# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ch. Elschenbroich' 'Klaus Harms' 'Jorg Six' _publ_contact_author_name 'Ch Elschenbroich' _publ_contact_author_address ; Fachbereich Chemie Philipps-Universitat Marburg FB Chemie Hans-Meerwein-Strasse Marburg D-35032 GERMANY ; _publ_contact_author_email EB@CHEMIE.UNI-MARBURG.DE _publ_requested_journal 'Chemical Communications' _publ_section_title ; On a Novel Coordination Mode of Phosphinine C5H5P ; data_six07s _database_code_depnum_ccdc_archive 'CCDC 602394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H30 Mn4 O13 P2' _chemical_formula_weight 1030.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9492(8) _cell_length_b 14.8524(13) _cell_length_c 16.7326(15) _cell_angle_alpha 105.427(7) _cell_angle_beta 95.207(7) _cell_angle_gamma 92.097(7) _cell_volume 2130.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1038 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min 0.6522 _exptl_absorpt_correction_T_max 0.9499 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24204 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 24.94 _reflns_number_total 7422 _reflns_number_gt 5516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe Expose' _computing_cell_refinement 'Stoe Cell' _computing_data_reduction 'Stoe Integrate' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7422 _refine_ls_number_parameters 660 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 0.10105(4) 0.22327(3) 0.40456(3) 0.03112(11) Uani 1 1 d . . . Mn2 Mn 0.40781(4) 0.27900(3) 0.42223(3) 0.03192(11) Uani 1 1 d . . . Mn3 Mn 0.13521(5) 0.28859(3) 0.13848(3) 0.04256(12) Uani 1 1 d . . . Mn4 Mn 0.24852(4) 0.18984(3) 0.68163(3) 0.03608(11) Uani 1 1 d . . . P1 P 0.21128(7) 0.26519(5) 0.30744(5) 0.03301(16) Uani 1 1 d . . . C2 C 0.2460(3) 0.19545(19) 0.20545(19) 0.0394(7) Uani 1 1 d . . . C3 C 0.3456(3) 0.2304(2) 0.1583(2) 0.0407(7) Uani 1 1 d . . . H3 H 0.393(3) 0.185(2) 0.110(2) 0.048(8) Uiso 1 1 d . . . C4 C 0.3728(3) 0.3277(2) 0.16529(19) 0.0404(7) Uani 1 1 d . . . C5 C 0.2897(3) 0.3927(2) 0.2197(2) 0.0407(7) Uani 1 1 d . . . H5 H 0.294(3) 0.461(2) 0.216(2) 0.051(9) Uiso 1 1 d . . . C6 C 0.1891(3) 0.36971(19) 0.27154(19) 0.0389(7) Uani 1 1 d . . . C7 C 0.4775(3) 0.3619(2) 0.1141(2) 0.0443(7) Uani 1 1 d . . . C8 C 0.4719(4) 0.3225(3) 0.0289(2) 0.0571(9) Uani 1 1 d . . . H8 H 0.401(4) 0.269(2) 0.000(2) 0.063(10) Uiso 1 1 d . . . C9 C 0.5714(5) 0.3562(3) -0.0186(3) 0.0680(10) Uani 1 1 d . . . H9 H 0.573(4) 0.317(2) -0.084(2) 0.063(10) Uiso 1 1 d . . . C10 C 0.6756(4) 0.4286(3) 0.0209(3) 0.0650(10) Uani 1 1 d . . . H10 H 0.747(4) 0.444(3) -0.010(2) 0.070(11) Uiso 1 1 d . . . C11 C 0.6809(5) 0.4676(3) 0.1048(3) 0.0672(11) Uani 1 1 d . . . H11 H 0.755(5) 0.514(3) 0.130(3) 0.087(14) Uiso 1 1 d . . . C12 C 0.5834(4) 0.4339(2) 0.1517(3) 0.0561(9) Uani 1 1 d . . . H12 H 0.591(4) 0.463(2) 0.212(3) 0.063(10) Uiso 1 1 d . . . C13 C 0.2092(4) 0.0906(2) 0.1794(2) 0.0480(8) Uani 1 1 d . . . H13A H 0.275(4) 0.065(2) 0.211(2) 0.047(9) Uiso 1 1 d . . . H13B H 0.108(4) 0.076(2) 0.192(2) 0.064(11) Uiso 1 1 d . . . H13C H 0.228(4) 0.062(3) 0.118(3) 0.078(12) Uiso 1 1 d . . . C14 C 0.0904(4) 0.4452(2) 0.3137(3) 0.0493(8) Uani 1 1 d . . . H14A H 0.137(3) 0.476(2) 0.373(2) 0.040(8) Uiso 1 1 d . . . H14B H -0.004(4) 0.413(2) 0.313(2) 0.044(8) Uiso 1 1 d . . . H14C H 0.081(4) 0.493(2) 0.281(2) 0.064(10) Uiso 1 1 d . . . P15 P 0.25208(7) 0.22660(4) 0.51540(5) 0.03051(15) Uani 1 1 d . . . C16 C 0.2622(3) 0.30496(18) 0.61961(18) 0.0350(6) Uani 1 1 d . . . C17 C 0.3888(3) 0.30661(19) 0.6761(2) 0.0355(6) Uani 1 1 d . . . H17 H 0.408(3) 0.3583(19) 0.7227(18) 0.029(7) Uiso 1 1 d . . . C18 C 0.4801(3) 0.22868(18) 0.67433(18) 0.0347(6) Uani 1 1 d . . . C19 C 0.4349(3) 0.14240(19) 0.61454(19) 0.0357(6) Uani 1 1 d . . . H19 H 0.484(3) 0.086(2) 0.620(2) 0.050(9) Uiso 1 1 d . . . C20 C 0.3105(3) 0.12907(18) 0.55389(18) 0.0355(6) Uani 1 1 d . . . C21 C 0.6142(3) 0.23855(19) 0.7356(2) 0.0393(7) Uani 1 1 d . . . C22 C 0.7049(3) 0.3218(2) 0.7588(2) 0.0459(7) Uani 1 1 d . . . H22 H 0.683(3) 0.366(2) 0.730(2) 0.049(9) Uiso 1 1 d . . . C23 C 0.8300(4) 0.3322(3) 0.8163(2) 0.0548(9) Uani 1 1 d . . . H23 H 0.883(4) 0.388(2) 0.831(2) 0.058(10) Uiso 1 1 d . . . C24 C 0.8669(4) 0.2609(3) 0.8510(2) 0.0561(9) Uani 1 1 d . . . H24 H 0.954(4) 0.268(2) 0.890(2) 0.048(9) Uiso 1 1 d . . . C25 C 0.7817(4) 0.1778(3) 0.8265(2) 0.0583(9) Uani 1 1 d . . . H25 H 0.806(4) 0.128(3) 0.850(2) 0.071(11) Uiso 1 1 d . . . C26 C 0.6559(4) 0.1666(2) 0.7701(2) 0.0500(8) Uani 1 1 d . . . H26 H 0.599(4) 0.111(3) 0.755(2) 0.062(10) Uiso 1 1 d . . . C27 C 0.1615(4) 0.3858(2) 0.6397(2) 0.0446(7) Uani 1 1 d . . . H27A H 0.185(3) 0.430(2) 0.613(2) 0.041(8) Uiso 1 1 d . . . H27B H 0.175(4) 0.416(2) 0.701(2) 0.054(9) Uiso 1 1 d . . . H27C H 0.055(4) 0.363(2) 0.621(2) 0.053(9) Uiso 1 1 d . . . C28 C 0.2612(4) 0.0293(2) 0.5058(2) 0.0426(7) Uani 1 1 d . . . H28A H 0.302(3) 0.010(2) 0.453(2) 0.044(9) Uiso 1 1 d . . . H28B H 0.290(4) -0.011(3) 0.535(3) 0.077(12) Uiso 1 1 d . . . H28C H 0.148(4) 0.027(2) 0.490(2) 0.067(11) Uiso 1 1 d . . . O29 O 0.1013(2) 0.01854(13) 0.32709(14) 0.0450(5) Uani 1 1 d . . . C29 C 0.1119(3) 0.0981(2) 0.35700(19) 0.0364(6) Uani 1 1 d . . . O30 O -0.2186(2) 0.16543(18) 0.3919(2) 0.0876(10) Uani 1 1 d . . . C30 C -0.0922(3) 0.1881(2) 0.3963(2) 0.0503(8) Uani 1 1 d . . . C31 C 0.0232(3) 0.33616(19) 0.44748(19) 0.0368(6) Uani 1 1 d . . . O31 O -0.0444(2) 0.40013(14) 0.47291(14) 0.0470(5) Uani 1 1 d . . . O32 O 0.6630(2) 0.30838(18) 0.55427(16) 0.0589(6) Uani 1 1 d . . . C32 C 0.5623(3) 0.2944(2) 0.5048(2) 0.0403(7) Uani 1 1 d . . . O33 O 0.3317(2) 0.47606(14) 0.49558(17) 0.0602(7) Uani 1 1 d . . . C33 C 0.3572(3) 0.3998(2) 0.4671(2) 0.0421(7) Uani 1 1 d . . . O34 O 0.6178(2) 0.34745(18) 0.32095(16) 0.0608(6) Uani 1 1 d . . . C34 C 0.5328(3) 0.3197(2) 0.3574(2) 0.0415(7) Uani 1 1 d . . . O35 O 0.4702(2) 0.07875(14) 0.35011(16) 0.0521(6) Uani 1 1 d . . . C35 C 0.4456(3) 0.1556(2) 0.3776(2) 0.0393(7) Uani 1 1 d . . . C36 C -0.0515(4) 0.2658(3) 0.1665(2) 0.0604(9) Uani 1 1 d . . . O36 O -0.1684(3) 