C46 C47 1.386(11) . ? C47 C48 1.386(12) . ? C48 C49 1.356(13) . ? C49 C50 1.399(11) . ? C51 C56 1.392(10) . ? C51 C52 1.395(10) . ? C52 C53 1.385(11) . ? C53 C54 1.376(12) . ? C54 C55 1.408(13) . ? C55 C56 1.373(12) . ? C57 C58 1.395(11) . ? C57 C62 1.396(10) . ? C58 C59 1.402(12) . ? C59 C60 1.380(14) . ? C60 C61 1.377(14) . ? C61 C62 1.414(11) . ? C63 C68 1.368(10) . ? C63 C64 1.395(10) . ? C64 C65 1.378(11) . ? C65 C66 1.386(14) . ? C67 C68 1.380(11) . ? C67 C66 1.421(13) . ? C69 N5 1.068(16) . ? C69 C70 1.59(2) . ? 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 N3 Mn2 O9 85.8(4) . . ? N3 Mn2 N4 82.6(4) . . ? O9 Mn2 N4 168.1(4) . . ? N3 Mn2 O12 161.8(4) . . ? O9 Mn2 O12 112.2(4) . . ? N4 Mn2 O12 79.3(4) . . ? N3 Mn2 O15 93.8(3) . . ? O9 Mn2 O15 91.0(3) . . ? N4 Mn2 O15 92.4(3) . . ? O12 Mn2 O15 88.7(3) . . ? N3 Mn2 O2 92.3(3) . . ? O9 Mn2 O2 83.0(3) . . ? N4 Mn2 O2 94.8(3) . . ? O12 Mn2 O2 87.6(2) . . ? O15 Mn2 O2 171.2(2) . . ? N3 Mn2 C12 61.0(4) . . ? O9 Mn2 C12 24.9(4) . . ? N4 Mn2 C12 143.4(4) . . ? O12 Mn2 C12 136.9(4) . . ? O15 Mn2 C12 93.5(3) . . ? O2 Mn2 C12 83.8(3) . . ? C14 O12 Mn2 106.5(6) . . ? C15 N3 C11 129.7(9) . . ? C15 N3 Mn2 118.1(6) . . ? C11 N3 Mn2 111.8(7) . . ? O7 C11 N3 123.9(15) . . ? O7 C11 C12 128.3(14) . . ? N3 C11 C12 107.9(7) . . ? O9 C12 O8 125.5(14) . . ? O9 C12 C11 122.0(11) . . ? O8 C12 C11 112.4(12) . . ? O9 C12 Mn2 42.8(6) . . ? O8 C12 Mn2 167.2(11) . . ? C11 C12 Mn2 79.3(6) . . ? C13 N4 C20 125.1(10) . . ? C13 N4 Mn2 123.4(8) . . ? C20 N4 Mn2 111.5(6) . . ? O10 C13 N4 130.4(13) . . ? O10 C13 C14 122.9(11) . . ? N4 C13 C14 106.8(10) . . ? O11 C14 C13 124.1(9) . . ? O11 C14 O12 112.0(11) . . ? C13 C14 O12 123.9(9) . . ? C12 O9 Mn2 112.3(8) . . ? C2 O2 Mn2 132.0(5) . . ? C15 C20 C19 124.1(12) . . ? C15 C20 N4 113.7(8) . . ? C19 C20 N4 122.1(12) . . ? C20 C15 N3 114.0(8) . . ? C20 C15 C16 120.4(12) . . ? N3 C15 C16 125.6(12) . . ? C18 C19 C20 113.5(15) . . ? C17 C16 C15 118.1(15) . . ? C19 C18 C17 122.9(13) . . ? C16 C17 C18 120.9(12) . . ? N1 Mn1 N2 82.0(2) . . ? N1 Mn1 O6 164.2(2) . . ? N2 Mn1 O6 82.8(2) . . ? N1 Mn1 O3 82.7(2) . . ? N2 Mn1 O3 164.7(2) . . ? O6 Mn1 O3 112.5(2) . . ? N1 Mn1 O13 88.9(2) . . ? N2 Mn1 O13 87.6(2) . . ? O6 Mn1 O13 86.4(2) . . ? O3 Mn1 O13 91.8(2) . . ? N1 Mn1 O14 101.7(2) . . ? N2 Mn1 O14 97.2(2) . . ? O6 Mn1 O14 84.3(2) . . ? O3 Mn1 O14 86.2(2) . . ? O13 Mn1 O14 168.9(2) . . ? C2 O3 Mn1 114.7(4) . . ? O2 C2 O3 126.4(7) . . ? O2 C2 C1 118.0(6) . . ? O3 C2 C1 115.6(6) . . ? O1 C1 N1 129.0(7) . . ? O1 C1 C2 121.5(6) . . ? N1 C1 C2 109.6(5) . . ? C1 N1 C5 126.0(5) . . ? C1 N1 Mn1 117.0(4) . . ? C5 N1 Mn1 116.1(4) . . ? C4 O6 