Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions ' _publ_section_title ; Different coordination modes of a 1,2,1',2'-ferrocenyltetraphosphine: di or tridentat behaviour with group 6 or 7 transition metals ; loop_ _publ_author_name 'Emmanuelle Andre-Bentabet' 'Roland Broussier' 'Regine Amardeil' 'Jean-Cyrille Hierso' 'P. Richard' 'Dominique Fasseur' 'Bernard Gautheron' 'Phillippe Meunier' _publ_contact_author_name 'Prof Phillippe Meunier' _publ_contact_author_address ; Prof Phillippe Meunier Laboratoire de Synthese et d'Electrosynthese Organometalliques (UMR 5632) Universite de Bourgogne 6 boulevard Gabriel Dijon 21000 FRANCE ; _publ_contact_author_email 'PHILIPPE.MEUNIER@U-BOURGOGNE.FR' data_brou2a _database_code_CSD 163669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H70 Fe Mo O3 P4' _chemical_formula_weight 1306.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'O' 'O' 0.0106 0.0060 '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' _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 15.045(3) _cell_length_b 17.246(3) _cell_length_c 25.762(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.899(14) _cell_angle_gamma 90.00 _cell_volume 6621(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.5 _cell_measurement_theta_max 18.2 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type psi-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 CAD4 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% 3 _diffrn_reflns_number 13744 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.31 _reflns_number_total 13430 _reflns_number_gt 7422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction XCAD4PC _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _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^)+(0.0614P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 13430 _refine_ls_number_parameters 720 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1645 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.009 _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 Fe Fe 0.22351(3) 1.02806(3) 0.26253(2) 0.03005(14) Uani 1 1 d . . . Mo Mo 0.34203(2) 0.829173(19) 0.198063(14) 0.03290(10) Uani 1 1 d . . . P1 P 0.41355(6) 0.96256(6) 0.20538(4) 0.0320(2) Uani 1 1 d . . . P2 P 0.22192(6) 0.91820(6) 0.15286(4) 0.0323(2) Uani 1 1 d . . . P3 P 0.30957(7) 0.84580(6) 0.29333(4) 0.0338(2) Uani 1 1 d . . . P4 P 0.35528(7) 1.02149(7) 0.38929(4) 0.0402(3) Uani 1 1 d . . . C1 C 0.2282(3) 1.1339(2) 0.22065(15) 0.0357(9) Uani 1 1 d . . . C2 C 0.3153(2) 1.1045(2) 0.23664(15) 0.0346(9) Uani 1 1 d . . . H2 H 0.3608 1.1306 0.2578 0.045 Uiso 1 1 calc R . . C3 C 0.3229(2) 1.0286(2) 0.21543(14) 0.0298(8) Uani 1 1 d . . . C4 C 0.2361(2) 1.0099(2) 0.18625(14) 0.0296(8) Uani 1 1 d . . . C5 C 0.1790(3) 1.0757(2) 0.19015(15) 0.0349(9) Uani 1 1 d . . . H5 H 0.1193 1.0796 0.1751 0.045 Uiso 1 1 calc R . . C6 C 0.2016(3) 1.2185(2) 0.22607(18) 0.0474(11) Uani 1 1 d . . . C7 C 0.1031(3) 1.2314(3) 0.2078(2) 0.0792(17) Uani 1 1 d . . . H7A H 0.0886 1.2134 0.1724 0.103 Uiso 1 1 calc R . . H7B H 0.0897 1.2857 0.2094 0.103 Uiso 1 1 calc R . . H7C H 0.0682 1.2032 0.2301 0.103 Uiso 1 1 calc R . . C8 C 0.2262(4) 1.2464(3) 0.2822(2) 0.0726(16) Uani 1 1 d . . . H8A H 0.2890 1.2378 0.2932 0.094 Uiso 1 1 calc R . . H8B H 0.1918 1.2183 0.3047 0.094 Uiso 1 1 calc R . . H8C H 0.2133 1.3008 0.2841 0.094 Uiso 1 1 calc R . . C9 C 0.2565(4) 1.2638(3) 0.1903(2) 0.0700(15) Uani 1 1 d . . . H9A H 0.3193 1.2559 0.2017 0.091 Uiso 1 1 calc R . . H9B H 0.2428 1.3181 0.1919 0.091 Uiso 1 1 calc R . . H9C H 0.2418 1.2458 0.1549 0.091 Uiso 1 1 calc R . . C10 C 0.4529(2) 1.0093(2) 0.14841(15) 0.0368(9) Uani 1 1 d . . . C11 C 0.4810(3) 0.9649(3) 0.10925(17) 0.0508(12) Uani 1 1 d . . . H11 H 0.4734 0.9113 0.1095 0.066 Uiso 1 1 calc R . . C12 C 0.5206(4) 0.9997(4) 0.0693(2) 0.0702(15) Uani 1 1 d . . . H12 H 0.5407 0.9695 0.0434 0.091 Uiso 1 1 calc R . . C13 C 0.5298(4) 1.0795(4) 0.0686(2) 0.0728(16) Uani 1 1 d . . . H13 H 0.5553 1.1031 0.0417 0.095 Uiso 1 1 calc R . . C14 C 0.5018(4) 1.1234(3) 0.1067(2) 0.0700(15) Uani 1 1 d . . . H14 H 0.5084 1.1770 0.1061 0.091 Uiso 1 1 calc R . . C15 C 0.4635(3) 1.0888(3) 0.14663(19) 0.0531(12) Uani 1 1 d . . . H15 H 0.4446 1.1194 0.1727 0.069 Uiso 1 1 calc R . . C16 C 0.5147(2) 0.9863(2) 0.25062(15) 0.0339(9) Uani 1 1 d . . . C17 C 0.5934(3) 0.9504(3) 0.24029(18) 0.0499(12) Uani 1 1 d . . . H17 H 0.5911 0.9136 0.2137 0.065 Uiso 1 1 calc R . . C18 C 0.6748(3) 0.9691(3) 0.2692(2) 0.0566(13) Uani 1 1 d . . . H18 H 0.7272 0.9454 0.2618 0.074 Uiso 1 1 calc R . . C19 C 0.6783(3) 1.0223(3) 0.3084(2) 0.0619(14) Uani 1 1 d . . . H19 H 0.7331 1.0343 0.3281 0.080 Uiso 1 1 calc R . . C20 C 0.6028(3) 1.0579(3) 0.31910(19) 0.0600(13) Uani 1 1 d . . . H20 H 0.6062 1.0952 0.3454 0.078 Uiso 1 1 calc R . . C21 C 0.5201(3) 1.0390(2) 0.29092(17) 0.0451(11) Uani 1 1 d . . . H21 H 0.4682 1.0622 0.2994 0.059 Uiso 1 1 calc R . . C22 C 0.2365(3) 0.9436(3) 0.08548(16) 0.0408(10) Uani 1 1 d . . . C23 C 0.2569(3) 1.0188(3) 0.07069(18) 0.0566(13) Uani 1 1 d . . . H23 H 0.2627 1.0585 0.0954 0.074 Uiso 1 1 calc R . . C24 C 0.2684(4) 1.0346(4) 0.0190(2) 0.0789(18) Uani 1 1 d . . . H24 H 0.2822 1.0848 0.0094 0.103 Uiso 1 1 calc R . . C25 C 0.2597(4) 0.9769(5) -0.0179(2) 0.090(2) Uani 1 1 d . . . H25 H 0.2673 0.9876 -0.0524 0.117 Uiso 1 1 calc R . . C26 C 0.2394(4) 0.9025(4) -0.0033(2) 0.0804(19) Uani 1 1 d . . . H26 H 0.2335 0.8631 -0.0281 0.105 Uiso 1 1 calc R . . C27 C 0.2279(3) 0.8864(3) 0.04786(18) 0.0597(13) Uani 1 1 d . . . H27 H 0.2142 0.8361 0.0570 0.078 Uiso 1 1 calc R . . C28 C 0.1005(2) 0.9004(2) 0.14177(15) 0.0370(10) Uani 1 1 d . . . C29 C 0.0636(3) 0.8363(3) 0.16318(18) 0.0499(11) Uani 1 1 d . . . H29 H 0.1003 0.8027 0.1847 0.065 Uiso 1 1 calc R . . C30 C -0.0279(3) 0.8219(3) 0.1527(2) 0.0739(16) Uani 1 1 d . . . H30 H -0.0521 0.7783 0.1668 0.096 Uiso 1 1 calc R . . C31 C -0.0825(3) 0.8718(4) 0.1216(2) 0.0738(17) Uani 1 