0.2541(3) 0.1851(2) 0.0962(10) Uani 1 1 d . . . O37 O 0.0803(4) 0.1481(2) -0.02498(19) 0.0852(9) Uani 1 1 d . . . C37 C 0.1022(4) 0.2033(3) 0.0388(3) 0.0579(9) Uani 1 1 d . . . O38 O 0.0493(3) 0.43097(19) 0.0517(2) 0.0780(8) Uani 1 1 d . . . C38 C 0.0802(4) 0.3763(2) 0.0871(2) 0.0541(8) Uani 1 1 d . . . C39 C 0.2286(3) 0.2518(2) 0.7874(2) 0.0479(8) Uani 1 1 d . . . O39 O 0.2235(3) 0.2905(2) 0.85658(17) 0.0704(7) Uani 1 1 d . . . O40 O 0.2461(3) 0.01993(18) 0.74265(19) 0.0715(7) Uani 1 1 d . . . C40 C 0.2463(3) 0.0844(2) 0.7167(2) 0.0490(8) Uani 1 1 d . . . O41 O -0.0759(2) 0.16900(16) 0.62144(15) 0.0533(6) Uani 1 1 d . . . C41 C 0.0480(3) 0.17583(19) 0.6454(2) 0.0410(7) Uani 1 1 d . . . C901 C 0.3731(10) -0.0268(6) -0.0495(6) 0.143(3) Uani 1 1 d . . . H90F H 0.2815 -0.0428 -0.0862 0.172 Uiso 0.50 1 d PR A 2 C907 C 0.2433(10) -0.0532(6) -0.0856(6) 0.295(17) Uani 0.50 1 d PR A 1 H90C H 0.1992 -0.1071 -0.0731 0.443 Uiso 0.50 1 d PR A 1 H90D H 0.1789 -0.0022 -0.0714 0.443 Uiso 0.50 1 d PR A 1 H90E H 0.2552 -0.0677 -0.1440 0.443 Uiso 0.50 1 d PR A 1 C902 C 0.4029(13) -0.0789(6) 0.0024(6) 0.161(4) Uani 1 1 d . A . H90A H 0.3378 -0.1314 0.0032 0.193 Uiso 1 1 d R . . C903 C 0.5381(12) -0.0490(7) 0.0549(5) 0.131(3) Uani 1 1 d . . . H90B H 0.5712 -0.0809 0.0956 0.158 Uiso 1 1 d R A . 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 0.02582(19) 0.0299(2) 0.0395(3) 0.01255(18) 0.00361(17) 0.00196(15) Mn2 0.0261(2) 0.0305(2) 0.0410(3) 0.01229(18) 0.00565(18) 0.00194(15) Mn3 0.0427(2) 0.0445(3) 0.0457(3) 0.0218(2) 0.0025(2) 0.00459(19) Mn4 0.0332(2) 0.0378(2) 0.0395(3) 0.01459(19) 0.00377(19) -0.00004(17) P1 0.0326(3) 0.0306(3) 0.0388(4) 0.0137(3) 0.0052(3) 0.0045(3) C2 0.0425(15) 0.0393(15) 0.0397(17) 0.0161(13) 0.0037(13) 0.0070(12) C3 0.0444(16) 0.0422(16) 0.0370(18) 0.0126(14) 0.0049(14) 0.0066(13) C4 0.0418(15) 0.0414(15) 0.0401(17) 0.0147(13) 0.0032(13) 0.0053(12) C5 0.0447(16) 0.0356(15) 0.0451(19) 0.0168(13) 0.0037(14) 0.0038(12) C6 0.0420(15) 0.0344(14) 0.0445(18) 0.0164(13) 0.0065(14) 0.0079(12) C7 0.0456(17) 0.0474(17) 0.046(2) 0.0209(15) 0.0118(15) 0.0068(13) C8 0.058(2) 0.067(2) 0.048(2) 0.0158(18) 0.0115(17) -0.0044(18) C9 0.071(2) 0.082(3) 0.057(3) 0.024(2) 0.022(2) -0.001(2) C10 0.063(2) 0.074(2) 0.068(3) 0.033(2) 0.025(2) -0.0019(19) C11 0.068(2) 0.064(2) 0.070(3) 0.017(2) 0.017(2) -0.015(2) C12 0.064(2) 0.053(2) 0.053(2) 0.0147(17) 0.0153(18) -0.0032(16) C13 0.062(2) 0.0358(16) 0.048(2) 0.0151(15) 0.0066(18) 0.0066(15) C14 0.057(2) 0.0419(17) 0.058(2) 0.0225(17) 0.0169(18) 0.0162(15) P15 0.0275(3) 0.0284(3) 0.0373(4) 0.0113(3) 0.0040(3) 0.0027(3) C16 0.0336(14) 0.0324(14) 0.0408(17) 0.0113(12) 0.0076(12) 0.0042(11) C17 0.0358(14) 0.0323(14) 0.0378(17) 0.0083(13) 0.0041(13) 0.0016(11) C18 0.0319(13) 0.0365(14) 0.0385(16) 0.0137(12) 0.0064(12) 0.0038(11) C19 0.0340(14) 0.0333(14) 0.0434(18) 0.0154(13) 0.0069(13) 0.0045(11) C20 0.0347(14) 0.0328(14) 0.0408(17) 0.0122(12) 0.0066(12) 0.0041(11) C21 0.0346(14) 0.0400(15) 0.0425(18) 0.0098(13) 0.0032(13) 0.0023(12) C22 0.0432(17) 0.0466(18) 0.048(2) 0.0146(16) 0.0039(15) 0.0008(14) C23 0.0441(18) 0.060(2) 0.056(2) 0.0111(18) 0.0008(16) -0.0083(16) C24 0.0412(17) 0.075(2) 0.051(2) 0.0178(18) -0.0028(16) 0.0040(16) C25 0.054(2) 0.064(2) 0.060(2) 0.0236(19) -0.0051(17) 0.0125(17) C26 0.0506(18) 0.0457(18) 0.053(2) 0.0177(16) -0.0079(16) 0.0027(15) C27 0.0444(18) 0.0394(17) 0.050(2) 0.0103(16) 0.0075(16) 0.0124(14) C28 0.0535(19) 0.0306(15) 0.043(2) 0.0122(14) -0.0032(16) 0.0026(13) O29 0.0533(12) 0.0315(11) 0.0494(13) 0.0108(10) 0.0041(10) -0.0027(9) C29 0.0278(13) 0.0441(17) 0.0412(17) 0.0183(14) 0.0037(12) 0.0009(11) O30 0.0293(12) 0.0604(16) 0.158(3) 0.0012(17) 0.0163(15) -0.0033(11) C30 0.0366(17) 0.0348(15) 0.075(3) 0.0051(15) 0.0082(16) 0.0051(12) C31 0.0318(14) 0.0399(15) 0.0421(18) 0.0183(13) 0.0002(12) 0.0004(12) O31 0.0433(11) 0.0412(11) 0.0600(15) 0.0164(10) 0.0115(10) 0.0132(9) O32 0.0373(12) 0.0861(17) 0.0563(16) 0.0285(13) -0.0033(12) -0.0067(11) C32 0.0341(15) 0.0453(16) 0.0458(19) 0.0181(14) 0.0097(15) 0.0010(12) O33 0.0478(12) 0.0301(12) 0.097(2) 0.0045(12) 0.0150(13) 0.0021(9) C33 0.0290(14) 0.0412(17) 0.057(2) 0.0160(15) 0.0051(13) -0.0045(12) O34 0.0472(12) 0.0811(16) 0.0630(16) 0.0334(14) 0.0149(12) -0.0060(12) C34 0.0338(14) 0.0453(16) 0.0473(19) 0.0160(14) 0.0045(14) 0.0018(12) O35 0.0390(11) 0.0352(11) 0.0794(18) 0.0093(11) 0.0089(11) 0.0082(9) C35 0.0274(13) 0.0443(17) 0.0491(19) 0.0174(14) 0.0052(13) 0.0007(12) C36 0.050(2) 0.074(2) 0.063(3) 0.031(2) 0.0047(18) 0.0036(17) O36 0.0475(15) 0.146(3) 0.104(3) 0.048(2) 0.0151(16) -0.0044(17) O37 0.101(2) 0.087(2) 0.0563(19) 0.0082(17) -0.0158(16) 0.0100(17) C37 0.056(2) 0.060(2) 0.061(3) 0.027(2) -0.0057(18) 0.0055(16) O38 0.0752(17) 0.0754(17) 0.098(2) 0.0571(17) -0.0154(16) 0.0016(14) C38 0.0474(18) 0.057(2) 0.061(2) 0.0247(18) -0.0025(16) 0.0031(15) C39 0.0397(16) 0.0565(19) 0.048(2) 0.0164(17) 0.0062(15) -0.0051(14) O39 0.0649(15) 0.0922(19) 0.0472(17) 0.0068(14) 0.0119(13) -0.0115(14) O40 0.0803(17) 0.0618(15) 0.087(2) 0.0454(15) 0.0101(15) 0.0006(13) C40 0.0443(17) 0.0545(19) 0.053(2) 0.0232(16) 0.0038(15) -0.0006(14) O41 0.0372(12) 0.0637(14) 0.0624(16) 0.0246(12) 0.0024(11) -0.0028(10) C41 0.0425(17) 0.0385(15) 0.0454(19) 0.0155(14) 0.0105(14) 0.0011(12) C901 0.137(6) 0.107(5) 0.167(9) -0.007(5) 0.047(6) 0.017(5) C907 0.29(3) 0.152(19) 0.37(4) -0.03(2) -0.02(3) -0.05(2) C902 0.232(11) 0.147(7) 0.136(7) 0.059(6) 0.083(8) 0.111(7) C903 0.163(7) 0.155(7) 0.085(5) 0.036(4) 0.025(5) 0.080(6) _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 C30 1.771(3) . ? Mn1 C29 1.828(3) . ? Mn1 C31 1.830(3) . ? Mn1 P15 2.1818(9) . ? Mn1 P1 2.1878(8) . ? Mn1 Mn2 2.8045(6) . ? Mn2 C34 1.820(3) . ? Mn2 C32 1.825(3) . ? Mn2 C33 1.842(3) . ? Mn2 C35 1.843(3) . ? Mn2 P15 2.4369(8) . ? Mn2 P1 2.4446(9) . ? Mn3 C37 1.798(4) . ? Mn3 C38 1.802(3) . ? Mn3 C36 1.820(4) . ? Mn3 C5 2.129(3) . ? Mn3 C3 2.135(3) . ? Mn3 C4 2.158(3) . ? Mn3 C2 2.208(3) . ? Mn3 C6 2.231(3) . ? Mn3 P1 2.9610(9) . ? Mn4 C39 1.793(4) . ? Mn4 C40 1.813(3) . ? Mn4 C41 1.827(3) . ? Mn4 