# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Javier Ruiz' _publ_contact_author_email JRUIZ@UNIOVI.ES _publ_section_title ; NHC-manganese(I) complexes as carbene transfer agents ; _publ_requested_category FM loop_ _publ_author_name 'Javier Ruiz' 'Angela Berros' 'Bernabe F. Perandones' 'Marilin Vivanco' # Attachment '8a11a1318.cif.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-03-23 at 10:26:41 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : d:\monocristal\wingx\files\archive.reqdat # CIF files read : jv02jj1n struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_8a _database_code_depnum_ccdc_archive 'CCDC 725955' _audit_creation_date 2009-03-23T10:26:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H16 Mn N4 O3, F6 P' _chemical_formula_sum 'C21 H16 F6 Mn N4 O3 P' _chemical_formula_weight 572.29 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_Int_Tables_number 56 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 17.9823(7) _cell_length_b 20.1857(9) _cell_length_c 12.4699(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4526.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1954 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.05 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.68 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.985 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_unetI/netI 0.0632 _diffrn_reflns_number 61187 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.41 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4653 _reflns_number_gt 2859 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR-97 (Giacovazzo et all, 1999' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0311P)^2^+1.0725P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4653 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.083 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.542 _refine_diff_density_min -0.38 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 H3 H -0.095(2) 0.021(2) 0.235(3) 0.036(12) Uiso 1 1 d . . . Mn1 Mn -0.08970(3) 0.17021(3) 0.27942(4) 0.02048(14) Uani 1 1 d . . . N1 N 0.03206(16) 0.09382(14) 0.1474(2) 0.0219(7) Uani 1 1 d . . . C2 C -0.03235(19) 0.09509(17) 0.2042(3) 0.0202(8) Uani 1 1 d . . . N3 N -0.05364(18) 0.03061(15) 0.2096(2) 0.0222(7) Uani 1 1 d . . . C4 C -0.0043(2) -0.01136(17) 0.1575(3) 0.0212(8) Uani 1 1 d . . . C5 C 0.05140(19) 0.02934(18) 0.1183(3) 0.0222(8) Uani 1 1 d . . . C6 C 0.1116(2) 0.0039(2) 0.0618(3) 0.0283(9) Uani 1 1 d . . . H6 H 0.1498 0.0318 0.035 0.034 Uiso 1 1 calc R . . C7 C 0.1132(2) -0.0636(2) 0.0465(3) 0.0307(9) Uani 1 1 d . . . H7 H 0.1537 -0.0828 0.0087 0.037 Uiso 1 1 calc R . . C8 C 0.0564(2) -0.1047(2) 0.0855(3) 0.0308(9) Uani 1 1 d . . . H8 H 0.0592 -0.1511 0.073 0.037 Uiso 1 1 calc R . . C9 C -0.0033(2) -0.07960(19) 0.1414(3) 0.0287(9) Uani 1 1 d . . . H9 H -0.0418 -0.1074 0.1677 0.034 Uiso 1 1 calc R . . C10 C 0.0771(2) 0.15030(18) 0.1128(3) 0.0287(9) Uani 1 1 d . . . H10A H 0.0463 0.1904 0.1121 0.043 Uiso 1 1 calc R . . H10B H 0.0964 0.142 0.0406 0.043 Uiso 1 1 calc R . . H10C H 0.1187 0.1564 0.1626 0.043 Uiso 1 1 calc R . . N11 N 0.00734(16) 0.19041(14) 0.3601(2) 0.0210(7) Uani 1 1 d . . . C12 C 0.0586(2) 0.23631(18) 0.3340(3) 0.0259(9) Uani 1 1 d . . . H12 H 0.0478 0.2662 0.2773 0.031 Uiso 1 1 calc R . . C13 C 0.1258(2) 0.24186(19) 0.3858(3) 0.0281(9) Uani 1 1 d . . . H13 H 0.1604 0.2749 0.3648 0.034 Uiso 1 1 calc R . . C14 C 0.1424(2) 0.19897(19) 0.4684(3) 0.0303(9) Uani 1 1 d . . . H14 H 0.189 0.2014 0.5042 0.036 Uiso 1 1 calc R . . C15 C 0.0899(2) 0.15232(18) 0.4982(3) 0.0274(9) Uani 1 1 d . . . H15 H 0.0999 0.1222 0.5549 0.033 Uiso 1 1 calc R . . C16 C 0.02257(19) 0.15006(17) 0.4444(3) 0.0201(8) Uani 1 1 d . . . C17 C -0.03892(19) 0.10552(17) 0.4743(3) 0.0214(8) Uani 1 1 d . . . C18 C -0.0382(2) 0.06696(18) 0.5666(3) 0.0266(9) Uani 1 1 d . . . H18 H 0.0041 0.0667 0.6122 0.032 Uiso 1 1 calc R . . C19 C -0.0996(2) 0.02903(19) 0.5914(3) 0.0320(9) Uani 1 1 d . . . H19 H -0.1002 0.0023 0.654 0.038 Uiso 1 1 calc R . . C20 C -0.1599(2) 0.03057(19) 0.5243(3) 0.0281(9) Uani 1 1 d . . . H20 H -0.2027 0.0047 0.5396 0.034 Uiso 1 1 calc R . . C21 C -0.1578(2) 0.07002(18) 0.4342(3) 0.0249(8) Uani 1 1 d . . . H21 H -0.2 0.0709 0.3884 0.03 Uiso 1 1 calc R . . N22 N -0.09851(15) 0.10732(14) 0.4086(2) 0.0202(6) Uani 1 1 d . . . C23 C -0.0774(2) 0.22771(19) 0.1712(3) 0.0277(9) Uani 1 1 d . . . O24 O -0.07309(16) 0.26514(14) 0.1012(2) 0.0424(8) Uani 1 1 d . . . C25 C -0.1758(2) 0.14614(18) 0.2143(3) 0.0276(9) Uani 1 1 d . . . O26 O -0.23000(15) 0.13373(13) 0.1709(2) 0.0377(7) Uani 1 1 d . . . C27 C -0.1414(2) 0.23437(19) 0.3524(3) 0.0266(9) Uani 1 1 d . . . O28 O -0.17524(15) 0.27516(14) 0.3937(3) 0.0431(8) Uani 1 1 d . . . P1 P 0.27254(5) 0.09169(5) 0.25190(8) 0.0277(2) Uani 1 1 d . . . F1 F 0.25615(13) 0.07875(13) 0.12817(17) 0.0479(7) Uani 1 1 d . . . F2 F 0.35880(13) 0.09971(18) 0.2241(2) 0.0744(10) Uani 1 1 d . . . F3 F 0.28628(15) 0.01417(12) 0.2721(2) 0.0579(7) Uani 1 1 d . . . F4 F 0.29110(13) 0.10465(12) 0.37499(17) 0.0435(6) Uani 1 1 d . . . F5 F 0.18755(12) 0.08208(11) 0.27984(18) 0.0395(6) Uani 1 1 d . . . F6 F 0.25966(15) 0.16823(11) 0.2329(2) 0.0532(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0249(3) 0.0174(3) 0.0191(3) 0.0012(2) -0.0008(2) -0.0005(2) N1 0.0258(16) 0.0214(17) 0.0186(16) 0.0008(13) -0.0006(13) -0.0021(13) C2 0.0266(19) 0.0202(19) 0.0139(18) 0.0026(15) -0.0042(15) -0.0030(15) N3 0.0268(18) 0.0224(17) 0.0175(16) 0.0005(14) 0.0046(14) -0.0005(14) C4 0.0274(19) 0.022(2) 0.0146(18) 0.0003(15) -0.0012(15) 0.0034(16) C5 0.0252(19) 0.023(2) 0.0187(19) 0.0019(16) -0.0051(16) 0.0005(16) C6 0.026(2) 0.034(2) 0.024(2) -0.0013(18) -0.0016(16) 0.0003(18) C7 0.032(2) 0.038(2) 0.022(2) -0.0053(18) -0.0050(17) 0.0116(19) C8 0.038(2) 0.027(2) 0.027(2) 0.0010(17) -0.0079(18) 0.0086(19) C9 0.036(2) 0.026(2) 0.024(2) -0.0004(17) 0.0002(17) -0.0025(18) C10 0.030(2) 0.027(2) 0.029(2) 0.0018(17) 0.0059(17) -0.0058(17) N11 0.0290(17) 0.0160(15) 0.0181(16) -0.0006(12) 0.0055(13) -0.0007(13) C12 0.032(2) 0.017(2) 0.029(2) 0.0014(16) 0.0041(18) -0.0023(16) C13 0.028(2) 0.025(2) 0.031(2) -0.0066(18) 0.0074(18) -0.0070(17) C14 0.027(2) 0.035(2) 0.029(2) -0.0064(19) -0.0022(18) -0.0036(18) C15 0.031(2) 0.026(2) 0.025(2) -0.0003(16) -0.0033(17) -0.0006(19) C16 0.0265(19) 0.0166(18) 0.0172(18) -0.0043(15) 0.0028(15) -0.0002(15) C17 0.0267(19) 0.0192(19) 0.0183(19) -0.0043(15) 0.0053(16) 0.0007(16) C18 0.034(2) 0.026(2) 0.020(2) 0.0018(16) -0.0001(17) -0.0022(18) C19 0.044(2) 0.031(2) 0.021(2) 0.0057(17) 0.0044(19) -0.007(2) C20 0.035(2) 0.028(2) 0.022(2) -0.0043(17) 0.0065(17) -0.0094(18) C21 0.027(2) 0.029(2) 0.0185(19) -0.0038(17) 0.0023(16) -0.0045(17) N22 0.0254(16) 0.0197(15) 0.0155(15) -0.0031(12) 0.0014(13) -0.0007(13) C23 0.028(2) 0.026(2) 0.029(2) -0.0002(18) -0.0045(17) 0.0001(17) O24 0.0476(18) 0.0391(18) 0.0406(18) 0.0221(15) 0.0002(14) 0.0000(14) C25 0.040(2) 0.0182(18) 0.025(2) 0.0012(17) 0.0024(19) 0.0041(17) O26 0.0354(17) 0.0385(17) 0.0392(17) -0.0022(14) -0.0132(14) -0.0004(14) C27 0.0222(19) 0.023(2) 0.034(2) -0.0018(18) -0.0030(17) -0.0081(17) O28 0.0303(15) 0.0325(17) 0.066(2) -0.0185(16) 0.0043(15) -0.0007(13) P1 0.0281(5) 0.0309(6) 0.0241(5) 0.0014(4) 0.0009(4) -0.0005(4) F1 0.0449(14) 0.0728(18) 0.0258(13) -0.0090(13) -0.0009(11) -0.0009(13) F2 0.0274(13) 0.153(3) 0.0425(16) 0.0355(19) 0.0021(12) -0.0064(16) F3 0.0768(19) 0.0367(14) 0.0601(18) -0.0034(13) 0.0016(15) 0.0227(13) F4 0.0543(15) 0.0520(16) 0.0243(13) 0.0053(11) -0.0081(11) -0.0101(12) F5 0.0336(12) 0.0451(14) 0.0400(14) 0.0081(12) 0.0062(11) -0.0041(11) F6 0.0767(18) 0.0292(13) 0.0538(16) 0.0140(13) -0.0201(14) -0.0160(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C23 1.794(4) . ? Mn1 C25 1.814(4) . ? Mn1 C27 1.836(4) . ? Mn1 N11 2.055(3) . ? Mn1 N22 2.057(3) . ? Mn1 C2 2.060(4) . ? N1 C2 1.358(4) . ? N1 C5 1.395(4) . ? N1 C10 1.464(4) . ? C2 N3 1.358(4) . ? N3 C4 1.388(4) . ? N3 H3 0.83(4) . ? C4 C5 1.384(5) . ? C4 C9 1.392(5) . ? C5 C6 1.390(5) . ? C6 C7 1.376(5) . ? C6 H6 0.95 . ? C7 C8 1.403(5) . ? C7 H7 0.95 . ? C8 C9 1.377(5) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? N11 C12 1.346(4) . ? N11 C16 1.358(4) . ? C12 C13 1.374(5) . ? C12 H12 0.95 . ? C13 C14 1.379(5) . ? C13 H13 0.95 . ? C14 C15 1.384(5) . ? C14 H14 0.95 . ? C15 C16 1.385(5) . ? C15 H15 0.95 . ? C16 C17 1.473(5) . ? C17 N22 1.349(4) . ? C17 C18 1.390(5) . ? C18 C19 1.379(5) . ? C18 H18 0.95 . ? C19 C20 1.369(5) . ? C19 H19 0.95 . ? C20 C21 1.377(5) . ? C20 H20 0.95 . ? C21 N22 1.344(4) . ? C21 H21 0.95 . ? C23 O24 1.157(4) . ? C25 O26 1.143(4) . ? C27 O28 1.146(4) . ? P1 F6 1.580(2) . ? P1 F5 1.580(2) . ? P1 F1 1.592(2) . ? P1 F4 1.592(2) . ? P1 F2 1.598(3) . ? P1 F3 1.604(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Mn1 C25 86.66(17) . . ? C23 Mn1 C27 88.81(17) . . ? C25 Mn1 C27 88.81(16) . . ? C23 Mn1 N11 97.76(14) . . ? C25 Mn1 N11 175.36(14) . . ? C27 Mn1 N11 92.70(13) . . ? C23 Mn1 N22 176.38(14) . . ? C25 Mn1 N22 96.87(14) . . ? C27 Mn1 N22 90.45(14) . . ? N11 Mn1 N22 78.73(11) . . ? C23 Mn1 C2 94.13(15) . . ? C25 Mn1 C2 91.50(15) . . ? C27 Mn1 C2 177.05(15) . . ? N11 Mn1 C2 86.77(12) . . ? N22 Mn1 C2 86.60(12) . . ? C2 N1 C5 111.5(3) . . ? C2 N1 C10 127.7(3) . . ? C5 N1 C10 120.8(3) . . ? N3 C2 N1 104.3(3) . . ? N3 C2 Mn1 122.8(3) . . ? N1 C2 Mn1 132.7(3) . . ? C2 N3 C4 112.4(3) . . ? C2 N3 H3 120(3) . . ? C4 N3 H3 127(3) . . ? C5 C4 N3 105.4(3) . . ? C5 C4 C9 121.8(3) . . ? N3 C4 C9 132.8(3) . . ? C4 C5 C6 121.5(3) . . ? C4 C5 N1 106.4(3) . . ? C6 C5 N1 132.1(3) . . ? C7 C6 C5 117.0(4) . . ? C7 C6 H6 121.5 . . ? C5 C6 H6 121.5 . . ? C6 C7 C8 121.4(4) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 121.7(4) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C4 116.6(4) . . ? C8 C9 H9 121.7 . . ? C4 C9 H9 121.7 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 N11 C16 117.5(3) . . ? C12 N11 Mn1 126.9(2) . . ? C16 N11 Mn1 115.5(2) . . ? N11 C12 C13 123.0(3) . . ? N11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 118.7(4) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N11 C16 C15 122.1(3) . . ? N11 C16 C17 114.3(3) . . ? C15 C16 C17 123.6(3) . . ? N22 C17 C18 121.7(3) . . ? N22 C17 C16 115.2(3) . . ? C18 C17 C16 123.0(3) . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 119.4(4) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? N22 C21 C20 122.6(3) . . ? N22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 N22 C17 118.1(3) . . ? C21 N22 Mn1 126.4(2) . . ? C17 N22 Mn1 115.5(2) . . ? O24 C23 Mn1 176.7(3) . . ? O26 C25 Mn1 176.8(3) . . ? O28 C27 Mn1 176.8(4) . . ? F6 P1 F5 90.65(14) . . ? F6 P1 F1 89.29(14) . . ? F5 P1 F1 90.83(13) . . ? F6 P1 F4 90.86(14) . . ? F5 P1 F4 90.59(13) . . ? F1 P1 F4 178.57(14) . . ? F6 P1 F2 90.61(17) . . ? F5 P1 F2 178.74(17) . . ? F1 P1 F2 89.20(14) . . ? F4 P1 F2 89.38(14) . . ? F6 P1 F3 179.41(16) . . ? F5 P1 F3 89.68(14) . . ? F1 P1 F3 91.19(15) . . ? F4 P1 F3 88.64(14) . . ? F2 P1 F3 89.05(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C2 N3 -0.6(4) . . . . ? C10 N1 C2 N3 176.5(3) . . . . ? C5 N1 C2 Mn1 175.7(3) . . . . ? C10 N1 C2 Mn1 -7.3(5) . . . . ? C23 Mn1 C2 N3 -141.1(3) . . . . ? C25 Mn1 C2 N3 -54.4(3) . . . . ? N11 Mn1 C2 N3 121.3(3) . . . . ? N22 Mn1 C2 N3 42.4(3) . . . . ? C23 Mn1 C2 N1 43.2(3) . . . . ? C25 Mn1 C2 N1 129.9(3) . . . . ? N11 Mn1 C2 N1 -54.4(3) . . . . ? N22 Mn1 C2 N1 -133.3(3) . . . . ? N1 C2 N3 C4 0.0(4) . . . . ? Mn1 C2 N3 C4 -176.8(2) . . . . ? C2 N3 C4 C5 0.6(4) . . . . ? C2 N3 C4 C9 -179.4(4) . . . . ? N3 C4 C5 C6 179.3(3) . . . . ? C9 C4 C5 C6 -0.6(5) . . . . ? N3 C4 C5 N1 -0.9(4) . . . . ? C9 C4 C5 N1 179.1(3) . . . . ? C2 N1 C5 C4 1.0(4) . . . . ? C10 N1 C5 C4 -176.3(3) . . . . ? C2 N1 C5 C6 -179.3(4) . . . . ? C10 N1 C5 C6 3.4(6) . . . . ? C4 C5 C6 C7 0.0(5) . . . . ? N1 C5 C6 C7 -179.6(4) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? C6 C7 C8 C9 -0.4(6) . . . . ? C7 C8 C9 C4 -0.1(5) . . . . ? C5 C4 C9 C8 0.6(5) . . . . ? N3 C4 C9 C8 -179.3(4) . . . . ? C23 Mn1 N11 C12 2.6(3) . . . . ? C27 Mn1 N11 C12 -86.6(3) . . . . ? N22 Mn1 N11 C12 -176.5(3) . . . . ? C2 Mn1 N11 C12 96.3(3) . . . . ? C23 Mn1 N11 C16 -173.1(3) . . . . ? C27 Mn1 N11 C16 97.7(3) . . . . ? N22 Mn1 N11 C16 7.8(2) . . . . ? C2 Mn1 N11 C16 -79.4(2) . . . . ? C16 N11 C12 C13 2.8(5) . . . . ? Mn1 N11 C12 C13 -172.9(3) . . . . ? N11 C12 C13 C14 -0.1(6) . . . . ? C12 C13 C14 C15 -1.3(6) . . . . ? C13 C14 C15 C16 0.1(5) . . . . ? C12 N11 C16 C15 -4.1(5) . . . . ? Mn1 N11 C16 C15 172.0(3) . . . . ? C12 N11 C16 C17 174.5(3) . . . . ? Mn1 N11 C16 C17 -9.4(4) . . . . ? C14 C15 C16 N11 2.8(5) . . . . ? C14 C15 C16 C17 -175.7(3) . . . . ? N11 C16 C17 N22 5.3(4) . . . . ? C15 C16 C17 N22 -176.1(3) . . . . ? N11 C16 C17 C18 -171.1(3) . . . . ? C15 C16 C17 C18 7.5(5) . . . . ? N22 C17 C18 C19 0.7(5) . . . . ? C16 C17 C18 C19 176.8(3) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? C18 C19 C20 C21 -0.3(6) . . . . ? C19 C20 C21 N22 0.3(6) . . . . ? C20 C21 N22 C17 0.1(5) . . . . ? C20 C21 N22 Mn1 -178.1(3) . . . . ? C18 C17 N22 C21 -0.6(5) . . . . ? C16 C17 N22 C21 -177.1(3) . . . . ? C18 C17 N22 Mn1 177.8(3) . . . . ? C16 C17 N22 Mn1 1.3(4) . . . . ? C25 Mn1 N22 C21 -8.1(3) . . . . ? C27 Mn1 N22 C21 80.8(3) . . . . ? N11 Mn1 N22 C21 173.5(3) . . . . ? C2 Mn1 N22 C21 -99.2(3) . . . . ? C25 Mn1 N22 C17 173.7(2) . . . . ? C27 Mn1 N22 C17 -97.4(3) . . . . ? N11 Mn1 N22 C17 -4.8(2) . . . . ? C2 Mn1 N22 C17 82.6(2) . . . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-04-02 at 13:15:24 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.dat # CIF files read : jv03bk3n struct data_11a _database_code_depnum_ccdc_archive 'CCDC 725956' _audit_creation_date 2007-04-02T13:15:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H32 Au Mn N4 O3 P, Cl O4 ' _chemical_formula_sum 'C41 H32 Au Cl Mn N4 O7 P' _chemical_formula_weight 1011.04 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.6998(3) _cell_length_b 16.4964(4) _cell_length_c 34.3632(8) _cell_angle_alpha 90 _cell_angle_beta 95.510(2) _cell_angle_gamma 90 _cell_volume 7730.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1891 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 20.08 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.8822 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_unetI/netI 0.084 _diffrn_reflns_number 69647 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 15238 _reflns_number_gt 10969 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'DIRDIF 99 (Beurskens et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.3059P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15238 _refine_ls_number_parameters 873 _refine_ls_number_restraints 928 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.989 _refine_ls_restrained_S_all 1.934 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.884 _refine_diff_density_min -1.830 _refine_diff_density_rms 0.213 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.84859(10) 0.67866(8) 0.54768(4) 0.0172(4) Uani 1 1 d U . . N3 N 0.7176(5) 0.6255(4) 0.5582(2) 0.0143(16) Uani 1 1 d U . . C2 C 0.6996(7) 0.5710(5) 0.5873(3) 0.0163(10) Uani 1 1 d U . . N1 N 0.6048(5) 0.5499(4) 0.5819(2) 0.0181(17) Uani 1 1 d U . . C5 C 0.5586(7) 0.5888(5) 0.5493(3) 0.0163(10) Uani 1 1 d U . . C4 C 0.6300(6) 0.6349(5) 0.5361(3) 0.015(2) Uani 1 1 d U . . H6 H 0.6204 0.6698 0.5140 0.018 Uiso 1 1 calc R . . Au1 Au 0.79380(3) 0.52607(2) 0.631148(11) 0.01690(10) Uani 1 1 d U . . P1 P 0.88521(18) 0.46413(15) 0.68181(7) 0.0195(6) Uani 1 1 d U . . C7 C 0.9671(6) 0.5267(5) 0.7136(3) 0.018(2) Uani 1 1 d U . . C8 C 1.0238(7) 0.5851(5) 0.6973(3) 0.022(2) Uani 1 1 d U . . H8 H 1.0140 0.5952 0.6700 0.027 Uiso 1 1 calc R . . C9 C 1.0940(7) 0.6291(5) 0.7199(3) 0.021(2) Uani 1 1 d U . . H9 H 1.1326 0.6686 0.7083 0.026 Uiso 1 1 calc R . . C10 C 1.1070(7) 0.6143(5) 0.7598(3) 0.023(2) Uani 1 1 d U . . H10 H 1.1554 0.6437 0.7756 0.027 Uiso 1 1 calc R . . C11 C 1.0503(7) 0.5572(5) 0.7770(3) 0.023(2) Uani 1 1 d U . . H11 H 1.0588 0.5480 0.8044 0.028 Uiso 1 1 calc R . . C12 C 0.9805(7) 0.5134(5) 0.7532(3) 0.025(2) Uani 1 1 d U . . H12 H 0.9417 0.4739 0.7646 0.030 Uiso 1 1 calc R . . C13 C 0.9613(7) 0.3818(5) 0.6641(3) 0.016(2) Uani 1 1 d U . . C14 C 1.0615(7) 0.3832(5) 0.6707(3) 0.022(2) Uani 1 1 d U . . H14 H 1.0929 0.4243 0.6867 0.027 Uiso 1 1 calc R . . C15 C 1.1169(7) 0.3256(5) 0.6542(3) 0.029(3) Uani 1 1 d U . . H15 H 1.1863 0.3271 0.6587 0.034 Uiso 1 1 calc R . . C16 C 1.0718(8) 0.2653(6) 0.6310(3) 0.030(3) Uani 1 1 d U . . H16 H 1.1103 0.2256 0.6195 0.037 Uiso 1 1 calc R . . C17 C 0.9703(8) 0.2629(6) 0.6245(3) 0.030(2) Uani 1 1 d U . . H17 H 0.9388 0.2208 0.6092 0.036 Uiso 1 1 calc R . . C18 C 0.9147(7) 0.3232(5) 0.6408(3) 0.022(2) Uani 1 1 d U . . H18 H 0.8453 0.3235 0.6358 0.026 Uiso 1 1 calc R . . C19 C 0.8013(7) 0.4183(5) 0.7128(3) 0.020(2) Uani 1 1 d U . . C20 C 0.8001(7) 0.3355(6) 0.7213(3) 0.0296(12) Uani 1 1 d U . . H20 H 0.8492 0.3010 0.7126 0.036 Uiso 1 1 calc R . . C21 C 0.7284(7) 0.3035(6) 0.7422(3) 0.0296(12) Uani 1 1 d U . . H21 H 0.7268 0.2467 0.7469 0.036 Uiso 1 1 calc R . . C22 C 0.6595(7) 0.3524(5) 0.7564(3) 0.0296(12) Uani 1 1 d U . . H22 H 0.6112 0.3300 0.7712 0.036 Uiso 1 1 calc R . . C23 C 0.6606(7) 0.4349(6) 0.7488(3) 0.0296(12) Uani 1 1 d U . . H23 H 0.6126 0.4693 0.7583 0.036 Uiso 1 1 calc R . . C24 C 0.7313(7) 0.4670(6) 0.7276(3) 0.0296(12) Uani 1 1 d U . . H24 H 0.7321 0.5237 0.7229 0.036 Uiso 1 1 calc R . . N25 N 0.9007(5) 0.5622(4) 0.5446(2) 0.0163(17) Uani 1 1 d U . . C26 C 0.9624(6) 0.5263(5) 0.5725(3) 0.017(2) Uani 1 1 d U . . H26 H 0.9873 0.5566 0.5948 0.021 Uiso 1 1 calc R . . C27 C 0.9902(6) 0.4446(5) 0.5689(3) 0.018(2) Uani 1 1 d U . . H27 H 1.0347 0.4198 0.5883 0.022 Uiso 1 1 calc R . . C28 C 0.9512(7) 0.4016(5) 0.5368(3) 0.018(2) Uani 1 1 d U . . H28 H 0.9670 0.3459 0.5342 0.022 Uiso 1 1 calc R . . C29 C 0.8887(6) 0.4397(5) 0.5078(3) 0.017(2) Uani 1 1 d U . . H29 H 0.8619 0.4106 0.4854 0.021 Uiso 1 1 calc R . . C30 C 0.8666(6) 0.5204(5) 0.5125(3) 0.0152(10) Uani 1 1 d U . . C31 C 0.8094(6) 0.5686(5) 0.4820(3) 0.0152(10) Uani 1 1 d U . . C32 C 0.7688(6) 0.5383(5) 0.4475(3) 0.019(2) Uani 1 1 d U . . H32 H 0.7723 0.4819 0.4423 0.023 Uiso 1 1 calc R . . C33 C 0.7220(7) 0.5900(6) 0.4198(3) 0.024(2) Uani 1 1 d U . . H33 H 0.6916 0.5694 0.3959 0.028 Uiso 1 1 calc R . . C34 C 0.7207(7) 0.6711(5) 0.4278(3) 0.020(2) Uani 1 1 d U . . H34 H 0.6908 0.7077 0.4089 0.024 Uiso 1 1 calc R . . C35 C 0.7628(6) 0.7000(5) 0.4632(3) 0.015(2) Uani 1 1 d U . . H35 H 0.7611 0.7565 0.4684 0.018 Uiso 1 1 calc R . . N36 N 0.8066(5) 0.6494(4) 0.4908(2) 0.0165(17) Uani 1 1 d U . . C37 C 0.9644(7) 0.7214(5) 0.5374(3) 0.020(2) Uani 1 1 d U . . O37 O 1.0372(5) 0.7518(4) 0.53063(18) 0.0260(17) Uani 1 1 d U . . C38 C 0.7996(7) 0.7782(6) 0.5460(3) 0.019(2) Uani 1 1 d U . . O38 O 0.7778(5) 0.8466(4) 0.5465(2) 0.037(2) Uani 1 1 d U . . C39 C 0.8793(7) 0.6959(5) 0.5991(3) 0.020(2) Uani 1 1 d U . . O39 O 0.8928(4) 0.7130(3) 0.63202(19) 0.0227(17) Uani 1 1 d U . . C41 C 0.5618(6) 0.4904(5) 0.6061(3) 0.020(2) Uani 1 1 d U . . C42 C 0.5326(7) 0.5134(5) 0.6403(3) 0.0259(12) Uani 1 1 d U . . H42 H 0.5361 0.5690 0.6475 0.031 Uiso 1 1 calc R . . C43 C 0.4967(7) 0.4563(5) 0.6658(3) 0.0259(12) Uani 1 1 d U . . H43 H 0.4786 0.4726 0.6906 0.031 Uiso 1 1 calc R . . C44 C 0.4879(7) 0.3744(5) 0.6540(3) 0.0259(12) Uani 1 1 d U . . H44 H 0.4633 0.3345 0.6704 0.031 Uiso 1 1 calc R . . C45 C 0.5154(7) 0.3549(5) 0.6187(3) 0.0259(12) Uani 1 1 d U . . H45 H 0.5095 0.3001 0.6104 0.031 Uiso 1 1 calc R . . C46 C 0.5525(7) 0.4115(5) 0.5937(3) 0.0259(12) Uani 1 1 d U . . H46 H 0.5706 0.3958 0.5687 0.031 Uiso 1 1 calc R . . C6 C 0.4517(6) 0.5770(5) 0.5356(3) 0.026(2) Uani 1 1 d U . . H50A H 0.4302 0.6196 0.5169 0.039 Uiso 1 1 calc R . . H50B H 0.4128 0.5797 0.5581 0.039 Uiso 1 1 calc R . . H50C H 0.4425 0.5239 0.5230 0.039 Uiso 1 1 calc R . . Mn2 Mn 0.32186(10) -0.16175(8) 0.44530(4) 0.0173(4) Uani 1 1 d U . . N3B N 0.1863(5) -0.1071(4) 0.4354(2) 0.0180(17) Uani 1 1 d U . . C2B C 0.1522(7) -0.0544(5) 0.4080(3) 0.0163(10) Uani 1 1 d U . . N1B N 0.0553(5) -0.0398(4) 0.4123(2) 0.0164(17) Uani 1 1 d U . . C5B C 0.0287(7) -0.0831(5) 0.4438(3) 0.0163(10) Uani 1 1 d U . . C4B C 0.1103(6) -0.1242(5) 0.4582(3) 0.019(2) Uani 1 1 d U . . H6B H 0.1147 -0.1592 0.4802 0.022 Uiso 1 1 calc R . . Au1B Au 0.22159(3) 0.00160(2) 0.364922(11) 0.01769(10) Uani 1 1 d U . . P1B P 0.29901(18) 0.06593(15) 0.31739(7) 0.0197(6) Uani 1 1 d U . . C7B C 0.3500(6) -0.0040(5) 0.2845(3) 0.0184(10) Uani 1 1 d U . . C8B C 0.4228(7) -0.0581(5) 0.2996(3) 0.023(2) Uani 1 1 d U . . H8B H 0.4483 -0.0543 0.3263 0.027 Uiso 1 1 calc R . . C9B C 0.4583(8) -0.1177(6) 0.2755(3) 0.035(3) Uani 1 1 d U . . H9B H 0.5065 -0.1551 0.2861 0.042 Uiso 1 1 calc R . . C10B C 0.4242(8) -0.1224(6) 0.2371(3) 0.036(3) Uani 1 1 d U . . H10B H 0.4495 -0.1620 0.2207 0.043 Uiso 1 1 calc R . . C11B C 0.3512(8) -0.0681(6) 0.2218(3) 0.035(3) Uani 1 1 d U . . H11B H 0.3267 -0.0712 0.1950 0.042 Uiso 1 1 calc R . . C12B C 0.3158(7) -0.0114(6) 0.2453(3) 0.027(2) Uani 1 1 d U . . H12B H 0.2661 0.0245 0.2346 0.033 Uiso 1 1 calc R . . C13B C 0.3963(7) 0.1316(5) 0.3378(3) 0.0184(10) Uani 1 1 d U . . C14B C 0.3680(7) 0.1977(5) 0.3615(3) 0.021(2) Uani 1 1 d U . . H14B H 0.3010 0.2042 0.3657 0.025 Uiso 1 1 calc R . . C15B C 0.4362(7) 0.2516(5) 0.3781(3) 0.0229(12) Uani 1 1 d U . . H15B H 0.4164 0.2942 0.3942 0.027 Uiso 1 1 calc R . . C16B C 0.5328(7) 0.2440(5) 0.3713(3) 0.0229(12) Uani 1 1 d U . . H16B H 0.5795 0.2824 0.3821 0.027 Uiso 1 1 calc R . . C17B C 0.5626(7) 0.1801(5) 0.3487(3) 0.0229(12) Uani 1 1 d U . . H17B H 0.6299 0.1742 0.3448 0.027 Uiso 1 1 calc R . . C18B C 0.4953(7) 