1 d . . . H31 H -0.1439 0.8624 0.1152 0.096 Uiso 1 1 calc R . . C32 C -0.0477(3) 0.9350(3) 0.1000(2) 0.0619(14) Uani 1 1 d . . . H32 H -0.0853 0.9687 0.0791 0.080 Uiso 1 1 calc R . . C33 C 0.0440(3) 0.9492(3) 0.10933(17) 0.0485(11) Uani 1 1 d . . . H33 H 0.0678 0.9916 0.0937 0.063 Uiso 1 1 calc R . . C34 C 0.1098(2) 1.0018(2) 0.29974(15) 0.0355(9) Uani 1 1 d . . . C35 C 0.1766(2) 1.0418(2) 0.33385(14) 0.0359(9) Uani 1 1 d . . . H35 H 0.1680 1.0892 0.3496 0.047 Uiso 1 1 calc R . . C36 C 0.2586(2) 0.9993(2) 0.34057(14) 0.0355(9) Uani 1 1 d . . . C37 C 0.2431(2) 0.9305(2) 0.30803(14) 0.0331(9) Uani 1 1 d . . . C38 C 0.1518(2) 0.9350(2) 0.28254(15) 0.0350(9) Uani 1 1 d . . . H38 H 0.1246 0.8994 0.2583 0.046 Uiso 1 1 calc R . . C39 C 0.0090(3) 1.0175(3) 0.29230(18) 0.0464(11) Uani 1 1 d . . . C40 C -0.0351(3) 0.9967(4) 0.2385(2) 0.101(2) Uani 1 1 d . . . H40A H -0.0220 0.9436 0.2312 0.132 Uiso 1 1 calc R . . H40B H -0.0128 1.0298 0.2133 0.132 Uiso 1 1 calc R . . H40C H -0.0988 1.0033 0.2365 0.132 Uiso 1 1 calc R . . C41 C -0.0276(3) 0.9663(4) 0.3326(2) 0.093(2) Uani 1 1 d . . . H41A H 0.0008 0.9798 0.3671 0.121 Uiso 1 1 calc R . . H41B H -0.0154 0.9129 0.3256 0.121 Uiso 1 1 calc R . . H41C H -0.0912 0.9738 0.3304 0.121 Uiso 1 1 calc R . . C42 C -0.0116(4) 1.1006(3) 0.3034(3) 0.106(2) Uani 1 1 d . . . H42A H 0.0166 1.1142 0.3379 0.137 Uiso 1 1 calc R . . H42B H -0.0753 1.1072 0.3013 0.137 Uiso 1 1 calc R . . H42C H 0.0108 1.1335 0.2781 0.137 Uiso 1 1 calc R . . C43 C 0.4013(3) 0.8416(2) 0.34876(16) 0.0394(10) Uani 1 1 d . . . C44 C 0.3851(3) 0.8235(3) 0.39867(17) 0.0480(11) Uani 1 1 d . . . H44 H 0.3265 0.8136 0.4045 0.062 Uiso 1 1 calc R . . C45 C 0.4534(4) 0.8196(3) 0.44048(18) 0.0604(13) Uani 1 1 d . . . H45 H 0.4406 0.8075 0.4738 0.078 Uiso 1 1 calc R . . C46 C 0.5397(4) 0.8338(3) 0.4324(2) 0.0647(15) Uani 1 1 d . . . H46 H 0.5857 0.8330 0.4604 0.084 Uiso 1 1 calc R . . C47 C 0.5589(3) 0.8495(3) 0.3821(2) 0.0631(14) Uani 1 1 d . . . H47 H 0.6179 0.8577 0.3765 0.082 Uiso 1 1 calc R . . C48 C 0.4899(3) 0.8529(2) 0.34039(18) 0.0479(11) Uani 1 1 d . . . H48 H 0.5029 0.8627 0.3068 0.062 Uiso 1 1 calc R . . C49 C 0.2427(3) 0.7637(2) 0.31529(16) 0.0452(11) Uani 1 1 d . . . H49 H 0.2699 0.8068 0.3025 0.059 Uiso 1 1 calc R . . C50 C 0.1681(3) 0.7728(3) 0.34017(18) 0.0548(12) Uani 1 1 d . . . H50 H 0.1445 0.8219 0.3443 0.071 Uiso 1 1 calc R . . C51 C 0.1284(4) 0.7075(4) 0.3592(2) 0.0752(17) Uani 1 1 d . . . H51 H 0.0778 0.7131 0.3758 0.098 Uiso 1 1 calc R . . C52 C 0.1632(5) 0.6354(4) 0.3535(2) 0.0805(19) Uani 1 1 d . . . H52 H 0.1364 0.5923 0.3665 0.105 Uiso 1 1 calc R . . C53 C 0.2368(5) 0.6263(3) 0.3290(2) 0.0810(18) Uani 1 1 d . . . H53 H 0.2604 0.5771 0.3253 0.105 Uiso 1 1 calc R . . C54 C 0.2770(4) 0.6910(3) 0.30936(19) 0.0601(14) Uani 1 1 d . . . H54 H 0.3271 0.6848 0.2923 0.078 Uiso 1 1 calc R . . C55 C 0.3157(3) 0.9821(3) 0.44772(16) 0.0471(11) Uani 1 1 d . . . C56 C 0.3711(4) 0.9929(3) 0.49523(19) 0.0709(15) Uani 1 1 d . . . H56 H 0.4229 1.0223 0.4956 0.092 Uiso 1 1 calc R . . C57 C 0.3523(5) 0.9621(4) 0.5408(2) 0.105(2) Uani 1 1 d . . . H57 H 0.3896 0.9717 0.5720 0.137 Uiso 1 1 calc R . . C58 C 0.2777(6) 0.9169(4) 0.5403(2) 0.112(3) Uani 1 1 d . . . H58 H 0.2662 0.8929 0.5710 0.146 Uiso 1 1 calc R . . C59 C 0.2186(5) 0.9062(4) 0.4944(2) 0.090(2) Uani 1 1 d . . . H59 H 0.1665 0.8773 0.4948 0.117 Uiso 1 1 calc R . . C60 C 0.2376(4) 0.9387(3) 0.44780(19) 0.0614(14) Uani 1 1 d . . . H60 H 0.1985 0.9316 0.4169 0.080 Uiso 1 1 calc R . . C61 C 0.3392(3) 1.1255(3) 0.40244(16) 0.0469(11) Uani 1 1 d . . . C62 C 0.2734(3) 1.1548(3) 0.42925(18) 0.0556(12) Uani 1 1 d . . . H62 H 0.2313 1.1214 0.4403 0.072 Uiso 1 1 calc R . . C63 C 0.2692(4) 1.2326(3) 0.4398(2) 0.0676(15) Uani 1 1 d . . . H63 H 0.2251 1.2512 0.4586 0.088 Uiso 1 1 calc R . . C64 C 0.3286(4) 1.2823(3) 0.4231(2) 0.0787(17) Uani 1 1 d . . . H64 H 0.3245 1.3350 0.4300 0.102 Uiso 1 1 calc R . . C65 C 0.3952(4) 1.2557(3) 0.3961(3) 0.0812(18) Uani 1 1 d . . . H65 H 0.4362 1.2901 0.3849 0.106 Uiso 1 1 calc R . . C66 C 0.4004(3) 1.1774(3) 0.3859(2) 0.0621(14) Uani 1 1 d . . . H66 H 0.4454 1.1591 0.3676 0.081 Uiso 1 1 calc R . . O1 O 0.3881(2) 0.7699(2) 0.09087(15) 0.0802(12) Uani 1 1 d . . . O2 O 0.5111(2) 0.7301(2) 0.23779(15) 0.0735(11) Uani 1 1 d . . . O3 O 0.2185(2) 0.68425(19) 0.17814(16) 0.0745(11) Uani 1 1 d . . . C67 C 0.3712(3) 0.7969(3) 0.12930(19) 0.0478(11) Uani 1 1 d . . . C68 C 0.4485(3) 0.7676(2) 0.22548(17) 0.0452(11) Uani 1 1 d . . . C69 C 0.2651(3) 0.7371(3) 0.18851(19) 0.0488(11) Uani 1 1 d . . . C70 C 0.0433(9) 1.3369(9) 0.5344(5) 0.240(6) Uiso 1 1 d . . . C71 C 0.0498(6) 1.2605(4) 0.5211(3) 0.187(4) Uiso 1 1 d G . . C72 C 0.1047(5) 1.2053(6) 0.5467(3) 0.196(5) Uiso 1 1 d G . . H72 H 0.1435 1.2183 0.5767 0.255 Uiso 1 1 calc R . . C73 C 0.1023(5) 1.1308(5) 0.5281(3) 0.216(5) Uiso 1 1 d G . . H73 H 0.1396 1.0933 0.5455 0.281 Uiso 1 1 calc R . . C74 C 0.0452(6) 1.1116(4) 0.4840(3) 0.195(5) Uiso 1 1 d G . . H74 H 0.0436 1.0610 0.4715 0.253 Uiso 1 1 calc R . . C75 C -0.0096(5) 1.1668(5) 0.4584(3) 0.202(5) Uiso 1 1 d G . . H75 H -0.0485 1.1537 0.4284 0.263 Uiso 1 1 calc R . . C76 C -0.0073(5) 1.2412(5) 0.4769(3) 0.166(4) Uiso 1 1 d G . . H76 H -0.0446 1.2787 0.4595 0.216 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 Fe 0.0275(3) 0.0272(3) 0.0356(3) -0.0002(2) 0.0047(2) 0.0015(2) Mo 0.02851(18) 0.02678(18) 0.0430(2) -0.00344(17) 0.00343(14) 0.00080(15) P1 0.0256(5) 0.0298(5) 0.0408(6) -0.0009(5) 0.0056(4) -0.0001(4) P2 0.0292(5) 0.0318(6) 0.0355(6) -0.0020(5) 0.0027(4) -0.0008(4) P3 0.0315(5) 0.0264(6) 0.0428(6) 0.0027(5) 0.0029(5) 0.0004(4) P4 0.0377(6) 0.0403(7) 0.0416(6) -0.0049(5) 0.0017(5) 0.0022(5) C1 0.034(2) 0.030(2) 0.044(2) 0.0045(19) 0.0094(18) 0.0016(18) C2 0.033(2) 0.028(2) 0.042(2) 0.0004(18) 0.0039(18) -0.0034(17) C3 0.0256(19) 0.028(2) 0.035(2) 0.0037(17) 0.0035(15) -0.0005(16) C4 0.0296(19) 0.029(2) 0.029(2) 0.0025(17) 