C17 2.130(3) . ? Mn4 C19 2.132(3) . ? Mn4 C18 2.154(3) . ? Mn4 C20 2.217(3) . ? Mn4 C16 2.229(3) . ? P1 C2 1.806(3) . ? P1 C6 1.819(3) . ? C2 C3 1.413(4) . ? C2 C13 1.516(4) . ? C3 C4 1.428(4) . ? C3 H3 1.05(3) . ? C4 C5 1.422(4) . ? C4 C7 1.487(4) . ? C5 C6 1.399(4) . ? C5 H5 1.04(3) . ? C6 C14 1.517(4) . ? C7 C12 1.378(5) . ? C7 C8 1.386(5) . ? C8 C9 1.408(5) . ? C8 H8 0.98(4) . ? C9 C10 1.378(6) . ? C9 H9 1.09(4) . ? C10 C11 1.364(6) . ? C10 H10 0.92(4) . ? C11 C12 1.389(5) . ? C11 H11 0.92(4) . ? C12 H12 0.99(4) . ? C13 H13A 0.92(4) . ? C13 H13B 0.98(4) . ? C13 H13C 1.04(4) . ? C14 H14A 1.01(3) . ? C14 H14B 0.95(3) . ? C14 H14C 1.01(4) . ? P15 C20 1.810(3) . ? P15 C16 1.813(3) . ? C16 C17 1.403(4) . ? C16 C27 1.512(4) . ? C17 C18 1.437(4) . ? C17 H17 0.93(3) . ? C18 C19 1.419(4) . ? C18 C21 1.482(4) . ? C19 C20 1.408(4) . ? C19 H19 0.99(3) . ? C20 C28 1.514(4) . ? C21 C26 1.390(4) . ? C21 C22 1.397(4) . ? C22 C23 1.385(5) . ? C22 H22 0.93(3) . ? C23 C24 1.373(5) . ? C23 H23 0.90(3) . ? C24 C25 1.370(5) . ? C24 H24 0.95(3) . ? C25 C26 1.378(5) . ? C25 H25 0.94(4) . ? C26 H26 0.91(4) . ? C27 H27A 0.91(3) . ? C27 H27B 1.00(4) . ? C27 H27C 0.99(3) . ? C28 H28A 0.95(3) . ? C28 H28B 0.90(4) . ? C28 H28C 1.02(4) . ? O29 C29 1.150(3) . ? O30 C30 1.158(3) . ? C31 O31 1.150(3) . ? O32 C32 1.141(4) . ? O33 C33 1.146(3) . ? O34 C34 1.148(3) . ? O35 C35 1.149(3) . ? C36 O36 1.139(4) . ? O37 C37 1.155(5) . ? O38 C38 1.152(4) . ? C39 O39 1.153(4) . ? O40 C40 1.151(4) . ? O41 C41 1.136(4) . ? C901 C907 1.2575 . ? C901 C902 1.325(11) . ? C901 C903 1.382(10) 2_655 ? C901 H90F 0.9600 . ? C907 H90F 0.3714 . ? C907 H90C 0.9599 . ? C907 H90D 0.9599 . ? C907 H90E 0.9599 . ? C902 C903 1.411(12) . ? C902 H90A 0.9600 . ? C903 C901 1.382(10) 2_655 ? C903 H90B 0.9602 . ? 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 C30 Mn1 C29 81.22(12) . . ? C30 Mn1 C31 79.53(12) . . ? C29 Mn1 C31 160.73(11) . . ? C30 Mn1 P15 121.61(13) . . ? C29 Mn1 P15 94.83(9) . . ? C31 Mn1 P15 95.99(9) . . ? C30 Mn1 P1 124.47(13) . . ? C29 Mn1 P1 94.15(9) . . ? C31 Mn1 P1 95.97(9) . . ? P15 Mn1 P1 113.91(3) . . ? C30 Mn1 Mn2 178.47(13) . . ? C29 Mn1 Mn2 99.05(8) . . ? C31 Mn1 Mn2 100.22(8) . . ? P15 Mn1 Mn2 56.88(2) . . ? P1 Mn1 Mn2 57.04(2) . . ? C34 Mn2 C32 90.23(13) . . ? C34 Mn2 C33 90.38(13) . . ? C32 Mn2 C33 90.14(13) . . ? C34 Mn2 C35 92.59(13) . . ? C32 Mn2 C35 92.12(13) . . ? C33 Mn2 C35 176.25(11) . . ? C34 Mn2 P15 176.75(10) . . ? C32 Mn2 P15 86.54(9) . . ? C33 Mn2 P15 89.32(9) . . ? C35 Mn2 P15 87.83(9) . . ? C34 Mn2 P1 85.98(10) . . ? C32 Mn2 P1 176.04(9) . . ? C33 Mn2 P1 88.74(10) . . ? C35 Mn2 P1 89.21(10) . . ? P15 Mn2 P1 97.24(3) . . ? C34 Mn2 Mn1 134.64(10) . . ? C32 Mn2 Mn1 135.08(9) . . ? C33 Mn2 Mn1 87.95(8) . . ? C35 Mn2 Mn1 88.34(8) . . ? P15 Mn2 Mn1 48.58(2) . . ? P1 Mn2 Mn1 48.67(2) . . ? C37 Mn3 C38 88.02(16) . . ? C37 Mn3 C36 93.06(17) . . ? C38 Mn3 C36 95.20(16) . . ? C37 Mn3 C5 145.72(14) . . ? C38 Mn3 C5 87.33(14) . . ? C36 Mn3 C5 121.19(15) . . ? C37 Mn3 C3 88.75(14) . . ? C38 Mn3 C3 132.42(13) . . ? C36 Mn3 C3 132.37(14) . . ? C5 Mn3 C3 69.97(11) . . ? C37 Mn3 C4 109.02(14) . . ? C38 Mn3 C4 98.94(13) . . ? C36 Mn3 C4 154.04(15) . . ? C5 Mn3 C4 38.74(11) . . ? C3 Mn3 C4 38.84(11) . . ? C37 Mn3 C2 96.29(13) . . ? C38 Mn3 C2 168.91(13) . . ? C36 Mn3 C2 94.76(14) . . ? C5 Mn3 C2 83.35(11) . . ? C3 Mn3 C2 37.93(11) . . ? C4 Mn3 C2 70.00(11) . . ? C37 Mn3 C6 168.42(13) . . ? C38 Mn3 C6 103.56(14) . . ? C36 Mn3 C6 86.06(15) . . ? C5 Mn3 C6 37.33(11) . . ? C3 Mn3 C6 83.38(11) . . ? C4 Mn3 C6 69.55(11) . . ? C2 Mn3 C6 72.30(10) . . ? C37 Mn3 P1 130.70(11) . . ? C38 Mn3 P1 140.86(12) . . ? C36 Mn3 P1 79.39(12) . . ? C5 Mn3 P1 64.15(8) . . ? C3 Mn3 P1 64.28(9) . . ? C4 Mn3 P1 75.88(8) . . ? C2 Mn3 P1 37.44(8) . . ? C6 Mn3 P1 37.81(7) . . ? C39 Mn4 C40 86.48(15) . . ? C39 Mn4 C41 96.32(14) . . ? C40 Mn4 C41 93.85(13) . . ? C39 Mn4 C17 87.29(13) . . ? C40 Mn4 C17 143.35(13) . . ? C41 Mn4 C17 122.74(12) . . ? C39 Mn4 C19 134.37(13) . . ? C40 Mn4 C19 89.15(13) . . ? C41 Mn4 C19 129.30(13) . . ? C17 Mn4 C19 70.12(10) . . ? C39 Mn4 C18 100.40(13) . . ? C40 Mn4 C18 107.11(12) . . ? C41 Mn4 C18 153.80(12) . . ? C17 Mn4 C18 39.18(10) . . ? C19 Mn4 C18 38.66(11) . . ? C39 Mn4 C20 169.84(12) . . ? C40 Mn4 C20 98.65(13) . . ? C41 Mn4 C20 92.10(12) . . ? C17 Mn4 C20 83.37(11) . . ? C19 Mn4 C20 37.71(11) . . ? C18 Mn4 C20 69.75(10) . . ? C39 Mn4 C16 102.52(13) . . ? C40 Mn4 C16 170.84(13) . . ? C41 Mn4 C16 86.88(11) . . ? C17 Mn4 C16 37.46(11) . . ? C19 Mn4 C16 83.36(10) . . ? C18 Mn4 C16 69.94(10) . . ? C20 Mn4 C16 72.19(10) . . ? C2 P1 C6 92.52(13) . . ? C2 P1 Mn1 129.23(9) . . ? C6 P1 Mn1 128.75(10) . . ? C2 P1 Mn2 117.52(10) . . ? C6 P1 Mn2 115.49(10) . . ? Mn1 P1 Mn2 74.28(3) . . ? C2 P1 Mn3 48.02(9) . . ? C6 P1 Mn3 48.77(10) . . ? Mn1 P1 Mn3 139.33(3) . . ? Mn2 P1 Mn3 146.38(3) . . ? C3 C2 C13 116.5(3) . . ? C3 C2 P1 120.4(2) . . ? C13 C2 P1 120.6(2) . . ? C3 C2 Mn3 68.24(16) . . ? C13 C2 Mn3 121.7(2) . . ? P1 C2 Mn3 94.54(12) . . ? C2 C3 C4 123.7(3) . . ? C2 C3 Mn3 73.83(17) . . ? C4 C3 Mn3 71.45(17) . . ? C2 C3 H3 120.3(16) . . ? C4 C3 H3 115.5(16) . . ? Mn3 C3 H3 121.6(17) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 C7 119.6(3) . . ? C3 C4 C7 122.2(3) . . ? C5 C4 Mn3 69.52(17) . . ? C3 C4 Mn3 69.70(17) . . ? C7 C4 Mn3 129.5(2) . . ? C6 C5 C4 125.1(3) . . ? C6 C5 Mn3 75.29(18) . . ? C4 C5 Mn3 71.74(17) . . ? C6 C5 H5 116.7(17) . . ? C4 C5 H5 117.8(17) . . ? Mn3 C5 H5 121.7(18) . . ? C5 C6 C14 117.6(3) . . ? C5 C6 P1 119.9(2) . . ? C14 C6 P1 120.6(2) . . ? C5 C6 Mn3 67.38(17) . . ? C14 C6 Mn3 121.6(2) . . ? P1 C6 Mn3 93.42(12) . . ? C12 C7 C8 118.8(3) . . ? C12 C7 C4 119.8(3) . . ? C8 C7 C4 121.5(3) . . ? C7 C8 C9 120.6(3) . . ? C7 C8 H8 121(2) . . ? C9 C8 H8 118(2) . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9 122.5(18) . . ? C8 C9 H9 117.7(18) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 122(2) . . ? C9 C10 H10 117(2) . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119(3) . . ? C12 C11 H11 120(3) . . ? C7 C12 C11 120.6(4) . . ? C7 C12 H12 121(2) . . ? C11 C12 H12 119(2) . . ? C2 C13 H13A 107(2) . . ? C2 C13 H13B 110(2) . . ? H13A C13 H13B 108(3) . . ? C2 C13 H13C 111(2) . . ? H13A C13 H13C 107(3) . . ? H13B C13 H13C 114(3) . . ? C6 C14 H14A 109.5(17) . . ? C6 C14 H14B 104.8(18) . . ? H14A C14 H14B 112(3) . . ? C6 C14 H14C 109(2) . . ? H14A C14 H14C 109(3) . . ? H14B C14 H14C 112(3) . . ? C20 P15 C16 92.59(13) . . ? C20 P15 Mn1 128.14(10) . . ? C16 P15 Mn1 129.77(9) . . ? C20 P15 Mn2 118.22(9) . . ? C16 P15 Mn2 114.52(9) . . ? Mn1 P15 Mn2 74.55(3) . . ? C17 C16 C27 117.6(3) . . ? C17 C16 P15 119.2(2) . . ? C27 C16 P15 121.1(2) . . ? C17 C16 Mn4 67.46(15) . . ? C27 C16 Mn4 120.9(2) . . ? P15 C16 Mn4 94.29(11) . . ? C16 C17 C18 124.5(3) . . ? C16 C17 Mn4 75.08(16) . . ? C18 C17 Mn4 71.28(15) . . ? C16 C17 H17 118.6(17) . . ? C18 C17 H17 116.3(17) . . ? Mn4 C17 H17 120.3(16) . . ? C19 C18 C17 118.1(3) . . ? C19 C18 C21 121.7(2) . . ? C17 C18 C21 120.2(2) . . ? C19 C18 Mn4 69.84(15) . . ? C17 C18 Mn4 69.53(15) . . ? C21 C18 Mn4 130.6(2) . . ? C20 C19 C18 124.4(3) . . ? C20 C19 Mn4 74.43(16) . . ? C18 C19 Mn4 71.50(16) . . ? C20 C19 H19 116.5(19) . . ? C18 C19 H19 118.6(19) . . ? Mn4 C19 H19 121.4(18) . . ? C19 C20 C28 117.2(2) . . ? C19 C20 P15 119.3(2) . . ? C28 C20 P15 121.0(2) . . ? C19 C20 Mn4 67.86(16) . . ? C28 C20 Mn4 121.4(2) . . ? P15 C20 Mn4 94.76(12) . . ? C26 C21 C22 118.1(3) . . ? C26 C21 C18 122.2(3) . . ? C22 C21 C18 119.7(3) . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 122(2) . . ? C21 C22 H22 117(2) . . ? C24 C23 C22 120.6(3) . . ? C24 C23 H23 122(2) . . ? C22 C23 H23 117(2) . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24 120.0(19) . . ? C23 C24 H24 120.3(19) . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25 120(2) . . ? C26 C25 H25 119(2) . . ? C25 C26 C21 120.8(3) . . ? C25 C26 H26 119(2) . . ? C21 C26 H26 120(2) . . ? C16 C27 H27A 111.2(19) . . ? C16 C27 H27B 109.2(19) . . ? H27A C27 H27B 108(3) . . ? C16 C27 H27C 109.8(19) . . ? H27A C27 H27C 108(3) . . ? H27B C27 H27C 110(3) . . ? C20 C28 H28A 113.1(18) . . ? C20 C28 H28B 111(3) . . ? H28A C28 H28B 107(3) . . ? C20 C28 H28C 107.4(19) . . ? H28A C28 H28C 104(3) . . ? H28B C28 H28C 114(3) . . ? O29 C29 Mn1 172.2(2) . . ? O30 C30 Mn1 179.1(4) . . ? O31 C31 Mn1 170.6(2) . . ? O32 C32 Mn2 175.5(3) . . ? O33 C33 Mn2 177.2(2) . . ? O34 C34 Mn2 175.7(3) . . ? O35 C35 Mn2 179.5(3) . . ? O36 C36 Mn3 178.2(4) . . ? O37 C37 Mn3 179.5(4) . . ? O38 C38 Mn3 177.0(3) . . ? O39 C39 Mn4 176.4(3) . . ? O40 C40 Mn4 176.9(3) . . ? O41 C41 Mn4 177.8(3) . . ? C907 C901 C902 107.1(8) . . ? C907 C901 C903 127.0(7) . 2_655 ? C902 C901 C903 125.6(10) . 2_655 ? C907 C901 H90F 11.6 . . ? C902 C901 H90F 117.1 . . ? C903 C901 H90F 117.3 2_655 . ? C901 C907 H90F 31.3 . . ? C901 C907 H90C 114.4 . . ? H90F C907 H90C 137.9 . . ? C901 C907 H90D 109.0 . . ? H90F C907 H90D 107.2 . . ? H90C C907 H90D 109.5 . . ? C901 C907 H90E 104.8 . . ? H90F C907 H90E 76.3 . . ? H90C C907 H90E 109.5 . . ? H90D C907 H90E 109.5 . . ? C901 C902 C903 113.1(10) . . ? C901 C902 H90A 122.2 . . ? C903 C902 H90A 124.6 . . ? C901 C903 C902 121.3(8) 2_655 . ? C901 C903 H90B 117.8 2_655 . ? C902 C903 H90B 120.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 Mn1 Mn2 C34 -169(4) . . . . ? C29 Mn1 Mn2 C34 90.70(16) . . . . ? C31 Mn1 Mn2 C34 -88.90(16) . . . . ? P15 Mn1 Mn2 C34 -179.42(13) . . . . ? P1 Mn1 Mn2 C34 1.61(13) . . . . ? C30 Mn1 Mn2 C32 7(4) . . . . ? C29 Mn1 Mn2 C32 -92.65(16) . . . . ? C31 Mn1 Mn2 C32 87.74(16) . . . . ? P15 Mn1 Mn2 C32 -2.77(13) . . . . ? P1 Mn1 Mn2 C32 178.26(13) . . . . ? C30 Mn1 Mn2 C33 -81(4) . . . . ? C29 Mn1 Mn2 C33 179.22(14) . . . . ? C31 Mn1 Mn2 C33 -0.39(14) . . . . ? P15 Mn1 Mn2 C33 -90.90(10) . . . . ? P1 Mn1 Mn2 C33 90.12(10) . . . . ? C30 Mn1 Mn2 C35 99(4) . . . . ? C29 Mn1 Mn2 C35 -1.31(13) . . . . ? C31 Mn1 Mn2 C35 179.09(13) . . . . ? P15 Mn1 Mn2 C35 88.57(10) . . . . ? P1 Mn1 Mn2 C35 -90.40(10) . . . . ? C30 Mn1 Mn2 P15 10(4) . . . . ? C29 Mn1 Mn2 P15 -89.88(10) . . . . ? C31 Mn1 Mn2 P15 90.51(10) . . . . ? P1 Mn1 Mn2 P15 -178.97(3) . . . . ? C30 Mn1 Mn2 P1 -171(4) . . . . ? C29 Mn1 Mn2 P1 89.09(10) . . . . ? C31 Mn1 Mn2 P1 -90.51(10) . . . . ? P15 Mn1 Mn2 P1 178.97(3) . . . . ? C30 Mn1 P1 C2 -67.35(17) . . . . ? C29 Mn1 P1 C2 14.85(15) . . . . ? C31 Mn1 P1 C2 -148.73(15) . . . . ? P15 Mn1 P1 C2 112.00(13) . . . . ? Mn2 Mn1 P1 C2 112.95(13) . . . . ? C30 Mn1 P1 C6 69.37(18) . . . . ? C29 Mn1 P1 C6 151.57(15) . . . . ? C31 Mn1 P1 C6 -12.00(16) . . . . ? P15 Mn1 P1 C6 -111.27(13) . . . . ? Mn2 Mn1 P1 C6 -110.33(13) . . . . ? C30 Mn1 P1 Mn2 179.71(12) . . . . ? C29 Mn1 P1 Mn2 -98.09(9) . . . . ? C31 Mn1 P1 Mn2 98.33(9) . . . . ? P15 Mn1 P1 Mn2 -0.94(3) . . . . ? C30 Mn1 P1 Mn3 0.64(13) . . . . ? C29 Mn1 P1 Mn3 82.84(10) . . . . ? C31 Mn1 P1 Mn3 -80.74(10) . . . . ? P15 Mn1 P1 Mn3 179.99(4) . . . . ? Mn2 Mn1 P1 Mn3 -179.07(6) . . . . ? C34 Mn2 P1 C2 54.69(14) . . . . ? C32 Mn2 P1 C2 71.6(14) . . . . ? C33 Mn2 P1 C2 145.17(13) . . . . ? C35 Mn2 P1 C2 -37.96(13) . . . . ? P15 Mn2 P1 C2 -125.68(10) . . . . ? Mn1 Mn2 P1 C2 -126.45(11) . . . . ? C34 Mn2 P1 C6 -52.96(14) . . . . ? C32 Mn2 P1 C6 -36.0(14) . . . . ? C33 Mn2 P1 C6 37.51(14) . . . . ? C35 Mn2 P1 C6 -145.62(13) . . . . ? P15 Mn2 P1 C6 126.67(10) . . . . ? Mn1 Mn2 P1 C6 125.89(11) . . . . ? C34 Mn2 P1 Mn1 -178.85(9) . . . . ? C32 Mn2 P1 Mn1 -161.9(14) . . . . ? C33 Mn2 P1 Mn1 -88.38(9) . . . . ? C35 Mn2 P1 Mn1 88.49(9) . . . . ? P15 Mn2 P1 Mn1 0.78(3) . . . . ? C34 Mn2 P1 Mn3 0.05(11) . . . . ? C32 Mn2 P1 Mn3 17.0(14) . . . . ? C33 Mn2 P1 Mn3 90.53(10) . . . . ? C35 Mn2 P1 Mn3 -92.60(10) . . . . ? P15 Mn2 P1 Mn3 179.68(5) . . . . ? Mn1 Mn2 P1 Mn3 178.91(7) . . . . ? C37 Mn3 P1 C2 27.68(19) . . . . ? C38 Mn3 P1 C2 -162.3(2) . . . . ? C36 Mn3 P1 C2 112.55(18) . . . . ? C5 Mn3 P1 C2 -114.90(15) . . . . ? C3 Mn3 P1 C2 -35.81(15) . . . . ? C4 Mn3 P1 C2 -75.43(14) . . . . ? C6 Mn3 P1 C2 -150.14(17) . . . . ? C37 Mn3 P1 C6 177.83(19) . . . . ? C38 Mn3 P1 C6 -12.1(2) . . . . ? C36 Mn3 P1 C6 -97.31(17) . . . . ? C5 Mn3 P1 C6 35.24(14) . . . . ? C3 Mn3 P1 C6 114.34(15) . . . . ? C4 Mn3 P1 C6 