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' loop_ _publ_author_name 'Hor, T. S. Andy' 'Lee, Kim Hun' 'Liu, Ye' 'Vittal, Jagadese J.' _publ_contact_author_name 'Prof T. S. Andy Hor' _publ_contact_author_address ; Chemistry National University of Singapore Kent Ridge, Singapore Singapore Singapore 119260 SINGAPORE ; _publ_contact_author_email 'CHMHEAD@NUS.EDU.SG' _publ_section_title ; Cleavage of Homometallic and Formation of Heterometallic M-M Bonds. Serendipitous Syntheses of Bimetallic PdMn(m-PPh2)(CO)4(¦Ç2-P-P) (P-P = dppm, dppe, dppf) and Polymetallic Mn2Pd2Ag(m-Cl)(m-PPh2)2(m-dppm)(CO)8 ; data_1010 _database_code_CSD 180412 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H48 Ag Cl Mn2 O9 P4 Pd2' _chemical_formula_weight 1502.86 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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 11.3130(4) _cell_length_b 26.5117(10) _cell_length_c 19.9718(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.478(1) _cell_angle_gamma 90.00 _cell_volume 5988.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4861 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.5 _exptl_crystal_description 'plates, cut' _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 0.8559 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34997 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10548 _reflns_number_gt 7110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0200P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10548 _refine_ls_number_parameters 691 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.992 _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 Ag1 Ag 0.89180(5) 0.455922(16) 0.14279(2) 0.04324(14) Uani 1 1 d . . . Pd1 Pd 0.81877(4) 0.391274(16) 0.23948(2) 0.03227(12) Uani 1 1 d . . . Pd2 Pd 0.81732(4) 0.511445(16) 0.25335(2) 0.03291(12) Uani 1 1 d . . . Mn1 Mn 0.94197(8) 0.35596(3) 0.12948(4) 0.0352(2) Uani 1 1 d . . . Mn2 Mn 0.88634(8) 0.55594(3) 0.13087(4) 0.0382(2) Uani 1 1 d . . . Cl1 Cl 0.96367(13) 0.44848(5) 0.29441(7) 0.0408(4) Uani 1 1 d . . . P1 P 0.76282(14) 0.33322(6) 0.16436(7) 0.0350(4) Uani 1 1 d . . . P2 P 0.69271(15) 0.39253(6) 0.33063(7) 0.0377(4) Uani 1 1 d . . . P3 P 0.73394(15) 0.50881(6) 0.35788(7) 0.0388(4) Uani 1 1 d . . . P4 P 0.73650(14) 0.57509(6) 0.19772(7) 0.0344(4) Uani 1 1 d . . . O1 O 1.0497(4) 0.31966(17) 0.2580(2) 0.0670(14) Uani 1 1 d . . . C1 C 1.0041(6) 0.3350(2) 0.2097(3) 0.0450(17) Uani 1 1 d . . . O2 O 0.8346(4) 0.38612(17) -0.0020(2) 0.0629(14) Uani 1 1 d . . . C2 C 0.8739(6) 0.3774(2) 0.0498(3) 0.0397(16) Uani 1 1 d . . . O3 O 1.0361(5) 0.26800(18) 0.0593(2) 0.0805(18) Uani 1 1 d . . . C3 C 0.9990(6) 0.3024(2) 0.0864(3) 0.0503(18) Uani 1 1 d . . . O4 O 1.1627(5) 0.4144(2) 0.1115(3) 0.0875(18) Uani 1 1 d . . . C4 C 1.0742(6) 0.3943(2) 0.1194(4) 0.0551(19) Uani 1 1 d . . . O5 O 1.0854(4) 0.51545(17) 0.0534(2) 0.0701(15) Uani 1 1 d . . . C5 C 1.0059(6) 0.5284(2) 0.0835(3) 0.0495(18) Uani 1 1 d . . . O6 O 1.0729(5) 0.57265(18) 0.2367(3) 0.0771(16) Uani 1 1 d . . . C6 C 0.9969(7) 0.5665(2) 0.1975(4) 0.0508(19) Uani 1 1 d . . . O7 O 0.9012(6) 0.65550(19) 0.0683(3) 0.114(3) Uani 1 1 d . . . C7 C 0.8956(6) 0.6168(3) 0.0928(4) 0.063(2) Uani 1 1 d . . . O8 O 0.7058(4) 0.51844(19) 0.0310(2) 0.0697(15) Uani 1 1 d . . . C8 C 0.7740(6) 0.5316(2) 0.0696(3) 0.0456(17) Uani 1 1 d . . . C9 C 0.7284(5) 0.4436(2) 0.3900(3) 0.0421(16) Uani 1 1 d . . . H9A H 0.8055 0.4360 0.4111 0.050 Uiso 1 1 calc R . . H9B H 0.6700 0.4427 0.4253 0.050 Uiso 1 1 calc R . . C1A C 0.7410(5) 0.2709(2) 0.2009(3) 0.0389(15) Uani 1 1 d . . . C2A C 0.8129(6) 0.2320(2) 0.1843(4) 0.066(2) Uani 1 1 d . . . H2A H 0.8727 0.2378 0.1534 0.079 Uiso 1 1 calc R . . C3A C 0.8011(8) 0.1844(3) 0.2113(4) 0.090(3) Uani 1 1 d . . . H3A H 0.8505 0.1579 0.1981 0.108 Uiso 1 1 calc R . . C4A C 0.7159(7) 0.1764(3) 0.2577(4) 0.076(3) Uani 1 1 d . . . H4A H 0.7089 0.1446 0.2780 0.091 Uiso 1 1 calc R . . C5A C 0.6415(7) 0.2145(2) 0.2745(4) 0.068(2) Uani 1 1 d . . . H5A H 0.5816 0.2088 0.3053 0.082 Uiso 1 1 calc R . . C6A C 0.6544(6) 0.2612(2) 0.2460(3) 0.0534(19) Uani 1 1 d . . . H6A H 0.6025 0.2873 0.2577 0.064 Uiso 1 1 calc R . . C1B C 0.6279(5) 0.3437(2) 0.1143(3) 0.0368(15) Uani 1 1 d . . . C2B C 0.5490(6) 0.3056(2) 0.0985(3) 0.0507(18) Uani 1 1 d . . . H2B H 0.5649 0.2724 0.1129 0.061 Uiso 1 1 calc R . . C3B C 0.4470(7) 0.3158(3) 0.0618(4) 0.069(2) Uani 1 1 d . . . H3B H 0.3933 0.2897 0.0517 0.083 Uiso 1 1 calc R . . C4B C 0.4232(7) 0.3636(3) 0.0400(3) 0.066(2) Uani 1 1 d . . . H4B H 0.3534 0.3704 0.0150 0.080 Uiso 1 1 calc R . . C5B C 0.5009(7) 0.4014(3) 0.0545(3) 0.058(2) Uani 1 1 d . . . H5B H 0.4854 0.4343 0.0391 0.070 Uiso 1 1 calc R . . C6B C 0.6015(6) 0.3917(2) 0.0915(3) 0.0478(17) Uani 1 1 d . . . H6B H 0.6539 0.4183 0.1016 0.057 Uiso 1 1 calc R . . C1C C 0.7195(6) 0.3371(2) 0.3840(3) 0.0467(17) Uani 1 1 d . . . C2C C 0.8294(7) 0.3151(3) 0.3840(4) 0.074(2) Uani 1 1 d . . . H2C H 0.8889 0.3293 0.3580 0.089 Uiso 1 1 calc R . . C3C C 0.8536(8) 0.2729(3) 0.4212(5) 0.097(3) Uani 1 1 d . . . H3C H 0.9290 0.2580 0.4200 0.116 Uiso 1 1 calc R . . C4C C 0.7697(9) 0.2524(3) 0.4597(5) 0.107(4) Uani 1 1 d . . . H4C H 0.7882 0.2246 0.4873 0.129 Uiso 1 1 calc R . . C5C C 0.6592(10) 0.2717(3) 0.4585(4) 0.106(3) Uani 1 1 d . . . H5C H 0.5994 0.2563 0.4831 0.127 Uiso 1 1 calc R . . C6C C 0.6348(7) 0.3144(3) 0.4211(4) 0.077(3) Uani 1 1 d . . . H6C H 0.5582 0.3281 0.4212 0.092 Uiso 1 1 calc R . . C1D C 0.5342(5) 0.3966(2) 0.3193(3) 0.0396(15) Uani 1 1 d . . . C2D C 0.4850(6) 0.3911(2) 0.2563(3) 0.0502(17) Uani 1 1 d . . . H2D H 0.5345 0.3842 0.2203 0.060 Uiso 1 1 calc R . . C3D C 0.3637(7) 0.3955(3) 0.2440(4) 0.073(2) Uani 1 1 d . . . H3D H 0.3320 0.3911 0.2004 0.088 Uiso 1 1 calc R . . C4D C 0.2913(7) 0.4062(3) 0.2957(5) 0.082(3) Uani 1 1 d . . . H4D H 0.2096 0.4100 0.2876 0.098 Uiso 1 1 calc R . . C5D C 0.3373(7) 0.4112(3) 0.3589(5) 0.076(2) Uani 1 1 d . . . H5D H 0.2869 0.4173 0.3947 0.091 Uiso 1 1 calc R . . C6D C 0.4570(7) 0.4073(2) 0.3705(3) 0.058(2) Uani 1 1 d . . . H6D H 0.4878 0.4121 0.4142 0.069 Uiso 1 1 calc R . . C1E C 0.5897(6) 0.5364(2) 0.3735(3) 0.0493(18) Uani 1 1 d . . . C2E C 0.4951(7) 0.5255(3) 0.3321(4) 0.063(2) Uani 1 1 d . . . H2E H 0.5045 0.5026 0.2967 0.075 Uiso 1 1 calc R . . C3E C 0.3850(7) 0.5478(3) 0.3412(5) 0.087(3) Uani 1 1 d . . . H3E H 0.3198 0.5386 0.3138 0.104 Uiso 1 1 calc R . . C4E C 0.3729(9) 0.5826(4) 0.3900(5) 0.105(4) Uani 1 1 d . . . H4E H 0.2993 0.5984 0.3952 0.126 Uiso 1 1 calc R . . C5E C 0.4649(10) 0.5953(4) 0.4314(4) 0.114(4) Uani 1 1 d . . . H5E H 0.4551 0.6193 0.4654 0.137 Uiso 1 1 calc R . . C6E C 0.5737(7) 0.5723(3) 0.4232(3) 0.080(3) Uani 1 1 d . . . H6E H 0.6378 0.5813 0.4517 0.096 Uiso 1 1 calc R . . C1F C 0.8322(6) 0.5397(2) 0.4196(3) 0.0477(17) Uani 1 1 d . . . C2F C 0.8379(6) 0.5254(3) 0.4864(3) 0.061(2) Uani 1 1 d . . . H2F H 0.7916 0.4985 0.5014 0.073 Uiso 1 1 calc R . . C3F C 0.9121(8) 0.5510(3) 0.5308(4) 0.080(3) Uani 1 1 d . . . H3F H 0.9177 0.5410 0.5760 0.096 Uiso 1 1 calc R . . C4F C 0.9770(9) 0.5906(4) 0.5088(5) 0.101(4) Uani 1 1 d . . . H4F H 1.0264 0.6082 0.5393 0.121 Uiso 1 1 calc R . . C5F C 0.9717(9) 0.6050(3) 0.4444(5) 0.106(3) Uani 1 1 d . . . H5F H 1.0169 0.6325 0.4300 0.127 Uiso 1 1 calc R . . C6F C 0.8991(8) 0.5791(3) 0.3989(4) 0.080(3) Uani 1 1 d . . . H6F H 0.8963 0.5889 0.3537 0.096 Uiso 1 1 calc R . . C1G C 0.7348(6) 0.6333(2) 0.2465(3) 0.0378(15) Uani 1 1 d . . . C2G C 0.6377(6) 0.6458(2) 0.2841(3) 0.0532(19) Uani 1 1 d . . . H2G H 0.5692 0.6258 0.2818 0.064 Uiso 1 1 calc R . . C3G C 0.6421(8) 0.6880(3) 0.3253(4) 0.086(3) Uani 1 1 d . . . H3G H 0.5754 0.6969 0.3498 0.104 Uiso 1 1 calc R . . C4G C 0.7425(9) 0.7169(3) 0.3307(5) 0.095(3) Uani 1 1 d . . . H4G H 0.7462 0.7446 0.3601 0.114 Uiso 1 1 calc R . . C5G C 0.8356(7) 0.7049(3) 0.2930(4) 0.084(3) Uani 1 1 d . . . H5G H 0.9037 0.7252 0.2954 0.100 Uiso 1 1 calc R . . C6G C 0.8339(6) 0.6637(2) 0.2509(3) 0.061(2) Uani 1 1 d . . . H6G H 0.9002 0.6562 0.2252 0.073 Uiso 1 1 calc R . . C1H C 0.5870(5) 0.5696(2) 0.1661(3) 0.0369(15) Uani 1 1 d . . . C2H C 0.5305(6) 0.5229(2) 0.1635(3) 0.0510(18) Uani 1 1 d . . . H2H H 0.5694 0.4942 0.1805 0.061 Uiso 1 1 calc R . . C3H C 0.4174(7) 0.5185(3) 0.1360(3) 0.063(2) Uani 1 1 d . . . H3H H 0.3795 0.4870 0.1355 0.076 Uiso 1 1 calc R . . C4H C 0.3607(7) 0.5595(3) 0.1096(3) 0.064(2) Uani 1 1 d . . . H4H H 0.2839 0.5564 0.0909 0.077 Uiso 1 1 calc R . . C5H C 0.4170(7) 0.6054(3) 0.1105(3) 0.063(2) Uani 1 1 d . . . H5H H 0.3786 0.6337 0.0918 0.076 Uiso 1 1 calc R . . C6H C 0.5277(6) 0.6104(2) 0.1381(3) 0.0482(17) Uani 1 1 d . . . H6H H 0.5645 0.6422 0.1381 0.058 Uiso 1 1 calc R . . O1S O 0.3638(7) 0.2959(3) 0.4725(4) 0.178(2) Uiso 1 1 d D . . C1S C 0.3004(9) 0.2791(4) 0.4300(5) 0.178(2) Uiso 1 1 d D . . C2S C 0.1749(9) 0.2957(4) 0.4295(6) 0.178(2) Uiso 1 1 d D . . H2SA H 0.1470 0.2963 0.4750 0.267 Uiso 1 1 calc R . . H2SB H 0.1272 0.2723 0.4030 0.267 Uiso 1 1 calc R . . H2SC H 0.1685 0.3291 0.4102 0.267 Uiso 1 1 calc R . . C3S C 0.3364(11) 0.2580(4) 0.3674(5) 0.178(2) Uiso 1 1 d D . . H3SA H 0.3913 0.2808 0.3463 0.267 Uiso 1 1 calc R . . H3SB H 0.2675 0.2532 0.3381 0.267 Uiso 1 1 calc R . . H3SC H 0.3747 0.2257 0.3755 0.267 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 Ag1 0.0595(4) 0.0296(3) 0.0413(3) -0.0010(2) 0.0138(2) 0.0010(2) Pd1 0.0332(3) 0.0332(3) 0.0305(3) -0.0002(2) 0.0019(2) 0.0012(2) Pd2 0.0347(3) 0.0330(3) 0.0310(3) -0.0033(2) 0.0015(2) 0.0036(2) Mn1 0.0352(6) 0.0323(5) 0.0383(5) -0.0012(4) 0.0032(4) 0.0044(4) Mn2 0.0409(6) 0.0323(5) 0.0416(6) -0.0003(4) 0.0091(5) -0.0009(4) Cl1 0.0350(10) 0.0439(9) 0.0431(9) -0.0069(7) -0.0070(7) 0.0049(7) P1 0.0391(11) 0.0308(9) 0.0350(9) -0.0004(7) 0.0018(8) 0.0007(7) P2 0.0406(11) 0.0406(10) 0.0319(9) 0.0034(8) 0.0030(8) 0.0013(8) P3 0.0406(11) 0.0452(10) 0.0306(9) -0.0036(8) -0.0007(7) 0.0079(8) P4 0.0367(11) 0.0303(9) 0.0363(9) -0.0013(7) 0.0031(8) 0.0022(7) O1 0.077(4) 0.069(3) 0.054(3) 0.003(3) -0.016(3) 0.029(3) C1 0.042(5) 0.044(4) 0.049(4) -0.009(3) 0.003(4) 0.005(3) O2 0.076(4) 0.075(3) 0.037(3) 0.016(2) -0.004(3) 0.002(3) C2 0.043(4) 0.031(4) 0.046(4) -0.001(3) 0.012(3) -0.003(3) O3 0.116(5) 0.059(3) 0.067(3) -0.015(3) 0.015(3) 0.037(3) C3 0.057(5) 0.054(5) 0.040(4) 0.007(3) -0.005(3) 0.008(4) O4 0.038(4) 0.087(4) 0.138(5) 0.033(3) 0.002(3) -0.008(3) C4 0.040(5) 0.049(4) 0.076(5) 0.003(4) 0.001(4) 0.007(4) O5 0.059(4) 0.064(3) 0.089(4) -0.015(3) 0.037(3) -0.002(3) C5 0.054(5) 0.044(4) 0.051(4) -0.001(3) 0.008(4) -0.002(3) O6 0.060(4) 0.077(4) 0.093(4) -0.012(3) -0.017(3) -0.013(3) C6 0.052(5) 0.035(4) 0.066(5) -0.006(3) 0.017(4) 0.005(3) O7 0.166(7) 0.049(4) 0.130(5) 0.043(4) 0.056(5) 0.006(4) C7 0.065(6) 0.053(5) 0.072(5) 0.004(4) 0.026(4) 0.002(4) O8 0.058(4) 0.099(4) 0.051(3) -0.017(3) -0.012(3) 0.011(3) C8 0.050(5) 0.052(4) 0.035(4) -0.003(3) 0.006(3) 0.014(3) C9 0.044(4) 0.054(4) 0.027(3) 0.001(3) -0.001(3) 0.006(3) C1A 0.041(4) 0.036(4) 0.040(4) 0.001(3) 0.002(3) -0.004(3) C2A 0.066(6) 0.049(5) 0.082(6) 0.013(4) 0.022(4) 0.000(4) C3A 0.101(8) 0.039(5) 0.132(8) 0.018(5) 0.042(6) 0.020(4) C4A 0.090(7) 0.043(5) 0.097(6) 0.026(4) 0.014(5) -0.007(4) C5A 0.082(6) 0.040(5) 0.084(6) 0.007(4) 0.027(5) -0.013(4) C6A 0.058(5) 0.041(4) 0.062(5) -0.004(3) 0.022(4) -0.005(3) C1B 0.036(4) 0.044(4) 0.031(3) -0.006(3) 0.002(3) 0.004(3) C2B 0.052(5) 0.051(4) 0.049(4) -0.003(3) -0.003(4) -0.009(3) C3B 0.060(6) 0.091(7) 0.056(5) -0.013(4) 0.000(4) -0.025(5) C4B 0.042(5) 0.104(7) 0.052(5) -0.004(5) -0.009(4) 0.003(5) C5B 0.062(6) 0.069(5) 0.044(4) 0.004(4) 0.002(4) 0.016(4) C6B 0.042(5) 0.056(4) 0.045(4) -0.001(3) -0.003(3) 0.001(3) C1C 0.057(5) 0.048(4) 0.034(4) 0.012(3) -0.001(3) -0.002(3) C2C 0.047(6) 0.078(6) 0.098(6) 0.040(5) -0.003(5) 0.002(4) C3C 0.067(7) 0.091(7) 0.131(8) 0.051(6) -0.018(6) 0.013(5) C4C 0.095(9) 0.096(7) 0.129(9) 0.072(6) -0.009(7) 0.006(6) C5C 0.122(10) 0.098(8) 0.098(7) 0.055(6) 0.025(7) -0.008(6) C6C 0.088(7) 0.068(5) 0.076(6) 0.032(4) 0.030(5) 0.013(4) C1D 0.041(4) 0.042(4) 0.036(4) 0.006(3) 0.012(3) 0.003(3) C2D 0.041(5) 0.060(4) 0.050(4) -0.006(3) 0.008(4) 0.011(3) C3D 0.052(6) 0.093(6) 0.074(6) -0.018(5) -0.014(5) 0.012(4) C4D 0.033(5) 0.099(7) 0.113(8) 0.003(6) 0.006(5) 0.004(4) C5D 0.045(6) 0.093(6) 0.092(7) -0.004(5) 0.031(5) -0.004(4) C6D 0.052(5) 0.074(5) 0.047(4) 0.005(4) 0.012(4) -0.003(4) C1E 0.047(5) 0.062(5) 0.040(4) 0.006(3) 0.009(4) 0.014(3) C2E 0.045(5) 0.075(5) 0.068(5) 0.008(4) 0.004(4) 0.014(4) C3E 0.052(6) 0.096(7) 0.112(7) 0.027(6) -0.013(5) 0.014(5) C4E 0.104(10) 0.130(9) 0.083(7) 0.020(6) 0.028(7) 0.074(7) C5E 0.114(10) 0.169(10) 0.059(6) -0.012(6) 0.004(6) 0.093(8) C6E 0.080(7) 0.116(7) 0.043(4) -0.016(5) -0.005(4) 0.050(5) C1F 0.043(5) 0.057(5) 0.043(4) -0.014(3) -0.007(3) 0.016(3) C2F 0.069(6) 0.073(5) 0.040(4) -0.018(4) -0.011(4) 0.027(4) C3F 0.087(7) 0.111(7) 0.040(4) -0.034(5) -0.028(5) 0.050(6) C4F 0.082(8) 0.104(9) 0.115(9) -0.065(7) -0.051(7) 0.024(6) C5F 0.119(9) 0.098(8) 0.099(8) -0.028(6) -0.034(7) -0.024(6) C6F 0.104(8) 0.075(6) 0.061(5) -0.017(5) -0.014(5) -0.014(5) C1G 0.043(4) 0.032(4) 0.038(4) -0.005(3) -0.003(3) 0.005(3) C2G 0.056(5) 0.048(4) 0.055(4) -0.021(3) 0.007(4) 0.002(3) C3G 0.088(8) 0.073(6) 0.100(7) -0.046(5) 0.018(6) 