0.1258(5) 0.3323(3) 0.0229(12) Uani 1 1 d U . . H18B H 0.5167 0.0830 0.3166 0.027 Uiso 1 1 calc R . . C19B C 0.2226(7) 0.1370(5) 0.2879(3) 0.0184(10) Uani 1 1 d U . . C20B C 0.1253(7) 0.1466(5) 0.2927(3) 0.019(2) Uani 1 1 d U . . H20B H 0.0947 0.1115 0.3098 0.023 Uiso 1 1 calc R . . C21B C 0.0712(8) 0.2070(6) 0.2729(3) 0.029(2) Uani 1 1 d U . . H21B H 0.0039 0.2139 0.2767 0.035 Uiso 1 1 calc R . . C22B C 0.1150(8) 0.2572(6) 0.2478(3) 0.035(3) Uani 1 1 d U . . H22B H 0.0772 0.2982 0.2341 0.042 Uiso 1 1 calc R . . C23B C 0.2122(8) 0.2490(5) 0.2421(3) 0.033(3) Uani 1 1 d U . . H23B H 0.2418 0.2847 0.2250 0.039 Uiso 1 1 calc R . . C24B C 0.2667(7) 0.1879(6) 0.2617(3) 0.032(3) Uani 1 1 d U . . H24B H 0.3336 0.1805 0.2574 0.039 Uiso 1 1 calc R . . N25B N 0.3063(5) -0.1346(4) 0.5026(2) 0.0176(17) Uani 1 1 d U . . C26B C 0.2733(6) -0.1861(6) 0.5300(3) 0.021(2) Uani 1 1 d U . . H26B H 0.2655 -0.2420 0.5238 0.025 Uiso 1 1 calc R . . C27B C 0.2514(6) -0.1596(6) 0.5656(3) 0.022(2) Uani 1 1 d U . . H27B H 0.2294 -0.1963 0.5842 0.026 Uiso 1 1 calc R . . C28B C 0.2621(6) -0.0761(6) 0.5743(3) 0.023(2) Uani 1 1 d U . . H28B H 0.2458 -0.0555 0.5987 0.028 Uiso 1 1 calc R . . C29B C 0.2960(6) -0.0255(6) 0.5473(3) 0.021(2) Uani 1 1 d U . . H29B H 0.3031 0.0308 0.5525 0.025 Uiso 1 1 calc R . . C30B C 0.3198(6) -0.0568(5) 0.5124(3) 0.0152(10) Uani 1 1 d U . . C31B C 0.3664(6) -0.0075(5) 0.4832(3) 0.0152(10) Uani 1 1 d U . . C32B C 0.3992(6) 0.0713(5) 0.4894(3) 0.0186(11) Uani 1 1 d U . . H32B H 0.3874 0.0989 0.5128 0.022 Uiso 1 1 calc R . . C33B C 0.4491(6) 0.1099(5) 0.4615(3) 0.0186(11) Uani 1 1 d U . . H33B H 0.4697 0.1646 0.4648 0.022 Uiso 1 1 calc R . . C34B C 0.4679(6) 0.0658(5) 0.4287(3) 0.0186(11) Uani 1 1 d U . . H34B H 0.5059 0.0894 0.4099 0.022 Uiso 1 1 calc R . . C35B C 0.4321(6) -0.0118(5) 0.4230(3) 0.0186(11) Uani 1 1 d U . . H35B H 0.4439 -0.0403 0.3999 0.022 Uiso 1 1 calc R . . N36B N 0.3805(5) -0.0481(4) 0.4498(2) 0.0189(17) Uani 1 1 d U . . C37B C 0.2701(7) -0.2607(6) 0.4460(3) 0.022(2) Uani 1 1 d U . . O37B O 0.2418(5) -0.3278(4) 0.4458(2) 0.034(2) Uani 1 1 d U . . C38B C 0.4411(7) -0.2074(5) 0.4560(3) 0.021(2) Uani 1 1 d U . . O38B O 0.5148(5) -0.2393(4) 0.46339(18) 0.0253(17) Uani 1 1 d U . . C39B C 0.3264(7) -0.1743(5) 0.3926(3) 0.020(2) Uani 1 1 d U . . O39B O 0.3255(5) -0.1895(4) 0.35996(19) 0.0265(17) Uani 1 1 d U . . C41B C -0.0106(6) 0.0102(5) 0.3858(3) 0.0184(10) Uani 1 1 d U . . C42B C -0.0815(7) -0.0230(5) 0.3620(3) 0.023(2) Uani 1 1 d U . . H42B H -0.0878 -0.0804 0.3617 0.028 Uiso 1 1 calc R . . C43B C -0.1466(7) 0.0222(5) 0.3374(3) 0.025(2) Uani 1 1 d U . . H43B H -0.1969 -0.0031 0.3207 0.030 Uiso 1 1 calc R . . C44B C -0.1358(7) 0.1033(6) 0.3382(3) 0.022(2) Uani 1 1 d U . . H44B H -0.1784 0.1358 0.3212 0.027 Uiso 1 1 calc R . . C45B C -0.0639(7) 0.1404(6) 0.3632(3) 0.028(2) Uani 1 1 d U . . H45B H -0.0583 0.1978 0.3639 0.033 Uiso 1 1 calc R . . C46B C 0.0011(7) 0.0919(5) 0.3877(3) 0.024(2) Uani 1 1 d U . . H46B H 0.0514 0.1157 0.4050 0.028 Uiso 1 1 calc R . . C6B C -0.0705(7) -0.0786(5) 0.4588(3) 0.031(3) Uani 1 1 d U . . H50D H -0.1195 -0.1026 0.4396 0.046 Uiso 1 1 calc R . . H50E H -0.0873 -0.0217 0.4631 0.046 Uiso 1 1 calc R . . H50F H -0.0694 -0.1084 0.4835 0.046 Uiso 1 1 calc R . . Cl1 Cl 0.3513(2) 0.12993(15) 0.63105(8) 0.0306(7) Uani 1 1 d U . . O101 O 0.3183(8) 0.1741(6) 0.6609(3) 0.124(4) Uani 1 1 d U . . O102 O 0.2774(6) 0.1364(4) 0.5989(3) 0.072(3) Uani 1 1 d U . . O103 O 0.3673(5) 0.0474(4) 0.6414(3) 0.064(3) Uani 1 1 d U . . O104 O 0.4406(6) 0.1608(4) 0.6212(3) 0.078(3) Uani 1 1 d U . . Cl2 Cl 0.79871(18) 0.14152(14) 0.88035(7) 0.0232(6) Uani 1 1 d U . . O105 O 0.7533(5) 0.1960(3) 0.85120(19) 0.0311(18) Uani 1 1 d U . . O106 O 0.7521(5) 0.1484(4) 0.9164(2) 0.040(2) Uani 1 1 d U . . O107 O 0.8995(5) 0.1643(4) 0.8888(2) 0.0368(19) Uani 1 1 d U . . O108 O 0.7924(5) 0.0599(3) 0.86713(19) 0.041(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0130(9) 0.0210(9) 0.0174(9) -0.0001(7) 0.0007(7) -0.0006(7) N3 0.012(4) 0.017(4) 0.013(4) -0.001(3) -0.001(3) 0.001(3) C2 0.015(2) 0.014(3) 0.019(3) -0.0026(19) 0.000(2) 0.001(2) N1 0.019(4) 0.014(4) 0.021(4) 0.001(3) 0.005(3) 0.001(3) C5 0.015(2) 0.014(3) 0.019(3) -0.0026(19) 0.000(2) 0.001(2) C4 0.010(4) 0.025(6) 0.012(5) 0.001(4) 0.005(4) 0.006(4) Au1 0.0157(2) 0.0195(2) 0.0158(2) 0.00194(18) 0.00284(17) 0.00011(18) P1 0.0173(15) 0.0252(15) 0.0163(15) 0.0008(12) 0.0038(12) 0.0022(12) C7 0.016(5) 0.020(5) 0.018(5) 0.005(4) -0.001(4) 0.006(4) C8 0.022(6) 0.033(6) 0.012(5) 0.004(4) 0.002(4) -0.001(4) C9 0.023(6) 0.021(6) 0.019(5) 0.002(4) -0.004(5) 0.004(4) C10 0.022(6) 0.020(6) 0.024(5) -0.013(5) -0.006(5) 0.002(4) C11 0.031(7) 0.018(6) 0.019(5) 0.002(4) -0.008(4) 0.010(4) C12 0.023(6) 0.026(6) 0.028(5) 0.002(4) 0.004(4) 0.001(4) C13 0.020(5) 0.015(5) 0.014(6) 0.008(4) 0.006(4) 0.002(4) C14 0.020(5) 0.025(6) 0.023(6) 0.000(4) 0.001(5) 0.006(4) C15 0.024(6) 0.025(6) 0.038(7) 0.011(5) 0.015(5) 0.003(4) C16 0.038(6) 0.022(6) 0.033(7) 0.005(5) 0.012(5) 0.007(5) C17 0.043(6) 0.021(6) 0.027(6) 0.003(5) 0.006(5) -0.002(5) C18 0.025(6) 0.031(6) 0.010(6) 0.002(4) 0.009(4) -0.003(4) C19 0.020(5) 0.022(5) 0.020(6) -0.004(4) 0.010(4) -0.004(4) C20 0.031(3) 0.032(3) 0.029(3) 0.008(2) 0.015(2) 0.008(2) C21 0.031(3) 0.032(3) 0.029(3) 0.008(2) 0.015(2) 0.008(2) C22 0.031(3) 0.032(3) 0.029(3) 0.008(2) 0.015(2) 0.008(2) C23 0.031(3) 0.032(3) 0.029(3) 0.008(2) 0.015(2) 0.008(2) C24 0.031(3) 0.032(3) 0.029(3) 0.008(2) 0.015(2) 0.008(2) N25 0.018(5) 0.022(4) 0.010(4) 0.004(3) 0.005(3) 0.001(3) C26 0.009(5) 0.024(5) 0.020(5) 0.003(4) 0.007(4) 0.000(4) C27 0.011(5) 0.023(5) 0.020(5) 0.003(4) 0.003(4) 0.001(4) C28 0.019(6) 0.011(5) 0.027(6) 0.004(4) 0.010(4) -0.001(4) C29 0.016(6) 0.026(5) 0.012(5) -0.007(4) 0.009(4) -0.001(4) C30 0.008(3) 0.022(2) 0.016(2) 0.0006(19) 0.0044(19) -0.001(2) C31 0.008(3) 0.022(2) 0.016(2) 0.0006(19) 0.0044(19) -0.001(2) C32 0.015(5) 0.017(5) 0.025(5) -0.004(4) 0.002(4) 0.006(4) C33 0.020(6) 0.042(6) 0.008(5) -0.003(4) 0.002(4) -0.007(5) C34 0.022(6) 0.025(5) 0.014(5) 0.009(4) 0.008(4) 0.007(5) C35 0.006(5) 0.019(5) 0.022(5) 0.001(4) 0.009(4) -0.001(4) N36 0.015(5) 0.017(4) 0.017(4) 0.001(3) 0.003(3) 0.001(3) C37 0.023(5) 0.024(6) 0.013(5) -0.002(4) 0.000(4) 0.000(4) O37 0.023(4) 0.031(4) 0.024(4) 0.000(3) 0.002(3) -0.005(3) C38 0.010(5) 0.024(4) 0.022(6) -0.005(4) 0.000(4) -0.008(4) O38 0.029(5) 0.029(4) 0.050(6) -0.006(4) -0.009(4) 0.014(4) C39 0.016(6) 0.019(6) 0.025(5) -0.002(4) 0.001(4) -0.001(4) O39 0.025(4) 0.019(4) 0.023(4) -0.003(3) -0.004(4) 0.000(3) C41 0.009(5) 0.022(5) 0.030(5) -0.005(4) 0.002(4) -0.004(4) C42 0.033(3) 0.016(3) 0.031(3) 0.001(2) 0.014(2) -0.005(2) C43 0.033(3) 0.016(3) 0.031(3) 0.001(2) 0.014(2) -0.005(2) C44 0.033(3) 0.016(3) 0.031(3) 0.001(2) 0.014(2) -0.005(2) C45 0.033(3) 0.016(3) 0.031(3) 0.001(2) 0.014(2) -0.005(2) C46 0.033(3) 0.016(3) 0.031(3) 0.001(2) 0.014(2) -0.005(2) C6 0.018(5) 0.034(6) 0.027(7) 0.000(5) 0.008(5) 0.001(5) Mn2 0.0139(9) 0.0234(9) 0.0145(9) 0.0019(7) 0.0014(7) -0.0007(7) N3B 0.011(4) 0.023(4) 0.020(5) 0.001(3) 0.002(3) -0.003(3) C2B 0.015(2) 0.014(3) 0.019(3) -0.0026(19) 0.000(2) 0.001(2) N1B 0.015(4) 0.023(4) 0.011(4) 0.001(3) 0.002(3) -0.006(3) C5B 0.015(2) 0.014(3) 0.019(3) -0.0026(19) 0.000(2) 0.001(2) C4B 0.011(5) 0.034(6) 0.010(5) 0.005(4) -0.001(4) -0.002(4) Au1B 0.0149(2) 0.0223(2) 0.0161(2) 0.00371(18) 0.00247(16) -0.00214(18) P1B 0.0154(15) 0.0281(16) 0.0155(15) 0.0037(12) 0.0017(12) -0.0038(12) C7B 0.017(2) 0.021(3) 0.018(3) 0.0032(19) 0.004(2) -0.002(2) C8B 0.039(7) 0.020(6) 0.009(5) -0.002(4) 0.005(4) -0.003(4) C9B 0.050(8) 0.021(6) 0.035(6) 0.001(5) 0.007(6) 0.008(5) C10B 0.053(8) 0.025(6) 0.032(6) -0.017(5) 0.019(6) -0.014(5) C11B 0.044(8) 0.038(7) 0.022(6) -0.005(5) 0.003(5) -0.018(5) C12B 0.022(6) 0.040(6) 0.019(5) 0.001(4) -0.002(4) -0.010(5) C13B 0.017(2) 0.021(3) 0.018(3) 0.0032(19) 0.004(2) -0.002(2) C14B 0.017(5) 0.031(6) 0.016(6) 0.001(4) 0.002(4) 0.001(4) C15B 0.021(3) 0.027(3) 0.022(3) 0.002(2) 0.008(2) -0.004(2) C16B 0.021(3) 0.027(3) 0.022(3) 0.002(2) 0.008(2) -0.004(2) C17B 0.021(3) 0.027(3) 0.022(3) 0.002(2) 0.008(2) -0.004(2) C18B 0.021(3) 0.027(3) 0.022(3) 0.002(2) 0.008(2) -0.004(2) C19B 0.017(2) 0.021(3) 0.018(3) 0.0032(19) 0.004(2) -0.002(2) C20B 0.018(5) 0.024(6) 0.015(6) 0.000(4) 0.004(4) -0.006(4) C21B 0.027(6) 0.035(7) 0.024(7) -0.011(4) 0.001(5) 0.000(4) C22B 0.040(6) 0.040(7) 0.024(6) 0.006(5) -0.004(5) 0.007(6) C23B 0.041(6) 0.022(6) 0.035(7) 0.014(5) -0.001(5) -0.007(5) C24B 0.023(6) 0.044(7) 0.030(7) 0.011(5) 0.007(5) 0.001(5) N25B 0.011(4) 0.029(4) 0.013(4) 0.005(3) 0.003(3) 0.003(3) C26B 0.014(6) 0.031(5) 0.018(5) 0.008(4) 0.002(5) 0.003(4) C27B 0.009(5) 0.041(5) 0.015(5) 0.015(5) 0.002(4) 0.009(5) C28B 0.015(6) 0.047(6) 0.008(5) 0.001(4) 0.001(4) 0.013(5) C29B 0.017(5) 0.033(5) 0.013(5) 0.000(4) 0.000(4) 0.009(5) C30B 0.008(3) 0.022(2) 0.016(2) 0.0006(19) 0.0044(19) -0.001(2) C31B 0.008(3) 0.022(2) 0.016(2) 0.0006(19) 0.0044(19) -0.001(2) C32B 0.012(3) 0.024(3) 0.019(3) 0.008(2) -0.002(2) 0.004(2) C33B 0.012(3) 0.024(3) 0.019(3) 0.008(2) -0.002(2) 0.004(2) C34B 0.012(3) 0.024(3) 0.019(3) 0.008(2) -0.002(2) 0.004(2) C35B 0.012(3) 0.024(3) 0.019(3) 0.008(2) -0.002(2) 0.004(2) N36B 0.013(4) 0.030(4) 0.013(4) 0.004(3) -0.001(3) 0.000(3) C37B 0.020(6) 0.022(5) 0.025(6) 0.000(4) 0.005(5) 0.010(4) O37B 0.025(5) 0.025(4) 0.053(6) 0.003(4) 0.016(4) -0.003(3) C38B 0.019(5) 0.029(6) 0.015(6) -0.004(4) 0.008(4) -0.001(4) O38B 0.022(4) 0.026(4) 0.028(4) -0.005(3) 0.002(3) 0.006(3) C39B 0.014(6) 0.022(6) 0.023(4) -0.001(4) 0.003(4) 0.001(4) O39B 0.030(4) 0.031(4) 0.019(4) -0.007(3) 0.006(4) -0.011(3) C41B 0.017(2) 0.021(3) 0.018(3) 0.0032(19) 0.004(2) -0.002(2) C42B 0.040(6) 0.017(5) 0.014(5) -0.001(4) 0.002(4) 0.008(4) C43B 0.033(6) 0.028(5) 0.013(5) -0.002(4) 0.002(4) 0.003(5) C44B 0.019(6) 0.030(5) 0.019(6) 0.009(5) 0.007(4) 0.014(5) C45B 0.021(6) 0.026(6) 0.038(7) 0.006(5) 0.011(5) 0.000(4) C46B 0.015(6) 0.028(5) 0.027(6) 0.002(4) 0.001(4) -0.004(4) C6B 0.026(6) 0.041(7) 0.027(7) 0.017(5) 0.011(5) 0.008(5) Cl1 0.0257(17) 0.0284(17) 0.0374(19) -0.0040(13) 0.0013(14) -0.0014(13) O101 0.151(10) 0.167(9) 0.055(7) -0.032(6) 0.022(6) 0.105(8) O102 0.068(6) 0.034(5) 0.102(7) -0.020(5) -0.060(5) 0.014(4) O103 0.051(6) 0.032(4) 0.104(8) 0.031(4) -0.018(5) -0.004(4) O104 0.036(5) 0.067(6) 0.133(9) 0.040(6) 0.019(5) -0.007(4) Cl2 0.0214(15) 0.0253(16) 0.0230(16) 0.0024(12) 0.0032(12) 0.0046(12) O105 0.036(5) 0.032(4) 0.025(4) 0.009(3) 0.000(3) 0.006(3) O106 0.064(5) 0.025(4) 0.036(5) 0.008(3) 0.036(4) 0.011(4) O107 0.019(4) 0.046(5) 0.044(5) -0.003(4) -0.005(3) 0.005(3) O108 0.083(6) 0.014(4) 0.025(4) -0.009(3) 0.006(4) 0.015(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C38 1.773(10) . ? Mn1 C39 1.799(10) . ? Mn1 C37 1.802(10) . ? Mn1 N36 2.041(7) . ? Mn1 N25 2.056(7) . ? Mn1 