74.71(14) . . . . ? C2 Mn3 P1 C6 150.14(17) . . . . ? C37 Mn3 P1 Mn1 -77.27(16) . . . . ? C38 Mn3 P1 Mn1 92.78(17) . . . . ? C36 Mn3 P1 Mn1 7.59(13) . . . . ? C5 Mn3 P1 Mn1 140.14(10) . . . . ? C3 Mn3 P1 Mn1 -140.76(10) . . . . ? C4 Mn3 P1 Mn1 179.62(9) . . . . ? C2 Mn3 P1 Mn1 -104.96(13) . . . . ? C6 Mn3 P1 Mn1 104.90(13) . . . . ? C37 Mn3 P1 Mn2 104.34(16) . . . . ? C38 Mn3 P1 Mn2 -85.60(17) . . . . ? C36 Mn3 P1 Mn2 -170.79(14) . . . . ? C5 Mn3 P1 Mn2 -38.25(10) . . . . ? C3 Mn3 P1 Mn2 40.85(10) . . . . ? C4 Mn3 P1 Mn2 1.23(9) . . . . ? C2 Mn3 P1 Mn2 76.66(13) . . . . ? C6 Mn3 P1 Mn2 -73.48(13) . . . . ? C6 P1 C2 C3 45.4(2) . . . . ? Mn1 P1 C2 C3 -166.98(18) . . . . ? Mn2 P1 C2 C3 -75.2(2) . . . . ? Mn3 P1 C2 C3 67.4(2) . . . . ? C6 P1 C2 C13 -153.2(3) . . . . ? Mn1 P1 C2 C13 -5.6(3) . . . . ? Mn2 P1 C2 C13 86.2(3) . . . . ? Mn3 P1 C2 C13 -131.2(3) . . . . ? C6 P1 C2 Mn3 -22.01(13) . . . . ? Mn1 P1 C2 Mn3 125.63(8) . . . . ? Mn2 P1 C2 Mn3 -142.59(6) . . . . ? C37 Mn3 C2 C3 79.8(2) . . . . ? C38 Mn3 C2 C3 -32.7(8) . . . . ? C36 Mn3 C2 C3 173.4(2) . . . . ? C5 Mn3 C2 C3 -65.70(18) . . . . ? C4 Mn3 C2 C3 -28.19(18) . . . . ? C6 Mn3 C2 C3 -102.28(19) . . . . ? P1 Mn3 C2 C3 -121.0(2) . . . . ? C37 Mn3 C2 C13 -28.8(3) . . . . ? C38 Mn3 C2 C13 -141.3(7) . . . . ? C36 Mn3 C2 C13 64.8(3) . . . . ? C5 Mn3 C2 C13 -174.3(3) . . . . ? C3 Mn3 C2 C13 -108.6(3) . . . . ? C4 Mn3 C2 C13 -136.8(3) . . . . ? C6 Mn3 C2 C13 149.2(3) . . . . ? P1 Mn3 C2 C13 130.5(3) . . . . ? C37 Mn3 C2 P1 -159.25(15) . . . . ? C38 Mn3 C2 P1 88.3(8) . . . . ? C36 Mn3 C2 P1 -65.63(17) . . . . ? C5 Mn3 C2 P1 55.26(12) . . . . ? C3 Mn3 C2 P1 121.0(2) . . . . ? C4 Mn3 C2 P1 92.77(14) . . . . ? C6 Mn3 C2 P1 18.69(11) . . . . ? C13 C2 C3 C4 169.4(3) . . . . ? P1 C2 C3 C4 -28.5(4) . . . . ? Mn3 C2 C3 C4 53.8(3) . . . . ? C13 C2 C3 Mn3 115.6(3) . . . . ? P1 C2 C3 Mn3 -82.23(19) . . . . ? C37 Mn3 C3 C2 -101.9(2) . . . . ? C38 Mn3 C3 C2 171.9(2) . . . . ? C36 Mn3 C3 C2 -8.9(3) . . . . ? C5 Mn3 C3 C2 105.51(19) . . . . ? C4 Mn3 C3 C2 134.9(3) . . . . ? C6 Mn3 C3 C2 69.57(18) . . . . ? P1 Mn3 C3 C2 35.35(15) . . . . ? C37 Mn3 C3 C4 123.1(2) . . . . ? C38 Mn3 C3 C4 37.0(3) . . . . ? C36 Mn3 C3 C4 -143.9(2) . . . . ? C5 Mn3 C3 C4 -29.44(18) . . . . ? C2 Mn3 C3 C4 -134.9(3) . . . . ? C6 Mn3 C3 C4 -65.37(18) . . . . ? P1 Mn3 C3 C4 -99.59(18) . . . . ? C2 C3 C4 C5 -3.2(5) . . . . ? Mn3 C3 C4 C5 51.6(3) . . . . ? C2 C3 C4 C7 -179.4(3) . . . . ? Mn3 C3 C4 C7 -124.7(3) . . . . ? C2 C3 C4 Mn3 -54.8(3) . . . . ? C37 Mn3 C4 C5 165.24(19) . . . . ? C38 Mn3 C4 C5 74.3(2) . . . . ? C36 Mn3 C4 C5 -48.0(4) . . . . ? C3 Mn3 C4 C5 -132.5(3) . . . . ? C2 Mn3 C4 C5 -104.87(19) . . . . ? C6 Mn3 C4 C5 -26.97(16) . . . . ? P1 Mn3 C4 C5 -66.11(16) . . . . ? C37 Mn3 C4 C3 -62.3(2) . . . . ? C38 Mn3 C4 C3 -153.3(2) . . . . ? C36 Mn3 C4 C3 84.5(4) . . . . ? C5 Mn3 C4 C3 132.5(3) . . . . ? C2 Mn3 C4 C3 27.58(17) . . . . ? C6 Mn3 C4 C3 105.48(19) . . . . ? P1 Mn3 C4 C3 66.34(16) . . . . ? C37 Mn3 C4 C7 53.2(3) . . . . ? C38 Mn3 C4 C7 -37.8(3) . . . . ? C36 Mn3 C4 C7 -160.0(3) . . . . ? C5 Mn3 C4 C7 -112.0(3) . . . . ? C3 Mn3 C4 C7 115.5(3) . . . . ? C2 Mn3 C4 C7 143.1(3) . . . . ? C6 Mn3 C4 C7 -139.0(3) . . . . ? P1 Mn3 C4 C7 -178.1(3) . . . . ? C3 C4 C5 C6 4.3(5) . . . . ? C7 C4 C5 C6 -179.3(3) . . . . ? Mn3 C4 C5 C6 56.0(3) . . . . ? C3 C4 C5 Mn3 -51.7(3) . . . . ? C7 C4 C5 Mn3 124.7(3) . . . . ? C37 Mn3 C5 C6 -160.8(2) . . . . ? C38 Mn3 C5 C6 116.62(19) . . . . ? C36 Mn3 C5 C6 22.2(2) . . . . ? C3 Mn3 C5 C6 -106.00(18) . . . . ? C4 Mn3 C5 C6 -135.5(2) . . . . ? C2 Mn3 C5 C6 -69.40(17) . . . . ? P1 Mn3 C5 C6 -35.68(13) . . . . ? C37 Mn3 C5 C4 -25.3(3) . . . . ? C38 Mn3 C5 C4 -107.9(2) . . . . ? C36 Mn3 C5 C4 157.67(19) . . . . ? C3 Mn3 C5 C4 29.51(17) . . . . ? C2 Mn3 C5 C4 66.12(17) . . . . ? C6 Mn3 C5 C4 135.5(2) . . . . ? P1 Mn3 C5 C4 99.84(17) . . . . ? C4 C5 C6 C14 -169.5(3) . . . . ? Mn3 C5 C6 C14 -115.0(3) . . . . ? C4 C5 C6 P1 26.0(4) . . . . ? Mn3 C5 C6 P1 80.5(2) . . . . ? C4 C5 C6 Mn3 -54.5(3) . . . . ? C2 P1 C6 C5 -44.0(3) . . . . ? Mn1 P1 C6 C5 168.1(2) . . . . ? Mn2 P1 C6 C5 78.2(3) . . . . ? Mn3 P1 C6 C5 -65.8(2) . . . . ? C2 P1 C6 C14 151.9(3) . . . . ? Mn1 P1 C6 C14 4.0(3) . . . . ? Mn2 P1 C6 C14 -85.8(3) . . . . ? Mn3 P1 C6 C14 130.2(3) . . . . ? C2 P1 C6 Mn3 21.74(12) . . . . ? Mn1 P1 C6 Mn3 -126.14(8) . . . . ? Mn2 P1 C6 Mn3 143.97(6) . . . . ? C37 Mn3 C6 C5 112.9(7) . . . . ? C38 Mn3 C6 C5 -66.72(19) . . . . ? C36 Mn3 C6 C5 -161.1(2) . . . . ? C3 Mn3 C6 C5 65.39(17) . . . . ? C4 Mn3 C6 C5 27.90(16) . . . . ? C2 Mn3 C6 C5 102.59(17) . . . . ? P1 Mn3 C6 C5 121.1(2) . . . . ? C37 Mn3 C6 C14 -137.7(7) . . . . ? C38 Mn3 C6 C14 42.7(3) . . . . ? C36 Mn3 C6 C14 -51.7(3) . . . . ? C5 Mn3 C6 C14 109.5(3) . . . . ? C3 Mn3 C6 C14 174.9(2) . . . . ? C4 Mn3 C6 C14 137.4(3) . . . . ? C2 Mn3 C6 C14 -147.9(3) . . . . ? P1 Mn3 C6 C14 -129.4(3) . . . . ? C37 Mn3 C6 P1 -8.2(7) . . . . ? C38 Mn3 C6 P1 172.16(13) . . . . ? C36 Mn3 C6 P1 77.75(15) . . . . ? C5 Mn3 C6 P1 -121.1(2) . . . . ? C3 Mn3 C6 P1 -55.73(12) . . . . ? C4 Mn3 C6 P1 -93.21(13) . . . . ? C2 Mn3 C6 P1 -18.53(11) . . . . ? C5 C4 C7 C12 51.6(4) . . . . ? C3 C4 C7 C12 -132.2(3) . . . . ? Mn3 C4 C7 C12 138.5(3) . . . . ? C5 C4 C7 C8 -128.8(3) . . . . ? C3 C4 C7 C8 47.4(4) . . . . ? Mn3 C4 C7 C8 -41.9(4) . . . . ? C12 C7 C8 C9 -0.8(5) . . . . ? C4 C7 C8 C9 179.6(3) . . . . ? C7 C8 C9 C10 0.6(6) . . . . ? C8 C9 C10 C11 -0.7(6) . . . . ? C9 C10 C11 C12 1.1(7) . . . . ? C8 C7 C12 C11 1.2(5) . . . . ? C4 C7 C12 C11 -179.2(3) . . . . ? C10 C11 C12 C7 -1.4(6) . . . . ? C30 Mn1 P15 C20 66.32(16) . . . . ? C29 Mn1 P15 C20 -16.34(14) . . . . ? C31 Mn1 P15 C20 147.69(14) . . . . ? P1 Mn1 P15 C20 -113.06(11) . . . . ? Mn2 Mn1 P15 C20 -114.00(12) . . . . ? C30 Mn1 P15 C16 -70.41(16) . . . . ? C29 Mn1 P15 C16 -153.06(14) . . . . ? C31 Mn1 P15 C16 10.97(14) . . . . ? P1 Mn1 P15 C16 110.22(11) . . . . ? Mn2 Mn1 P15 C16 109.28(12) . . . . ? C30 Mn1 P15 Mn2 -179.68(11) . . . . ? C29 Mn1 P15 Mn2 97.66(8) . . . . ? C31 Mn1 P15 Mn2 -98.31(8) . . . . ? P1 Mn1 P15 Mn2 0.94(3) . . . . ? C34 Mn2 P15 C20 -62.0(17) . . . . ? C32 Mn2 P15 C20 -56.59(14) . . . . ? C33 Mn2 P15 C20 -146.77(14) . . . . ? C35 Mn2 P15 C20 35.66(14) . . . . ? P1 Mn2 P15 C20 124.59(11) . . . . ? Mn1 Mn2 P15 C20 125.37(11) . . . . ? C34 Mn2 P15 C16 45.5(17) . . . . ? C32 Mn2 P15 C16 50.93(13) . . . . ? C33 Mn2 P15 C16 -39.24(14) . . . . ? C35 Mn2 P15 C16 143.19(13) . . . . ? P1 Mn2 P15 C16 -127.89(10) . . . . ? Mn1 Mn2 P15 C16 -127.11(10) . . . . ? C34 Mn2 P15 Mn1 172.6(17) . . . . ? C32 Mn2 P15 Mn1 178.04(9) . . . . ? C33 Mn2 P15 Mn1 87.86(10) . . . . ? C35 Mn2 P15 Mn1 -89.70(9) . . . . ? P1 Mn2 P15 Mn1 -0.78(3) . . . . ? C20 P15 C16 C17 46.3(2) . . . . ? Mn1 P15 C16 C17 -166.35(17) . . . . ? Mn2 P15 C16 C17 -76.4(2) . . . . ? C20 P15 C16 C27 -150.6(2) . . . . ? Mn1 P15 C16 C27 -3.2(3) . . . . ? Mn2 P15 C16 C27 86.7(2) . . . . ? C20 P15 C16 Mn4 -20.21(11) . . . . ? Mn1 P15 C16 Mn4 127.13(8) . . . . ? Mn2 P15 C16 Mn4 -142.95(6) . . . . ? C39 Mn4 C16 C17 68.31(19) . . . . ? C40 Mn4 C16 C17 -101.1(8) . . . . ? C41 Mn4 C16 C17 164.09(19) . . . . ? C19 Mn4 C16 C17 -65.74(17) . . . . ? C18 Mn4 C16 C17 -28.34(17) . . . . ? C20 Mn4 C16 C17 -102.69(18) . . . . ? C39 Mn4 C16 C27 -41.3(3) . . . . ? C40 Mn4 C16 C27 149.3(7) . . . . ? C41 Mn4 C16 C27 54.5(3) . . . . ? C17 Mn4 C16 C27 -109.6(3) . . . . ? C19 Mn4 C16 C27 -175.4(3) . . . . ? C18 Mn4 C16 C27 -138.0(3) . . . . ? C20 Mn4 C16 C27 147.7(3) . . . . ? C39 Mn4 C16 P15 -171.78(13) . . . . ? C40 Mn4 C16 P15 18.8(8) . . . . ? C41 Mn4 C16 P15 -76.00(13) . . . . ? C17 Mn4 C16 P15 119.9(2) . . . . ? C19 Mn4 C16 P15 54.16(12) . . . . ? C18 Mn4 C16 P15 91.57(12) . . . . ? C20 Mn4 C16 P15 17.21(10) . . . . ? C27 C16 C17 C18 168.4(3) . . . . ? P15 C16 C17 C18 -27.8(4) . . . . ? Mn4 C16 C17 C18 54.2(2) . . . . ? C27 C16 C17 Mn4 114.3(3) . . . . ? P15 C16 C17 Mn4 -82.00(17) . . . . ? C39 Mn4 C17 C16 -114.76(19) . . . . ? C40 Mn4 C17 C16 164.8(2) . . . . ? C41 Mn4 C17 C16 -19.0(2) . . . . ? C19 Mn4 C17 C16 105.65(18) . . . . ? C18 Mn4 C17 C16 135.1(3) . . . . ? C20 Mn4 C17 C16 69.24(17) . . . . ? C39 Mn4 C17 C18 110.13(19) . . . . ? C40 Mn4 C17 C18 29.7(3) . . . . ? C41 Mn4 C17 C18 -154.10(18) . . . . ? C19 Mn4 C17 C18 -29.47(17) . . . . ? C20 Mn4 C17 C18 -65.87(17) . . . . ? C16 Mn4 C17 C18 -135.1(3) . . . . ? C16 C17 C18 C19 -3.8(4) . . . . ? Mn4 C17 C18 C19 52.0(2) . . . . ? C16 C17 C18 C21 178.3(3) . . . . ? Mn4 C17 C18 C21 -126.0(2) . . . . ? C16 C17 C18 Mn4 -55.8(3) . . . . ? C39 Mn4 C18 C19 155.31(19) . . . . ? C40 Mn4 C18 C19 65.8(2) . . . . ? C41 Mn4 C18 C19 -75.9(3) . . . . ? C17 Mn4 C18 C19 -132.2(3) . . . . ? C20 Mn4 C18 C19 -27.29(16) . . . . ? C16 Mn4 C18 C19 -105.04(18) . . . . ? C39 Mn4 C18 C17 -72.5(2) . . . . ? C40 Mn4 C18 C17 -161.96(19) . . . . ? C41 Mn4 C18 C17 56.3(3) . . . . ? C19 Mn4 C18 C17 132.2(3) . . . . ? C20 Mn4 C18 C17 104.93(19) . . . . ? C16 Mn4 C18 C17 27.19(17) . . . . ? C39 Mn4 C18 C21 40.3(3) . . . . ? C40 Mn4 C18 C21 -49.2(3) . . . . ? C41 Mn4 C18 C21 169.1(3) . . . . ? C17 Mn4 C18 C21 112.8(3) . . . . ? C19 Mn4 C18 C21 -115.0(3) . . . . ? C20 Mn4 C18 C21 -142.3(3) . . . . ? C16 Mn4 C18 C21 140.0(3) . . . . ? C17 C18 C19 C20 3.3(4) . . . . ? C21 C18 C19 C20 -178.8(3) . . . . ? Mn4 C18 C19 C20 55.1(3) . . . . ? C17 C18 C19 Mn4 -51.8(2) . . . . ? C21 C18 C19 Mn4 126.1(3) . . . . ? C39 Mn4 C19 C20 -170.38(19) . . . . ? C40 Mn4 C19 C20 105.38(18) . . . . ? C41 Mn4 C19 C20 11.1(2) . . . . ? C17 Mn4 C19 C20 -105.47(18) . . . . ? C18 Mn4 C19 C20 -135.3(2) . . . . ? C16 Mn4 C19 C20 -69.34(16) . . . . ? C39 Mn4 C19 C18 -35.1(2) . . . . ? C40 Mn4 C19 C18 -119.32(19) . . . . ? C41 Mn4 C19 C18 146.41(18) . . . . ? C17 Mn4 C19 C18 29.84(17) . . . . ? C20 Mn4 C19 C18 135.3(2) . . . . ? C16 Mn4 C19 C18 65.96(17) . . . . ? C18 C19 C20 C28 -168.9(3) . . . . ? Mn4 C19 C20 C28 -115.0(3) . . . . ? C18 C19 C20 P15 28.9(4) . . . . ? Mn4 C19 C20 P15 82.77(18) . . . . ? C18 C19 C20 Mn4 -53.9(2) . . . . ? C16 P15 C20 C19 -46.9(2) . . . . ? Mn1 P15 C20 C19 164.94(18) . . . . ? Mn2 P15 C20 C19 72.8(2) . . . . ? C16 P15 C20 C28 151.6(2) . . . . ? Mn1 P15 C20 C28 3.4(3) . . . . ? Mn2 P15 C20 C28 -88.7(2) . . . . ? C16 P15 C20 Mn4 20.33(12) . . . . ? Mn1 P15 C20 Mn4 -127.83(8) . . . . ? Mn2 P15 C20 Mn4 140.05(6) . . . . ? C39 Mn4 C20 C19 42.6(8) . . . . ? C40 Mn4 C20 C19 -77.21(18) . . . . ? C41 Mn4 C20 C19 -171.43(17) . . . . ? C17 Mn4 C20 C19 65.85(17) . . . . ? C18 Mn4 C20 C19 27.93(16) . . . . ? C16 Mn4 C20 C19 102.53(17) . . . . ? C39 Mn4 C20 C28 151.9(7) . . . . ? C40 Mn4 C20 C28 32.0(3) . . . . ? C41 Mn4 C20 C28 -62.2(2) . . . . ? C17 Mn4 C20 C28 175.1(2) . . . . ? C19 Mn4 C20 C28 109.3(3) . . . . ? C18 Mn4 C20 C28 137.2(2) . . . . ? C16 Mn4 C20 C28 -148.2(2) . . . . ? C39 Mn4 C20 P15 -77.2(8) . . . . ? C40 Mn4 C20 P15 163.01(13) . . . . ? C41 Mn4 C20 P15 68.79(13) . . . . ? C17 Mn4 C20 P15 -53.93(12) . . . . ? C19 Mn4 C20 P15 -119.78(19) . . . . ? C18 Mn4 C20 P15 -91.85(12) . . . . ? C16 Mn4 C20 P15 -17.25(10) . . . . ? C19 C18 C21 C26 -35.0(4) . . . . ? C17 C18 C21 C26 142.9(3) . . . . ? Mn4 C18 C21 C26 54.8(4) . . . . ? C19 C18 C21 C22 143.6(3) . . . . ? C17 C18 C21 C22 -38.5(4) . . . . ? Mn4 C18 C21 C22 -126.6(3) . . . . ? C26 C21 C22 C23 -1.7(5) . . . . ? C18 C21 C22 C23 179.6(3) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C22 C23 C24 C25 1.9(6) . . . . ? C23 C24 C25 C26 -2.6(6) . . . . ? C24 C25 C26 C21 1.2(6) . . . . ? C22 C21 C26 C25 1.0(5) . . . . ? C18 C21 C26 C25 179.7(3) . . . . ? C30 Mn1 C29 O29 0.8(19) . . . . ? C31 Mn1 C29 O29 -2(2) . . . . ? P15 Mn1 C29 O29 122.1(19) . . . . ? P1 Mn1 C29 O29 -123.4(19) . . . . ? Mn2 Mn1 C29 O29 179(100) . . . . ? C29 Mn1 C30 O30 114(18) . . . . ? C31 Mn1 C30 O30 -67(18) . . . . ? P15 Mn1 C30 O30 23(19) . . . . ? P1 Mn1 C30 O30 -157(18) . . . . ? Mn2 Mn1 C30 O30 13(21) . . . . ? C30 Mn1 C31 O31 2.9(16) . . . . ? C29 Mn1 C31 O31 5.6(18) . . . . ? P15 Mn1 C31 O31 -118.2(16) . . . . ? P1 Mn1 C31 O31 126.9(16) . . . . ? Mn2 Mn1 C31 O31 -175.6(16) . . . . ? C34 Mn2 C32 O32 25(4) . . . . ? C33 Mn2 C32 O32 -65(4) . . . . ? C35 Mn2 C32 O32 118(4) . . . . ? P15 Mn2 C32 O32 -154(4) . . . . ? P1 Mn2 C32 