0.015(5) C4G 0.090(8) 0.070(6) 0.126(8) -0.061(5) 0.013(6) 0.000(5) C5G 0.070(6) 0.048(5) 0.133(8) -0.037(5) 0.006(6) -0.019(4) C6G 0.062(6) 0.045(4) 0.076(5) -0.014(4) 0.003(4) -0.005(4) C1H 0.044(4) 0.031(4) 0.036(3) -0.004(3) 0.008(3) 0.006(3) C2H 0.044(5) 0.051(4) 0.059(4) 0.002(3) 0.002(4) 0.002(3) C3H 0.060(6) 0.066(5) 0.064(5) -0.012(4) -0.002(4) -0.015(4) C4H 0.045(5) 0.094(7) 0.052(5) -0.011(4) -0.015(4) 0.006(4) C5H 0.068(6) 0.073(6) 0.047(4) -0.006(4) -0.010(4) 0.024(4) C6H 0.055(5) 0.048(4) 0.041(4) -0.005(3) -0.004(3) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C5 2.616(6) . ? Ag1 Mn2 2.6629(9) . ? Ag1 C4 2.683(7) . ? Ag1 Mn1 2.7246(9) . ? Ag1 Pd1 2.7259(6) . ? Ag1 Pd2 2.8014(6) . ? Pd1 P1 2.2295(16) . ? Pd1 P2 2.3416(15) . ? Pd1 Cl1 2.4695(15) . ? Pd1 Mn1 2.7934(9) . ? Pd1 Pd2 3.1981(6) . ? Pd2 P4 2.2057(16) . ? Pd2 P3 2.3140(15) . ? Pd2 Cl1 2.4760(15) . ? Pd2 Mn2 2.8432(9) . ? Mn1 C3 1.789(7) . ? Mn1 C1 1.820(7) . ? Mn1 C4 1.824(7) . ? Mn1 C2 1.840(7) . ? Mn1 P1 2.2426(18) . ? Mn2 C7 1.788(7) . ? Mn2 C5 1.823(7) . ? Mn2 C6 1.825(8) . ? Mn2 C8 1.858(7) . ? Mn2 P4 2.2430(17) . ? P1 C1B 1.824(6) . ? P1 C1A 1.826(6) . ? P2 C1D 1.805(6) . ? P2 C1C 1.836(6) . ? P2 C9 1.838(6) . ? P3 C1E 1.822(6) . ? P3 C1F 1.831(7) . ? P3 C9 1.845(5) . ? P4 C1H 1.796(6) . ? P4 C1G 1.824(6) . ? O1 C1 1.156(7) . ? O2 C2 1.140(7) . ? O3 C3 1.145(7) . ? O4 C4 1.148(7) . ? O5 C5 1.147(6) . ? O6 C6 1.159(8) . ? O7 C7 1.139(7) . ? O8 C8 1.131(7) . ? C1A C2A 1.359(8) . ? C1A C6A 1.372(7) . ? C2A C3A 1.382(8) . ? C3A C4A 1.370(9) . ? C4A C5A 1.361(9) . ? C5A C6A 1.373(8) . ? C1B C2B 1.381(8) . ? C1B C6B 1.382(7) . ? C2B C3B 1.378(9) . ? C3B C4B 1.364(9) . ? C4B C5B 1.360(9) . ? C5B C6B 1.364(9) . ? C1C C6C 1.367(8) . ? C1C C2C 1.372(9) . ? C2C C3C 1.367(9) . ? C3C C4C 1.352(10) . ? C4C C5C 1.351(11) . ? C5C C6C 1.379(9) . ? C1D C2D 1.370(8) . ? C1D C6D 1.392(8) . ? C2D C3D 1.392(9) . ? C3D C4D 1.365(9) . ? C4D C5D 1.359(10) . ? C5D C6D 1.373(9) . ? C1E C2E 1.367(9) . ? C1E C6E 1.391(9) . ? C2E C3E 1.394(9) . ? C3E C4E 1.352(11) . ? C4E C5E 1.355(13) . ? C5E C6E 1.386(10) . ? C1F C6F 1.362(9) . ? C1F C2F 1.386(8) . ? C2F C3F 1.383(10) . ? C3F C4F 1.361(11) . ? C4F C5F 1.342(12) . ? C5F C6F 1.388(10) . ? C1G C6G 1.382(8) . ? C1G C2G 1.388(7) . ? C2G C3G 1.387(8) . ? C3G C4G 1.373(10) . ? C4G C5G 1.350(9) . ? C5G C6G 1.379(8) . ? C1H C6H 1.385(8) . ? C1H C2H 1.393(8) . ? C2H C3H 1.383(9) . ? C3H C4H 1.361(9) . ? C4H C5H 1.373(9) . ? C5H C6H 1.362(9) . ? O1S C1S 1.184(8) . ? C1S C3S 1.439(8) . ? C1S C2S 1.486(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ag1 Mn2 40.38(15) . . ? C5 Ag1 C4 88.7(2) . . ? Mn2 Ag1 C4 127.37(15) . . ? C5 Ag1 Mn1 124.34(15) . . ? Mn2 Ag1 Mn1 164.62(3) . . ? C4 Ag1 Mn1 39.43(15) . . ? C5 Ag1 Pd1 160.86(15) . . ? Mn2 Ag1 Pd1 133.06(3) . . ? C4 Ag1 Pd1 89.37(15) . . ? Mn1 Ag1 Pd1 61.66(2) . . ? C5 Ag1 Pd2 97.61(14) . . ? Mn2 Ag1 Pd2 62.65(2) . . ? C4 Ag1 Pd2 134.88(16) . . ? Mn1 Ag1 Pd2 130.97(3) . . ? Pd1 Ag1 Pd2 70.688(16) . . ? P1 Pd1 P2 111.40(6) . . ? P1 Pd1 Cl1 153.71(6) . . ? P2 Pd1 Cl1 93.24(5) . . ? P1 Pd1 Ag1 92.49(4) . . ? P2 Pd1 Ag1 138.03(4) . . ? Cl1 Pd1 Ag1 73.67(4) . . ? P1 Pd1 Mn1 51.56(4) . . ? P2 Pd1 Mn1 160.46(5) . . ? Cl1 Pd1 Mn1 102.49(4) . . ? Ag1 Pd1 Mn1 59.15(2) . . ? P1 Pd1 Pd2 138.07(4) . . ? P2 Pd1 Pd2 85.06(4) . . ? Cl1 Pd1 Pd2 49.80(4) . . ? Ag1 Pd1 Pd2 55.759(14) . . ? Mn1 Pd1 Pd2 113.94(2) . . ? P4 Pd2 P3 107.71(6) . . ? P4 Pd2 Cl1 161.37(6) . . ? P3 Pd2 Cl1 88.02(5) . . ? P4 Pd2 Ag1 97.71(4) . . ? P3 Pd2 Ag1 146.42(4) . . ? Cl1 Pd2 Ag1 72.22(4) . . ? P4 Pd2 Mn2 50.85(4) . . ? P3 Pd2 Mn2 156.37(5) . . ? Cl1 Pd2 Mn2 111.63(4) . . ? Ag1 Pd2 Mn2 56.29(2) . . ? P4 Pd2 Pd1 136.18(5) . . ? P3 Pd2 Pd1 92.94(4) . . ? Cl1 Pd2 Pd1 49.62(4) . . ? Ag1 Pd2 Pd1 53.553(14) . . ? Mn2 Pd2 Pd1 109.67(2) . . ? C3 Mn1 C1 92.6(3) . . ? C3 Mn1 C4 94.7(3) . . ? C1 Mn1 C4 88.2(3) . . ? C3 Mn1 C2 88.6(3) . . ? C1 Mn1 C2 177.9(3) . . ? C4 Mn1 C2 93.4(3) . . ? C3 Mn1 P1 106.0(2) . . ? C1 Mn1 P1 88.6(2) . . ? C4 Mn1 P1 159.1(2) . . ? C2 Mn1 P1 89.43(19) . . ? C3 Mn1 Ag1 153.8(2) . . ? C1 Mn1 Ag1 106.75(18) . . ? C4 Mn1 Ag1 69.1(2) . . ? C2 Mn1 Ag1 72.60(17) . . ? P1 Mn1 Ag1 92.23(5) . . ? C3 Mn1 Pd1 146.9(2) . . ? C1 Mn1 Pd1 66.38(18) . . ? C4 Mn1 Pd1 109.1(2) . . ? C2 Mn1 Pd1 111.76(18) . . ? P1 Mn1 Pd1 51.14(4) . . ? Ag1 Mn1 Pd1 59.19(2) . . ? C7 Mn2 C5 95.1(3) . . ? C7 Mn2 C6 97.2(3) . . ? C5 Mn2 C6 86.3(3) . . ? C7 Mn2 C8 94.6(3) . . ? C5 Mn2 C8 91.3(3) . . ? C6 Mn2 C8 168.1(3) . . ? C7 Mn2 P4 95.8(2) . . ? C5 Mn2 P4 169.07(19) . . ? C6 Mn2 P4 92.6(2) . . ? C8 Mn2 P4 87.49(19) . . ? C7 Mn2 Ag1 159.3(2) . . ? C5 Mn2 Ag1 68.42(19) . . ? C6 Mn2 Ag1 94.20(19) . . ? C8 Mn2 Ag1 74.12(19) . . ? P4 Mn2 Ag1 100.85(5) . . ? C7 Mn2 Pd2 139.5(2) . . ? C5 Mn2 Pd2 120.3(2) . . ? C6 Mn2 Pd2 68.5(2) . . ? C8 Mn2 Pd2 102.95(19) . . ? P4 Mn2 Pd2 49.70(4) . . ? Ag1 Mn2 Pd2 61.06(2) . . ? Pd1 Cl1 Pd2 80.58(5) . . ? C1B P1 C1A 103.7(3) . . ? C1B P1 Pd1 118.83(19) . . ? C1A P1 Pd1 113.3(2) . . ? C1B P1 Mn1 122.62(19) . . ? C1A P1 Mn1 120.0(2) . . ? Pd1 P1 Mn1 77.31(6) . . ? C1D P2 C1C 105.6(3) . . ? C1D P2 C9 103.8(3) . . ? C1C P2 C9 100.7(3) . . ? C1D P2 Pd1 121.7(2) . . ? C1C P2 Pd1 110.2(2) . . ? C9 P2 Pd1 112.6(2) . . ? C1E P3 C1F 103.7(3) . . ? C1E P3 C9 106.1(3) . . ? C1F P3 C9 102.1(3) . . ? C1E P3 Pd2 122.0(2) . . ? C1F P3 Pd2 109.8(2) . . ? C9 P3 Pd2 111.11(18) . . ? C1H P4 C1G 103.5(3) . . ? C1H P4 Pd2 119.3(2) . . ? C1G P4 Pd2 112.8(2) . . ? C1H P4 Mn2 119.45(18) . . ? C1G P4 Mn2 121.8(2) . . ? Pd2 P4 Mn2 79.45(6) . . ? O1 C1 Mn1 174.9(6) . . ? O2 C2 Mn1 173.3(5) . . ? O3 C3 Mn1 179.3(6) . . ? O4 C4 Mn1 173.6(6) . . ? O4 C4 Ag1 114.8(5) . . ? Mn1 C4 Ag1 71.5(2) . . ? O5 C5 Mn2 173.8(6) . . ? O5 C5 Ag1 114.8(5) . . ? Mn2 C5 Ag1 71.2(2) . . ? O6 C6 Mn2 175.4(6) . . ? O7 C7 Mn2 179.6(8) . . ? O8 C8 Mn2 177.4(6) . . ? P2 C9 P3 118.4(3) . . ? C2A C1A C6A 117.4(6) . . ? C2A C1A P1 120.0(5) . . ? C6A C1A P1 122.5(5) . . ? C1A C2A C3A 122.2(7) . . ? C4A C3A C2A 118.7(7) . . ? C5A C4A C3A 120.2(7) . . ? C4A C5A C6A 119.6(7) . . ? C1A C6A C5A 121.8(6) . . ? C2B C1B C6B 117.8(6) . . ? C2B C1B P1 122.7(5) . . ? C6B C1B P1 119.5(5) . . ? C3B C2B C1B 120.3(7) . . ? C4B C3B C2B 120.6(7) . . ? C5B C4B C3B 119.6(8) . . ? C4B C5B C6B 120.2(7) . . ? C5B C6B C1B 121.5(6) . . ? C6C C1C C2C 117.4(6) . . ? C6C C1C P2 124.0(6) . . ? C2C C1C P2 118.4(5) . . ? C3C C2C C1C 121.1(7) . . ? C4C C3C C2C 120.3(9) . . ? C5C C4C C3C 120.0(8) . . ? C4C C5C C6C 119.5(8) . . ? C1C C6C C5C 121.5(8) . . ? C2D C1D C6D 116.7(6) . . ? C2D C1D P2 119.2(5) . . ? C6D C1D P2 124.0(5) . . ? C1D C2D C3D 