N3 2.060(7) . ? N3 C4 1.366(10) . ? N3 C2 1.386(10) . ? C2 N1 1.339(10) . ? C2 Au1 2.027(9) . ? N1 C5 1.390(11) . ? N1 C41 1.448(10) . ? C5 C4 1.352(11) . ? C5 C6 1.508(12) . ? C4 H6 0.9500 . ? Au1 P1 2.286(2) . ? P1 C19 1.806(9) . ? P1 C7 1.811(9) . ? P1 C13 1.850(9) . ? C7 C12 1.374(12) . ? C7 C8 1.389(11) . ? C8 C9 1.382(12) . ? C8 H8 0.9500 . ? C9 C10 1.387(12) . ? C9 H9 0.9500 . ? C10 C11 1.389(12) . ? C10 H10 0.9500 . ? C11 C12 1.398(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.370(12) . ? C13 C18 1.373(11) . ? C14 C15 1.372(11) . ? C14 H14 0.9500 . ? C15 C16 1.382(12) . ? C15 H15 0.9500 . ? C16 C17 1.388(13) . ? C16 H16 0.9500 . ? C17 C18 1.402(12) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.383(11) . ? C19 C20 1.398(11) . ? C20 C21 1.377(12) . ? C20 H20 0.9500 . ? C21 C22 1.366(12) . ? C21 H21 0.9500 . ? C22 C23 1.386(11) . ? C22 H22 0.9500 . ? C23 C24 1.374(12) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? N25 C30 1.348(10) . ? N25 C26 1.350(10) . ? C26 C27 1.408(11) . ? C26 H26 0.9500 . ? C27 C28 1.377(12) . ? C27 H27 0.9500 . ? C28 C29 1.399(12) . ? C28 H28 0.9500 . ? C29 C30 1.378(11) . ? C29 H29 0.9500 . ? C30 C31 1.478(11) . ? C31 C32 1.356(11) . ? C31 N36 1.369(10) . ? C32 C33 1.387(12) . ? C32 H32 0.9500 . ? C33 C34 1.367(11) . ? C33 H33 0.9500 . ? C34 C35 1.381(12) . ? C34 H34 0.9500 . ? C35 N36 1.360(10) . ? C35 H35 0.9500 . ? C37 O37 1.160(10) . ? C38 O38 1.168(9) . ? C39 O39 1.163(10) . ? C41 C42 1.332(11) . ? C41 C46 1.371(11) . ? C42 C43 1.408(11) . ? C42 H42 0.9500 . ? C43 C44 1.412(11) . ? C43 H43 0.9500 . ? C44 C45 1.341(12) . ? C44 H44 0.9500 . ? C45 C46 1.399(11) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C6 H50A 0.9800 . ? C6 H50B 0.9800 . ? C6 H50C 0.9800 . ? Mn2 C37B 1.781(10) . ? Mn2 C38B 1.805(10) . ? Mn2 C39B 1.829(10) . ? Mn2 N36B 2.040(7) . ? Mn2 N25B 2.049(7) . ? Mn2 N3B 2.064(7) . ? N3B C2B 1.332(10) . ? N3B C4B 1.391(10) . ? C2B N1B 1.371(10) . ? C2B Au1B 2.053(9) . ? N1B C5B 1.376(10) . ? N1B C41B 1.471(10) . ? C5B C4B 1.359(11) . ? C5B C6B 1.500(12) . ? C4B H6B 0.9500 . ? Au1B P1B 2.292(3) . ? P1B C7B 1.803(9) . ? P1B C13B 1.807(9) . ? P1B C19B 1.814(9) . ? C7B C12B 1.387(12) . ? C7B C8B 1.401(11) . ? C8B C9B 1.403(12) . ? C8B H8B 0.9500 . ? C9B C10B 1.359(13) . ? C9B H9B 0.9500 . ? C10B C11B 1.406(13) . ? C10B H10B 0.9500 . ? C11B C12B 1.356(12) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C18B 1.390(12) . ? C13B C14B 1.435(11) . ? C14B C15B 1.374(11) . ? C14B H14B 0.9500 . ? C15B C16B 1.371(11) . ? C15B H15B 0.9500 . ? C16B C17B 1.393(11) . ? C16B H16B 0.9500 . ? C17B C18B 1.369(11) . ? C17B H17B 0.9500 . ? C18B H18B 0.9500 . ? C19B C20B 1.367(11) . ? C19B C24B 1.411(12) . ? C20B C21B 1.380(12) . ? C20B H20B 0.9500 . ? C21B C22B 1.376(12) . ? C21B H21B 0.9500 . ? C22B C23B 1.370(13) . ? C22B H22B 0.9500 . ? C23B C24B 1.389(12) . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? N25B C30B 1.335(10) . ? N25B C26B 1.378(10) . ? C26B C27B 1.360(12) . ? C26B H26B 0.9500 . ? C27B C28B 1.415(12) . ? C27B H27B 0.9500 . ? C28B C29B 1.363(11) . ? C28B H28B 0.9500 . ? C29B C30B 1.373(11) . ? C29B H29B 0.9500 . ? C30B C31B 1.482(11) . ? C31B N36B 1.359(10) . ? C31B C32B 1.386(11) . ? C32B C33B 1.384(11) . ? C32B H32B 0.9500 . ? C33B C34B 1.387(11) . ? C33B H33B 0.9500 . ? C34B C35B 1.378(11) . ? C34B H34B 0.9500 . ? C35B N36B 1.353(10) . ? C35B H35B 0.9500 . ? C37B O37B 1.173(9) . ? C38B O38B 1.145(10) . ? C39B O39B 1.149(10) . ? C41B C42B 1.328(12) . ? C41B C46B 1.357(11) . ? C42B C43B 1.386(12) . ? C42B H42B 0.9500 . ? C43B C44B 1.346(11) . ? C43B H43B 0.9500 . ? C44B C45B 1.388(12) . ? C44B H44B 0.9500 . ? C45B C46B 1.413(12) . ? C45B H45B 0.9500 . ? C46B H46B 0.9500 . ? C6B H50D 0.9800 . ? C6B H50E 0.9800 . ? C6B H50F 0.9800 . ? Cl1 O101 1.371(8) . ? Cl1 O104 1.395(8) . ? Cl1 O103 1.419(7) . ? Cl1 O102 1.429(8) . ? Cl2 O108 1.420(6) . ? Cl2 O107 1.434(7) . ? Cl2 O105 1.441(6) . ? Cl2 O106 1.451(6) . ? 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 C38 Mn1 C39 86.4(4) . . ? C38 Mn1 C37 88.2(4) . . ? C39 Mn1 C37 90.3(4) . . ? C38 Mn1 N36 96.7(4) . . ? C39 Mn1 N36 174.5(4) . . ? C37 Mn1 N36 94.4(4) . . ? C38 Mn1 N25 175.0(4) . . ? C39 Mn1 N25 98.5(4) . . ? C37 Mn1 N25 92.2(3) . . ? N36 Mn1 N25 78.3(3) . . ? C38 Mn1 N3 93.8(3) . . ? C39 Mn1 N3 91.2(4) . . ? C37 Mn1 N3 177.6(3) . . ? N36 Mn1 N3 84.1(3) . . ? N25 Mn1 N3 85.7(3) . . ? C4 N3 C2 105.6(7) . . ? C4 N3 Mn1 125.9(6) . . ? C2 N3 Mn1 128.4(6) . . ? N1 C2 N3 107.8(8) . . ? N1 C2 Au1 123.2(7) . . ? N3 C2 Au1 129.0(7) . . ? C2 N1 C5 110.7(8) . . ? C2 N1 C41 122.6(8) . . ? C5 N1 C41 126.6(8) . . ? C4 C5 N1 104.0(8) . . ? C4 C5 C6 132.9(9) . . ? N1 C5 C6 123.1(8) . . ? C5 C4 N3 111.9(8) . . ? C5 C4 H6 124.0 . . ? N3 C4 H6 124.0 . . ? C2 Au1 P1 172.9(3) . . ? C19 P1 C7 106.0(4) . . ? C19 P1 C13 107.3(4) . . ? C7 P1 C13 106.3(4) . . ? C19 P1 Au1 107.6(3) . . ? C7 P1 Au1 117.8(3) . . ? C13 P1 Au1 111.3(3) . . ? C12 C7 C8 118.8(9) . . ? C12 C7 P1 121.5(7) . . ? C8 C7 P1 119.4(7) . . ? C9 C8 C7 121.7(9) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 118.6(9) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C9 C10 C11 121.1(9) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 118.7(9) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 121.1(9) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C18 120.7(9) . . ? C14 C13 P1 121.4(7) . . ? C18 C13 P1 117.6(7) . . ? C13 C14 C15 120.3(9) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.2(10) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.9(10) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 119.4(10) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 119.5(9) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C24 C19 C20 117.9(9) . . ? C24 C19 P1 118.5(7) . . ? C20 C19 P1 123.6(7) . . ? C21 C20 C19 120.5(9) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.7(9) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.6(10) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 119.9(9) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 121.4(9) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C30 N25 C26 120.0(8) . . ? C30 N25 Mn1 115.1(6) . . ? C26 N25 Mn1 124.8(6) . . ? N25 C26 C27 121.0(9) . . ? N25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 118.3(9) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 120.2(8) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 118.5(9) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? N25 C30 C29 121.8(8) . . ? N25 C30 C31 115.2(8) . . ? C29 C30 C31 122.9(9) . . ? C32 C31 N36 122.3(8) . . ? C32 C31 C30 124.6(8) . . ? N36 C31 C30 113.0(8) . . ? C31 C32 C33 119.8(9) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 118.7(9) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C33 C34 C35 120.1(9) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? N36 C35 C34 121.5(8) . . ? N36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 N36 C31 117.6(8) . . ? C35 N36 Mn1 126.0(6) . . ? C31 N36 Mn1 115.5(6) . . ? O37 C37 Mn1 177.4(8) . . ? O38 C38 Mn1 172.4(8) . . ? O39 C39 Mn1 173.6(8) . . ? C42 C41 C46 121.2(9) . . ? C42 C41 N1 119.0(8) . . ? C46 C41 N1 119.7(8) . . ? C41 C42 C43 120.7(9) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.1(9) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 117.7(9) . . ? C45 C44 H44 121.1 . . ? C43 C44 H44 121.1 . . ? C44 C45 C46 123.1(9) . . ? C44 C45 H45 118.4 . . ? C46 C45 H45 118.4 . . ? C41 C46 C45 118.0(9) . . ? C41 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? C5 C6 H50A 109.5 . . ? C5 C6 H50B 109.5 . . ? H50A C6 H50B 109.5 . . ? C5 C6 H50C 109.5 . . ? H50A C6 H50C 109.5 . . ? H50B C6 H50C 109.5 . . ? C37B Mn2 C38B 88.2(4) . . ? C37B Mn2 C39B 87.7(4) . . ? C38B Mn2 C39B 92.2(4) . . ? C37B Mn2 N36B 174.9(4) . . ? C38B Mn2 N36B 91.5(4) . . ? C39B Mn2 N36B 97.4(4) . . ? C37B Mn2 N25B 96.3(4) . . ? C38B Mn2 N25B 94.1(4) . . ? C39B Mn2 N25B 172.6(4) . . ? N36B Mn2 N25B 78.6(3) . . ? C37B Mn2 N3B 92.8(3) . . ? C38B Mn2 N3B 177.6(4) . . ? C39B Mn2 N3B 90.1(4) . . ? N36B Mn2 N3B 87.3(3) . . ? N25B Mn2 N3B 83.6(3) . . ? C2B N3B C4B 107.5(8) . . ? C2B N3B Mn2 130.6(6) . . ? C4B N3B Mn2 121.9(6) . . ? N3B C2B N1B 108.4(8) . . ? N3B C2B Au1B 130.3(7) . . ? N1B C2B Au1B 121.2(6) . . ? C2B N1B C5B 109.0(7) . . ? C2B N1B C41B 125.1(7) . . ? C5B N1B C41B 125.8(7) . . ? C4B C5B N1B 105.9(8) . . ? C4B C5B C6B 129.8(9) . . ? N1B C5B C6B 124.2(8) . . ? C5B C4B N3B 109.1(8) . . ? C5B C4B H6B 125.4 . . ? N3B C4B H6B 125.4 . . ? C2B Au1B P1B 179.1(2) . . ? C7B P1B C13B 108.2(4) . . ? C7B P1B C19B 107.5(4) . . ? C13B P1B C19B 101.2(4) . . ? C7B P1B Au1B 112.6(3) . . ? C13B P1B Au1B 112.1(3) . . ? C19B P1B Au1B 114.5(3) . . ? C12B C7B C8B 117.8(9) . . ? C12B C7B P1B 123.4(7) . . ? C8B C7B P1B 118.6(7) . . ? C7B C8B C9B 120.1(9) . . ? C7B C8B H8B 119.9 . . ? C9B C8B H8B 119.9 . . ? C10B C9B C8B 120.5(10) . . ? C10B C9B H9B 119.8 . . ? C8B C9B H9B 119.8 . . ? C9B C10B C11B 119.5(10) . . ? C9B C10B H10B 120.3 . . ? C11B C10B H10B 120.3 . . ? C12B C11B C10B 120.0(10) . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C12B C7B 122.1(10) . . ? C11B C12B H12B 118.9 . . ? C7B C12B H12B 118.9 . . ? C18B C13B C14B 116.8(8) . . ? C18B C13B P1B 126.7(7) . . ? C14B C13B P1B 116.5(7) . . ? C15B C14B C13B 121.1(9) . . ? C15B C14B H14B 119.4 . . ? C13B C14B H14B 119.4 . . ? C14B C15B C16B 120.0(9) . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C15B C16B C17B 120.2(9) . . ? C15B C16B H16B 119.9 . . ? C17B C16B H16B 119.9 . . ? C18B C17B C16B 120.2(9) . . ? C18B C17B H17B 119.9 . . ? C16B C17B H17B 119.9 . . ? C17B C18B C13B 121.7(9) . . ? C17B C18B H18B 119.2 . . ? C13B C18B H18B 119.2 . . ? C20B C19B C24B 119.3(9) . . ? C20B C19B P1B 121.7(7) . . ? C24B C19B P1B 118.8(7) . . ? C19B C20B C21B 120.6(9) . . ? C19B C20B H20B 119.7 . . ? C21B C20B H20B 119.7 . . ? C22B C21B C20B 119.8(10) . . ? C22B C21B H21B 120.1 . . ? C20B C21B H21B 120.1 . . ? C23B C22B C21B 121.2(10) . . ? C23B C22B H22B 119.4 . . ? C21B C22B H22B 119.4 . . ? C22B C23B C24B 119.2(10) . . ? C22B C23B H23B 120.4 . . ? C24B C23B H23B 120.4 . . ? C23B C24B C19B 119.8(10) . . ? C23B C24B H24B 120.1 . . ? C19B C24B H24B 120.1 . . ? C30B N25B C26B 117.8(8) . . ? C30B N25B Mn2 115.4(6) . . ? C26B N25B Mn2 126.4(6) . . ? C27B C26B N25B 122.2(9) . . ? C27B C26B H26B 118.9 . . ? N25B C26B H26B 118.9 . . ? C26B C27B C28B 118.5(9) . . ? C26B C27B H27B 120.8 . . ? C28B C27B H27B 120.8 . . ? C29B C28B C27B 119.1(9) . . ? C29B C28B H28B 120.4 . . ? C27B C28B H28B 120.4 . . ? C28B C29B C30B 119.4(9) . . ? C28B C29B H29B 120.3 . . ? C30B C29B H29B 120.3 . . ? N25B C30B C29B 122.9(9) . . ? N25B C30B C31B 114.4(8) . . ? C29B C30B C31B 122.6(8) . . ? N36B C31B C32B 121.5(8) . . ? N36B C31B C30B 114.1(8) . . ? C32B C31B C30B 124.3(8) . . ? C33B C32B C31B 119.9(9) . . ? C33B C32B H32B 120.1 . . ? C31B C32B H32B 120.1 . . ? C32B C33B C34B 117.8(9) . . ? C32B C33B H33B 121.1 . . ? C34B C33B H33B 121.1 . . ? C35B C34B C33B 120.7(9) . . ? C35B C34B H34B 119.6 . . ? C33B C34B H34B 119.6 . . ? N36B C35B C34B 121.1(9) . . ? N36B C35B H35B 119.5 . . ? C34B C35B H35B 119.5 . . ? C35B N36B C31B 118.9(8) . . ? C35B N36B Mn2 125.7(6) . . ? C31B N36B Mn2 115.4(6) . . ? O37B C37B Mn2 175.6(8) . . ? O38B C38B Mn2 177.0(9) . . ? O39B C39B Mn2 173.5(8) . . ? C42B C41B C46B 121.0(9) . . ? C42B C41B N1B 121.2(8) . . ? C46B C41B N1B 117.7(8) . . ? C41B C42B C43B 122.9(9) . . ? C41B C42B H42B 118.5 . . ? C43B C42B H42B 118.5 . . ? C44B C43B C42B 117.4(9) . . ? C44B C43B H43B 121.3 . . ? C42B C43B H43B 121.3 . . ? C43B C44B C45B 121.4(9) . . ? C43B C44B H44B 119.3 . . ? C45B C44B H44B 119.3 . . ? C44B C45B C46B 119.2(9) . . ? C44B C45B H45B 120.4 . . ? C46B C45B H45B 120.4 . . ? C41B C46B C45B 118.0(9) . . ? C41B C46B H46B 121.0 . . ? C45B C46B H46B 121.0 . . ? C5B C6B H50D 109.5 . . ? C5B C6B H50E 109.5 . . ? H50D C6B H50E 109.5 . . ? C5B C6B H50F 109.5 . . ? H50D C6B H50F 109.5 . . ? H50E C6B H50F 109.5 . . ? O101 Cl1 O104 110.3(7) . . ? O101 Cl1 O103 112.1(6) . . ? O104 Cl1 O103 107.0(5) . . ? O101 Cl1 O102 106.2(6) . . ? O104 Cl1 O102 111.0(6) . . ? O103 Cl1 O102 110.3(4) . . ? O108 Cl2 O107 109.9(4) . . ? O108 Cl2 O105 111.1(4) . . ? O107 Cl2 O105 108.7(4) . . ? O108 Cl2 O106 109.2(4) . . ? O107 Cl2 O106 107.5(4) . . ? O105 Cl2 O106 110.