O32 8(5) . . . . ? Mn1 Mn2 C32 O32 -152(4) . . . . ? C34 Mn2 C33 O33 -50(6) . . . . ? C32 Mn2 C33 O33 40(6) . . . . ? C35 Mn2 C33 O33 167(5) . . . . ? P15 Mn2 C33 O33 127(6) . . . . ? P1 Mn2 C33 O33 -136(6) . . . . ? Mn1 Mn2 C33 O33 175(100) . . . . ? C32 Mn2 C34 O34 -15(4) . . . . ? C33 Mn2 C34 O34 76(4) . . . . ? C35 Mn2 C34 O34 -107(4) . . . . ? P15 Mn2 C34 O34 -9(5) . . . . ? P1 Mn2 C34 O34 164(4) . . . . ? Mn1 Mn2 C34 O34 163(3) . . . . ? C34 Mn2 C35 O35 78(37) . . . . ? C32 Mn2 C35 O35 -12(37) . . . . ? C33 Mn2 C35 O35 -139(36) . . . . ? P15 Mn2 C35 O35 -99(37) . . . . ? P1 Mn2 C35 O35 164(100) . . . . ? Mn1 Mn2 C35 O35 -148(100) . . . . ? C37 Mn3 C36 O36 -144(11) . . . . ? C38 Mn3 C36 O36 -56(11) . . . . ? C5 Mn3 C36 O36 34(11) . . . . ? C3 Mn3 C36 O36 125(11) . . . . ? C4 Mn3 C36 O36 67(11) . . . . ? C2 Mn3 C36 O36 119(11) . . . . ? C6 Mn3 C36 O36 47(11) . . . . ? P1 Mn3 C36 O36 85(11) . . . . ? C38 Mn3 C37 O37 -128(48) . . . . ? C36 Mn3 C37 O37 -33(48) . . . . ? C5 Mn3 C37 O37 150(48) . . . . ? C3 Mn3 C37 O37 99(48) . . . . ? C4 Mn3 C37 O37 133(48) . . . . ? C2 Mn3 C37 O37 62(48) . . . . ? C6 Mn3 C37 O37 52(48) . . . . ? P1 Mn3 C37 O37 46(48) . . . . ? C37 Mn3 C38 O38 -51(6) . . . . ? C36 Mn3 C38 O38 -143(6) . . . . ? C5 Mn3 C38 O38 95(6) . . . . ? C3 Mn3 C38 O38 36(6) . . . . ? C4 Mn3 C38 O38 58(6) . . . . ? C2 Mn3 C38 O38 63(7) . . . . ? C6 Mn3 C38 O38 129(6) . . . . ? P1 Mn3 C38 O38 137(6) . . . . ? C40 Mn4 C39 O39 70(5) . . . . ? C41 Mn4 C39 O39 163(5) . . . . ? C17 Mn4 C39 O39 -74(5) . . . . ? C19 Mn4 C39 O39 -16(5) . . . . ? C18 Mn4 C39 O39 -37(5) . . . . ? C20 Mn4 C39 O39 -51(5) . . . . ? C16 Mn4 C39 O39 -109(5) . . . . ? C39 Mn4 C40 O40 -16(5) . . . . ? C41 Mn4 C40 O40 -112(5) . . . . ? C17 Mn4 C40 O40 65(6) . . . . ? C19 Mn4 C40 O40 119(5) . . . . ? C18 Mn4 C40 O40 84(5) . . . . ? C20 Mn4 C40 O40 156(5) . . . . ? C16 Mn4 C40 O40 154(5) . . . . ? C39 Mn4 C41 O41 112(8) . . . . ? C40 Mn4 C41 O41 -161(8) . . . . ? C17 Mn4 C41 O41 21(8) . . . . ? C19 Mn4 C41 O41 -69(8) . . . . ? C18 Mn4 C41 O41 -18(8) . . . . ? C20 Mn4 C41 O41 -62(8) . . . . ? C16 Mn4 C41 O41 10(8) . . . . ? C907 C901 C902 C903 -172.5(5) . . . . ? C903 C901 C902 C903 0.6(12) 2_655 . . . ? C901 C902 C903 C901 -0.6(11) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.350 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.058 # Attachment 'six09a.cif' data_six09a _database_code_depnum_ccdc_archive 'CCDC 602395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Mn2 O10 P2' _chemical_formula_weight 878.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 19.7993(14) _cell_length_b 27.5435(18) _cell_length_c 7.6297(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4160.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Flat plate' _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7319 _exptl_absorpt_correction_T_max 0.9640 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13989 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4014 _reflns_number_gt 2329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe Expose' _computing_cell_refinement 'Stoe Cell' _computing_data_reduction 'Stoe Integrate' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 4014 _refine_ls_number_parameters 255 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.05899(3) 0.46870(2) 0.19854(13) 0.04144(17) Uani 1 1 d . . . P1 P 0.14947(5) 0.42054(4) 0.2051(2) 0.0391(3) Uani 1 1 d . . . C2 C 0.2320(2) 0.43608(18) 0.1644(5) 0.0341(12) Uani 1 1 d . . . C3 C 0.2843(2) 0.40234(18) 0.1825(8) 0.0391(11) Uani 1 1 d . . . H3A H 0.3290 0.4134 0.1610 0.047 Uiso 1 1 calc R . . C4 C 0.2762(2) 0.35392(18) 0.2293(7) 0.0396(13) Uani 1 1 d . . . C5 C 0.2124(2) 0.3346(2) 0.2671(6) 0.0412(12) Uani 1 1 d . . . H5A H 0.2102 0.3014 0.3001 0.049 Uiso 1 1 calc R . . C6 C 0.1517(2) 0.36051(18) 0.2602(6) 0.0389(12) Uani 1 1 d . . . C7 C 0.2504(3) 0.48669(19) 0.1066(6) 0.0457(13) Uani 1 1 d . . . H7A H 0.2982 0.4876 0.0736 0.069 Uiso 1 1 calc R . . H7B H 0.2423 0.5095 0.2029 0.069 Uiso 1 1 calc R . . H7C H 0.2226 0.4959 0.0055 0.069 Uiso 1 1 calc R . . C8 C 0.0864(3) 0.3341(2) 0.3025(7) 0.0494(13) Uani 1 1 d . . . H8A H 0.0968 0.3020 0.3502 0.074 Uiso 1 1 calc R . . H8B H 0.0595 0.3306 0.1955 0.074 Uiso 1 1 calc R . . H8C H 0.0608 0.3528 0.3892 0.074 Uiso 1 1 calc R . . C9 C 0.3366(2) 0.3210(2) 0.2388(6) 0.0430(14) Uani 1 1 d . . . C10 C 0.3983(3) 0.3386(2) 0.2995(7) 0.0517(14) Uani 1 1 d . . . H10I H 0.4016 0.3713 0.3379 0.062 Uiso 1 1 calc R . . C11 C 0.4551(3) 0.3089(3) 0.3046(8) 0.0684(18) Uani 1 1 d . . . H11A H 0.4969 0.3211 0.3470 0.082 Uiso 1 1 calc R . . C12 C 0.4502(3) 0.2616(3) 0.2478(8) 0.076(2) Uani 1 1 d . . . H12A H 0.4888 0.2411 0.2513 0.091 Uiso 1 1 calc R . . C13 C 0.3898(3) 0.2439(2) 0.1859(14) 0.0757(17) Uani 1 1 d . . . H13A H 0.3869 0.2114 0.1453 0.091 Uiso 1 1 calc R . . C14 C 0.3328(3) 0.27372(19) 0.1826(11) 0.0561(14) Uani 1 1 d . . . H14A H 0.2910 0.2612 0.1412 0.067 Uiso 1 1 calc R . . O15 O -0.0355(2) 0.39525(17) 0.0481(6) 0.0724(12) Uani 1 1 d . . . C15 C 0.0020(3) 0.4246(2) 0.1053(7) 0.0491(13) Uani 1 1 d . . . O16 O 0.0185(2) 0.43805(17) 0.5600(6) 0.0707(13) Uani 1 1 d . . . C16 C 0.0331(3) 0.4510(2) 0.4189(7) 0.0524(15) Uani 1 1 d . . . O17 O 0.1318(2) 0.55443(17) 0.3435(6) 0.0709(13) Uani 1 1 d . . . C17 C 0.1022(3) 0.5208(2) 0.2886(7) 0.0497(14) Uani 1 1 d . . . O18 O 0.0907(2) 0.50370(17) -0.1634(5) 0.0678(12) Uani 1 1 d . . . C18 C 0.0775(3) 0.4900(2) -0.0207(7) 0.0520(14) Uani 1 1 d . . . O100 O 0.3224(8) 0.2031(4) 0.7756(11) 0.218(6) Uani 1 1 d . . . C101 C 0.3526(6) 0.2060(4) 0.6255(19) 0.145(5) Uani 1 1 d . . . H10A H 0.3926 0.2274 0.6357 0.174 Uiso 1 1 calc R . . H10B H 0.3216 0.2205 0.5380 0.174 Uiso 1 1 calc R . . C102 C 0.3731(6) 0.1586(4) 0.5684(15) 0.122(3) Uani 1 1 d . . . H10C H 0.4229 0.1556 0.5717 0.147 Uiso 1 1 calc R . . H10D H 0.3574 0.1525 0.4472 0.147 Uiso 1 1 calc R . . C103 C 0.3415(7) 0.1239(4) 0.6916(18) 0.149(4) Uani 1 1 d . . . H10E H 0.3763 0.1038 0.7496 0.179 Uiso 1 1 calc R . . H10F H 0.3096 0.1023 0.6292 0.179 Uiso 1 1 calc R . . C104 C 0.3054(8) 