121.9(6) . . ? C4D C3D C2D 119.4(7) . . ? C5D C4D C3D 120.0(8) . . ? C4D C5D C6D 120.1(7) . . ? C5D C6D C1D 121.7(7) . . ? C2E C1E C6E 117.5(6) . . ? C2E C1E P3 120.2(5) . . ? C6E C1E P3 122.1(6) . . ? C1E C2E C3E 121.3(8) . . ? C4E C3E C2E 119.4(9) . . ? C3E C4E C5E 121.2(9) . . ? C4E C5E C6E 119.4(9) . . ? C5E C6E C1E 121.1(8) . . ? C6F C1F C2F 119.2(7) . . ? C6F C1F P3 118.1(5) . . ? C2F C1F P3 122.6(6) . . ? C3F C2F C1F 119.7(8) . . ? C4F C3F C2F 119.7(8) . . ? C5F C4F C3F 121.1(9) . . ? C4F C5F C6F 119.9(9) . . ? C1F C6F C5F 120.3(8) . . ? C6G C1G C2G 118.6(6) . . ? C6G C1G P4 120.5(5) . . ? C2G C1G P4 120.8(5) . . ? C1G C2G C3G 119.9(7) . . ? C4G C3G C2G 120.9(7) . . ? C5G C4G C3G 118.7(8) . . ? C4G C5G C6G 121.9(7) . . ? C5G C6G C1G 120.0(7) . . ? C6H C1H C2H 117.5(6) . . ? C6H C1H P4 121.4(5) . . ? C2H C1H P4 120.9(5) . . ? C3H C2H C1H 120.6(6) . . ? C4H C3H C2H 120.6(7) . . ? C3H C4H C5H 119.2(8) . . ? C6H C5H C4H 120.9(7) . . ? C5H C6H C1H 121.2(7) . . ? O1S C1S C3S 126.2(10) . . ? O1S C1S C2S 117.1(10) . . ? C3S C1S C2S 113.6(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.981 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.127 data_1280 _database_code_CSD 180413 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H44 Fe Mn O5 P3 Pd' _chemical_formula_weight 1070.98 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' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4500(6) _cell_length_b 10.7239(5) _cell_length_c 33.3018(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.5950(10) _cell_angle_gamma 90.00 _cell_volume 4798.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4623 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.2 _exptl_crystal_description 'thin plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8468 _exptl_absorpt_correction_T_max 0.9189 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27407 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8445 _reflns_number_gt 5967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0080P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8445 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0604 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _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 Pd1 Pd 0.27807(2) 0.34849(3) 0.624018(9) 0.03045(9) Uani 1 1 d . . . Mn1 Mn 0.07328(4) 0.32453(5) 0.624477(18) 0.03639(17) Uani 1 1 d . . . Fe1 Fe 0.55839(4) 0.23214(5) 0.579896(17) 0.03706(16) Uani 1 1 d . . . P1 P 0.17608(7) 0.38179(9) 0.67525(3) 0.0337(3) Uani 1 1 d . . . P2 P 0.30797(8) 0.27448(9) 0.55879(3) 0.0333(3) Uani 1 1 d . . . P3 P 0.43712(8) 0.40507(9) 0.64889(3) 0.0323(3) Uani 1 1 d . . . C1 C 0.0604(3) 0.4833(4) 0.60665(13) 0.0452(12) Uani 1 1 d . . . O1 O 0.0464(2) 0.5836(3) 0.59450(10) 0.0727(11) Uani 1 1 d . . . C2 C -0.0441(3) 0.3343(4) 0.64651(13) 0.0466(11) Uani 1 1 d . . . O2 O -0.1201(2) 0.3455(3) 0.66126(9) 0.0677(9) Uani 1 1 d . . . C3 C 0.0978(3) 0.1649(4) 0.64032(13) 0.0483(12) Uani 1 1 d . . . O3 O 0.1083(3) 0.0623(3) 0.65083(10) 0.0743(11) Uani 1 1 d . . . C4 C 0.0390(3) 0.2684(4) 0.57476(14) 0.0453(12) Uani 1 1 d . . . O4 O 0.0138(2) 0.2321(3) 0.54304(10) 0.0675(10) Uani 1 1 d . . . C5 C 0.4350(3) 0.2506(3) 0.54298(11) 0.0341(10) Uani 1 1 d . . . C6 C 0.5046(3) 0.3471(4) 0.53589(11) 0.0391(10) Uani 1 1 d . . . H6 H 0.4924 0.4377 0.5387 0.047 Uiso 1 1 calc R . . C7 C 0.5935(3) 0.2924(4) 0.52447(12) 0.0509(12) Uani 1 1 d . . . H7 H 0.6549 0.3376 0.5180 0.061 Uiso 1 1 calc R . . C8 C 0.5811(3) 0.1633(4) 0.52416(12) 0.0503(12) Uani 1 1 d . . . H8 H 0.6322 0.1012 0.5174 0.060 Uiso 1 1 calc R . . C9 C 0.4835(3) 0.1364(4) 0.53489(11) 0.0404(11) Uani 1 1 d . . . H9 H 0.4543 0.0521 0.5372 0.049 Uiso 1 1 calc R . . C10 C 0.5353(3) 0.3024(3) 0.63484(11) 0.0332(10) Uani 1 1 d . . . C11 C 0.6343(3) 0.3286(4) 0.62406(11) 0.0412(11) Uani 1 1 d . . . H11 H 0.6634 0.4128 0.6212 0.049 Uiso 1 1 calc R . . C12 C 0.6831(3) 0.2156(4) 0.61708(12) 0.0507(13) Uani 1 1 d . . . H12 H 0.7521 0.2064 0.6084 0.061 Uiso 1 1 calc R . . C13 C 0.6168(3) 0.1186(4) 0.62369(12) 0.0481(12) Uani 1 1 d . . . H13 H 0.6312 0.0286 0.6207 0.058 Uiso 1 1 calc R . . C14 C 0.5265(3) 0.1695(3) 0.63456(11) 0.0394(10) Uani 1 1 d . . . H14 H 0.4664 0.1216 0.6411 0.047 Uiso 1 1 calc R . . C1A C 0.1889(3) 0.2741(3) 0.71788(12) 0.0366(10) Uani 1 1 d . . . C2A C 0.2764(3) 0.2092(3) 0.72557(12) 0.0459(12) Uani 1 1 d . . . H2A H 0.3314 0.2241 0.7098 0.055 Uiso 1 1 calc R . . C3A C 0.2836(4) 0.1225(4) 0.75628(14) 0.0575(13) Uani 1 1 d . . . H3A H 0.3440 0.0803 0.7617 0.069 Uiso 1 1 calc R . . C4A C 0.2043(4) 0.0980(4) 0.77865(14) 0.0662(15) Uani 1 1 d . . . H4A H 0.2096 0.0385 0.7994 0.079 Uiso 1 1 calc R . . C5A C 0.1167(4) 0.1598(5) 0.77112(14) 0.0705(15) Uani 1 1 d . . . H5A H 0.0615 0.1427 0.7866 0.085 Uiso 1 1 calc R . . C6A C 0.1091(3) 0.2475(4) 0.74069(14) 0.0606(14) Uani 1 1 d . . . H6A H 0.0486 0.2896 0.7356 0.073 Uiso 1 1 calc R . . C1B C 0.1723(3) 0.5358(4) 0.69843(13) 0.0403(11) Uani 1 1 d . . . C2B C 0.1852(3) 0.6412(4) 0.67454(14) 0.0560(13) Uani 1 1 d . . . H2B H 0.1960 0.6318 0.6470 0.067 Uiso 1 1 calc R . . C3B C 0.1823(4) 0.7587(5) 0.6911(2) 0.0805(18) Uani 1 1 d . . . H3B H 0.1888 0.8288 0.6745 0.097 Uiso 1 1 calc R . . C4B C 0.1701(4) 0.7747(5) 0.7310(2) 0.091(2) Uani 1 1 d . . . H4B H 0.1690 0.8554 0.7419 0.109 Uiso 1 1 calc R . . C5B C 0.1596(4) 0.6732(5) 0.75495(18) 0.0831(18) Uani 1 1 d . . . H5B H 0.1517 0.6840 0.7826 0.100 Uiso 1 1 calc R . . C6B C 0.1605(3) 0.5545(4) 0.73891(14) 0.0581(14) Uani 1 1 d . . . H6B H 0.1529 0.4853 0.7558 0.070 Uiso 1 1 calc R . . C1C C 0.2591(3) 0.3639(4) 0.51579(12) 0.0360(10) Uani 1 1 d . . . C2C C 0.2865(3) 0.3416(4) 0.47687(13) 0.0516(12) Uani 1 1 d . . . H2C H 0.3327 0.2782 0.4720 0.062 Uiso 1 1 calc R . . C3C C 0.2470(4) 0.4113(4) 0.44504(14) 0.0638(14) Uani 1 1 d . . . H3C H 0.2662 0.3948 0.4188 0.077 Uiso 1 1 calc R . . C4C C 0.1804(4) 0.5039(4) 0.45168(15) 0.0606(14) Uani 1 1 d . . . H4C H 0.1530 0.5502 0.4299 0.073 Uiso 1 1 calc R . . C5C C 0.1535(3) 0.5297(4) 0.48971(16) 0.0594(14) Uani 1 1 d . . . H5C H 0.1082 0.5944 0.4943 0.071 Uiso 1 1 calc R . . C6C C 0.1933(3) 0.4600(4) 0.52175(13) 0.0446(11) Uani 1 1 d . . . H6D' H 0.1749 0.4787 0.5480 0.053 Uiso 1 1 calc R . . C1D C 0.2589(3) 0.1164(3) 0.55150(13) 0.0375(10) Uani 1 1 d . . . C2D C 0.2107(3) 0.0735(4) 0.51699(14) 0.0577(14) Uani 1 1 d . . . H2D H 0.2000 0.1276 0.4950 0.069 Uiso 1 1 calc R . . C3D C 0.1776(4) -0.0483(5) 0.51417(19) 0.0833(19) Uani 1 1 d . . . H3D H 0.1454 -0.0764 0.4902 0.100 Uiso 1 1 calc R . . C4D C 0.1914(4) -0.1278(5) 0.5457(2) 0.087(2) Uani 1 1 d . . . H4D H 0.1676 -0.2101 0.5438 0.104 Uiso 1 1 calc R . . C5D C 0.2395(4) -0.0882(5) 0.58009(18) 0.0807(18) Uani 1 1 d . . . H5D H 0.2506 -0.1433 0.6018 0.097 Uiso 1 1 calc R . . C6D C 0.2719(3) 0.0342(4) 0.58289(15) 0.0589(14) Uani 1 1 d . . . H6D H 0.3037 0.0617 0.6070 0.071 Uiso 1 1 calc R . . C1E C 0.4653(3) 0.4189(3) 0.70314(11) 0.0321(10) Uani 1 1 d . . . C2E C 0.5331(3) 0.3412(4) 0.72323(12) 0.0490(12) Uani 1 1 d . . . H2E H 0.5714 0.2853 0.7086 0.059 Uiso 1 1 calc R . . C3E C 0.5450(4) 0.3454(4) 0.76483(14) 0.0624(14) Uani 1 1 d . . . H3E H 0.5900 0.2910 0.7783 0.075 Uiso 1 1 calc R . . C4E C 0.4917(4) 0.4278(4) 0.78617(13) 0.0574(14) Uani 1 1 d . . . H4E H 0.5002 0.4308 0.8143 0.069 Uiso 1 1 calc R . . C5E C 0.4258(3) 0.5063(4) 0.76674(13) 0.0499(12) Uani 1 1 d . . . H5E H 0.3889 0.5633 0.7815 0.060 Uiso 1 1 calc R . . C6E C 0.4134(3) 0.5023(3) 0.72559(13) 0.0393(11) Uani 1 1 d . . . H6E H 0.3685 0.5577 0.7125 0.047 Uiso 1 1 calc R . . C1F C 0.4745(3) 0.5568(3) 0.63005(12) 0.0340(10) Uani 1 1 d . . . C2F C 0.5556(3) 0.6219(4) 0.64653(12) 0.0445(11) Uani 1 1 d . . . H2F H 0.5910 0.5896 0.6692 0.053 Uiso 1 1 calc R . . C3F C 0.5850(3) 0.7328(4) 0.63028(15) 0.0586(13) Uani 1 1 d . . . H3F H 0.6401 0.7757 0.6419 0.070 Uiso 1 1 calc R . . C4F C 0.5348(4) 0.7815(4) 0.59725(15) 0.0647(15) Uani 1 1 d . . . H4F H 0.5563 0.8564 0.5858 0.078 Uiso 1 1 calc R . . C5F C 0.4530(4) 0.7204(4) 0.58104(13) 0.0583(14) Uani 1 1 d . . . H5F H 0.4173 0.7543 0.5587 0.070 Uiso 1 1 calc R . . C6F C 0.4230(3) 0.6094(4) 0.59743(12) 0.0439(11) Uani 1 1 d . . . H6F H 0.3665 0.5686 0.5862 0.053 Uiso 1 1 calc R . . O1S O -0.2179(3) -0.0847(4) 0.59171(14) 0.1297(17) Uani 1 1 d . . . C1S C -0.0511(4) -0.1225(6) 0.5857(2) 0.144(3) Uani 1 1 d . . . H1S1 H -0.0730 -0.1593 0.5602 0.217 Uiso 1 1 calc R . . H1S2 H -0.0087 -0.1811 0.6006 0.217 Uiso 1 1 calc R . . H1S3 H -0.0141 -0.0467 0.5808 0.217 Uiso 1 1 calc R . . C2S C -0.1380(5) -0.0929(6) 0.6090(2) 0.096(2) Uani 1 1 d . . . C3S C -0.1311(6) -0.0820(9) 0.6510(2) 0.228(5) Uani 1 1 d . . . H3S1 H -0.1966 -0.0666 0.6609 0.342 Uiso 1 1 calc R . . H3S2 H -0.0873 -0.0132 0.6585 0.342 Uiso 1 1 calc R . . H3S3 H -0.1045 -0.1587 0.6626 0.342 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 Pd1 0.02951(17) 0.03349(17) 0.02825(19) -0.00242(15) 0.00030(14) 0.00087(16) Mn1 0.0325(4) 0.0383(4) 0.0380(4) -0.0011(3) -0.0018(3) 0.0006(3) Fe1 0.0331(3) 0.0434(4) 0.0347(4) -0.0081(3) 0.0003(3) 0.0020(3) P1 0.0316(6) 0.0371(6) 0.0323(7) -0.0012(5) 0.0020(5) 0.0017(5) P2 0.0325(6) 0.0376(6) 0.0296(7) -0.0035(5) -0.0003(5) -0.0011(5) P3 0.0334(6) 0.0342(6) 0.0291(7) -0.0032(5) -0.0013(5) -0.0006(5) C1 0.032(3) 0.060(3) 0.042(3) -0.006(2) -0.003(2) 0.002(2) O1 0.078(3) 0.052(2) 0.087(3) 0.0150(19) -0.011(2) 0.014(2) C2 0.046(3) 0.048(3) 0.046(3) 0.002(2) -0.001(2) -0.004(3) O2 0.045(2) 0.090(2) 0.070(3) 0.003(2) 0.0184(18) -0.002(2) C3 0.049(3) 0.050(3) 0.046(3) -0.008(2) -0.005(2) -0.007(3) O3 0.098(3) 0.0383(19) 0.086(3) 0.0054(18) -0.010(2) -0.001(2) C4 0.041(3) 0.044(3) 0.051(3) 0.001(2) -0.002(2) 0.003(2) O4 0.073(2) 0.077(2) 0.050(2) -0.0176(18) -0.0166(19) 0.0040(19) C5 0.040(2) 0.038(2) 0.025(2) -0.0061(19) 0.000(2) -0.001(2) C6 0.044(3) 0.043(2) 0.031(3) 0.000(2) 0.005(2) -0.006(2) C7 0.037(3) 0.080(4) 0.037(3) -0.006(2) 0.007(2) -0.011(3) C8 0.039(3) 0.072(3) 0.040(3) -0.019(3) 0.007(2) 0.004(3) C9 0.042(3) 0.044(3) 0.036(3) -0.014(2) -0.001(2) -0.002(2) C10 0.032(2) 0.036(2) 0.030(3) -0.0039(18) -0.007(2) -0.004(2) C11 0.040(3) 0.042(3) 0.041(3) -0.007(2) -0.004(2) -0.002(2) C12 0.037(3) 0.065(3) 0.049(3) -0.020(2) -0.007(2) 0.011(3) C13 0.053(3) 0.040(3) 0.050(3) -0.010(2) -0.009(2) 0.013(2) C14 0.045(3) 0.036(2) 0.038(3) -0.001(2) 0.000(2) 0.002(2) C1A 0.037(2) 0.044(3) 0.029(3) 0.000(2) 0.002(2) -0.003(2) C2A 0.049(3) 0.047(3) 0.042(3) 0.003(2) 0.000(2) -0.005(2) C3A 0.063(3) 0.054(3) 0.054(4) 0.013(3) -0.009(3) -0.004(3) C4A 0.093(4) 0.060(3) 0.045(4) 0.018(3) -0.008(3) -0.018(3) C5A 0.067(4) 0.094(4) 0.051(4) 0.019(3) 0.012(3) -0.023(3) C6A 0.051(3) 0.081(4) 0.050(4) 0.013(3) 0.006(3) -0.006(3) C1B 0.028(2) 0.047(3) 0.046(3) -0.013(2) 0.002(2) 0.003(2) C2B 0.060(3) 0.045(3) 0.063(4) -0.010(3) -0.001(3) -0.003(3) C3B 0.073(4) 0.046(3) 0.122(6) -0.013(4) -0.002(4) -0.003(3) C4B 0.077(4) 0.060(4) 0.135(7) -0.051(4) 0.007(5) -0.001(3) C5B 0.069(4) 0.095(4) 0.087(5) -0.054(4) 0.021(3) -0.004(4) C6B 0.055(3) 0.067(3) 0.052(4) -0.021(3) 0.008(3) 0.003(3) C1C 0.030(2) 0.045(3) 0.033(3) -0.001(2) -0.001(2) -0.004(2) C2C 0.054(3) 0.062(3) 0.039(3) -0.003(3) 0.002(2) 0.008(3) C3C 0.071(4) 0.086(4) 0.034(3) 0.005(3) 0.003(3) -0.002(3) C4C 0.057(3) 0.079(4) 0.045(4) 0.023(3) -0.016(3) -0.007(3) C5C 0.047(3) 0.064(3) 0.066(4) 0.012(3) -0.001(3) 0.005(3) C6C 0.045(3) 0.052(3) 0.036(3) 0.007(2) 0.002(2) 0.001(2) C1D 0.029(2) 0.043(3) 0.040(3) -0.008(2) 0.007(2) -0.003(2) C2D 0.054(3) 0.061(3) 0.057(4) -0.019(3) -0.006(3) -0.006(3) C3D 0.073(4) 0.078(4) 0.100(5) -0.049(4) 0.011(4) -0.030(4) C4D 0.088(5) 0.053(4) 0.124(6) -0.032(4) 0.056(4) -0.029(4) C5D 0.098(5) 0.050(3) 0.096(5) 0.000(3) 0.029(4) -0.005(3) C6D 0.065(3) 0.047(3) 0.065(4) -0.006(3) 0.008(3) -0.011(3) C1E 0.034(2) 0.032(2) 0.030(3) 0.0000(19) -0.002(2) -0.003(2) C2E 0.066(3) 0.048(3) 0.032(3) -0.008(2) -0.008(2) 0.016(3) C3E 0.090(4) 0.054(3) 0.041(3) -0.002(3) -0.020(3) 0.017(3) C4E 0.093(4) 0.052(3) 0.027(3) -0.001(2) -0.006(3) -0.014(3) C5E 0.062(3) 0.049(3) 0.039(3) -0.016(2) 0.007(3) -0.005(3) C6E 0.038(3) 0.045(3) 0.035(3) -0.002(2) 0.002(2) 0.001(2) C1F 0.038(3) 0.035(2) 0.029(3) -0.0052(19) 0.002(2) 0.002(2) C2F 0.048(3) 0.043(3) 0.041(3) 0.004(2) -0.003(2) -0.003(2) C3F 0.061(3) 0.051(3) 0.065(4) -0.005(3) 0.007(3) -0.019(3) C4F 0.100(4) 0.040(3) 0.057(4) 0.002(3) 0.023(3) -0.008(3) C5F 0.085(4) 0.047(3) 0.043(3) 0.007(2) 0.003(3) 0.008(3) C6F 0.054(3) 0.041(3) 0.036(3) -0.002(2) -0.004(2) 0.000(2) O1S 0.100(4) 0.165(4) 0.123(4) -0.038(3) 0.003(3) 0.038(3) C1S 0.075(5) 0.162(7) 0.194(8) -0.063(6) -0.019(5) 0.018(5) C2S 0.051(4) 0.124(5) 0.111(6) -0.011(5) -0.015(4) -0.002(4) C3S 0.146(8) 0.450(15) 0.084(7) 0.080(8) -0.033(6) -0.086(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2654(11) . ? Pd1 P3 2.3388(10) . ? Pd1 P2 2.3641(11) . ? Pd1 Mn1 2.7672(7) . ? Mn1 C2 1.774(5) . ? Mn1 C4 1.802(5) . ? Mn1 C1 1.809(5) . ? Mn1 C3 1.817(4) . ? Mn1 P1 2.2216(12) . ? Fe1 C14 2.005(4) . ? Fe1 C10 2.016(4) . ? Fe1 C6 2.024(4) . ? Fe1 C5 2.029(4) . ? Fe1 C13 2.031(4) . ? Fe1 C7 2.031(4) . ? Fe1 C8 2.034(4) . ? Fe1 C11 2.035(4) . ? Fe1 C9 2.044(4) . ? Fe1 C12 2.047(4) . ? P1 C1B 1.825(4) . ? P1 C1A 1.832(4) . ? P2 C1C 