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C38 Mn1 N3 C4 54.2(7) . . . . ? C39 Mn1 N3 C4 140.7(7) . . . . ? N1B C5B C4B N3B -0.6(10) . . . . ? C6B C5B C4B N3B -177.3(9) . . . . ? C2B N3B C4B C5B 1.5(10) . . . . ? Mn2 N3B C4B C5B -176.8(6) . . . . ? N36B Mn2 N25B C30B 13.4(6) . . . . ? N3B Mn2 N25B C30B -75.1(6) . . . . ? C37B Mn2 N25B C26B 5.0(8) . . . . ? N36B Mn2 N25B C26B -174.4(8) . . . . ? N3B Mn2 N25B C26B 97.1(7) . . . . ? C30B N25B C26B C27B 2.2(13) . . . . ? Mn2 N25B C26B C27B -169.9(7) . . . . ? N25B C26B C27B C28B 0.7(14) . . . . ? C26B C27B C28B C29B -1.5(13) . . . . ? C27B C28B C29B C30B -0.5(13) . . . . ? C26B N25B C30B C29B -4.4(13) . . . . ? Mn2 N25B C30B C29B 168.5(7) . . . . ? C26B N25B C30B C31B 173.1(7) . . . . ? Mn2 N25B C30B C31B -13.9(9) . . . . ? C28B C29B C30B N25B 3.7(14) . . . . ? C28B C29B C30B C31B -173.7(8) . . . . ? N25B C30B C31B N36B 5.1(11) . . . . ? C29B C30B C31B N36B -177.4(8) . . . . ? N25B C30B C31B C32B -171.0(8) . . . . ? C29B C30B C31B C32B 6.6(14) . . . . ? N36B C31B C32B C33B -1.1(13) . . . . ? C30B C31B C32B C33B 174.6(8) . . . . ? C31B C32B C33B C34B -2.6(12) . . . . ? C32B C33B C34B C35B 4.2(13) . . . . ? C33B C34B C35B N36B -2.1(13) . . . . ? C34B C35B N36B C31B -1.7(12) . . . . ? C34B C35B N36B Mn2 179.3(6) . . . . ? C32B C31B N36B C35B 3.3(12) . . . . ? C30B C31B N36B C35B -172.8(7) . . . . ? C32B C31B N36B Mn2 -177.6(6) . . . . ? C30B C31B N36B Mn2 6.3(9) . . . . ? N25B Mn2 N36B C35B 168.6(7) . . . . ? N3B Mn2 N36B C35B -107.4(7) . . . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-03-11 at 10:12:10 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : d:\monocristal\wingx\files\archive.reqdat # CIF files read : jv01jj01n struct #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_13 _database_code_depnum_ccdc_archive 'CCDC 725957' _audit_creation_date 2009-03-11T10:12:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '4(C56 H46 Au Mn N2 O3 P3), 4(F6 P), 3(C H2 Cl2), 4(O H2)' _chemical_formula_sum 'C227 H198 Au4 Cl6 F24 Mn4 N8 O16 P16' _chemical_formula_weight 5465.79 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.1731(8) _cell_length_b 34.8321(17) _cell_length_c 17.7003(9) _cell_angle_alpha 90 _cell_angle_beta 106.796(2) _cell_angle_gamma 90 _cell_volume 11316.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1880 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.4 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.6390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5526.0 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.345 _exptl_absorpt_correction_T_max 0.465 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_unetI/netI 0.0607 _diffrn_reflns_number 101972 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 22254 _reflns_number_gt 15792 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR-97 (Giacovazzo et all, 1999' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0536P)^2^+0.9980P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 22254 _refine_ls_number_parameters 1221 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.579 _refine_ls_restrained_S_all 1.579 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 4.207 _refine_diff_density_min -2.895 _refine_diff_density_rms 0.177 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 P1W P 0.10457(16) 0.41258(8) 0.2379(2) 0.0562(4) Uani 1 1 d . . . F1W F 0.1607(3) 0.44111(15) 0.2145(4) 0.0562(4) Uani 1 1 d . . . F2W F 0.0410(3) 0.43976(15) 0.1961(4) 0.0562(4) Uani 1 1 d . . . F3W F 0.0475(3) 0.38455(15) 0.2613(4) 0.0562(4) Uani 1 1 d . . . F4W F 0.1678(3) 0.38281(16) 0.2653(4) 0.0562(4) Uani 1 1 d . . . F5W F 0.0901(3) 0.38987(15) 0.1515(4) 0.0562(4) Uani 1 1 d . . . F6W F 0.1236(3) 0.43143(16) 0.3183(4) 0.0562(4) Uani 1 1 d . . . P2W P 0.37159(16) 0.56339(8) 0.1566(2) 0.0562(4) Uani 1 1 d . . . F7W F 0.4270(3) 0.52929(15) 0.1512(4) 0.0562(4) Uani 1 1 d . A . F8W F 0.3167(3) 0.59698(15) 0.1641(4) 0.0562(4) Uani 1 1 d . A . F1WA F 0.4344(5) 0.5927(3) 0.1652(5) 0.0562(4) Uani 0.705(5) 1 d PD A 1 F2WA F 0.3058(4) 0.5316(2) 0.1399(5) 0.0562(4) Uani 0.705(5) 1 d PD A 1 F3WA F 0.3499(4) 0.5704(2) 0.0590(5) 0.0562(4) Uani 0.705(5) 1 d PD A 1 F4WA F 0.3921(5) 0.5560(2) 0.2472(5) 0.0562(4) Uani 0.705(5) 1 d PD A 1 F1WB F 0.3396(10) 0.5396(5) 0.2165(12) 0.0562(4) Uani 0.295(5) 1 d PD A 2 F2WB F 0.4320(12) 0.5958(7) 0.1387(12) 0.0562(4) Uani 0.295(5) 1 d PD A 2 F3WB F 0.4261(10) 0.5799(5) 0.2559(11) 0.0562(4) Uani 0.295(5) 1 d PD A 2 F4WB F 0.3368(10) 0.5538(6) 0.0802(11) 0.0562(4) Uani 0.295(5) 1 d PD A 2 O1W O 0.5049(6) 0.7504(3) 0.6907(6) 0.0240(13) Uani 0.518(7) 1 d P B 1 O2W O 0.5682(6) 0.7323(3) 0.5701(6) 0.0240(13) Uani 0.482(7) 1 d P B 2 O3W O 0.6352(5) 0.7815(3) 0.5675(5) 0.0240(13) Uani 0.546(8) 1 d P C 3 O4W O 0.5758(7) 0.7073(4) 0.5550(7) 0.0240(13) Uani 0.454(8) 1 d P C 4 C4W C 0.3900(11) 0.6642(6) 0.0264(12) 0.052(3) Uani 0.50 1 d P . . H4W1 H 0.3892 0.6406 0.0572 0.062 Uiso 0.50 1 calc PR . . H4W2 H 0.3647 0.6845 0.0475 0.062 Uiso 0.50 1 calc PR . . Cl5W Cl 0.3441(4) 0.65615(13) -0.0641(3) 0.0599(17) Uani 0.50 1 d P . . Cl6W Cl 0.4758(3) 0.67729(19) 0.0416(4) 0.080(2) Uani 0.50 1 d P . . C7W C 0.9176(6) 0.6168(3) 0.5530(6) 0.052(3) Uani 1 1 d . . . H7W1 H 0.8940 0.6349 0.5813 0.062 Uiso 1 1 calc R . . H7W2 H 0.9172 0.5909 0.5760 0.062 Uiso 1 1 calc R . . Cl8W Cl 1.00744(18) 0.63123(11) 0.56443(19) 0.0838(11) Uani 1 1 d . . . Cl9W Cl 0.8689(2) 0.61608(8) 0.45152(16) 0.0743(10) Uani 1 1 d . . . Mn1 Mn 1.05777(6) 0.61305(3) 0.25634(7) 0.0194(3) Uani 1 1 d . . . Au1 Au 0.872280(16) 0.655026(8) 0.261529(17) 0.01696(9) Uani 1 1 d . D . P1 P 0.84036(12) 0.71650(5) 0.28376(13) 0.0215(5) Uani 1 1 d . . . P2 P 1.06808(11) 0.57945(6) 0.14696(12) 0.0224(5) Uani 1 1 d . . . P3 P 1.13653(11) 0.56623(6) 0.32730(12) 0.0220(5) Uani 1 1 d . . . N1 N 0.8487(3) 0.56997(17) 0.2448(4) 0.0181(14) Uani 1 1 d . D . C2 C 0.8984(4) 0.5990(2) 0.2507(4) 0.0178(17) Uani 1 1 d . . . N3 N 0.9629(3) 0.58295(17) 0.2564(4) 0.0209(15) Uani 1 1 d . D . C4 C 0.9532(4) 0.5435(2) 0.2572(4) 0.0203(18) Uani 1 1 d . . . H4 H 0.9908 0.5251 0.2624 0.024 Uiso 1 1 calc R D . C5 C 0.8844(4) 0.5353(2) 0.2498(4) 0.0214(18) Uani 1 1 d . D . H5 H 0.8637 0.5104 0.2482 0.026 Uiso 1 1 calc R . . C6 C 0.7734(4) 0.5749(2) 0.2373(4) 0.0196(18) Uani 1 1 d . . . C7 C 0.7437(5) 0.5566(2) 0.2911(5) 0.030(2) Uani 1 1 d . D . H7 H 0.7729 0.5410 0.3322 0.036 Uiso 1 1 calc R . . C8 C 0.6698(5) 0.5622(3) 0.2822(5) 0.036(2) Uani 1 1 d . . . H8 H 0.6483 0.5498 0.3178 0.044 Uiso 1 1 calc R D . C9 C 0.6268(5) 0.5850(2) 0.2235(5) 0.034(2) Uani 1 1 d . D . H9 H 0.5767 0.5889 0.2190 0.040 Uiso 1 1 calc R . . C10 C 0.6583(5) 0.6019(2) 0.1719(5) 0.032(2) Uani 1 1 d . . . H10 H 0.6292 0.6174 0.1306 0.038 Uiso 1 1 calc R D . C11 C 0.7313(4) 0.5971(2) 0.1779(5) 0.028(2) Uani 1 1 d . D . H11 H 0.7519 0.6091 0.1412 0.033 Uiso 1 1 calc R . . C12 C 0.9868(4) 0.5528(2) 0.0959(4) 0.0211(18) Uani 1 1 d . . . C13 C 0.9854(5) 0.5131(2) 0.0879(5) 0.029(2) Uani 1 1 d . . . H13 H 1.0294 0.4989 0.1056 0.035 Uiso 1 1 calc R . . C14 C 0.9208(5) 0.4943(2) 0.0546(5) 0.032(2) Uani 1 1 d . . . H14 H 0.9206 0.4671 0.0492 0.038 Uiso 1 1 calc R . . C15 C 0.8562(5) 0.5145(2) 0.0288(5) 0.032(2) Uani 1 1 d . . . H15 H 0.8116 0.5012 0.0069 0.039 Uiso 1 1 calc R . . C16 C 0.8564(5) 0.5530(2) 0.0346(5) 0.034(2) Uani 1 1 d . . . H16 H 0.8122 0.5670 0.0159 0.041 Uiso 1 1 calc R . . C17 C 0.9209(4) 0.5722(2) 0.0677(5) 0.0233(18) Uani 1 1 d . . . H17 H 0.9204 0.5994 0.0714 0.028 Uiso 1 1 calc R . . C18 C 1.0930(4) 0.6066(2) 0.0705(5) 0.0255(19) Uani 1 1 d . . . C19 C 1.1598(5) 0.6276(3) 0.0920(5) 0.036(2) Uani 1 1 d . . . H19 H 1.1888 0.6281 0.1455 0.044 Uiso 1 1 calc R . . C20 C 1.1828(5) 0.6475(3) 0.0348(6) 0.044(3) Uani 1 1 d . . . H20 H 1.2272 0.6616 0.0497 0.053 Uiso 1 1 calc R . . C21 C 1.1417(5) 0.6468(3) -0.0430(6) 0.040(2) Uani 1 1 d . . . H21 H 1.1576 0.6599 -0.0821 0.048 Uiso 1 1 calc R . . C22 C 1.0768(5) 0.6266(2) -0.0633(5) 0.030(2) Uani 1 1 d . . . H22 H 1.0482 0.6263 -0.1170 0.036 Uiso 1 1 calc R . . C23 C 1.0519(4) 0.6068(2) -0.0081(5) 0.0256(19) Uani 1 1 d . . . H23 H 1.0068 0.5935 -0.0242 0.031 Uiso 1 1 calc R . . C24 C 1.2256(4) 0.5867(2) 0.3759(5) 0.0248(19) Uani 1 1 d . . . C25 C 1.2851(5) 0.5839(2) 0.3453(5) 0.031(2) Uani 1 1 d . . . H25 H 1.2813 0.5682 0.3004 0.038 Uiso 1 1 calc R . . C26 C 1.3494(5) 0.6035(3) 0.3797(5) 0.034(2) Uani 1 1 d . . . H26 H 1.3896 0.6014 0.3587 0.041 Uiso 1 1 calc R . . C27 C 1.3538(5) 0.6256(3) 0.4428(6) 0.042(3) Uani 1 1 d . . . H27 H 1.3978 0.6392 0.4658 0.050 Uiso 1 1 calc R . . C28 C 1.2953(5) 0.6297(3) 0.4773(5) 0.040(2) Uani 1 1 d . . . H28 H 1.3002 0.6454 0.5223 0.047 Uiso 1 1 calc R . . C29 C 1.2315(5) 0.6100(2) 0.4429(5) 0.031(2) Uani 1 1 d . . . H29 H 1.1916 0.6121 0.4644 0.037 Uiso 1 1 calc R . . C30 C 1.1194(4) 0.5389(2) 0.4081(5) 0.0259(19) Uani 1 1 d . . . C31 C 1.1625(5) 0.5066(2) 0.4369(5) 0.033(2) Uani 1 1 d . . . H31 H 1.1960 0.4978 0.4102 0.040 Uiso 1 1 calc R . . C32 C 1.1574(5) 0.4874(3) 0.5027(5) 0.040(2) Uani 1 1 d . . . H32 H 1.1869 0.4655 0.5217 0.048 Uiso 1 1 calc R . . C33 C 1.1080(5) 0.5006(3) 0.5411(5) 0.042(3) Uani 1 1 d . . . H33 H 1.1042 0.4877 0.5871 0.050 Uiso 1 1 calc R . . C34 C 1.0652(5) 0.5318(3) 0.5133(5) 0.045(3) Uani 1 1 d . . . H34 H 1.0316 0.5403 0.5402 0.054 Uiso 1 1 calc R . . C35 C 1.0698(5) 0.5513(3) 0.4467(5) 0.035(2) Uani 1 1 d . . . H35 H 