0.1542(6) 0.8217(17) 0.185(6) Uani 1 1 d . . . H10G H 0.2560 0.1490 0.8142 0.222 Uiso 1 1 calc R . . H10H H 0.3207 0.1466 0.9422 0.222 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0391(3) 0.0419(4) 0.0433(3) -0.0027(6) -0.0029(6) 0.0042(3) P1 0.0384(5) 0.0376(7) 0.0413(6) -0.0031(10) 0.0003(10) 0.0012(5) C2 0.042(2) 0.033(3) 0.027(3) -0.0002(18) 0.0018(18) -0.002(2) C3 0.038(2) 0.045(3) 0.035(3) -0.002(3) 0.001(3) 0.000(2) C4 0.039(2) 0.041(3) 0.039(4) -0.003(2) -0.002(2) 0.007(2) C5 0.042(3) 0.037(3) 0.045(3) -0.003(2) 0.001(2) 0.002(2) C6 0.038(3) 0.036(3) 0.043(3) -0.0029(19) 0.004(2) -0.006(2) C7 0.045(3) 0.042(4) 0.050(3) 0.001(2) 0.008(2) 0.003(3) C8 0.046(3) 0.044(4) 0.058(3) 0.000(3) 0.003(2) -0.004(3) C9 0.041(3) 0.046(3) 0.041(4) 0.000(2) -0.001(2) 0.009(2) C10 0.044(3) 0.060(4) 0.051(3) -0.016(3) 0.000(2) 0.009(3) C11 0.050(4) 0.083(6) 0.072(4) -0.007(4) -0.008(3) 0.019(3) C12 0.057(4) 0.076(5) 0.094(6) -0.005(4) -0.009(4) 0.033(4) C13 0.078(4) 0.056(4) 0.093(4) -0.004(6) -0.002(6) 0.020(3) C14 0.055(3) 0.044(3) 0.070(4) -0.003(4) -0.003(4) 0.011(2) O15 0.060(3) 0.062(3) 0.096(3) -0.024(3) -0.019(2) 0.002(2) C15 0.044(3) 0.052(4) 0.051(3) -0.005(3) -0.001(3) 0.006(3) O16 0.078(3) 0.080(4) 0.055(2) 0.006(2) 0.009(2) 0.016(3) C16 0.049(3) 0.054(4) 0.054(4) -0.009(3) 0.003(3) 0.006(3) O17 0.063(3) 0.052(3) 0.098(3) -0.022(2) -0.017(2) 0.004(2) C17 0.047(3) 0.051(4) 0.052(3) -0.005(3) -0.004(2) 0.010(3) O18 0.067(3) 0.083(3) 0.054(3) 0.007(2) 0.005(2) 0.006(2) C18 0.055(4) 0.048(4) 0.054(4) -0.003(3) -0.003(3) 0.005(3) O100 0.391(17) 0.179(11) 0.084(5) -0.005(6) 0.062(7) 0.122(11) C101 0.155(10) 0.090(9) 0.190(13) -0.062(8) 0.026(8) -0.017(7) C102 0.138(8) 0.090(8) 0.139(9) -0.044(7) -0.021(7) 0.009(7) C103 0.242(12) 0.110(8) 0.095(6) 0.011(9) 0.035(11) 0.030(8) C104 0.200(14) 0.232(19) 0.124(10) 0.038(11) 0.063(9) 0.011(14) _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 C15 1.804(6) . ? Mn1 C17 1.807(6) . ? Mn1 C18 1.810(6) . ? Mn1 C16 1.824(6) . ? Mn1 P1 2.2296(12) . ? Mn1 Mn1 2.9032(12) 2_565 ? P1 C6 1.707(5) . ? P1 C2 1.718(5) . ? C2 C3 1.397(6) . ? C2 C7 1.507(7) . ? C3 C4 1.390(7) . ? C4 C5 1.401(6) . ? C4 C9 1.502(6) . ? C5 C6 1.399(7) . ? C6 C8 1.518(7) . ? C9 C14 1.374(7) . ? C9 C10 1.394(7) . ? C10 C11 1.392(8) . ? C11 C12 1.374(9) . ? C12 C13 1.376(9) . ? C13 C14 1.397(7) . ? O15 C15 1.181(7) . ? O16 C16 1.171(6) . ? O17 C17 1.173(7) . ? O18 C18 1.181(6) . ? O100 C101 1.294(13) . ? O100 C104 1.432(16) . ? C101 C102 1.435(13) . ? C102 C103 1.479(14) . ? C103 C104 1.480(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Mn1 C17 168.8(3) . . ? C15 Mn1 C18 88.9(3) . . ? C17 Mn1 C18 89.9(3) . . ? C15 Mn1 C16 90.5(3) . . ? C17 Mn1 C16 89.7(3) . . ? C18 Mn1 C16 174.4(3) . . ? C15 Mn1 P1 96.36(18) . . ? C17 Mn1 P1 94.82(18) . . ? C18 Mn1 P1 92.92(19) . . ? C16 Mn1 P1 92.64(19) . . ? C15 Mn1 Mn1 84.06(18) . 2_565 ? C17 Mn1 Mn1 84.77(17) . 2_565 ? C18 Mn1 Mn1 88.30(18) . 2_565 ? C16 Mn1 Mn1 86.14(18) . 2_565 ? P1 Mn1 Mn1 178.71(6) . 2_565 ? C6 P1 C2 105.1(2) . . ? C6 P1 Mn1 127.07(17) . . ? C2 P1 Mn1 127.75(18) . . ? C3 C2 C7 117.8(4) . . ? C3 C2 P1 121.4(4) . . ? C7 C2 P1 120.9(4) . . ? C4 C3 C2 125.3(4) . . ? C3 C4 C5 121.4(4) . . ? C3 C4 C9 120.0(4) . . ? C5 C4 C9 118.6(4) . . ? C6 C5 C4 125.0(5) . . ? C5 C6 C8 118.7(4) . . ? C5 C6 P1 121.7(4) . . ? C8 C6 P1 119.6(4) . . ? C14 C9 C10 118.8(5) . . ? C14 C9 C4 120.9(4) . . ? C10 C9 C4 120.3(5) . . ? C11 C10 C9 120.9(6) . . ? C12 C11 C10 119.4(6) . . ? C11 C12 C13 120.4(5) . . ? C12 C13 C14 120.0(6) . . ? C9 C14 C13 120.5(6) . . ? O15 C15 Mn1 178.4(5) . . ? O16 C16 Mn1 177.1(5) . . ? O17 C17 Mn1 178.0(5) . . ? O18 C18 Mn1 178.9(5) . . ? C101 O100 C104 112.6(11) . . ? O100 C101 C102 110.0(13) . . ? C101 C102 C103 106.0(10) . . ? C102 C103 C104 105.4(10) . . ? O100 C104 C103 104.6(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Mn1 P1 C6 -40.2(3) . . . . ? C17 Mn1 P1 C6 140.5(3) . . . . ? C18 Mn1 P1 C6 -129.4(3) . . . . ? C16 Mn1 P1 C6 50.6(3) . . . . ? Mn1 Mn1 P1 C6 69(2) 2_565 . . . ? C15 Mn1 P1 C2 142.5(3) . . . . ? C17 Mn1 P1 C2 -36.8(3) . . . . ? C18 Mn1 P1 C2 53.3(3) . . . . ? C16 Mn1 P1 C2 -126.7(3) . . . . ? Mn1 Mn1 P1 C2 -108(2) 2_565 . . . ? C6 P1 C2 C3 -1.1(5) . . . . ? Mn1 P1 C2 C3 176.6(4) . . . . ? C6 P1 C2 C7 178.4(3) . . . . ? Mn1 P1 C2 C7 -3.9(4) . . . . ? C7 C2 C3 C4 -178.0(5) . . . . ? P1 C2 C3 C4 1.6(8) . . . . ? C2 C3 C4 C5 -1.4(9) . . . . ? C2 C3 C4 C9 178.2(5) . . . . ? C3 C4 C5 C6 0.9(8) . . . . ? C9 C4 C5 C6 -178.6(4) . . . . ? C4 C5 C6 C8 179.1(5) . . . . ? C4 C5 C6 P1 -0.7(6) . . . . ? C2 P1 C6 C5 0.8(4) . . . . ? Mn1 P1 C6 C5 -177.0(3) . . . . ? C2 P1 C6 C8 -179.1(4) . . . . ? Mn1 P1 C6 C8 3.2(5) . . . . ? C3 C4 C9 C14 -141.3(6) . . . . ? C5 C4 C9 C14 38.3(8) . . . . ? C3 C4 C9 C10 36.5(8) . . . . ? C5 C4 C9 C10 -143.9(5) . . . . ? C14 C9 C10 C11 -0.5(9) . . . . ? C4 C9 C10 C11 -178.3(5) . . . . ? C9 C10 C11 C12 0.5(9) . . . . ? C10 C11 C12 C13 0.2(11) . . . . ? C11 C12 C13 C14 -0.8(13) . . . . ? C10 C9 C14 C13 -0.2(11) . . . . ? C4 C9 C14 C13 177.6(7) . . . . ? C12 C13 C14 C9 0.8(14) . . . . ? C17 Mn1 C15 O15 -105(19) . . . . ? C18 Mn1 C15 O15 172(100) . . . . ? C16 Mn1 C15 O15 -14(19) . . . . ? P1 Mn1 C15 O15 79(19) . . . . ? Mn1 Mn1 C15 O15 -100(19) 2_565 . . . ? C15 Mn1 C16 O16 83(12) . . . . ? C17 Mn1 C16 O16 -108(12) . . . . ? C18 Mn1 C16 O16 167(10) . . . . ? P1 Mn1 C16 O16 -13(12) . . . . ? Mn1 Mn1 C16 O16 167(12) 2_565 . . . ? C15 Mn1 C17 O17 -130(14) . . . . ? C18 Mn1 C17 O17 -46(15) . . . . ? C16 Mn1 C17 O17 140(15) . . . . ? P1 Mn1 C17 O17 47(15) . . . . ? Mn1 Mn1 C17 O17 -134(15) 2_565 . . . ? C15 Mn1 C18 O18 -117(28) . . . . ? C17 Mn1 C18 O18 74(28) . . . . ? C16 Mn1 C18 O18 160(26) . . . . ? P1 Mn1 C18 O18 -21(28) . . . . ? Mn1 Mn1 C18 O18 159(28) 2_565 . . . ? C104 O100 C101 C102 -12.7(18) . . . . ? O100 C101 C102 C103 9.1(15) . . . . ? C101 C102 C103 C104 -2.2(16) . . . . ? C101 O100 C104 C103 11(2) . . . . ? C102 C103 C104 O100 -4.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.368 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.057