0.0027(16) -0.0010(16) C5 0.033(2) 0.032(2) 0.039(2) 0.0033(19) 0.0039(17) 0.0023(18) C6 0.046(3) 0.030(2) 0.065(3) 0.001(2) 0.002(2) 0.005(2) C7 0.058(3) 0.043(3) 0.131(5) 0.000(3) -0.005(3) 0.018(3) C8 0.090(4) 0.045(3) 0.081(4) -0.016(3) 0.007(3) 0.018(3) C9 0.085(4) 0.031(3) 0.095(4) 0.013(3) 0.016(3) -0.003(3) C10 0.029(2) 0.037(2) 0.045(2) 0.001(2) 0.0057(18) 0.0031(18) C11 0.055(3) 0.046(3) 0.054(3) 0.000(2) 0.016(2) 0.003(2) C12 0.082(4) 0.078(4) 0.058(3) 0.006(3) 0.038(3) 0.010(3) C13 0.077(4) 0.084(4) 0.064(4) 0.020(3) 0.032(3) -0.009(3) C14 0.085(4) 0.049(3) 0.083(4) 0.013(3) 0.034(3) -0.014(3) C15 0.055(3) 0.043(3) 0.065(3) 0.001(2) 0.020(2) -0.005(2) C16 0.027(2) 0.031(2) 0.042(2) 0.0033(19) 0.0003(17) -0.0067(17) C17 0.034(2) 0.051(3) 0.064(3) -0.009(2) 0.005(2) 0.002(2) C18 0.032(2) 0.057(3) 0.079(4) 0.002(3) 0.002(2) 0.005(2) C19 0.043(3) 0.052(3) 0.083(4) 0.008(3) -0.019(3) -0.007(2) C20 0.062(3) 0.048(3) 0.063(3) -0.009(3) -0.017(3) 0.002(3) C21 0.041(2) 0.041(3) 0.051(3) -0.001(2) -0.001(2) 0.007(2) C22 0.032(2) 0.052(3) 0.037(2) -0.003(2) 0.0025(18) 0.002(2) C23 0.047(3) 0.072(4) 0.049(3) 0.012(3) 0.001(2) 0.004(2) C24 0.076(4) 0.103(5) 0.059(4) 0.036(4) 0.017(3) -0.003(3) C25 0.072(4) 0.159(8) 0.041(3) 0.015(4) 0.012(3) 0.016(4) C26 0.073(4) 0.127(6) 0.041(3) -0.014(4) 0.009(3) 0.014(4) C27 0.053(3) 0.078(4) 0.047(3) -0.009(3) 0.002(2) 0.008(3) C28 0.030(2) 0.037(2) 0.045(2) -0.008(2) 0.0057(18) -0.0050(18) C29 0.045(3) 0.040(3) 0.065(3) -0.004(2) 0.010(2) -0.005(2) C30 0.050(3) 0.062(4) 0.113(5) -0.010(3) 0.024(3) -0.022(3) C31 0.035(3) 0.080(4) 0.104(5) -0.029(4) 0.001(3) -0.006(3) C32 0.040(3) 0.068(4) 0.073(4) -0.012(3) -0.008(2) 0.008(3) C33 0.038(2) 0.048(3) 0.057(3) -0.007(2) 0.000(2) -0.001(2) C34 0.030(2) 0.036(2) 0.042(2) 0.0052(19) 0.0101(18) 0.0041(18) C35 0.039(2) 0.037(2) 0.034(2) -0.0039(18) 0.0121(18) 0.0049(18) C36 0.035(2) 0.037(2) 0.034(2) 0.0001(19) 0.0048(17) 0.0008(18) C37 0.032(2) 0.032(2) 0.036(2) 0.0056(18) 0.0077(17) 0.0044(17) C38 0.035(2) 0.035(2) 0.035(2) 0.0035(18) 0.0040(18) -0.0018(18) C39 0.029(2) 0.052(3) 0.060(3) -0.004(2) 0.011(2) 0.004(2) C40 0.036(3) 0.187(7) 0.076(4) -0.027(4) -0.008(3) 0.025(4) C41 0.040(3) 0.127(6) 0.119(5) 0.038(4) 0.030(3) -0.006(3) C42 0.049(3) 0.076(4) 0.194(7) -0.016(5) 0.026(4) 0.025(3) C43 0.044(2) 0.023(2) 0.049(3) 0.0006(19) -0.003(2) 0.0065(18) C44 0.050(3) 0.042(3) 0.050(3) -0.004(2) 0.001(2) 0.008(2) C45 0.075(4) 0.059(3) 0.044(3) -0.003(2) -0.002(3) 0.019(3) C46 0.066(3) 0.053(3) 0.065(4) -0.014(3) -0.028(3) 0.015(3) C47 0.048(3) 0.058(3) 0.078(4) 0.000(3) -0.012(3) 0.000(2) C48 0.045(3) 0.035(2) 0.062(3) 0.003(2) 0.001(2) 0.000(2) C49 0.051(3) 0.033(2) 0.050(3) 0.011(2) 0.000(2) -0.013(2) C50 0.052(3) 0.050(3) 0.061(3) 0.019(3) 0.004(2) -0.009(2) C51 0.059(3) 0.094(5) 0.070(4) 0.032(3) 0.001(3) -0.025(3) C52 0.099(5) 0.064(4) 0.073(4) 0.029(3) -0.011(3) -0.040(4) C53 0.126(6) 0.034(3) 0.078(4) 0.007(3) -0.002(4) -0.016(3) C54 0.084(4) 0.032(3) 0.063(3) 0.003(2) 0.007(3) -0.002(2) C55 0.060(3) 0.043(3) 0.037(2) -0.002(2) 0.002(2) 0.010(2) C56 0.086(4) 0.077(4) 0.047(3) 0.004(3) -0.001(3) 0.001(3) C57 0.150(7) 0.110(6) 0.049(4) 0.013(4) -0.011(4) -0.013(5) C58 0.180(8) 0.103(6) 0.054(4) 0.029(4) 0.018(5) -0.011(6) C59 0.117(5) 0.089(5) 0.068(4) 0.003(4) 0.025(4) -0.023(4) C60 0.075(4) 0.066(4) 0.045(3) 0.003(3) 0.018(3) -0.005(3) C61 0.047(3) 0.048(3) 0.044(3) -0.008(2) 0.001(2) 0.003(2) C62 0.057(3) 0.053(3) 0.058(3) -0.012(2) 0.014(2) 0.001(2) C63 0.069(4) 0.061(4) 0.073(4) -0.020(3) 0.011(3) 0.017(3) C64 0.080(4) 0.039(3) 0.113(5) -0.024(3) 0.002(4) -0.002(3) C65 0.059(3) 0.048(3) 0.137(6) -0.022(4) 0.013(3) -0.008(3) C66 0.046(3) 0.050(3) 0.091(4) -0.016(3) 0.012(3) -0.006(2) O1 0.071(2) 0.096(3) 0.077(3) -0.042(2) 0.021(2) 0.004(2) O2 0.054(2) 0.056(2) 0.106(3) -0.005(2) -0.0063(19) 0.0252(18) O3 0.053(2) 0.043(2) 0.124(3) -0.015(2) 0.000(2) -0.0131(17) C67 0.038(2) 0.047(3) 0.058(3) -0.014(2) 0.006(2) 0.000(2) C68 0.041(2) 0.035(2) 0.060(3) -0.008(2) 0.006(2) 0.003(2) C69 0.035(2) 0.036(3) 0.074(3) -0.003(2) 0.002(2) 0.001(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 Fe C4 2.024(4) . ? Fe C38 2.038(4) . ? Fe C37 2.049(4) . ? Fe C3 2.051(4) . ? Fe C5 2.063(4) . ? Fe C36 2.068(4) . ? Fe C35 2.071(4) . ? Fe C2 2.084(4) . ? Fe C34 2.122(4) . ? Fe C1 2.127(4) . ? Mo C69 1.961(4) . ? Mo C67 1.963(5) . ? Mo C68 1.971(4) . ? Mo P2 2.5299(11) . ? Mo P1 2.5355(11) . ? Mo P3 2.5835(12) . ? P1 C3 1.822(4) . ? P1 C16 1.832(4) . ? P1 C10 1.842(4) . ? P2 C4 1.799(4) . ? P2 C22 1.833(4) . ? P2 C28 1.836(4) . ? P3 C37 1.838(4) . ? P3 C43 1.846(4) . ? P3 C49 1.869(4) . ? P4 C55 1.824(5) . ? P4 C36 1.827(4) . ? P4 C61 1.848(5) . ? C1 C2 1.412(5) . ? C1 C5 1.419(5) . ? C1 C6 1.524(5) . ? C2 C3 1.430(5) . ? C3 C4 1.451(5) . ? C4 C5 1.435(5) . ? C6 C7 1.508(6) . ? C6 C8 1.521(6) . ? C6 C9 1.535(6) . ? C10 C11 1.379(6) . ? C10 C15 1.381(6) . ? C11 C12 1.394(6) . ? C12 C13 1.384(8) . ? C13 C14 1.352(7) . ? C14 C15 1.381(6) . ? C16 C21 1.375(5) . ? C16 C17 1.393(5) . ? C17 C18 1.381(6) . ? C18 C19 1.362(6) . ? C19 C20 1.352(6) . ? C20 C21 1.390(6) . ? C22 C27 1.377(6) . ? C22 C23 1.398(6) . ? C23 C24 1.394(6) . ? C24 C25 1.369(8) . ? C25 C26 1.382(9) . ? C26 C27 1.380(7) . ? C28 C29 1.386(6) . ? C28 C33 1.390(6) . ? C29 C30 1.388(6) . ? C30 C31 1.369(7) . ? C31 C32 1.361(7) . ? C32 C33 1.389(6) . ? C34 C38 1.414(5) . ? C34 C35 1.419(5) . ? C34 C39 1.526(5) . ? C35 C36 1.425(5) . ? C36 C37 1.453(5) . ? C37 C38 1.441(5) . ? C39 C40 1.496(6) . ? C39 C42 1.501(7) . ? C39 C41 1.522(6) . ? C43 C44 1.377(6) . ? C43 C48 1.393(6) . ? C44 C45 1.385(6) . ? C45 C46 1.366(7) . ? C46 C47 1.390(7) . ? C47 C48 1.390(6) . ? C49 C54 1.372(6) . ? C49 C50 1.376(6) . ? C50 C51 1.394(7) . ? C51 C52 1.365(8) . ? C52 C53 1.356(8) . ? C53 C54 1.397(7) . ? C55 C60 1.392(6) . ? C55 C56 1.396(6) . ? C56 C57 1.354(8) . ? C57 C58 1.366(9) . ? C58 C59 1.391(9) . ? C59 C60 