1.0394 0.5729 0.4276 0.042 Uiso 1 1 calc R . . C36A C 0.8237(12) 0.7465(7) 0.1960(12) 0.0319(9) Uani 0.498(8) 1 d PD D 1 C37A C 0.8578(10) 0.7411(4) 0.1416(10) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H37A H 0.8938 0.7216 0.1490 0.038 Uiso 0.498(8) 1 calc PR D 1 C38A C 0.8417(10) 0.7635(4) 0.0735(10) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H38A H 0.8657 0.7581 0.0347 0.038 Uiso 0.498(8) 1 calc PR D 1 C39A C 0.7937(9) 0.7922(5) 0.0607(10) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H39A H 0.7735 0.8033 0.0101 0.038 Uiso 0.498(8) 1 calc PR D 1 C40A C 0.7752(10) 0.8050(4) 0.1291(10) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H40A H 0.7560 0.8301 0.1296 0.038 Uiso 0.498(8) 1 calc PR D 1 C41A C 0.7846(10) 0.7815(4) 0.1954(10) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H41A H 0.7660 0.7884 0.2378 0.038 Uiso 0.498(8) 1 calc PR D 1 C42A C 0.9041(16) 0.7421(5) 0.3581(13) 0.0319(9) Uani 0.498(8) 1 d PD D 1 C43A C 0.9126(11) 0.7822(5) 0.3510(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H43A H 0.8840 0.7959 0.3065 0.038 Uiso 0.498(8) 1 calc PR D 1 C44A C 0.9638(10) 0.8004(5) 0.4109(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H44A H 0.9705 0.8273 0.4076 0.038 Uiso 0.498(8) 1 calc PR D 1 C45A C 1.0051(10) 0.7809(5) 0.4747(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H45A H 1.0397 0.7942 0.5155 0.038 Uiso 0.498(8) 1 calc PR D 1 C46A C 0.9967(10) 0.7415(4) 0.4803(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H46A H 1.0251 0.7279 0.5252 0.038 Uiso 0.498(8) 1 calc PR D 1 C47A C 0.9469(11) 0.7223(5) 0.4202(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H47A H 0.9425 0.6952 0.4224 0.038 Uiso 0.498(8) 1 calc PR D 1 C48A C 0.6319(11) 0.7145(5) 0.3627(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H48A H 0.5899 0.7133 0.3809 0.038 Uiso 0.498(8) 1 calc PR D 1 C49A C 0.6497(10) 0.6843(5) 0.3259(11) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H49A H 0.6189 0.6624 0.3154 0.038 Uiso 0.498(8) 1 calc PR D 1 C50A C 0.7129(10) 0.6845(6) 0.3028(12) 0.0319(9) Uani 0.498(8) 1 d PD D 1 H50A H 0.7262 0.6622 0.2792 0.038 Uiso 0.498(8) 1 calc PR D 1 C36B C 0.8266(12) 0.7497(7) 0.2018(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 C37B C 0.8780(9) 0.7534(5) 0.1654(10) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H37B H 0.9220 0.7394 0.1856 0.038 Uiso 0.502(8) 1 calc PR D 2 C38B C 0.8713(9) 0.7767(5) 0.0992(10) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H38B H 0.9077 0.7770 0.0724 0.038 Uiso 0.502(8) 1 calc PR D 2 C39B C 0.8124(8) 0.7982(5) 0.0755(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H39B H 0.8122 0.8193 0.0413 0.038 Uiso 0.502(8) 1 calc PR D 2 C40B C 0.7484(9) 0.7906(5) 0.0998(10) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H40B H 0.7029 0.8020 0.0729 0.038 Uiso 0.502(8) 1 calc PR D 2 C41B C 0.7546(9) 0.7658(4) 0.1648(10) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H41B H 0.7140 0.7599 0.1833 0.038 Uiso 0.502(8) 1 calc PR D 2 C42B C 0.9101(15) 0.7374(5) 0.3691(12) 0.0319(9) Uani 0.502(8) 1 d PD D 2 C43B C 0.9262(11) 0.7770(5) 0.3758(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H43B H 0.9024 0.7938 0.3340 0.038 Uiso 0.502(8) 1 calc PR D 2 C44B C 0.9759(10) 0.7917(5) 0.4422(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H44B H 0.9867 0.8183 0.4456 0.038 Uiso 0.502(8) 1 calc PR D 2 C45B C 1.0091(9) 0.7680(5) 0.5024(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H45B H 1.0437 0.7781 0.5479 0.038 Uiso 0.502(8) 1 calc PR D 2 C46B C 0.9931(10) 0.7291(5) 0.4981(10) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H46B H 1.0154 0.7129 0.5415 0.038 Uiso 0.502(8) 1 calc PR D 2 C47B C 0.9446(11) 0.7136(5) 0.4311(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H47B H 0.9353 0.6868 0.4278 0.038 Uiso 0.502(8) 1 calc PR D 2 C48B C 0.6226(11) 0.7243(5) 0.3371(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H48B H 0.5744 0.7279 0.3404 0.038 Uiso 0.502(8) 1 calc PR D 2 C49B C 0.6367(9) 0.6949(5) 0.2950(11) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H49B H 0.6008 0.6756 0.2755 0.038 Uiso 0.502(8) 1 calc PR D 2 C50B C 0.7039(10) 0.6925(5) 0.2800(12) 0.0319(9) Uani 0.502(8) 1 d PD D 2 H50B H 0.7121 0.6731 0.2457 0.038 Uiso 0.502(8) 1 calc PR D 2 C51 C 0.7577(4) 0.7176(2) 0.3140(5) 0.0231(18) Uani 1 1 d . D . C52 C 0.7417(5) 0.7477(2) 0.3560(5) 0.029(2) Uani 1 1 d . . . H52 H 0.7760 0.7679 0.3724 0.035 Uiso 1 1 calc R D . C53 C 0.6762(5) 0.7493(3) 0.3753(5) 0.042(2) Uani 1 1 d . D . H53 H 0.6612 0.7721 0.3958 0.051 Uiso 1 1 calc R E 1 C54 C 1.0537(4) 0.6378(2) 0.3470(5) 0.0259(19) Uani 1 1 d . . . C55 C 1.0056(4) 0.6488(2) 0.1871(5) 0.0219(18) Uani 1 1 d . . . C56 C 1.1365(5) 0.6425(2) 0.2622(5) 0.029(2) Uani 1 1 d . . . O57 O 1.0556(3) 0.65509(17) 0.4021(4) 0.0390(16) Uani 1 1 d . . . O58 O 0.9800(3) 0.67186(16) 0.1419(3) 0.0276(13) Uani 1 1 d . . . O59 O 1.1842(3) 0.66341(17) 0.2673(4) 0.0348(15) Uani 1 1 d . . . C60 C 1.1446(5) 0.5458(2) 0.1790(5) 0.032(2) Uani 1 1 d . . . H60A H 1.1384 0.5250 0.1395 0.038 Uiso 1 1 calc R . . H60B H 1.1905 0.5595 0.1815 0.038 Uiso 1 1 calc R . . C61 C 1.1502(5) 0.5283(2) 0.2595(5) 0.030(2) Uani 1 1 d . . . H61A H 1.1987 0.5164 0.2814 0.036 Uiso 1 1 calc R . . H61B H 1.1128 0.5080 0.2540 0.036 Uiso 1 1 calc R . . Au1' Au 0.659516(16) 0.348195(8) 0.273198(18) 0.02005(9) Uani 1 1 d . F . Mn1' Mn 0.45780(6) 0.37712(3) 0.24843(7) 0.0194(3) Uani 1 1 d . . . P1' P 0.71848(12) 0.29104(6) 0.30720(13) 0.0224(5) Uani 1 1 d . . . N1' N 0.6490(3) 0.43163(18) 0.2316(4) 0.0238(16) Uani 1 1 d . F . C2' C 0.6110(4) 0.4005(2) 0.2446(5) 0.0215(18) Uani 1 1 d . . . N3' N 0.5428(3) 0.41120(17) 0.2371(4) 0.0210(15) Uani 1 1 d . F . C4' C 0.5393(4) 0.4504(2) 0.2190(5) 0.030(2) Uani 1 1 d . . . H4' H 0.4970 0.4659 0.2108 0.036 Uiso 1 1 calc R F . C5' C 0.6041(4) 0.4631(2) 0.2151(5) 0.028(2) Uani 1 1 d . F . H5' H 0.6163 0.4884 0.2033 0.034 Uiso 1 1 calc R . . C6' C 0.7222(5) 0.4307(2) 0.2274(6) 0.028(2) Uani 1 1 d . . . C7' C 0.7803(5) 0.4295(2) 0.2940(6) 0.041(2) Uani 1 1 d . F . H7' H 0.7730 0.4293 0.3449 0.050 Uiso 1 1 calc R . . C8' C 0.8524(5) 0.4284(3) 0.2856(7) 0.052(3) Uani 1 1 d . . . H8' H 0.8940 0.4267 0.3303 0.062 Uiso 1 1 calc R F . C9' C 0.8588(6) 0.4300(3) 0.2119(8) 0.052(3) Uani 1 1 d . F . H9' H 0.9068 0.4305 0.2069 0.062 Uiso 1 1 calc R . . C10' C 0.8030(6) 0.4312(3) 0.1443(8) 0.056(3) Uani 1 1 d . . . H10' H 0.8112 0.4313 0.0939 0.067 Uiso 1 1 calc R F . C11' C 0.7327(5) 0.4320(2) 0.1529(7) 0.046(3) Uani 1 1 d . F . H11' H 0.6917 0.4336 0.1074 0.056 Uiso 1 1 calc R . . P2'A P 0.4159(4) 0.4203(2) 0.3303(4) 0.0221(4) Uani 0.413(5) 1 d P F 1 P3'A P 0.3748(9) 0.4092(3) 0.1466(9) 0.0221(4) Uani 0.413(5) 1 d P F 1 C12' C 0.4810(9) 0.4589(5) 0.3786(12) 0.0221(4) Uani 0.413(5) 1 d PD F 1 C13' C 0.5495(9) 0.4467(5) 0.4201(10) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H13' H 0.5618 0.4202 0.4235 0.027 Uiso 0.413(5) 1 calc PR F 1 C14' C 0.6005(10) 0.4745(4) 0.4574(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H14' H 0.6479 0.4669 0.4877 0.027 Uiso 0.413(5) 1 calc PR F 1 C15' C 0.5822(11) 0.5133(5) 0.4503(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H15' H 0.6168 0.5321 0.4760 0.027 Uiso 0.413(5) 1 calc PR F 1 C16' C 0.5132(10) 0.5244(5) 0.4054(12) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H16' H 0.5022 0.5509 0.3970 0.027 Uiso 0.413(5) 1 calc PR F 1 C17' C 0.4596(10) 0.4973(5) 0.3725(12) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H17' H 0.4108 0.5047 0.3470 0.027 Uiso 0.413(5) 1 calc PR F 1 C18' C 0.3832(9) 0.4019(6) 0.4105(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 C19' C 0.4285(9) 0.3803(5) 0.4706(10) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H19' H 0.4767 0.3746 0.4695 0.027 Uiso 0.413(5) 1 calc PR F 1 C20' C 0.4048(9) 0.3672(6) 0.5310(10) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H20' H 0.4379 0.3533 0.5723 0.027 Uiso 0.413(5) 1 calc PR F 1 C21' C 0.3360(9) 0.3730(6) 0.5352(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H21' H 0.3198 0.3630 0.5771 0.027 Uiso 0.413(5) 1 calc PR F 1 C22' C 0.2922(9) 0.3939(6) 0.4763(12) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H22' H 0.2442 0.3990 0.4786 0.027 Uiso 0.413(5) 1 calc PR F 1 C23' C 0.3118(9) 0.4084(6) 0.4130(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H23' H 0.2780 0.4222 0.3724 0.027 Uiso 0.413(5) 1 calc PR F 1 C24' C 0.2961(9) 0.3826(6) 0.0927(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 C25' C 0.2328(9) 0.3806(5) 0.1129(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H25' H 0.2280 0.3951 0.1566 0.027 Uiso 0.413(5) 1 calc PR F 1 C26' C 0.1748(9) 0.3577(5) 0.0710(10) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H26' H 0.1297 0.3578 0.0833 0.027 Uiso 0.413(5) 1 calc PR F 1 C27' C 0.1852(11) 0.3342(6) 0.0089(11) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H27' H 0.1499 0.3153 -0.0147 0.027 Uiso 0.413(5) 1 calc PR F 1 C28' C 0.2433(9) 0.3387(5) -0.0156(10) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H28' H 0.2458 0.3263 -0.0626 0.027 Uiso 0.413(5) 1 calc PR F 1 C29' C 0.3014(9) 0.3616(5) 0.0271(10) 0.0221(4) Uani 0.413(5) 1 d PD F 1 H29' H 0.3447 0.3628 0.0114 0.027 Uiso 0.413(5) 1 calc PR F 1 P2'B P 0.4315(2) 0.42741(14) 0.3185(3) 0.0221(4) Uani 0.587(5) 1 d P F 2 P3'B P 0.3728(6) 0.4046(2) 0.1407(6) 0.0221(4) Uani 0.587(5) 1 d P F 2 C12B C 0.5039(7) 0.4589(4) 0.3750(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 C13B C 0.5736(7) 0.4446(4) 0.4063(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H13B H 0.5838 0.4184 0.3985 0.027 Uiso 0.587(5) 1 calc PR F 2 C14B C 0.6285(7) 0.4686(3) 0.4491(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H14B H 0.6759 0.4586 0.4724 0.027 Uiso 0.587(5) 1 calc PR F 2 C15B C 0.6147(8) 0.5068(3) 0.4580(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H15B H 0.6529 0.5233 0.4860 0.027 Uiso 0.587(5) 1 calc PR F 2 C16B C 0.5451(8) 0.5211(4) 0.4261(9) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H16B H 0.5357 0.5475 0.4331 0.027 Uiso 0.587(5) 1 calc PR F 2 C17B C 0.4882(7) 0.4975(3) 0.3838(9) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H17B H 0.4405 0.5073 0.3618 0.027 Uiso 0.587(5) 1 calc PR F 2 C18B C 0.3881(7) 0.4118(4) 0.3934(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 C19B C 0.4305(7) 0.3969(4) 0.4658(7) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H19B H 0.4819 0.3953 0.4761 0.027 Uiso 0.587(5) 1 calc PR F 2 C20B C 0.3989(6) 0.3848(4) 0.5218(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H20B H 0.4284 0.3742 0.5698 0.027 Uiso 0.587(5) 1 calc PR F 2 C21B C 0.3250(7) 0.3878(4) 0.5092(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H21B H 0.3029 0.3787 0.5473 0.027 Uiso 0.587(5) 1 calc PR F 2 C22B C 0.2841(7) 0.4042(4) 0.4409(9) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H22B H 0.2333 0.4071 0.4331 