1.822(4) . ? P2 C5 1.829(4) . ? P2 C1D 1.831(4) . ? P3 C10 1.798(4) . ? P3 C1F 1.823(4) . ? P3 C1E 1.835(4) . ? C1 O1 1.161(4) . ? C2 O2 1.160(4) . ? C3 O3 1.161(4) . ? C4 O4 1.162(4) . ? C5 C9 1.419(5) . ? C5 C6 1.422(5) . ? C6 C7 1.399(5) . ? C7 C8 1.395(5) . ? C8 C9 1.406(5) . ? C10 C11 1.423(5) . ? C10 C14 1.430(4) . ? C11 C12 1.402(5) . ? C12 C13 1.393(5) . ? C13 C14 1.395(5) . ? C1A C6A 1.372(5) . ? C1A C2A 1.381(5) . ? C2A C3A 1.382(5) . ? C3A C4A 1.354(6) . ? C4A C5A 1.365(6) . ? C5A C6A 1.384(5) . ? C1B C6B 1.379(5) . ? C1B C2B 1.397(5) . ? C2B C3B 1.377(5) . ? C3B C4B 1.356(7) . ? C4B C5B 1.362(7) . ? C5B C6B 1.381(6) . ? C1C C6C 1.379(5) . ? C1C C2C 1.384(5) . ? C2C C3C 1.383(5) . ? C3C C4C 1.362(6) . ? C4C C5C 1.361(6) . ? C5C C6C 1.390(5) . ? C1D C6D 1.373(5) . ? C1D C2D 1.373(5) . ? C2D C3D 1.381(6) . ? C3D C4D 1.359(7) . ? C4D C5D 1.357(7) . ? C5D C6D 1.384(5) . ? C1E C6E 1.376(5) . ? C1E C2E 1.385(5) . ? C2E C3E 1.388(5) . ? C3E C4E 1.359(6) . ? C4E C5E 1.364(5) . ? C5E C6E 1.374(5) . ? C1F C6F 1.382(5) . ? C1F C2F 1.387(5) . ? C2F C3F 1.372(5) . ? C3F C4F 1.368(6) . ? C4F C5F 1.370(6) . ? C5F C6F 1.378(5) . ? O1S C2S 1.198(6) . ? C1S C2S 1.467(8) . ? C2S C3S 1.404(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P3 105.53(4) . . ? P1 Pd1 P2 151.50(4) . . ? P3 Pd1 P2 102.81(4) . . ? P1 Pd1 Mn1 51.21(3) . . ? P3 Pd1 Mn1 156.47(3) . . ? P2 Pd1 Mn1 100.64(3) . . ? C2 Mn1 C4 101.80(19) . . ? C2 Mn1 C1 90.35(19) . . ? C4 Mn1 C1 89.79(18) . . ? C2 Mn1 C3 95.10(19) . . ? C4 Mn1 C3 89.28(18) . . ? C1 Mn1 C3 174.55(19) . . ? C2 Mn1 P1 101.76(14) . . ? C4 Mn1 P1 156.35(14) . . ? C1 Mn1 P1 92.10(13) . . ? C3 Mn1 P1 86.61(13) . . ? C2 Mn1 Pd1 154.37(14) . . ? C4 Mn1 Pd1 103.83(14) . . ? C1 Mn1 Pd1 89.51(13) . . ? C3 Mn1 Pd1 85.50(13) . . ? P1 Mn1 Pd1 52.64(3) . . ? C14 Fe1 C10 41.68(13) . . ? C14 Fe1 C6 141.05(16) . . ? C10 Fe1 C6 111.41(15) . . ? C14 Fe1 C5 112.34(16) . . ? C10 Fe1 C5 110.99(15) . . ? C6 Fe1 C5 41.09(13) . . ? C14 Fe1 C13 40.44(15) . . ? C10 Fe1 C13 69.07(15) . . ? C6 Fe1 C13 178.15(18) . . ? C5 Fe1 C13 140.62(17) . . ? C14 Fe1 C7 178.56(17) . . ? C10 Fe1 C7 139.26(17) . . ? C6 Fe1 C7 40.37(14) . . ? C5 Fe1 C7 68.63(16) . . ? C13 Fe1 C7 138.15(18) . . ? C14 Fe1 C8 138.95(18) . . ? C10 Fe1 C8 179.31(17) . . ? C6 Fe1 C8 67.90(17) . . ? C5 Fe1 C8 68.60(15) . . ? C13 Fe1 C8 111.61(17) . . ? C7 Fe1 C8 40.13(15) . . ? C14 Fe1 C11 68.60(16) . . ? C10 Fe1 C11 41.12(14) . . ? C6 Fe1 C11 111.40(16) . . ? C5 Fe1 C11 139.30(15) . . ? C13 Fe1 C11 67.69(15) . . ? C7 Fe1 C11 111.44(17) . . ? C8 Fe1 C11 138.86(17) . . ? C14 Fe1 C9 112.26(16) . . ? C10 Fe1 C9 139.68(16) . . ? C6 Fe1 C9 68.10(15) . . ? C5 Fe1 C9 40.77(13) . . ? C13 Fe1 C9 112.78(16) . . ? C7 Fe1 C9 67.69(16) . . ? C8 Fe1 C9 40.33(14) . . ? C11 Fe1 C9 179.11(17) . . ? C14 Fe1 C12 67.96(17) . . ? C10 Fe1 C12 68.83(15) . . ? C6 Fe1 C12 138.34(17) . . ? C5 Fe1 C12 179.37(17) . . ? C13 Fe1 C12 39.96(14) . . ? C7 Fe1 C12 111.08(18) . . ? C8 Fe1 C12 111.58(17) . . ? C11 Fe1 C12 40.19(13) . . ? C9 Fe1 C12 139.73(16) . . ? C1B P1 C1A 104.2(2) . . ? C1B P1 Mn1 122.96(14) . . ? C1A P1 Mn1 116.67(13) . . ? C1B P1 Pd1 119.38(15) . . ? C1A P1 Pd1 116.43(14) . . ? Mn1 P1 Pd1 76.15(4) . . ? C1C P2 C5 98.99(18) . . ? C1C P2 C1D 105.56(19) . . ? C5 P2 C1D 99.66(17) . . ? C1C P2 Pd1 118.37(14) . . ? C5 P2 Pd1 120.76(12) . . ? C1D P2 Pd1 110.94(14) . . ? C10 P3 C1F 103.86(18) . . ? C10 P3 C1E 100.62(18) . . ? C1F P3 C1E 102.63(17) . . ? C10 P3 Pd1 114.83(12) . . ? C1F P3 Pd1 111.84(13) . . ? C1E P3 Pd1 120.98(13) . . ? O1 C1 Mn1 176.0(4) . . ? O2 C2 Mn1 177.3(4) . . ? O3 C3 Mn1 176.5(4) . . ? O4 C4 Mn1 177.8(4) . . ? C9 C5 C6 106.6(3) . . ? C9 C5 P2 128.2(3) . . ? C6 C5 P2 125.2(3) . . ? C9 C5 Fe1 70.2(2) . . ? C6 C5 Fe1 69.2(2) . . ? P2 C5 Fe1 126.0(2) . . ? C7 C6 C5 108.4(4) . . ? C7 C6 Fe1 70.1(2) . . ? C5 C6 Fe1 69.7(2) . . ? C8 C7 C6 108.4(4) . . ? C8 C7 Fe1 70.0(2) . . ? C6 C7 Fe1 69.5(2) . . ? C7 C8 C9 108.3(4) . . ? C7 C8 Fe1 69.8(2) . . ? C9 C8 Fe1 70.2(2) . . ? C8 C9 C5 108.3(4) . . ? C8 C9 Fe1 69.4(2) . . ? C5 C9 Fe1 69.1(2) . . ? C11 C10 C14 105.9(3) . . ? C11 C10 P3 130.7(3) . . ? C14 C10 P3 123.4(3) . . ? C11 C10 Fe1 70.1(2) . . ? C14 C10 Fe1 68.8(2) . . ? P3 C10 Fe1 127.6(2) . . ? C12 C11 C10 108.7(4) . . ? C12 C11 Fe1 70.4(2) . . ? C10 C11 Fe1 68.7(2) . . ? C13 C12 C11 108.2(4) . . ? C13 C12 Fe1 69.4(2) . . ? C11 C12 Fe1 69.5(2) . . ? C12 C13 C14 108.6(4) . . ? C12 C13 Fe1 70.6(2) . . ? C14 C13 Fe1 68.8(2) . . ? C13 C14 C10 108.6(4) . . ? C13 C14 Fe1 70.8(3) . . ? C10 C14 Fe1 69.6(2) . . ? C6A C1A C2A 118.3(4) . . ? C6A C1A P1 120.7(3) . . ? C2A C1A P1 120.7(3) . . ? C1A C2A C3A 120.4(4) . . ? C4A C3A C2A 120.5(5) . . ? C3A C4A C5A 120.0(5) . . ? C4A C5A C6A 119.9(5) . . ? C1A C6A C5A 120.9(5) . . ? C6B C1B C2B 117.5(4) . . ? C6B C1B P1 123.5(4) . . ? C2B C1B P1 119.0(3) . . ? C3B C2B C1B 120.4(5) . . ? C4B C3B C2B 121.0(6) . . ? C3B C4B C5B 119.6(6) . . ? C4B C5B C6B 120.5(6) . . ? C1B C6B C5B 121.0(5) . . ? C6C C1C C2C 117.7(4) . . ? C6C C1C P2 119.4(3) . . ? C2C C1C P2 122.9(3) . . ? C3C C2C C1C 121.0(4) . . ? C4C C3C C2C 120.1(5) . . ? C5C C4C C3C 120.2(5) . . ? C4C C5C C6C 119.7(5) . . ? C1C C6C C5C 121.2(4) . . ? C6D C1D C2D 117.4(4) . . ? C6D C1D P2 117.5(3) . . ? C2D C1D P2 125.1(4) . . ? C1D C2D C3D 120.8(5) . . ? C4D C3D C2D 120.5(5) . . ? C5D C4D C3D 119.9(5) . . ? C4D C5D C6D 119.4(5) . . ? C1D C6D C5D 121.9(5) . . ? C6E C1E C2E 117.9(4) . . ? C6E C1E P3 120.0(3) . . ? C2E C1E P3 121.9(3) . . ? C1E C2E C3E 120.4(4) . . ? C4E C3E C2E 120.2(4) . . ? C3E C4E C5E 120.0(4) . . ? C4E C5E C6E 120.1(4) . . ? C5E C6E C1E 121.4(4) . . ? C6F C1F C2F 117.5(4) . . ? C6F C1F P3 119.9(3) . . ? C2F C1F P3 122.5(3) . . ? C3F C2F C1F 121.1(4) . . ? C4F C3F C2F 120.5(4) . . ? C3F C4F C5F 119.5(4) . . ? C4F C5F C6F 120.1(4) . . ? C5F C6F C1F 121.2(4) . . ? O1S C2S C3S 119.3(7) . . ? O1S C2S C1S 118.8(7) . . ? C3S C2S C1S 121.8(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.172 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.071 data_pdmn _database_code_CSD 180414 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 Mn O4 P3 Pd' _chemical_formula_weight 856.94 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' 'Mn' 'Mn' 0.3368 0.7283 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0096(5) _cell_length_b 10.2022(5) _cell_length_c 18.7467(10) _cell_angle_alpha 92.3510(10) _cell_angle_beta 95.6200(10) _cell_angle_gamma 94.8090(10) _cell_volume 1896.16(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6899 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'thin needle' _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.975 