1.390(7) . ? C61 C62 1.379(6) . ? C61 C66 1.393(6) . ? C62 C63 1.371(7) . ? C63 C64 1.350(7) . ? C64 C65 1.374(8) . ? C65 C66 1.380(7) . ? O1 C67 1.153(5) . ? O2 C68 1.151(5) . ? O3 C69 1.157(5) . ? C70 C71 1.369(15) . ? C71 C76 1.369(4) . ? C71 C72 1.369(4) . ? C72 C73 1.369(4) . ? C73 C74 1.368(4) . ? C74 C75 1.369(4) . ? C75 C76 1.369(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 C4 Fe C38 104.31(15) . . ? C4 Fe C37 113.78(15) . . ? C38 Fe C37 41.29(14) . . ? C4 Fe C3 41.70(14) . . ? C38 Fe C3 127.37(15) . . ? C37 Fe C3 106.40(15) . . ? C4 Fe C5 41.10(14) . . ? C38 Fe C5 115.15(15) . . ? C37 Fe C5 147.96(16) . . ? C3 Fe C5 68.67(15) . . ? C4 Fe C36 149.49(15) . . ? C38 Fe C36 68.80(15) . . ? C37 Fe C36 41.34(15) . . ? C3 Fe C36 117.83(15) . . ? C5 Fe C36 169.10(16) . . ? C4 Fe C35 165.44(15) . . ? C38 Fe C35 66.97(16) . . ? C37 Fe C35 68.06(15) . . ? C3 Fe C35 152.84(15) . . ? C5 Fe C35 130.40(15) . . ? C36 Fe C35 40.29(14) . . ? C4 Fe C2 68.45(15) . . ? C38 Fe C2 167.33(15) . . ? C37 Fe C2 130.75(15) . . ? C3 Fe C2 40.44(14) . . ? C5 Fe C2 66.79(15) . . ? C36 Fe C2 111.78(15) . . ? C35 Fe C2 122.23(16) . . ? C4 Fe C34 126.47(15) . . ? C38 Fe C34 39.68(15) . . ? C37 Fe C34 68.17(14) . . ? C3 Fe C34 165.21(15) . . ? C5 Fe C34 108.15(15) . . ? C36 Fe C34 67.87(15) . . ? C35 Fe C34 39.55(14) . . ? C2 Fe C34 152.94(15) . . ? C4 Fe C1 68.04(15) . . ? C38 Fe C1 149.28(15) . . ? C37 Fe C1 169.42(15) . . ? C3 Fe C1 67.56(14) . . ? C5 Fe C1 39.54(14) . . ? C36 Fe C1 132.64(16) . . ? C35 Fe C1 113.02(15) . . ? C2 Fe C1 39.18(14) . . ? C34 Fe C1 119.84(15) . . ? C69 Mo C67 81.86(19) . . ? C69 Mo C68 92.59(17) . . ? C67 Mo C68 84.20(18) . . ? C69 Mo P2 93.54(13) . . ? C67 Mo P2 89.48(13) . . ? C68 Mo P2 170.49(13) . . ? C69 Mo P1 168.91(12) . . ? C67 Mo P1 100.32(13) . . ? C68 Mo P1 98.43(12) . . ? P2 Mo P1 75.68(3) . . ? C69 Mo P3 91.35(14) . . ? C67 Mo P3 169.61(14) . . ? C68 Mo P3 88.28(13) . . ? P2 Mo P3 98.84(4) . . ? P1 Mo P3 87.85(3) . . ? C3 P1 C16 110.07(18) . . ? C3 P1 C10 99.72(17) . . ? C16 P1 C10 94.54(17) . . ? C3 P1 Mo 105.01(12) . . ? C16 P1 Mo 123.84(13) . . ? C10 P1 Mo 121.16(14) . . ? C4 P2 C22 102.76(19) . . ? C4 P2 C28 105.72(17) . . ? C22 P2 C28 97.99(18) . . ? C4 P2 Mo 106.47(12) . . ? C22 P2 Mo 114.21(13) . . ? C28 P2 Mo 127.08(14) . . ? C37 P3 C43 103.96(18) . . ? C37 P3 C49 102.08(19) . . ? C43 P3 C49 96.46(18) . . ? C37 P3 Mo 117.58(12) . . ? C43 P3 Mo 120.79(14) . . ? C49 P3 Mo 112.54(14) . . ? C55 P4 C36 99.7(2) . . ? C55 P4 C61 98.3(2) . . ? C36 P4 C61 102.55(19) . . ? C2 C1 C5 107.5(3) . . ? C2 C1 C6 124.2(4) . . ? C5 C1 C6 127.1(4) . . ? C2 C1 Fe 68.8(2) . . ? C5 C1 Fe 67.8(2) . . ? C6 C1 Fe 138.4(3) . . ? C1 C2 C3 109.7(3) . . ? C1 C2 Fe 72.0(2) . . ? C3 C2 Fe 68.5(2) . . ? C2 C3 C4 106.7(3) . . ? C2 C3 P1 136.6(3) . . ? C4 C3 P1 115.2(3) . . ? C2 C3 Fe 71.0(2) . . ? C4 C3 Fe 68.2(2) . . ? P1 C3 Fe 134.6(2) . . ? C5 C4 C3 107.1(3) . . ? C5 C4 P2 134.1(3) . . ? C3 C4 P2 118.8(3) . . ? C5 C4 Fe 70.9(2) . . ? C3 C4 Fe 70.1(2) . . ? P2 C4 Fe 125.4(2) . . ? C1 C5 C4 109.0(3) . . ? C1 C5 Fe 72.6(2) . . ? C4 C5 Fe 68.0(2) . . ? C7 C6 C8 110.5(4) . . ? C7 C6 C1 111.9(4) . . ? C8 C6 C1 110.9(4) . . ? C7 C6 C9 109.0(4) . . ? C8 C6 C9 109.2(4) . . ? C1 C6 C9 105.2(4) . . ? C11 C10 C15 118.6(4) . . ? C11 C10 P1 120.3(3) . . ? C15 C10 P1 120.8(3) . . ? C10 C11 C12 120.4(5) . . ? C13 C12 C11 119.5(5) . . ? C14 C13 C12 120.3(5) . . ? C13 C14 C15 120.2(5) . . ? C14 C15 C10 121.0(5) . . ? C21 C16 C17 118.3(4) . . ? C21 C16 P1 125.9(3) . . ? C17 C16 P1 115.7(3) . . ? C18 C17 C16 120.5(4) . . ? C19 C18 C17 119.9(4) . . ? C20 C19 C18 120.6(4) . . ? C19 C20 C21 120.3(5) . . ? C16 C21 C20 120.4(4) . . ? C27 C22 C23 118.4(4) . . ? C27 C22 P2 118.9(4) . . ? C23 C22 P2 122.6(3) . . ? C24 C23 C22 120.2(5) . . ? C25 C24 C23 120.5(6) . . ? C24 C25 C26 119.3(5) . . ? C27 C26 C25 120.5(6) . . ? C22 C27 C26 121.0(5) . . ? C29 C28 C33 118.5(4) . . ? C29 C28 P2 121.1(3) . . ? C33 C28 P2 120.4(3) . . ? C28 C29 C30 120.4(5) . . ? C31 C30 C29 120.0(5) . . ? C32 C31 C30 120.6(5) . . ? C31 C32 C33 120.0(5) . . ? C32 C33 C28 120.5(5) . . ? C38 C34 C35 106.3(3) . . ? C38 C34 C39 125.8(4) . . ? C35 C34 C39 126.7(4) . . ? C38 C34 Fe 67.0(2) . . ? C35 C34 Fe 68.3(2) . . ? C39 C34 Fe 139.0(3) . . ? C34 C35 C36 110.7(4) . . ? C34 C35 Fe 72.2(2) . . ? C36 C35 Fe 69.7(2) . . ? C35 C36 C37 106.4(3) . . ? C35 C36 P4 124.8(3) . . ? C37 C36 P4 128.1(3) . . ? C35 C36 Fe 70.0(2) . . ? C37 C36 Fe 68.6(2) . . ? P4 C36 Fe 133.7(2) . . ? C38 C37 C36 106.6(3) . . ? C38 C37 P3 117.4(3) . . ? C36 C37 P3 136.0(3) . . ? C38 C37 Fe 69.0(2) . . ? C36 C37 Fe 70.0(2) . . ? P3 C37 Fe 125.06(19) . . ? C34 C38 C37 110.0(3) . . ? C34 C38 Fe 73.4(2) . . ? C37 C38 Fe 69.8(2) . . ? C40 C39 C42 109.2(5) . . ? C40 C39 C41 109.7(5) . . ? C42 C39 C41 108.7(5) . . ? C40 C39 C34 112.3(4) . . ? C42 C39 C34 111.9(4) . . ? C41 C39 C34 104.9(4) . . ? C44 C43 C48 118.2(4) . . ? C44 C43 P3 121.5(3) . . ? C48 C43 P3 120.3(3) . . ? C43 C44 C45 122.0(5) . . ? C46 C45 C44 119.5(5) . . ? C45 C46 C47 120.0(4) . . ? C48 C47 C46 120.0(5) . . ? C47 C48 C43 120.2(5) . . ? C54 C49 C50 120.0(4) . . ? C54 C49 P3 115.6(4) . . ? C50 C49 P3 124.2(4) . . ? C49 C50 C51 119.1(5) . . ? C52 C51 C50 120.6(6) . . ? C53 C52 C51 120.3(5) . . ? C52 C53 C54 119.9(6) . . ? C49 C54 C53 120.1(5) . . ? C60 C55 C56 118.2(5) . . ? C60 C55 P4 124.9(3) . . ? C56 C55 P4 116.8(4) . . ? C57 C56 C55 122.5(6) . . ? C56 C57 C58 119.0(6) . . ? C57 C58 C59 120.9(6) . . ? C60 C59 C58 119.8(6) . . ? C59 C60 C55 119.5(5) . . ? C62 C61 C66 118.0(4) . . ? C62 C61 P4 124.7(4) . . ? C66 C61 P4 117.3(3) . . ? C63 C62 C61 120.9(5) . . ? C64 C63 C62 120.5(5) . . ? C63 C64 C65 120.7(5) . . ? C64 C65 C66 119.2(5) . . ? C65 C66 C61 120.8(5) . . ? O1 C67 Mo 172.7(4) . . ? O2 C68 Mo 175.0(4) . . ? O3 C69 Mo 173.9(4) . . ? C70 C71 C76 112.6(10) . . ? C70 C71 C72 127.4(10) . . ? C76 C71 C72 120.0 . . ? C73 C72 C71 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.633 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.087 data_brou3 _database_code_CSD 163670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H79 Fe Mn O P4' _chemical_formula_weight 1255.