0.027 Uiso 0.587(5) 1 calc PR F 2 C23B C 0.3130(7) 0.4168(4) 0.3823(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H23B H 0.2830 0.4285 0.3358 0.027 Uiso 0.587(5) 1 calc PR F 2 C24B C 0.3065(7) 0.3712(4) 0.0771(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 C25B C 0.2379(6) 0.3655(4) 0.0832(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H25B H 0.2247 0.3781 0.1246 0.027 Uiso 0.587(5) 1 calc PR F 2 C26B C 0.1858(8) 0.3421(4) 0.0318(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H26B H 0.1368 0.3404 0.0336 0.027 Uiso 0.587(5) 1 calc PR F 2 C27B C 0.2121(7) 0.3211(4) -0.0236(8) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H27B H 0.1801 0.3033 -0.0569 0.027 Uiso 0.587(5) 1 calc PR F 2 C28B C 0.2792(7) 0.3250(4) -0.0316(7) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H28B H 0.2930 0.3109 -0.0709 0.027 Uiso 0.587(5) 1 calc PR F 2 C29B C 0.3289(3) 0.35016(15) 0.0186(3) 0.0221(4) Uani 0.587(5) 1 d PD F 2 H29B H 0.3767 0.3531 0.0138 0.027 Uiso 0.587(5) 1 calc PR F 2 C30' C 0.4040(3) 0.43087(15) 0.0668(3) 0.0217(18) Uani 1 1 d R . . C31' C 0.3655(3) 0.46194(15) 0.0254(3) 0.0273(19) Uani 1 1 d R F . H31' H 0.3233 0.4713 0.0372 0.033 Uiso 1 1 d R . . C32' C 0.3890(5) 0.4791(2) -0.0330(5) 0.032(2) Uani 1 1 d . . . H32' H 0.3626 0.5002 -0.0614 0.038 Uiso 1 1 calc R F . C33' C 0.4508(5) 0.4659(2) -0.0510(5) 0.035(2) Uani 1 1 d . F . H33' H 0.4667 0.4782 -0.0910 0.042 Uiso 1 1 calc R . . C34' C 0.4894(4) 0.4344(2) -0.0100(5) 0.027(2) Uani 1 1 d . . . H34' H 0.5313 0.4250 -0.0224 0.033 Uiso 1 1 calc R F . C35' C 0.4657(4) 0.4172(2) 0.0490(5) 0.0239(19) Uani 1 1 d . F . H35' H 0.4917 0.3959 0.0773 0.029 Uiso 1 1 calc R . . C36' C 0.7383(5) 0.2796(2) 0.4106(5) 0.029(2) Uani 1 1 d . . . C37' C 0.6797(6) 0.2714(3) 0.4408(6) 0.050(3) Uani 1 1 d . . . H37' H 0.6313 0.2717 0.4066 0.061 Uiso 1 1 calc R . . C38' C 0.6916(7) 0.2630(3) 0.5187(7) 0.063(3) Uani 1 1 d . . . H38' H 0.6518 0.2567 0.5382 0.075 Uiso 1 1 calc R . . C39' C 0.7614(7) 0.2635(3) 0.5693(6) 0.063(3) Uani 1 1 d . . . H39' H 0.7689 0.2581 0.6237 0.076 Uiso 1 1 calc R . . C40' C 0.8195(6) 0.2715(3) 0.5428(6) 0.055(3) Uani 1 1 d . . . H40' H 0.8676 0.2715 0.5777 0.066 Uiso 1 1 calc R . . C41' C 0.8062(5) 0.2798(3) 0.4617(5) 0.040(2) Uani 1 1 d . . . H41' H 0.8463 0.2858 0.4425 0.048 Uiso 1 1 calc R . . C42' C 0.8053(4) 0.2899(2) 0.2864(4) 0.0199(17) Uani 1 1 d . . . C43' C 0.8352(4) 0.3238(2) 0.2681(5) 0.029(2) Uani 1 1 d . . . H43' H 0.8095 0.3473 0.2662 0.034 Uiso 1 1 calc R . . C44' C 0.9016(5) 0.3236(3) 0.2527(5) 0.040(2) Uani 1 1 d . . . H44' H 0.9219 0.3470 0.2415 0.048 Uiso 1 1 calc R . . C45' C 0.9385(5) 0.2900(3) 0.2535(6) 0.040(2) Uani 1 1 d . . . H45' H 0.9844 0.2903 0.2429 0.048 Uiso 1 1 calc R . . C46' C 0.9100(5) 0.2557(3) 0.2693(6) 0.045(3) Uani 1 1 d . . . H46' H 0.9354 0.2324 0.2684 0.054 Uiso 1 1 calc R . . C47' C 0.8430(5) 0.2554(2) 0.2870(5) 0.032(2) Uani 1 1 d . . . H47' H 0.8235 0.2319 0.2992 0.039 Uiso 1 1 calc R . . C48' C 0.6652(5) 0.2501(2) 0.2574(5) 0.030(2) Uani 1 1 d . . . C49' C 0.6136(5) 0.2566(3) 0.1859(5) 0.034(2) Uani 1 1 d . . . H49' H 0.6070 0.2817 0.1638 0.040 Uiso 1 1 calc R . . C50' C 0.5702(5) 0.2256(3) 0.1454(6) 0.044(3) Uani 1 1 d . . . H50' H 0.5344 0.2299 0.0964 0.053 Uiso 1 1 calc R . . C51' C 0.5801(6) 0.1898(3) 0.1770(7) 0.052(3) Uani 1 1 d . . . H51' H 0.5502 0.1693 0.1504 0.062 Uiso 1 1 calc R . . C52' C 0.6316(6) 0.1831(3) 0.2456(8) 0.057(3) Uani 1 1 d . . . H52' H 0.6383 0.1576 0.2658 0.068 Uiso 1 1 calc R . . C53' C 0.6760(5) 0.2128(2) 0.2884(6) 0.045(3) Uani 1 1 d . . . H53' H 0.7122 0.2076 0.3367 0.054 Uiso 1 1 calc R . . C54' C 0.4754(4) 0.3411(2) 0.1821(5) 0.0246(19) Uani 1 1 d . F . C55' C 0.5169(4) 0.3527(2) 0.3349(5) 0.0226(18) Uani 1 1 d . F . C56' C 0.3838(5) 0.3486(2) 0.2602(5) 0.026(2) Uani 1 1 d . F . O57' O 0.4797(3) 0.31622(16) 0.1403(3) 0.0340(15) Uani 1 1 d . . . O58' O 0.5494(3) 0.33592(17) 0.3890(4) 0.0351(15) Uani 1 1 d . . . O59' O 0.3374(3) 0.32956(17) 0.2677(4) 0.0357(15) Uani 1 1 d . . . C60' C 0.3160(10) 0.4357(5) 0.1810(11) 0.031(3) Uani 0.587(5) 1 d P F 2 H60C H 0.2877 0.4534 0.1396 0.037 Uiso 0.587(5) 1 calc PR F 2 H60D H 0.2812 0.4201 0.1998 0.037 Uiso 0.587(5) 1 calc PR F 2 C61' C 0.3648(8) 0.4589(4) 0.2499(9) 0.031(3) Uani 0.587(5) 1 d P F 2 H61E H 0.3342 0.4719 0.2786 0.037 Uiso 0.587(5) 1 calc PR F 2 H61F H 0.3910 0.4789 0.2290 0.037 Uiso 0.587(5) 1 calc PR F 2 C60B C 0.3322(15) 0.4517(7) 0.1879(17) 0.031(3) Uani 0.413(5) 1 d P F 1 H60E H 0.3617 0.4751 0.1888 0.037 Uiso 0.413(5) 1 calc PR F 1 H60F H 0.2824 0.4566 0.1531 0.037 Uiso 0.413(5) 1 calc PR F 1 C61B C 0.3289(12) 0.4431(6) 0.2690(12) 0.031(3) Uani 0.413(5) 1 d P F 1 H61C H 0.2876 0.4256 0.2662 0.037 Uiso 0.413(5) 1 calc PR F 1 H61D H 0.3203 0.4672 0.2946 0.037 Uiso 0.413(5) 1 calc PR F 1 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 P1W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F1W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F2W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F3W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F4W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F5W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F6W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) P2W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F7W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F8W 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F1WA 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F2WA 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F3WA 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F4WA 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F1WB 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F2WB 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F3WB 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) F4WB 0.0463(8) 0.0445(8) 0.0802(11) 0.0174(7) 0.0222(8) 0.0056(6) O1W 0.036(3) 0.024(3) 0.010(3) 0.008(3) 0.004(2) -0.006(3) O2W 0.036(3) 0.024(3) 0.010(3) 0.008(3) 0.004(2) -0.006(3) O3W 0.036(3) 0.024(3) 0.010(3) 0.008(3) 0.004(2) -0.006(3) O4W 0.036(3) 0.024(3) 0.010(3) 0.008(3) 0.004(2) -0.006(3) C4W 0.072(7) 0.044(6) 0.047(6) 0.024(5) 0.029(5) 0.012(5) Cl5W 0.129(5) 0.034(3) 0.029(3) -0.006(2) 0.043(3) -0.039(3) Cl6W 0.067(4) 0.068(4) 0.119(6) -0.007(4) 0.047(4) -0.018(3) C7W 0.072(7) 0.044(6) 0.047(6) 0.024(5) 0.029(5) 0.012(5) Cl8W 0.078(2) 0.114(3) 0.055(2) 0.028(2) 0.0126(17) 0.027(2) Cl9W 0.127(3) 0.0527(18) 0.0375(17) 0.0161(14) 0.0149(17) -0.0170(18) Mn1 0.0195(6) 0.0179(6) 0.0217(7) 0.0042(5) 0.0074(5) 0.0021(5) Au1 0.02204(17) 0.01060(15) 0.02027(18) -0.00166(12) 0.00935(13) 0.00017(12) P1 0.0296(12) 0.0110(10) 0.0289(13) -0.0042(9) 0.0162(10) -0.0009(9) P2 0.0232(12) 0.0275(12) 0.0170(12) 0.0043(9) 0.0066(9) 0.0098(9) P3 0.0245(12) 0.0247(11) 0.0171(12) 0.0051(9) 0.0064(9) 0.0068(9) N1 0.025(4) 0.012(3) 0.018(4) -0.002(3) 0.008(3) -0.007(3) C2 0.023(4) 0.018(4) 0.014(4) 0.003(3) 0.008(3) 0.004(3) N3 0.029(4) 0.016(3) 0.021(4) 0.004(3) 0.012(3) 0.007(3) C4 0.030(5) 0.010(4) 0.023(5) 0.001(3) 0.010(4) 0.005(3) C5 0.030(5) 0.010(4) 0.029(5) 0.006(3) 0.016(4) 0.006(3) C6 0.029(5) 0.010(4) 0.019(5) -0.006(3) 0.006(4) -0.005(3) C7 0.031(5) 0.029(5) 0.031(5) 0.002(4) 0.012(4) 0.000(4) C8 0.035(6) 0.047(6) 0.035(6) -0.014(5) 0.022(5) -0.010(5) C9 0.021(5) 0.033(5) 0.044(6) -0.012(4) 0.005(4) -0.001(4) C10 0.028(5) 0.025(5) 0.038(6) -0.002(4) 0.003(4) 0.004(4) C11 0.029(5) 0.022(4) 0.031(5) -0.004(4) 0.006(4) -0.009(4) C12 0.028(5) 0.024(4) 0.015(4) 0.002(3) 0.011(4) 0.007(4) C13 0.030(5) 0.031(5) 0.029(5) 0.003(4) 0.012(4) 0.007(4) C14 0.049(6) 0.016(4) 0.039(6) -0.005(4) 0.026(5) 0.000(4) C15 0.035(5) 0.028(5) 0.035(6) 0.000(4) 0.010(4) -0.005(4) C16 0.041(6) 0.020(5) 0.036(6) 0.003(4) 0.003(5) 0.003(4) C17 0.030(5) 0.015(4) 0.022(5) 0.001(3) 0.002(4) 0.002(4) C18 0.024(5) 0.029(5) 0.027(5) 0.000(4) 0.012(4) 0.003(4) C19 0.040(6) 0.043(6) 0.028(5) -0.002(4) 0.013(4) -0.001(5) C20 0.043(6) 0.057(7) 0.035(6) 0.000(5) 0.017(5) -0.017(5) C21 0.045(6) 0.040(6) 0.036(6) 0.007(5) 0.013(5) 0.006(5) C22 0.040(5) 0.027(5) 0.023(5) 0.003(4) 0.008(4) 0.007(4) C23 0.029(5) 0.017(4) 0.026(5) 0.002(4) 0.001(4) 0.006(4) C24 0.027(5) 0.030(5) 0.016(5) 0.012(4) 0.003(4) 0.003(4) C25 0.030(5) 0.042(5) 0.023(5) 0.016(4) 0.011(4) 0.012(4) C26 0.031(5) 0.046(6) 0.026(5) 0.005(4) 0.008(4) -0.007(4) C27 0.024(5) 0.050(6) 0.044(7) 0.027(5) -0.003(5) -0.002(5) C28 0.044(6) 0.043(6) 0.024(5) 0.007(4) -0.002(5) -0.003(5) C29 0.028(5) 0.038(5) 0.024(5) 0.007(4) 0.003(4) 0.001(4) C30 0.026(5) 0.032(5) 0.016(5) 0.002(4) 0.002(4) -0.001(4) C31 0.034(5) 0.036(5) 0.029(5) 0.008(4) 0.009(4) 0.000(4) C32 0.046(6) 0.037(6) 0.034(6) 0.013(4) 0.006(5) -0.002(5) C33 0.057(7) 0.043(6) 0.030(6) 0.018(5) 0.018(5) 0.004(5) C34 0.043(6) 0.067(7) 0.035(6) 0.008(5) 0.027(5) 0.013(5) C35 0.039(6) 0.038(5) 0.035(6) 0.007(4) 0.019(5) 0.003(4) C36A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C37A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C38A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C39A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C40A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C41A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C42A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C43A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C44A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C45A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C46A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C47A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C48A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C49A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C50A 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C36B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C37B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C38B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C39B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C40B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C41B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C42B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C43B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C44B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C45B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C46B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C47B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C48B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C49B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C50B 0.038(2) 0.021(2) 0.042(3) -0.0038(15) 0.020(2) -0.0039(15) C51 0.026(5) 0.020(4) 0.027(5) 0.000(4) 0.014(4) 0.002(3) C52 0.032(5) 0.023(5) 0.035(5) -0.011(4) 0.013(4) -0.002(4) C53 0.041(6) 0.047(6) 0.042(6) -0.008(5) 0.019(5) 0.010(5) C54 0.024(5) 0.025(5) 0.030(5) 0.003(4) 0.010(4) 0.006(4) C55 