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7386 _exptl_absorpt_correction_T_max 0.8647 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD' _diffrn_measurement_method 'frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18173 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6660 _reflns_number_gt 5871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6660 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _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 Pd1 Pd 0.241771(16) 0.245169(16) 0.269759(9) 0.01493(7) Uani 1 1 d . . . Mn1 Mn 0.48958(3) 0.35869(3) 0.265198(19) 0.01665(9) Uani 1 1 d . . . P1 P 0.38544(6) 0.20261(6) 0.18609(3) 0.01507(13) Uani 1 1 d . . . P2 P 0.15500(6) 0.33767(6) 0.36801(3) 0.01741(14) Uani 1 1 d . . . P3 P 0.02957(6) 0.14404(6) 0.23802(3) 0.01705(14) Uani 1 1 d . . . C1 C 0.5553(2) 0.2288(2) 0.31856(13) 0.0203(5) Uani 1 1 d . . . O1 O 0.59717(17) 0.14862(17) 0.35435(9) 0.0270(4) Uani 1 1 d . . . C2 C 0.3741(2) 0.4708(2) 0.22435(13) 0.0195(5) Uani 1 1 d . . . O2 O 0.30198(17) 0.54288(17) 0.19926(10) 0.0273(4) Uani 1 1 d . . . C3 C 0.6378(2) 0.4108(2) 0.22342(14) 0.0233(5) Uani 1 1 d . . . O3 O 0.73128(19) 0.44576(18) 0.19558(11) 0.0368(5) Uani 1 1 d . . . C4 C 0.5173(3) 0.4718(3) 0.34418(14) 0.0259(6) Uani 1 1 d . . . O4 O 0.5370(2) 0.5441(2) 0.39321(11) 0.0412(5) Uani 1 1 d . . . C5 C -0.0292(2) 0.3235(2) 0.34426(13) 0.0204(5) Uani 1 1 d . . . H5A H -0.0750 0.3378 0.3880 0.024 Uiso 1 1 calc R . . H5B H -0.0532 0.3922 0.3107 0.024 Uiso 1 1 calc R . . C6 C -0.0776(2) 0.1870(2) 0.30916(13) 0.0219(5) Uani 1 1 d . . . H6A H -0.1723 0.1868 0.2881 0.026 Uiso 1 1 calc R . . H6B H -0.0740 0.1203 0.3460 0.026 Uiso 1 1 calc R . . C1A C 0.4390(2) 0.0369(2) 0.17551(12) 0.0173(5) Uani 1 1 d . . . C2A C 0.4372(2) -0.0466(2) 0.23246(13) 0.0217(5) Uani 1 1 d . . . H2A H 0.4059 -0.0175 0.2761 0.026 Uiso 1 1 calc R . . C3A C 0.4806(3) -0.1719(2) 0.22610(14) 0.0260(6) Uani 1 1 d . . . H3A H 0.4801 -0.2278 0.2654 0.031 Uiso 1 1 calc R . . C4A C 0.5246(3) -0.2153(2) 0.16188(14) 0.0282(6) Uani 1 1 d . . . H4A H 0.5542 -0.3011 0.1573 0.034 Uiso 1 1 calc R . . C5A C 0.5255(2) -0.1344(3) 0.10509(14) 0.0269(6) Uani 1 1 d . . . H5A' H 0.5548 -0.1647 0.0611 0.032 Uiso 1 1 calc R . . C6A C 0.4836(2) -0.0084(2) 0.11170(13) 0.0222(5) Uani 1 1 d . . . H6A' H 0.4855 0.0473 0.0723 0.027 Uiso 1 1 calc R . . C1B C 0.3301(2) 0.2427(2) 0.09447(12) 0.0180(5) Uani 1 1 d . . . C2B C 0.3855(3) 0.3573(2) 0.06638(13) 0.0233(5) Uani 1 1 d . . . H2B H 0.4582 0.4091 0.0932 0.028 Uiso 1 1 calc R . . C3B C 0.3351(3) 0.3964(3) -0.00046(14) 0.0301(6) Uani 1 1 d . . . H3B H 0.3729 0.4750 -0.0189 0.036 Uiso 1 1 calc R . . C4B C 0.2308(3) 0.3214(3) -0.03982(14) 0.0317(6) Uani 1 1 d . . . H4B H 0.1955 0.3490 -0.0851 0.038 Uiso 1 1 calc R . . C5B C 0.1769(3) 0.2058(3) -0.01362(14) 0.0294(6) Uani 1 1 d . . . H5B' H 0.1065 0.1529 -0.0415 0.035 Uiso 1 1 calc R . . C6B C 0.2259(2) 0.1670(3) 0.05337(13) 0.0233(5) Uani 1 1 d . . . H6B' H 0.1879 0.0880 0.0713 0.028 Uiso 1 1 calc R . . C1C C 0.1850(2) 0.2444(2) 0.44787(12) 0.0203(5) Uani 1 1 d . . . C2C C 0.3112(3) 0.1993(3) 0.46203(14) 0.0270(6) Uani 1 1 d . . . H2C H 0.3767 0.2141 0.4292 0.032 Uiso 1 1 calc R . . C3C C 0.3430(3) 0.1324(3) 0.52373(14) 0.0306(6) Uani 1 1 d . . . H3C H 0.4303 0.1030 0.5332 0.037 Uiso 1 1 calc R . . C4C C 0.2486(3) 0.1088(3) 0.57093(15) 0.0351(7) Uani 1 1 d . . . H4C H 0.2703 0.0631 0.6131 0.042 Uiso 1 1 calc R . . C5C C 0.1223(3) 0.1517(4) 0.55703(18) 0.0537(10) Uani 1 1 d . . . H5C H 0.0565 0.1344 0.5895 0.064 Uiso 1 1 calc R . . C6C C 0.0902(3) 0.2196(3) 0.49630(16) 0.0431(8) Uani 1 1 d . . . H6C H 0.0030 0.2494 0.4876 0.052 Uiso 1 1 calc R . . C1D C 0.1919(2) 0.5095(2) 0.39973(13) 0.0197(5) Uani 1 1 d . . . C2D C 0.2452(3) 0.5475(3) 0.46946(14) 0.0293(6) Uani 1 1 d . . . H2D H 0.2611 0.4828 0.5036 0.035 Uiso 1 1 calc R . . C3D C 0.2751(3) 0.6802(3) 0.48911(15) 0.0361(7) Uani 1 1 d . . . H3D H 0.3113 0.7058 0.5369 0.043 Uiso 1 1 calc R . . C4D C 0.2529(3) 0.7753(3) 0.44019(16) 0.0335(7) Uani 1 1 d . . . H4D H 0.2741 0.8659 0.4541 0.040 Uiso 1 1 calc R . . C5D C 0.1996(3) 0.7382(3) 0.37070(15) 0.0307(6) Uani 1 1 d . . . H5D H 0.1831 0.8033 0.3369 0.037 Uiso 1 1 calc R . . C6D C 0.1705(3) 0.6060(2) 0.35042(13) 0.0251(6) Uani 1 1 d . . . H6D H 0.1356 0.5809 0.3024 0.030 Uiso 1 1 calc R . . C1E C -0.0031(2) -0.0344(2) 0.22448(12) 0.0181(5) Uani 1 1 d . . . C2E C 0.0906(2) -0.1017(2) 0.19101(13) 0.0217(5) Uani 1 1 d . . . H2E H 0.1670 -0.0542 0.1751 0.026 Uiso 1 1 calc R . . C3E C 0.0735(3) -0.2379(2) 0.18062(14) 0.0251(6) Uani 1 1 d . . . H3E H 0.1373 -0.2833 0.1571 0.030 Uiso 1 1 calc R . . C4E C -0.0369(3) -0.3074(2) 0.20469(13) 0.0259(6) Uani 1 1 d . . . H4E H -0.0482 -0.4007 0.1983 0.031 Uiso 1 1 calc R . . C5E C -0.1305(3) -0.2416(2) 0.23785(14) 0.0265(6) Uani 1 1 d . . . H5E H -0.2059 -0.2898 0.2544 0.032 Uiso 1 1 calc R . . C6E C -0.1150(2) -0.1051(2) 0.24723(13) 0.0237(5) Uani 1 1 d . . . H6E H -0.1808 -0.0600 0.2692 0.028 Uiso 1 1 calc R . . C1F C -0.0507(2) 0.2082(2) 0.15666(12) 0.0187(5) Uani 1 1 d . . . C2F C -0.0002(2) 0.3304(2) 0.13530(13) 0.0206(5) Uani 1 1 d . . . H2F H 0.0734 0.3782 0.1635 0.025 Uiso 1 1 calc R . . C3F C -0.0559(3) 0.3828(3) 0.07366(14) 0.0261(6) Uani 1 1 d . . . H3F H -0.0219 0.4670 0.0603 0.031 Uiso 1 1 calc R . . C4F C -0.1615(3) 0.3122(3) 0.03124(14) 0.0298(6) Uani 1 1 d . . . H4F H -0.1990 0.3475 -0.0116 0.036 Uiso 1 1 calc R . . C5F C -0.2121(3) 0.1904(3) 0.05153(15) 0.0332(7) Uani 1 1 d . . . H5F H -0.2841 0.1421 0.0224 0.040 Uiso 1 1 calc R . . C6F C -0.1578(3) 0.1385(3) 0.11431(14) 0.0278(6) Uani 1 1 d . . . H6F H -0.1938 0.0554 0.1283 0.033 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 Pd1 0.01611(10) 0.01287(10) 0.01578(11) 0.00055(7) 0.00183(7) 0.00091(7) Mn1 0.01631(18) 0.01383(19) 0.0193(2) -0.00078(14) 0.00076(14) 0.00011(14) P1 0.0167(3) 0.0126(3) 0.0159(3) 0.0009(2) 0.0015(2) 0.0014(2) P2 0.0196(3) 0.0173(3) 0.0157(3) 0.0012(2) 0.0023(2) 0.0033(2) P3 0.0164(3) 0.0142(3) 0.0204(3) 0.0010(2) 0.0015(2) 0.0007(2) C1 0.0184(12) 0.0210(13) 0.0201(13) -0.0073(11) 0.0006(10) -0.0003(10) O1 0.0293(10) 0.0253(10) 0.0257(10) 0.0027(8) -0.0046(8) 0.0060(8) C2 0.0220(12) 0.0139(12) 0.0213(13) -0.0043(10) 0.0037(10) -0.0043(10) O2 0.0285(10) 0.0185(9) 0.0352(11) 0.0038(8) 0.0004(8) 0.0052(8) C3 0.0235(13) 0.0144(12) 0.0315(14) -0.0016(10) 0.0027(11) 0.0004(10) O3 0.0284(10) 0.0276(11) 0.0557(13) 0.0000(9) 0.0173(10) -0.0037(8) C4 0.0246(13) 0.0221(14) 0.0300(15) -0.0001(12) -0.0037(11) 0.0047(11) O4 0.0469(12) 0.0368(12) 