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'O' 'O' 0.0106 0.0060 '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' _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 11.390(3) _cell_length_b 24.300(8) _cell_length_c 24.760(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.91(3) _cell_angle_gamma 90.00 _cell_volume 6680(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.7 _cell_measurement_theta_max 18.2 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type psi-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 CAD4 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9146 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.1889 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 22.78 _reflns_number_total 8664 _reflns_number_gt 4126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction XCAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _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^)+(0.0929P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 8664 _refine_ls_number_parameters 732 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2058 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1979 _refine_ls_wR_factor_gt 0.1549 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.265 _refine_ls_shift/su_mean 0.007 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 Fe Fe 0.61288(9) 0.77879(4) 0.50097(4) 0.0393(3) Uani 1 1 d . . . Mn Mn 0.56533(11) 0.69034(6) 0.34174(5) 0.0577(4) Uani 1 1 d . . . O O 0.3527(5) 0.6575(3) 0.3812(2) 0.0751(19) Uani 1 1 d . . . C77 C 0.4407(8) 0.6703(3) 0.3689(3) 0.054(2) Uani 1 1 d . . . P1 P 0.52710(19) 0.63424(9) 0.50908(9) 0.0478(6) Uani 1 1 d . . . P2 P 0.70904(18) 0.67946(9) 0.41934(9) 0.0479(6) Uani 1 1 d . . . P3 P 0.51661(18) 0.77814(10) 0.35366(8) 0.0497(6) Uani 1 1 d . . . P4 P 0.7207(2) 0.88953(9) 0.43117(9) 0.0538(6) Uani 1 1 d . . . C1 C 0.7554(7) 0.7601(3) 0.5696(3) 0.042(2) Uani 1 1 d . . . C2 C 0.6512(6) 0.7283(3) 0.5694(3) 0.043(2) Uani 1 1 d . . . H2 H 0.6093 0.7282 0.5976 0.056 Uiso 1 1 calc R . . C3 C 0.6197(6) 0.6962(3) 0.5200(3) 0.0408(19) Uani 1 1 d . . . C4 C 0.7047(6) 0.7104(3) 0.4865(3) 0.0418(19) Uani 1 1 d . . . C5 C 0.7855(6) 0.7492(3) 0.5184(3) 0.0419(19) Uani 1 1 d . . . H5 H 0.8498 0.7653 0.5068 0.054 Uiso 1 1 calc R . . C6 C 0.8316(8) 0.7900(4) 0.6191(3) 0.058(2) Uani 1 1 d . . . C7 C 0.8516(10) 0.7522(5) 0.6685(4) 0.110(4) Uani 1 1 d . . . H7A H 0.8897 0.7190 0.6602 0.143 Uiso 1 1 calc R . . H7B H 0.7755 0.7434 0.6770 0.143 Uiso 1 1 calc R . . H7C H 0.9023 0.7701 0.6997 0.143 Uiso 1 1 calc R . . C8 C 0.9541(10) 0.8034(5) 0.6100(4) 0.119(4) Uani 1 1 d . . . H8A H 0.9463 0.8275 0.5787 0.155 Uiso 1 1 calc R . . H8B H 0.9936 0.7701 0.6031 0.155 Uiso 1 1 calc R . . H8C H 1.0008 0.8212 0.6423 0.155 Uiso 1 1 calc R . . C9 C 0.7721(11) 0.8416(5) 0.6336(5) 0.152(6) Uani 1 1 d . . . H9A H 0.7585 0.8664 0.6027 0.197 Uiso 1 1 calc R . . H9B H 0.8234 0.8589 0.6651 0.197 Uiso 1 1 calc R . . H9C H 0.6965 0.8324 0.6423 0.197 Uiso 1 1 calc R . . C10 C 0.4050(7) 0.6471(3) 0.5450(4) 0.050(2) Uani 1 1 d . . . C11 C 0.2899(8) 0.6498(4) 0.5131(4) 0.068(3) Uani 1 1 d . . . H11 H 0.2782 0.6477 0.4748 0.088 Uiso 1 1 calc R . . C12 C 0.1901(8) 0.6554(4) 0.5365(5) 0.085(3) Uani 1 1 d . . . H12 H 0.1125 0.6567 0.5144 0.111 Uiso 1 1 calc R . . C13 C 0.2094(11) 0.6590(4) 0.5929(6) 0.085(3) Uani 1 1 d . . . H13 H 0.1438 0.6631 0.6091 0.111 Uiso 1 1 calc R . . C14 C 0.3222(10) 0.6566(4) 0.6259(4) 0.079(3) Uani 1 1 d . . . H14 H 0.3335 0.6588 0.6642 0.103 Uiso 1 1 calc R . . C15 C 0.4184(8) 0.6510(4) 0.6018(4) 0.062(2) Uani 1 1 d . . . H15 H 0.4955 0.6496 0.6243 0.080 Uiso 1 1 calc R . . C16 C 0.6205(8) 0.5886(3) 0.5604(3) 0.054(2) Uani 1 1 d . . . C17 C 0.7310(8) 0.6004(4) 0.5943(4) 0.070(3) Uani 1 1 d . . . H17 H 0.7630 0.6357 0.5949 0.091 Uiso 1 1 calc R . . C18 C 0.7939(10) 0.5597(5) 0.6274(4) 0.094(4) Uani 1 1 d . . . H18 H 0.8679 0.5682 0.6505 0.122 Uiso 1 1 calc R . . C19 C 0.7501(14) 0.5065(6) 0.6271(6) 0.113(5) Uani 1 1 d . . . H19 H 0.7951 0.4790 0.6483 0.147 Uiso 1 1 calc R . . C20 C 0.6420(13) 0.4959(5) 0.5957(6) 0.109(4) Uani 1 1 d . . . H20 H 0.6089 0.4610 0.5966 0.142 Uiso 1 1 calc R . . C21 C 0.5786(9) 0.5352(4) 0.5624(4) 0.084(3) Uani 1 1 d . . . H21 H 0.5042 0.5259 0.5401 0.109 Uiso 1 1 calc R . . C22 C 0.8571(7) 0.7014(4) 0.4095(3) 0.050(2) Uani 1 1 d . . . C23 C 0.8885(7) 0.7564(4) 0.4097(3) 0.056(2) Uani 1 1 d . . . H23 H 0.8361 0.7826 0.4184 0.073 Uiso 1 1 calc R . . C24 C 0.9957(9) 0.7738(4) 0.3973(4) 0.075(3) Uani 1 1 d . . . H24 H 1.0141 0.8111 0.3973 0.098 Uiso 1 1 calc R . . C25 C 1.0743(9) 0.7354(5) 0.3851(4) 0.080(3) Uani 1 1 d . . . H25 H 1.1471 0.7469 0.3778 0.104 Uiso 1 1 calc R . . C26 C 1.0477(8) 0.6807(5) 0.3833(4) 0.081(3) Uani 1 1 d . . . H26 H 1.1005 0.6552 0.3738 0.105 Uiso 1 1 calc R . . C27 C 0.9402(7) 0.6634(4) 0.3962(3) 0.067(3) Uani 1 1 d . . . H27 H 0.9229 0.6260 0.3959 0.087 Uiso 1 1 calc R . . C28 C 0.7490(8) 0.6083(3) 0.4449(4) 0.056(2) Uani 1 1 d . . . C29 C 0.6849(9) 0.5630(5) 0.4203(4) 0.080(3) Uani 1 1 d . . . H29 H 0.6180 0.5677 0.3912 0.104 Uiso 1 1 calc R . . C30 C 0.7217(14) 0.5101(5) 0.4395(7) 0.113(5) Uani 1 1 d . . . H30 H 0.6790 0.4794 0.4234 0.146 Uiso 1 1 calc R . . C31 C 0.8207(13) 0.5038(6) 0.4821(7) 0.107(5) Uani 1 1 d . . . H31 H 0.8467 0.4687 0.4940 0.139 Uiso 1 1 calc R . . C32 C 0.8810(10) 0.5484(5) 0.5068(5) 0.094(3) Uani 1 1 d . . . H32 H 0.9461 0.5437 0.5368 0.122 Uiso 1 1 calc R . . C33 C 0.8467(8) 0.6005(4) 0.4880(4) 0.065(3) Uani 1 1 d . . . H33 H 0.8902 0.6307 0.5048 0.084 Uiso 1 1 calc R . . C34 C 0.4589(7) 0.8249(3) 0.5032(3) 0.043(2) Uani 1 1 d . . . C35 C 0.4435(6) 0.7922(3) 0.4551(3) 0.0367(18) Uani 1 1 d . . . H35 H 0.3863 0.7645 0.4453 0.048 Uiso 1 1 calc R . . C36 C 0.5305(6) 0.8082(3) 0.4232(3) 0.0423(19) Uani 1 1 d . . . C37 C 0.6046(6) 0.8503(3) 0.4547(3) 0.043(2) Uani 1 1 d . . . C38 C 0.5604(7) 0.8596(3) 0.5039(3) 0.044(2) Uani 1 1 d . . . H38 H 0.5928 0.8844 0.5318 0.057 Uiso 1 1 calc R . . C39 C 0.3704(7) 0.8319(3) 0.5413(3) 0.052(2) Uani 1 1 d . . . C40 C 0.2696(10) 0.7924(6) 0.5267(6) 0.165(7) Uani 1 1 d . . . H40A H 0.2312 0.7964 0.4883 0.214 Uiso 1 1 calc R . . H40B H 0.2122 0.7996 0.5490 0.214 Uiso 1 1 calc R . . H40C H 0.2999 0.7556 0.5335 0.214 Uiso 1 1 calc R . . C41 C 0.3229(11) 0.8905(4) 0.5334(5) 0.138(5) Uani 1 1 d . . . H41A H 0.3889 0.9159 0.5430 0.180 Uiso 1 1 calc R . . H41B H 0.2674 0.8968 0.5567 0.180 Uiso 1 1 calc R . . H41C H 0.2824 0.8959 0.4953 0.180 Uiso 1 1 calc R . . C42 C 0.4288(10) 0.8252(5) 0.6022(4) 0.131(5) Uani 1 1 d . . . H42A H 0.4950 0.8504 0.6122 0.171 Uiso 1 1 calc R . . H42B H 0.4577 0.7882 0.6090 0.171 Uiso 1 1 calc R . . H42C H 0.3707 0.8328 0.6239 0.171 Uiso 1 1 calc R . . C43 C 0.3543(7) 0.7962(4) 0.3271(3) 0.056(2) Uani 1 1 d . . . C44 C 0.2982(8) 0.8404(4) 0.3468(4) 0.063(2) Uani 1 1 d . . . H44 H 0.3392 0.8597 0.3778 0.081 Uiso 1 1 calc R . . C45 C 0.1835(9) 0.8560(4) 0.3213(4) 0.076(3) Uani 1 1 d . . . H45 H 0.1478 0.8857 0.3351 0.099 Uiso 1 1 calc R . . C46 C 0.1212(9) 0.8283(5) 0.2758(5) 0.086(3) Uani 1 1 d . . . H46 H 0.0437 0.8392 0.2583 0.112 Uiso 1 1 calc R . . C47 C 0.1736(9) 0.7849(5) 0.2565(4) 0.096(4) Uani 1 1 d . . . H47 H 0.1313 0.7655 0.2259 0.125 Uiso 1 1 calc R . . C48 C 0.2915(8) 0.7687(4) 0.2820(4) 0.076(3) Uani 1 1 d . . . H48 H 0.3266 0.7389 0.2680 0.099 Uiso 1 1 calc R . . C49 C 0.5781(8) 0.8301(4) 0.3125(3) 0.057(2) Uani 1 1 d . . . C50 C 0.5087(9) 0.8706(4) 0.2812(4) 0.075(3) Uani 1 1 d . . . H50 H 0.4294 0.8757 0.2840 0.098 Uiso 1 1 calc R . . C51 C 0.5570(12) 0.9040(5) 0.2452(4) 0.096(4) Uani 1 1 d . . . H51 H 0.5093 0.9304 0.2236 0.125 Uiso 1 1 calc R . . C52 C 0.6740(14) 0.8973(6) 0.2422(5) 0.113(4) Uani 1 1 d . . . H52 H 0.7065 0.9199 0.2190 0.148 Uiso 1 1 calc R . . C53 C 0.7438(12) 0.8582(6) 0.2727(5) 0.105(4) Uani 1 1 d . . . H53 H 0.8238 0.8545 0.2705 0.136 Uiso 1 1 calc R . . C54 C 0.6965(9) 0.8237(4) 0.3072(4) 0.080(3) Uani 1 1 d . . . H54 H 0.7442 0.7961 0.3269 0.105 Uiso 1 1 calc R . . C55 C 0.6298(8) 0.9465(3) 0.3953(3) 0.054(2) Uani 1 1 d . . . C56 C 0.6830(8) 0.9792(4) 0.3603(4) 0.071(3) Uani 1 1 d . . . H56 H 0.7619 0.9721 0.3580 0.092 Uiso 1 1 calc R . . C57 C 0.6209(12) 1.0218(5) 0.3294(4) 0.093(4) Uani 1 1 d . . . H57 H 0.6572 1.0424 0.3061 0.121 Uiso 1 1 calc R . . C58 C 0.5059(12) 1.0332(4) 0.3335(4) 0.093(3) Uani 1 1 d . . . H58 H 0.4640 1.0621 0.3133 0.121 Uiso 1 1 calc R . . C59 C 0.4522(10) 1.0018(4) 0.3674(4) 0.084(3) Uani 1 1 d . . . H59 H 0.3735 1.0095 0.3698 0.110 Uiso 1 1 calc R . . C60 C 0.5145(9) 0.9586(4) 0.3984(4) 0.068(3) Uani 1 1 d . . . H60 H 0.4772 0.9379 0.4214 0.089 Uiso 1 1 calc R . . C61 C 0.8006(7) 0.9274(3) 0.4922(3) 0.049(2) Uani 1 1 d . . . C62 C 0.7536(8) 0.9682(4) 0.5196(4) 0.062(2) Uani 1 1 d . . . H62 H 0.6714 0.9753 0.5091 0.081 Uiso 1 1 calc R . . C63 C 0.8220(11) 0.9988(4) 0.5614(4) 0.077(3) Uani 1 1 d . . . H63 H 0.7869 1.0264 0.5786 0.100 Uiso 1 1 calc R . . C64 C 0.9420(11) 0.9885(5) 0.5775(5) 0.087(3) Uani 1 1 d . . . H64 H 0.9894 1.0089 0.6060 0.114 Uiso 1 1 calc R . . C65 C 0.9927(9) 0.9485(5) 0.5521(5) 0.090(3) Uani 1 1 d . . . H65 H 1.0749 0.9418 0.5635 0.117 Uiso 1 1 calc R . . C66 C 0.9238(9) 0.9171(4) 0.5093(4) 0.074(3) Uani 1 1 d . . . H66 H 0.9597 0.8896 0.4923 0.097 Uiso 1 1 calc R . . C67 C 0.5503(12) 0.6188(5) 0.2893(5) 0.094(3) Uani 1 1 d . . . H67 H 0.5206 0.5849 0.2976 0.122 Uiso 1 1 calc R . . C68 C 0.6722(11) 0.6368(6) 0.3036(4) 0.087(3) Uani 1 1 d . . . H68 H 0.7363 0.6162 0.3235 0.113 Uiso 1 1 calc R . . C69 C 0.6813(10) 0.6901(6) 0.2833(4) 0.091(4) Uani 1 1 d . . . H69 H 0.7510 0.7109 0.2867 0.118 Uiso 1 1 calc R . . C70 C 0.5615(13) 0.7060(5) 0.2564(4) 0.091(3) Uani 1 1 d . . . H70 H 0.5393 0.7397 0.2394 0.118 Uiso 1 1 calc R . . C71 C 0.4838(10) 0.6624(6) 0.2598(4) 0.084(3) Uani 1 1 d . . . H71 H 0.4012 0.6622 0.2451 0.109 Uiso 1 1 calc R . . C72 C 0.8513(13) 0.3829(6) 0.7495(6) 0.159(5) Uiso 1 1 d D . . C73 C 0.9339(16) 0.4314(8) 0.7704(8) 0.222(8) Uiso 1 1 d D . . C74 C 1.0328(18) 0.4457(9) 0.7418(8) 0.237(9) Uiso 1 1 d D . . C75 C 1.121(2) 0.4947(9) 0.7454(10) 0.275(11) Uiso 1 1 d D . . C76 C 1.1930(18) 0.5243(8) 0.7075(9) 0.226(8) Uiso 1 1 d 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 Fe 0.0418(7) 0.0410(7) 0.0359(6) 0.0004(5) 0.0103(5) 0.0004(6) Mn 0.0528(8) 0.0748(10) 0.0473(8) -0.0207(7) 0.0148(6) -0.0049(7) O 0.053(4) 0.093(5) 0.080(5) 0.007(4) 0.019(3) -0.014(4) C77 0.052(6) 0.058(6) 0.049(5) -0.010(4) 0.004(5) -0.001(5) P1 0.0468(14) 0.0454(13) 0.0539(14) -0.0029(11) 0.0165(11) -0.0026(11) P2 0.0420(13) 0.0528(14) 0.0518(14) -0.0138(11) 0.0166(11) -0.0036(11) P3 0.0445(13) 0.0684(16) 0.0364(12) -0.0021(12) 0.0096(10) -0.0097(12) P4 0.0533(14) 0.0579(15) 0.0524(14) 0.0039(12) 0.0167(12) -0.0076(12) C1 0.045(5) 0.049(5) 0.029(5) 0.002(4) -0.002(4) 0.006(4) C2 0.041(5) 0.047(5) 0.045(5) 0.008(4) 0.015(4) 0.002(4) C3 0.037(5) 0.036(5) 0.048(5) -0.002(4) 0.007(4) 0.002(4) C4 0.042(5) 0.044(5) 0.039(4) -0.006(4) 0.009(4) 0.001(4) C5 0.030(4) 0.050(5) 0.043(5) 0.003(4) 0.004(4) 0.007(4) C6 0.060(6) 0.069(6) 0.038(5) -0.008(5) -0.004(4) -0.005(5) C7 0.133(10) 0.120(9) 0.056(7) 0.016(7) -0.026(6) -0.034(8) C8 0.109(9) 0.174(13) 0.066(7) -0.038(8) 0.000(7) -0.060(9) C9 0.174(13) 0.135(11) 0.106(10) -0.086(9) -0.055(9) 0.050(10) C10 0.040(5) 0.048(5) 0.064(6) 0.010(5) 0.016(5) 0.001(4) C11 0.057(6) 0.074(7) 0.077(7) 0.007(5) 0.025(6) 0.003(5) C12 0.042(6) 0.099(9) 0.112(9) 0.008(7) 0.013(6) 0.002(5) C13 0.087(9) 0.074(7) 0.117(10) 0.023(7) 0.067(8) 0.009(6) C14 0.079(8) 0.089(8) 0.076(7) 0.027(6) 0.031(7) 0.011(6) C15 0.052(6) 0.074(7) 0.066(7) 0.008(5) 