Mn1 115.0(4) . . ? O5 C4 O6 125.5(7) . . ? O5 C4 C3 118.9(7) . . ? O6 C4 C3 115.6(6) . . ? O4 C3 N2 127.7(7) . . ? O4 C3 C4 122.6(6) . . ? N2 C3 C4 109.7(6) . . ? C3 N2 C10 126.3(6) . . ? C3 N2 Mn1 116.7(5) . . ? C10 N2 Mn1 115.6(4) . . ? C5 C10 N2 113.9(6) . . ? C5 C10 C9 119.6(6) . . ? N2 C10 C9 126.5(6) . . ? C8 C9 C10 118.0(7) . . ? C6 C5 C10 121.4(6) . . ? C6 C5 N1 126.5(6) . . ? C10 C5 N1 112.1(5) . . ? C7 C6 C5 119.1(7) . . ? C7 C8 C9 120.8(7) . . ? C6 C7 C8 121.1(7) . . ? C33 P1 C27 108.3(3) . . ? C33 P1 C21 107.0(3) . . ? C27 P1 C21 112.7(3) . . ? C33 P1 C39 109.8(3) . . ? C27 P1 C39 108.9(3) . . ? C21 P1 C39 110.1(3) . . ? C26 C21 C22 119.5(6) . . ? C26 C21 P1 120.1(5) . . ? C22 C21 P1 120.4(5) . . ? C23 C22 C21 119.1(7) . . ? C22 C23 C24 121.2(7) . . ? C23 C24 C25 120.1(7) . . ? C26 C25 C24 118.9(8) . . ? C21 C26 C25 121.1(7) . . ? C32 C27 C28 118.6(7) . . ? C32 C27 P1 121.6(6) . . ? C28 C27 P1 119.8(6) . . ? C27 C28 C29 120.1(8) . . ? C30 C29 C28 120.5(8) . . ? C30 C31 C32 118.8(8) . . ? C29 C30 C31 120.2(8) . . ? C27 C32 C31 121.8(8) . . ? C38 C33 C34 120.6(6) . . ? C38 C33 P1 119.9(5) . . ? C34 C33 P1 119.5(5) . . ? C33 C34 C35 120.5(7) . . ? C36 C35 C34 118.8(8) . . ? C37 C36 C35 121.2(7) . . ? C36 C37 C38 120.4(8) . . ? C33 C38 C37 118.5(7) . . ? C44 C39 C40 120.1(6) . . ? C44 C39 P1 120.9(5) . . ? C40 C39 P1 118.9(5) . . ? C41 C40 C39 118.8(7) . . ? C40 C41 C42 121.6(8) . . ? C41 C42 C43 118.6(8) . . ? C44 C43 C42 121.1(8) . . ? C43 C44 C39 119.6(7) . . ? C63 P2 C57 107.6(3) . . ? C63 P2 C51 110.3(3) . . ? C57 P2 C51 110.3(3) . . ? C63 P2 C45 107.5(3) . . ? C57 P2 C45 111.3(3) . . ? C51 P2 C45 109.8(3) . . ? C46 C45 C50 119.9(7) . . ? C46 C45 P2 121.0(5) . . ? C50 C45 P2 119.1(6) . . ? C45 C46 C47 120.3(7) . . ? C46 C47 C48 119.8(8) . . ? C49 C48 C47 120.2(7) . . ? C48 C49 C50 120.4(8) . . ? C45 C50 C49 119.3(8) . . ? C56 C51 C52 119.7(7) . . ? C56 C51 P2 120.9(6) . . ? C52 C51 P2 119.3(5) . . ? C53 C52 C51 119.7(7) . . ? C54 C53 C52 120.6(8) . . ? C53 C54 C55 119.6(7) . . ? C56 C55 C54 119.9(8) . . ? C55 C56 C51 120.3(8) . . ? C58 C57 C62 121.0(7) . . ? C58 C57 P2 119.2(6) . . ? C62 C57 P2 119.3(6) . . ? C57 C58 C59 119.6(8) . . ? C60 C59 C58 119.9(8) . . ? C61 C60 C59 120.6(8) . . ? C60 C61 C62 120.9(8) . . ? C57 C62 C61 118.1(8) . . ? C68 C63 C64 119.3(7) . . ? C68 C63 P2 121.4(5) . . ? C64 C63 P2 119.2(5) . . ? C65 C64 C63 121.7(8) . . ? C64 C65 C66 118.9(8) . . ? C68 C67 C66 119.6(8) . . ? C65 C66 C67 119.7(8) . . ? C63 C68 C67 120.7(7) . . ? N5 C69 C70 177.4(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.805 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.122