0.0368(12) -0.0182(10) -0.0098(10) 0.0112(9) C5 0.0200(12) 0.0223(13) 0.0199(13) 0.0023(10) 0.0039(10) 0.0052(10) C6 0.0213(12) 0.0203(13) 0.0244(13) 0.0020(10) 0.0053(10) -0.0002(10) C1A 0.0143(11) 0.0142(12) 0.0228(13) -0.0003(10) -0.0008(9) 0.0005(9) C2A 0.0224(13) 0.0179(13) 0.0236(13) -0.0006(10) 0.0007(10) -0.0020(10) C3A 0.0296(14) 0.0150(13) 0.0329(15) 0.0055(11) 0.0000(11) 0.0010(10) C4A 0.0273(14) 0.0172(13) 0.0402(16) -0.0009(12) 0.0018(12) 0.0063(11) C5A 0.0252(13) 0.0251(14) 0.0312(15) -0.0041(12) 0.0052(11) 0.0065(11) C6A 0.0214(12) 0.0207(13) 0.0251(14) 0.0016(10) 0.0035(10) 0.0033(10) C1B 0.0217(12) 0.0186(12) 0.0147(12) -0.0006(9) 0.0029(9) 0.0082(10) C2B 0.0271(13) 0.0227(13) 0.0213(13) 0.0020(10) 0.0045(10) 0.0063(11) C3B 0.0425(16) 0.0276(15) 0.0242(14) 0.0082(11) 0.0105(12) 0.0146(12) C4B 0.0384(16) 0.0425(17) 0.0178(13) 0.0037(12) 0.0020(12) 0.0242(13) C5B 0.0264(14) 0.0388(16) 0.0227(14) -0.0074(12) -0.0025(11) 0.0124(12) C6B 0.0201(12) 0.0261(14) 0.0242(13) -0.0028(11) 0.0034(10) 0.0057(10) C1C 0.0251(13) 0.0188(13) 0.0175(12) 0.0019(10) 0.0028(10) 0.0041(10) C2C 0.0260(13) 0.0334(15) 0.0237(14) 0.0077(11) 0.0058(11) 0.0074(11) C3C 0.0312(15) 0.0334(16) 0.0293(15) 0.0071(12) 0.0022(12) 0.0130(12) C4C 0.0428(17) 0.0379(17) 0.0283(15) 0.0156(13) 0.0072(13) 0.0148(13) C5C 0.0405(18) 0.085(3) 0.046(2) 0.0396(19) 0.0222(15) 0.0257(18) C6C 0.0323(16) 0.066(2) 0.0382(18) 0.0288(16) 0.0147(13) 0.0227(15) C1D 0.0188(12) 0.0198(13) 0.0211(13) -0.0012(10) 0.0029(10) 0.0045(10) C2D 0.0365(15) 0.0281(15) 0.0221(14) -0.0006(11) -0.0029(11) 0.0037(12) C3D 0.0399(16) 0.0375(17) 0.0278(15) -0.0126(13) -0.0055(13) 0.0019(13) C4D 0.0309(15) 0.0221(14) 0.0464(18) -0.0105(13) 0.0048(13) 0.0004(11) C5D 0.0362(15) 0.0207(14) 0.0361(16) 0.0039(12) 0.0062(12) 0.0042(11) C6D 0.0316(14) 0.0226(14) 0.0209(13) -0.0003(11) 0.0012(11) 0.0046(11) C1E 0.0198(12) 0.0148(12) 0.0184(12) 0.0030(9) -0.0030(10) -0.0012(9) C2E 0.0193(12) 0.0205(13) 0.0244(13) 0.0033(10) -0.0017(10) 0.0001(10) C3E 0.0256(13) 0.0187(13) 0.0301(14) -0.0016(11) -0.0045(11) 0.0064(10) C4E 0.0302(14) 0.0164(13) 0.0285(14) 0.0042(11) -0.0099(11) 0.0003(11) C5E 0.0281(14) 0.0209(13) 0.0284(14) 0.0062(11) -0.0010(11) -0.0075(11) C6E 0.0234(13) 0.0223(13) 0.0246(14) 0.0012(11) 0.0008(10) -0.0016(10) C1F 0.0211(12) 0.0174(12) 0.0185(12) 0.0012(10) 0.0035(10) 0.0047(10) C2F 0.0207(12) 0.0185(13) 0.0230(13) -0.0009(10) 0.0049(10) 0.0030(10) C3F 0.0312(14) 0.0230(14) 0.0266(14) 0.0058(11) 0.0089(11) 0.0088(11) C4F 0.0367(15) 0.0319(15) 0.0229(14) 0.0058(11) 0.0006(12) 0.0153(12) C5F 0.0326(15) 0.0325(16) 0.0321(16) -0.0007(12) -0.0088(12) 0.0040(12) C6F 0.0279(14) 0.0236(14) 0.0304(15) 0.0030(11) -0.0028(11) -0.0003(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2820(6) . ? Pd1 P3 2.2945(6) . ? Pd1 P2 2.3121(6) . ? Pd1 Mn1 2.6589(4) . ? Mn1 C3 1.796(3) . ? Mn1 C1 1.820(3) . ? Mn1 C4 1.824(3) . ? Mn1 C2 1.831(3) . ? Mn1 P1 2.2465(7) . ? P1 C1A 1.825(2) . ? P1 C1B 1.826(2) . ? P2 C1C 1.820(2) . ? P2 C1D 1.824(2) . ? P2 C5 1.846(2) . ? P3 C1E 1.825(2) . ? P3 C1F 1.825(2) . ? P3 C6 1.853(2) . ? C1 O1 1.159(3) . ? C2 O2 1.154(3) . ? C3 O3 1.153(3) . ? C4 O4 1.145(3) . ? C5 C6 1.535(3) . ? C1A C6A 1.392(3) . ? C1A C2A 1.394(3) . ? C2A C3A 1.389(3) . ? C3A C4A 1.390(4) . ? C4A C5A 1.374(4) . ? C5A C6A 1.390(3) . ? C1B C6B 1.392(3) . ? C1B C2B 1.397(3) . ? C2B C3B 1.391(3) . ? C3B C4B 1.375(4) . ? C4B C5B 1.384(4) . ? C5B C6B 1.388(4) . ? C1C C2C 1.385(3) . ? C1C C6C 1.392(4) . ? C2C C3C 1.390(4) . ? C3C C4C 1.370(4) . ? C4C C5C 1.377(4) . ? C5C C6C 1.381(4) . ? C1D C2D 1.389(3) . ? C1D C6D 1.393(3) . ? C2D C3D 1.389(4) . ? C3D C4D 1.379(4) . ? C4D C5D 1.384(4) . ? C5D C6D 1.385(4) . ? C1E C2E 1.391(3) . ? C1E C6E 1.393(3) . ? C2E C3E 1.389(3) . ? C3E C4E 1.386(4) . ? C4E C5E 1.378(4) . ? C5E C6E 1.391(4) . ? C1F C6F 1.394(3) . ? C1F C2F 1.395(3) . ? C2F C3F 1.380(3) . ? C3F C4F 1.389(4) . ? C4F C5F 1.384(4) . ? C5F C6F 1.391(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 P1 Pd1 P3 111.81(2) . . ? P1 Pd1 P2 161.13(2) . . ? P3 Pd1 P2 86.74(2) . . ? P1 Pd1 Mn1 53.428(17) . . ? P3 Pd1 Mn1 163.204(19) . . ? P2 Pd1 Mn1 107.706(18) . . ? C3 Mn1 C1 99.44(11) . . ? C3 Mn1 C4 98.40(11) . . ? C1 Mn1 C4 89.78(11) . . ? C3 Mn1 C2 99.14(11) . . ? C1 Mn1 C2 161.41(11) . . ? C4 Mn1 C2 88.18(11) . . ? C3 Mn1 P1 102.46(8) . . ? C1 Mn1 P1 88.67(7) . . ? C4 Mn1 P1 159.06(9) . . ? C2 Mn1 P1 86.68(7) . . ? C3 Mn1 Pd1 155.61(8) . . ? C1 Mn1 Pd1 89.21(7) . . ? C4 Mn1 Pd1 104.43(8) . . ? C2 Mn1 Pd1 73.45(7) . . ? P1 Mn1 Pd1 54.667(17) . . ? C1A P1 C1B 103.54(11) . . ? C1A P1 Mn1 124.01(8) . . ? C1B P1 Mn1 120.67(8) . . ? C1A P1 Pd1 119.29(8) . . ? C1B P1 Pd1 115.66(7) . . ? Mn1 P1 Pd1 71.91(2) . . ? C1C P2 C1D 104.61(11) . . ? C1C P2 C5 106.46(11) . . ? C1D P2 C5 103.13(11) . . ? C1C P2 Pd1 112.23(8) . . ? C1D P2 Pd1 123.95(8) . . ? C5 P2 Pd1 104.98(8) . . ? C1E P3 C1F 104.28(10) . . ? C1E P3 C6 103.98(11) . . ? C1F P3 C6 104.74(11) . . ? C1E P3 Pd1 122.40(8) . . ? C1F P3 Pd1 112.08(8) . . ? C6 P3 Pd1 107.82(8) . . ? O1 C1 Mn1 178.0(2) . . ? O2 C2 Mn1 179.1(2) . . ? O3 C3 Mn1 178.5(2) . . ? O4 C4 Mn1 178.6(3) . . ? C6 C5 P2 110.59(16) . . ? C5 C6 P3 110.44(16) . . ? C6A C1A C2A 118.7(2) . . ? C6A C1A P1 121.49(18) . . ? C2A C1A P1 119.84(18) . . ? C3A C2A C1A 120.8(2) . . ? C2A C3A C4A 119.7(2) . . ? C5A C4A C3A 120.1(2) . . ? C4A C5A C6A 120.3(2) . . ? C5A C6A C1A 120.5(2) . . ? C6B C1B C2B 118.5(2) . . ? C6B C1B P1 121.46(19) . . ? C2B C1B P1 119.79(18) . . ? C3B C2B C1B 120.6(2) . . ? C4B C3B C2B 120.0(3) . . ? C3B C4B C5B 120.2(2) . . ? C4B C5B C6B 120.0(2) . . ? C5B C6B C1B 120.6(2) . . ? C2C C1C C6C 118.4(2) . . ? C2C C1C P2 117.74(19) . . ? C6C C1C P2 123.80(19) . . ? C1C C2C C3C 120.8(2) . . ? C4C C3C C2C 120.1(2) . . ? C3C C4C C5C 119.7(3) . . ? C4C C5C C6C 120.6(3) . . ? C5C C6C C1C 120.3(3) . . ? C2D C1D C6D 119.1(2) . . ? C2D C1D P2 123.03(19) . . ? C6D C1D P2 117.82(18) . . ? C3D C2D C1D 119.8(2) . . ? C4D C3D C2D 120.8(3) . . ? C3D C4D C5D 119.6(2) . . ? C4D C5D C6D 120.0(3) . . ? C5D C6D C1D 120.6(2) . . ? C2E C1E C6E 119.2(2) . . ? C2E C1E P3 117.64(18) . . ? C6E C1E P3 123.17(19) . . ? C3E C2E C1E 120.6(2) . . ? C4E C3E C2E 119.7(2) . . ? C5E C4E C3E 120.2(2) . . ? C4E C5E C6E 120.3(2) . . ? C5E C6E C1E 120.1(2) . . ? C6F C1F C2F 119.0(2) . . ? C6F C1F P3 122.64(19) . . ? C2F C1F P3 118.36(18) . . ? C3F C2F C1F 120.8(2) . . ? C2F C3F C4F 120.0(2) . . ? C5F C4F C3F 119.8(2) . . ? C4F C5F C6F 120.3(2) . . ? C5F C6F C1F 120.1(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.017 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.076