0.026(5) -0.002(5) C16 0.062(6) 0.048(6) 0.061(6) 0.006(5) 0.030(5) 0.009(5) C17 0.058(6) 0.071(7) 0.081(7) 0.009(6) 0.015(6) 0.017(6) C18 0.099(9) 0.096(9) 0.080(8) 0.008(7) 0.010(6) 0.058(8) C19 0.138(13) 0.095(11) 0.114(11) 0.044(9) 0.045(10) 0.074(10) C20 0.122(11) 0.063(8) 0.145(12) 0.051(8) 0.037(10) 0.042(9) C21 0.073(7) 0.065(7) 0.110(9) 0.009(7) 0.015(6) 0.002(6) C22 0.036(5) 0.067(6) 0.048(5) -0.005(4) 0.012(4) -0.001(5) C23 0.048(6) 0.070(7) 0.057(6) 0.003(5) 0.027(4) 0.000(5) C24 0.065(7) 0.086(8) 0.079(7) -0.006(6) 0.025(6) -0.026(6) C25 0.045(6) 0.119(10) 0.080(7) 0.000(7) 0.027(5) -0.021(7) C26 0.055(7) 0.118(10) 0.076(7) -0.017(7) 0.029(5) -0.002(7) C27 0.050(6) 0.100(8) 0.055(6) -0.005(5) 0.023(5) 0.003(5) C28 0.057(6) 0.053(6) 0.067(6) -0.014(5) 0.032(5) -0.001(5) C29 0.073(7) 0.078(8) 0.099(8) -0.029(7) 0.041(6) -0.016(6) C30 0.137(12) 0.044(8) 0.184(15) -0.029(9) 0.094(11) -0.018(8) C31 0.099(11) 0.080(10) 0.163(15) 0.010(10) 0.076(10) 0.022(9) C32 0.082(8) 0.085(9) 0.122(10) 0.004(8) 0.038(7) 0.023(8) C33 0.048(6) 0.056(7) 0.098(8) 0.010(6) 0.034(6) 0.013(5) C34 0.048(5) 0.037(5) 0.044(5) 0.000(4) 0.011(4) 0.003(4) C35 0.036(4) 0.033(5) 0.040(5) 0.002(4) 0.005(4) 0.000(4) C36 0.041(5) 0.045(5) 0.039(4) 0.004(4) 0.006(4) 0.003(4) C37 0.045(5) 0.049(5) 0.035(5) 0.001(4) 0.007(4) -0.006(4) C38 0.056(5) 0.035(5) 0.040(5) 0.000(4) 0.013(4) -0.001(4) C39 0.053(5) 0.054(6) 0.056(6) -0.002(4) 0.026(5) 0.012(5) C40 0.110(10) 0.220(16) 0.209(15) -0.126(13) 0.129(10) -0.094(10) C41 0.161(12) 0.087(9) 0.209(14) 0.035(9) 0.132(11) 0.063(8) C42 0.145(11) 0.214(15) 0.048(7) 0.023(8) 0.048(7) 0.073(10) C43 0.051(5) 0.066(6) 0.050(6) 0.007(5) 0.008(5) -0.010(5) C44 0.053(6) 0.073(7) 0.057(6) 0.009(5) 0.004(5) 0.005(5) C45 0.061(7) 0.084(8) 0.080(7) 0.019(6) 0.005(6) 0.012(6) C46 0.049(7) 0.104(10) 0.096(9) 0.006(7) -0.007(6) -0.002(7) C47 0.062(8) 0.127(10) 0.080(8) -0.004(8) -0.027(6) -0.020(7) C48 0.059(6) 0.095(8) 0.070(7) -0.016(6) 0.006(5) -0.015(6) C49 0.052(6) 0.079(7) 0.039(5) -0.006(5) 0.011(4) -0.012(5) C50 0.076(7) 0.096(8) 0.052(6) 0.015(6) 0.009(5) -0.013(6) C51 0.117(10) 0.107(9) 0.062(7) 0.025(6) 0.014(7) -0.022(8) C52 0.132(13) 0.145(13) 0.078(9) -0.001(8) 0.056(9) -0.042(10) C53 0.105(10) 0.147(12) 0.078(9) -0.002(8) 0.051(8) -0.033(9) C54 0.078(8) 0.109(9) 0.054(6) 0.007(6) 0.015(6) -0.017(7) C55 0.064(6) 0.056(6) 0.037(5) 0.002(4) 0.004(4) -0.015(5) C56 0.074(7) 0.074(7) 0.066(6) 0.015(6) 0.020(5) -0.016(6) C57 0.127(10) 0.094(9) 0.068(7) 0.034(6) 0.041(7) -0.017(8) C58 0.134(11) 0.077(8) 0.067(7) 0.021(6) 0.019(8) -0.016(8) C59 0.083(7) 0.087(8) 0.075(7) 0.007(6) -0.001(6) 0.007(6) C60 0.073(7) 0.058(6) 0.070(6) 0.025(5) 0.006(5) -0.001(6) C61 0.053(6) 0.042(5) 0.054(5) 0.009(4) 0.015(5) -0.006(4) C62 0.057(6) 0.063(6) 0.062(6) 0.008(5) 0.005(5) -0.009(5) C63 0.087(8) 0.066(7) 0.077(7) 0.001(6) 0.013(6) -0.010(6) C64 0.090(10) 0.076(8) 0.088(8) 0.009(7) 0.001(7) -0.026(7) C65 0.045(6) 0.112(10) 0.102(9) 0.011(8) -0.007(6) -0.018(7) C66 0.059(7) 0.072(7) 0.093(8) 0.004(6) 0.016(6) -0.012(6) C67 0.101(10) 0.106(10) 0.074(8) -0.047(8) 0.022(7) -0.002(9) C68 0.087(10) 0.113(10) 0.066(7) -0.034(7) 0.027(7) 0.015(8) C69 0.072(8) 0.158(13) 0.048(6) -0.019(7) 0.023(6) 0.022(8) C70 0.122(10) 0.119(10) 0.035(6) -0.015(6) 0.023(7) 0.012(9) C71 0.084(8) 0.106(9) 0.059(7) -0.038(7) 0.012(6) -0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C35 2.034(7) . ? Fe C4 2.039(7) . ? Fe C5 2.047(7) . ? Fe C38 2.058(7) . ? Fe C2 2.060(7) . ? Fe C3 2.059(7) . ? Fe C36 2.071(7) . ? Fe C37 2.072(7) . ? Fe C34 2.092(7) . ? Fe C1 2.120(7) . ? Mn C77 1.769(9) . ? Mn C68 2.140(9) . ? Mn C71 2.144(9) . ? Mn C70 2.139(9) . ? Mn C67 2.155(10) . ? Mn C69 2.165(9) . ? Mn P3 2.241(3) . ? Mn P2 2.244(3) . ? O C77 1.154(9) . ? P1 C3 1.824(7) . ? P1 C16 1.836(9) . ? P1 C10 1.837(8) . ? P2 C4 1.834(7) . ? P2 C22 1.835(8) . ? P2 C28 1.862(9) . ? P3 C36 1.846(7) . ? P3 C49 1.856(9) . ? P3 C43 1.871(9) . ? P4 C61 1.829(8) . ? P4 C37 1.828(7) . ? P4 C55 1.835(9) . ? C1 C5 1.411(9) . ? C1 C2 1.416(9) . ? C1 C6 1.519(10) . ? C2 C3 1.428(10) . ? C3 C4 1.451(9) . ? C4 C5 1.427(10) . ? C6 C9 1.506(12) . ? C6 C8 1.498(12) . ? C6 C7 1.506(12) . ? C10 C11 1.371(11) . ? C10 C15 1.384(10) . ? C11 C12 1.393(12) . ? C12 C13 1.367(13) . ? C13 C14 1.360(13) . ? C14 C15 1.367(11) . ? C16 C17 1.378(11) . ? C16 C21 1.388(11) . ? C17 C18 1.379(12) . ? C18 C19 1.386(15) . ? C19 C20 1.326(15) . ? C20 C21 1.360(13) . ? C22 C23 1.385(11) . ? C22 C27 1.413(10) . ? C23 C24 1.390(11) . ? C24 C25 1.375(12) . ? C25 C26 1.361(13) . ? C26 C27 1.397(11) . ? C28 C33 1.374(11) . ? C28 C29 1.384(11) . ? C29 C30 1.403(14) . ? C30 C31 1.370(16) . ? C31 C32 1.354(15) . ? C32 C33 1.375(13) . ? C34 C35 1.410(9) . ? C34 C38 1.427(9) . ? C34 C39 1.537(10) . ? C35 C36 1.451(9) . ? C36 C37 1.439(10) . ? C37 C38 1.435(9) . ? C39 C40 1.477(12) . ? C39 C42 1.514(11) . ? C39 C41 1.522(11) . ? C43 C48 1.359(11) . ? C43 C44 1.392(11) . ? C44 C45 1.371(11) . ? C45 C46 1.367(13) . ? C46 C47 1.350(13) . ? C47 C48 1.406(13) . ? C49 C50 1.385(11) . ? C49 C54 1.392(11) . ? C50 C51 1.404(12) . ? C51 C52 1.361(14) . ? C52 C53 1.355(15) . ? C53 C54 1.388(13) . ? C55 C60 1.365(11) . ? C55 C56 1.407(11) . ? C56 C57 1.383(13) . ? C57 C58 1.363(13) . ? C58 C59 1.375(13) . ? C59 C60 1.398(12) . ? C61 C62 1.375(11) . ? C61 C66 1.395(11) . ? C62 C63 1.369(12) . ? C63 C64 1.359(13) . ? C64 C65 1.354(13) . ? C65 C66 1.397(13) . ? C67 C71 1.408(14) . ? C67 C68 1.422(13) . ? C68 C69 1.401(14) . ? C69 C70 1.432(13) . ? C70 C71 1.396(13) . ? C72 C73 1.526(9) . ? C73 C74 1.499(10) . ? C74 C75 1.545(10) . ? C75 C76 1.557(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 C35 Fe C4 119.5(3) . . ? C35 Fe C5 156.9(3) . . ? C4 Fe C5 40.9(3) . . ? C35 Fe C38 67.7(3) . . ? C4 Fe C38 161.6(3) . . ? C5 Fe C38 126.9(3) . . ? C35 Fe C2 123.7(3) . . ? C4 Fe C2 68.6(3) . . ? C5 Fe C2 66.4(3) . . ? C38 Fe C2 123.4(3) . . ? C35 Fe C3 105.4(3) . . ? C4 Fe C3 41.5(3) . . ? C5 Fe C3 67.9(3) . . ? C38 Fe C3 156.7(3) . . ? C2 Fe C3 40.6(3) . . ? C35 Fe C36 41.4(3) . . ? C4 Fe C36 105.2(3) . . ? C5 Fe C36 122.1(3) . . ? C38 Fe C36 68.1(3) . . ? C2 Fe C36 160.0(3) . . ? C3 Fe C36 122.4(3) . . ? C35 Fe C37 68.7(3) . . ? C4 Fe C37 123.3(3) . . ? C5 Fe C37 109.5(3) . . ? C38 Fe C37 40.7(3) . . ? C2 Fe C37 158.5(3) . . ? C3 Fe C37 159.8(3) . . ? C36 Fe C37 40.6(3) . . ? C35 Fe C34 39.9(3) . . ? C4 Fe C34 155.1(3) . . ? C5 Fe C34 162.6(3) . . ? C38 Fe C34 40.2(3) . . ? C2 Fe C34 108.8(3) . . ? C3 Fe C34 120.3(3) . . ? C36 Fe C34 68.3(3) . . ? C37 Fe C34 68.3(3) . . ? C35 Fe C1 160.5(3) . . ? C4 Fe C1 68.6(3) . . ? C5 Fe C1 39.5(3) . . ? C38 Fe C1 110.6(3) . . ? C2 Fe C1 39.6(3) . . ? C3 Fe C1 68.0(3) . . ? C36 Fe C1 157.7(3) . . ? C37 Fe C1 123.7(3) . . ? C34 Fe C1 126.1(3) . . ? C77 Mn C68 125.7(5) . . ? C77 Mn C71 93.3(4) . . ? C68 Mn C71 63.8(4) . . ? C77 Mn C70 125.7(5) . . ? C68 Mn C70 63.9(4) . . ? C71 Mn C70 38.1(4) . . ? C77 Mn C67 92.6(4) . . ? C68 Mn C67 38.7(4) . . ? C71 Mn C67 38.2(4) . . ? C70 Mn C67 64.3(4) . . ? C77 Mn C69 156.0(4) . . ? C68 Mn C69 38.0(4) . . ? C71 Mn C69 64.4(4) . . ? C70 Mn C69 38.9(4) . . ? C67 Mn C69 64.7(5) . . ? C77 Mn P3 88.2(3) . . ? C68 Mn P3 145.0(4) . . ? C71 Mn P3 111.0(4) . . ? C70 Mn P3 90.6(3) . . ? C67 Mn P3 149.3(4) . . ? C69 Mn P3 107.3(4) . . ? C77 Mn P2 97.8(3) . . ? C68 Mn P2 85.9(3) . . ? C71 Mn P2 148.4(4) . . ? C70 Mn P2 135.8(4) . . ? C67 Mn P2 111.4(4) . . ? C69 Mn P2 97.7(3) . . ? P3 Mn P2 98.86(9) . . ? O C77 Mn 173.2(7) . . ? C3 P1 C16 99.8(4) . . ? C3 P1 C10 105.2(3) . . ? C16 P1 C10 98.8(4) . . ? C4 P2 C22 102.3(4) . . ? C4 P2 C28 97.3(4) . . ? C22 P2 C28 98.7(4) . . ? C4 P2 Mn 124.4(2) . . ? C22 P2 Mn 111.6(3) . . ? C28 P2 Mn 118.4(3) . . ? C36 P3 C49 106.2(4) . . ? C36 P3 C43 96.2(4) . . ? C49 P3 C43 96.4(4) . . ? C36 P3 Mn 121.9(2) . . ? C49 P3 Mn 116.1(3) . . ? C43 P3 Mn 115.6(3) . . ? C61 P4 C37 105.1(3) . . ? C61 P4 C55 98.3(4) . . ? C37 P4 C55 100.2(4) . . ? C5 C1 C2 105.4(6) . . ? C5 C1 C6 127.3(7) . . ? C2 C1 C6 126.2(7) . . ? C5 C1 Fe 67.4(4) . . ? C2 C1 Fe 67.9(4) . . ? C6 C1 Fe 137.9(6) . . ? C1 C2 C3 110.5(6) . . ? C1 C2 Fe 72.5(4) . . ? C3 C2 Fe 69.7(4) . . ? C2 C3 C4 106.8(6) . . ? C2 C3 P1 127.2(6) . . ? C4 C3 P1 123.3(5) . . ? C2 C3 Fe 69.8(4) . . ? C4 C3 Fe 68.5(4) . . ? P1 C3 Fe 141.3(4) . . ? C5 C4 C3 105.7(6) . . ? C5 C4 P2 128.9(6) . . ? C3 C4 P2 125.3(5) . . ? C5 C4 Fe 69.9(4) . . ? C3 C4 Fe 70.0(4) . . ? P2 C4 Fe 127.7(4) . . ? C1 C5 C4 111.5(7) . . ? C1 C5 Fe 73.0(4) . . ? C4 C5 Fe 69.3(4) . . ? C9 C6 C8 109.9(9) . . ? C9 C6 C7 108.0(9) . . ? C8 C6 C7 106.1(8) . . ? C9 C6 C1 112.6(7) . . ? C8 C6 C1 111.4(7) . . ? C7 C6 C1 108.6(7) . . ? C11 C10 C15 117.1(8) . . ? C11 C10 P1 117.4(7) . . ? C15 C10 P1 125.4(7) . . ? C10 C11 C12 122.0(9) . . ? C13 C12 C11 118.0(9) . . ? C14 C13 C12 121.8(9) . . ? C13 C14 C15 118.9(10) . . ? C14 C15 C10 122.2(9) . . ? C17 C16 C21 116.6(8) . . ? C17 C16 P1 127.2(7) . . ? C21 C16 P1 116.0(8) . . ? C16 C17 C18 119.7(10) . . ? C17 C18 C19 121.9(12) . . ? C20 C19 C18 118.1(11) . . ? C19 C20 C21 121.1(12) . . ? C20 C21 C16 122.6(10) . . ? C23 C22 C27 116.5(7) . . ? C23 C22 P2 121.6(6) . . ? C27 C22 P2 121.7(7) . . ? C22 C23 C24 122.2(8) . . ? C25 C24 C23 119.3(9) . . ? C26 C25 C24 121.3(9) . . ? C25 C26 C27 119.2(9) . . ? C26 C27 C22 121.6(9) . . ? C33 C28 C29 119.2(9) . . ? C33 C28 P2 119.2(7) . . ? C29 C28 P2 121.6(8) . . ? C28 C29 C30 119.4(11) . . ? C31 C30 C29 119.7(12) . . ? C32 C31 C30 120.4(13) . . ? C33 C32 C31 120.4(12) . . ? C32 C33 C28 120.7(10) . . ? C35 C34 C38 106.9(6) . . ? C35 C34 C39 127.3(7) . . ? C38 C34 C39 124.6(7) . . ? C35 C34 Fe 67.9(4) . . ? C38 C34 Fe 68.6(4) . . ? C39 C34 Fe 138.1(5) . . ? C34 C35 C36 109.6(6) . . ? C34 C35 Fe 72.2(4) . . ? C36 C35 Fe 70.7(4) . . ? C37 C36 C35 106.6(6) . . ? C37 C36 P3 134.8(6) . . ? C35 C36 P3 118.3(5) . . ? C37 C36 Fe 69.7(4) . . ? C35 C36 Fe 68.0(4) . . ? P3 C36 Fe 131.1(4) . . ? C38 C37 C36 107.2(6) . . ? C38 C37 P4 127.2(6) . . ? C36 C37 P4 125.2(5) . . ? C38 C37 Fe 69.1(4) . . ? C36 C37 Fe 69.7(4) . . ? P4 C37 Fe 131.8(4) . . ? C34 C38 C37 109.5(6) . . ? C34 C38 Fe 71.2(4) . . ? C37 C38 Fe 70.2(4) . . ? C40 C39 C42 108.5(9) . . ? C40 C39 C41 110.0(9) . . ? C42 C39 C41 107.1(9) . . ? C40 C39 C34 111.0(7) . . ? C42 C39 C34 113.4(7) . . ? C41 C39 C34 106.7(7) . . ? C48 C43 C44 117.9(8) . . ? C48 C43 P3 118.1(7) . . ? C44 C43 P3 123.5(7) . . ? C45 C44 C43 121.1(9) . . ? C46 C45 C44 120.7(10) . . ? C47 C46 C45 119.1(10) . . ? C46 C47 C48 120.9(10) . . ? C43 C48 C47 120.4(10) . . ? C50 C49 C54 118.1(8) . . ? C50 C49 P3 123.5(7) . . ? C54 C49 P3 117.9(7) . . ? C49 C50 C51 120.6(10) . . ? C52 C51 C50 119.5(11) . . ? C51 C52 C53 120.8(12) . . ? C52 C53 C54 120.4(12) . . ? C53 C54 C49 120.5(10) . . ? C60 C55 C56 117.7(8) . . ? C60 C55 P4 125.5(6) . . ? C56 C55 P4 116.8(7) . . ? C57 C56 C55 121.7(9) . . ? C58 C57 C56 119.5(9) . . ? C57 C58 C59 119.9(11) . . ? C58 C59 C60 120.7(10) . . ? C55 C60 C59 120.5(9) . . ? C62 C61 C66 117.2(8) . . ? C62 C61 P4 126.3(7) . . ? C66 C61 P4 116.2(7) . . ? C61 C62 C63 123.1(9) . . ? C64 C63 C62 119.1(10) . . ? C65 C64 C63 120.2(11) . . ? C64 C65 C66 121.3(10) . . ? C61 C66 C65 119.2(10) . . ? C71 C67 C68 106.3(11) . . ? C71 C67 Mn 70.4(6) . . ? C68 C67 Mn 70.1(6) . . ? C69 C68 C67 110.0(11) . . ? C69 C68 Mn 72.0(6) . . ? C67 C68 Mn 71.2(6) . . ? C68 C69 C70 106.2(11) . . ? C68 C69 Mn 70.0(6) . . ? C70 C69 Mn 69.6(5) . . ? C71 C70 C69 108.5(11) . . ? C71 C70 Mn 71.1(6) . . ? C69 C70 Mn 71.6(5) . . ? C70 C71 C67 109.2(11) . . ? C70 C71 Mn 70.8(5) . . ? C67 C71 Mn 71.3(6) . . ? C74 C73 C72 119.4(17) . . ? C73 C74 C75 134.2(19) . . ? C74 C75 C76 138(2) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 22.78 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.732 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.076