0.019(4) 0.026(5) 0.024(5) -0.002(4) 0.010(4) -0.004(4) C56 0.030(5) 0.024(5) 0.035(6) 0.010(4) 0.010(4) 0.012(4) O57 0.035(4) 0.042(4) 0.039(4) -0.016(3) 0.009(3) 0.007(3) O58 0.027(3) 0.026(3) 0.034(4) 0.011(3) 0.014(3) 0.007(3) O59 0.029(4) 0.031(3) 0.044(4) 0.009(3) 0.009(3) -0.006(3) C60 0.037(5) 0.036(5) 0.025(5) 0.009(4) 0.014(4) 0.019(4) C61 0.036(5) 0.029(5) 0.027(5) 0.008(4) 0.013(4) 0.013(4) Au1' 0.02061(17) 0.01320(16) 0.02596(19) 0.00157(13) 0.00615(14) 0.00120(13) Mn1' 0.0196(6) 0.0145(6) 0.0214(7) 0.0001(5) 0.0018(5) -0.0002(5) P1' 0.0279(12) 0.0133(10) 0.0279(13) 0.0016(9) 0.0110(10) 0.0020(9) N1' 0.021(4) 0.017(4) 0.030(4) 0.003(3) 0.001(3) -0.002(3) C2' 0.018(4) 0.019(4) 0.025(5) -0.006(3) 0.002(4) 0.001(3) N3' 0.018(4) 0.011(3) 0.029(4) 0.002(3) -0.001(3) -0.003(3) C4' 0.021(5) 0.016(4) 0.044(6) 0.003(4) -0.005(4) 0.001(4) C5' 0.020(4) 0.018(4) 0.042(6) 0.009(4) 0.003(4) 0.003(4) C6' 0.032(5) 0.008(4) 0.048(6) 0.004(4) 0.017(5) 0.000(4) C7' 0.036(6) 0.029(5) 0.056(7) -0.004(5) 0.007(5) -0.006(4) C8' 0.037(6) 0.031(6) 0.073(9) 0.003(6) -0.008(6) -0.003(5) C9' 0.041(7) 0.023(5) 0.091(10) 0.008(6) 0.019(7) -0.006(5) C10' 0.058(8) 0.027(6) 0.095(10) 0.009(6) 0.043(8) 0.009(5) C11' 0.032(6) 0.026(5) 0.084(9) 0.006(5) 0.022(6) 0.001(4) P2'A 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) P3'A 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C12' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C13' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C14' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C15' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C16' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C17' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C18' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C19' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C20' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C21' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C22' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C23' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C24' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C25' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C26' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C27' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C28' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C29' 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) P2'B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) P3'B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C12B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C13B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C14B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C15B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C16B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C17B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C18B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C19B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C20B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C21B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C22B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C23B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C24B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C25B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C26B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C27B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C28B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C29B 0.0228(9) 0.0228(12) 0.0211(10) 0.0016(7) 0.0071(7) 0.0011(9) C30' 0.024(4) 0.021(4) 0.020(5) -0.001(3) 0.005(4) -0.008(3) C31' 0.034(5) 0.025(5) 0.022(5) 0.001(4) 0.007(4) -0.003(4) C32' 0.048(6) 0.022(5) 0.024(5) 0.009(4) 0.009(4) -0.004(4) C33' 0.056(6) 0.032(5) 0.017(5) 0.000(4) 0.008(4) -0.022(5) C34' 0.028(5) 0.033(5) 0.025(5) -0.002(4) 0.015(4) -0.006(4) C35' 0.034(5) 0.020(4) 0.019(5) -0.004(3) 0.010(4) 0.001(4) C36' 0.036(5) 0.024(5) 0.030(5) -0.001(4) 0.014(4) 0.001(4) C37' 0.049(7) 0.061(7) 0.051(7) 0.026(6) 0.030(6) 0.013(5) C38' 0.073(9) 0.078(9) 0.056(8) 0.026(7) 0.048(7) 0.011(7) C39' 0.082(9) 0.089(9) 0.025(6) 0.016(6) 0.025(6) 0.012(7) C40' 0.060(7) 0.062(7) 0.041(7) 0.013(6) 0.013(6) -0.007(6) C41' 0.047(6) 0.047(6) 0.029(6) 0.002(5) 0.014(5) -0.001(5) C42' 0.022(4) 0.020(4) 0.018(4) 0.000(3) 0.006(4) 0.001(3) C43' 0.024(5) 0.026(5) 0.039(6) 0.011(4) 0.014(4) 0.004(4) C44' 0.041(6) 0.039(6) 0.042(6) 0.016(5) 0.017(5) 0.000(5) C45' 0.034(6) 0.044(6) 0.049(7) 0.007(5) 0.025(5) 0.011(5) C46' 0.039(6) 0.052(7) 0.052(7) 0.006(5) 0.026(5) 0.022(5) C47' 0.030(5) 0.027(5) 0.041(6) 0.000(4) 0.013(4) 0.008(4) C48' 0.029(5) 0.020(5) 0.043(6) -0.010(4) 0.014(4) -0.001(4) C49' 0.029(5) 0.038(5) 0.040(6) -0.011(4) 0.018(5) -0.010(4) C50' 0.035(6) 0.058(7) 0.043(6) -0.022(5) 0.018(5) -0.011(5) C51' 0.034(6) 0.046(7) 0.079(9) -0.029(6) 0.023(6) -0.015(5) C52' 0.064(8) 0.021(5) 0.099(10) -0.009(6) 0.045(8) -0.010(5) C53' 0.048(6) 0.024(5) 0.063(7) -0.001(5) 0.018(6) -0.005(4) C54' 0.019(4) 0.030(5) 0.025(5) 0.010(4) 0.005(4) 0.001(4) C55' 0.023(4) 0.017(4) 0.027(5) -0.004(4) 0.006(4) 0.000(3) C56' 0.030(5) 0.027(5) 0.021(5) 0.001(4) 0.007(4) 0.010(4) O57' 0.040(4) 0.029(3) 0.033(4) -0.012(3) 0.011(3) -0.004(3) O58' 0.034(4) 0.037(4) 0.030(4) 0.009(3) 0.003(3) 0.013(3) O59' 0.031(4) 0.039(4) 0.039(4) 0.010(3) 0.014(3) -0.009(3) C60' 0.031(7) 0.035(7) 0.026(5) 0.000(5) 0.010(4) 0.017(5) C61' 0.031(7) 0.035(7) 0.026(5) 0.000(5) 0.010(4) 0.017(5) C60B 0.031(7) 0.035(7) 0.026(5) 0.000(5) 0.010(4) 0.017(5) C61B 0.031(7) 0.035(7) 0.026(5) 0.000(5) 0.010(4) 0.017(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P1W F6W 1.514(7) . ? P1W F2W 1.552(6) . ? P1W F4W 1.562(6) . ? P1W F1W 1.604(6) . ? P1W F3W 1.608(6) . ? P1W F5W 1.671(7) . ? P2W F4WB 1.366(18) . ? P2W F1WA 1.553(10) . ? P2W F4WA 1.557(9) . ? P2W F1WB 1.601(17) . ? P2W F8W 1.605(6) . ? P2W F7W 1.614(6) . ? P2W F2WA 1.641(8) . ? P2W F3WA 1.674(9) . ? P2W F2WB 1.712(19) . ? P2W F3WB 1.857(19) . ? C4W Cl5W 1.61(2) . ? C4W Cl6W 1.65(2) . ? C4W H4W1 0.9900 . ? C4W H4W2 0.9900 . ? C7W Cl8W 1.749(11) . ? C7W Cl9W 1.770(11) . ? C7W H7W1 0.9900 . ? C7W H7W2 0.9900 . ? Mn1 C56 1.802(9) . ? Mn1 C55 1.829(8) . ? Mn1 C54 1.843(9) . ? Mn1 N3 2.101(6) . ? Mn1 P2 2.319(2) . ? Mn1 P3 2.329(2) . ? Au1 C2 2.038(7) . ? Au1 P1 2.2922(19) . ? P1 C42A 1.758(18) . ? P1 C51 1.814(8) . ? P1 C36B 1.815(17) . ? P1 C36A 1.823(16) . ? P1 C42B 1.852(18) . ? P2 C12 1.816(8) . ? P2 C18 1.824(8) . ? P2 C60 1.834(8) . ? P3 C24 1.821(8) . ? P3 C30 1.824(8) . ? P3 C61 1.854(8) . ? N1 C2 1.372(9) . ? N1 C5 1.380(9) . ? N1 C6 1.421(9) . ? C2 N3 1.334(9) . ? N3 C4 1.387(9) . ? C4 C5 1.318(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.365(11) . ? C6 C7 1.394(10) . ? C7 C8 1.394(11) . ? C7 H7 0.9500 . ? C8 C9 1.378(12) . ? C8 H8 0.9500 . ? C9 C10 1.365(12) . ? C9 H9 0.9500 . ? C10 C11 1.382(11) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.388(11) . ? C12 C17 1.391(10) . ? C13 C14 1.375(11) . ? C13 H13 0.9500 . ? C14 C15 1.384(11) . ? C14 H14 0.9500 . ? C15 C16 1.345(11) . ? C15 H15 0.9500 . ? C16 C17 1.378(11) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.388(11) . ? C18 C19 1.428(11) . ? C19 C20 1.400(12) . ? C19 H19 0.9500 . ? C20 C21 1.374(13) . ? C20 H20 0.9500 . ? C21 C22 1.384(12) . ? C21 H21 0.9500 . ? C22 C23 1.387(11) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.400(11) . ? C24 C29 1.414(11) . ? C25 C26 1.388(12) . ? C25 H25 0.9500 . ? C26 C27 1.339(12) . ? C26 H26 0.9500 . ? C27 C28 1.429(12) . ? C27 H27 0.9500 . ? C28 C29 1.380(12) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C35 1.391(11) . ? C30 C31 1.403(11) . ? C31 C32 1.371(11) . ? C31 H31 0.9500 . ? C32 C33 1.394(12) . ? C32 H32 0.9500 . ? C33 C34 1.367(12) . ? C33 H33 0.9500 . ? C34 C35 1.386(12) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36A C37A 1.324(16) . ? C36A C41A 1.429(18) . ? C37A C38A 1.394(16) . ? C37A H37A 0.9500 . ? C38A C39A 1.334(16) . ? C38A H38A 0.9500 . ? C39A C40A 1.428(16) . ? C39A H39A 0.9500 . ? C40A C41A 1.400(17) . ? C40A H40A 0.9500 . ? C41A H41A 0.9500 . ? C42A C47A 1.355(16) . ? C42A C43A 1.414(15) . ? C43A C44A 1.376(18) . ? C43A H43A 0.9500 . ? C44A C45A 1.359(19) . ? C44A H44A 0.9500 . ? C45A C46A 1.389(18) . ? C45A H45A 0.9500 . ? C46A C47A 1.379(16) . ? C46A H46A 0.9500 . ? C47A H47A 0.9500 . ? C48A C49A 1.333(15) . ? C48A C53 1.46(2) . ? C48A H48A 0.9500 . ? C49A C50A 1.385(15) . ? C49A H49A 0.9500 . ? C50A C51 1.42(2) . ? C50A H50A 0.9500 . ? C36B C37B 1.330(16) . ? C36B C41B 1.458(18) . ? C37B C38B 1.402(16) . ? C37B H37B 0.9500 . ? C38B C39B 1.319(16) . ? C38B H38B 0.9500 . ? C39B C40B 1.438(16) . ? C39B H39B 0.9500 . ? C40B C41B 1.416(17) . ? C40B H40B 0.9500 . ? C41B H41B 0.9500 . ? C42B C47B 1.382(16) . ? C42B C43B 1.411(15) . ? C43B C44B 1.380(18) . ? C43B H43B 0.9500 . ? C44B C45B 1.352(19) . ? C44B H44B 0.9500 . ? C45B C46B 1.389(18) . ? C45B H45B 0.9500 . ? C46B C47B 1.387(16) . ? C46B H46B 0.9500 . ? C47B H47B 0.9500 . ? C48B C49B 1.339(15) . ? C48B C53 1.37(2) . ? C48B H48B 0.9500 . ? C49B C50B 1.392(16) . ? C49B H49B 0.9500 . ? C50B C51 1.35(2) . ? C50B H50B 0.9500 . ? C51 C52 1.370(10) . ? C52 C53 1.393(11) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 O57 1.138(9) . ? C55 O58 1.140(9) . ? C56 O59 1.153(10) . ? C60 C61 1.526(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? Au1' C2' 2.041(8) . ? Au1' P1' 2.283(2) . ? Mn1' C56' 1.794(9) . ? Mn1' C54' 1.815(9) . ? Mn1' C55' 1.829(9) . ? Mn1' N3' 2.072(6) . ? Mn1' P2'B 2.286(5) . ? Mn1' P3'A 2.318(16) . ? Mn1' P3'B 2.326(11) . ? Mn1' P2'A 2.382(7) . ? P1' C36' 1.804(9) . ? P1' C42' 1.807(8) . ? P1' C48' 1.826(8) . ? N1' C2' 1.363(9) . ? N1' C5' 1.371(9) . ? N1' C6' 1.428(10) . ? C2' N3' 1.329(9) . ? N3' C4' 1.401(9) . ? C4' C5' 1.337(11) . ? C4' H4' 0.9500 . ? C5' H5' 0.9500 . ? C6' C7' 1.369(12) . ? C6' C11' 1.389(13) . ? C7' C8' 1.432(13) . ? C7' H7' 0.9500 . ? C8' C9' 1.345(15) . ? C8' H8' 0.9500 . ? C9' C10' 1.356(15) . ? C9' H9' 0.9500 . ? C10' C11' 1.401(13) . ? C10' H10' 0.9500 . ? C11' H11' 0.9500 . ? P2'A C18' 1.826(17) . ? P2'A C12' 1.867(18) . ? P2'A C61B 1.88(2) . ? P3'A C24' 1.79(2) . ? P3'A C30' 1.826(18) . ? P3'A C60B 1.93(3) . ? C12' C13' 1.374(17) . ? C12' C17' 1.394(16) . ? C13' C14' 1.399(17) . ? C13' H13' 0.9500 . ? C14' C15' 1.393(18) . ? C14' H14' 0.9500 . ? C15' C16' 1.387(19) . ? C15' H15' 0.9500 . ? C16' C17' 1.391(18) . ? C16' H16' 0.9500 . ? C17' H17' 0.9500 . ? C18' C19' 1.385(17) . ? C18' C23' 1.402(16) . ? C19' C20' 1.356(17) . ? C19' H19' 0.9500 . ? C20' C21' 1.358(16) . ? C20' H20' 0.9500 . ? C21' C22' 1.35(2) . ? C21' H21' 0.9500 . ? C22' C23' 1.375(19) . ? C22' H22' 0.9500 . ? C23' H23' 0.9500 . ? C24' C25' 1.363(17) . ? C24' C29' 1.403(17) . ? C25' C26' 1.395(18) . ? C25' H25' 0.9500 . ? C26' C27' 1.43(2) . ? C26' H26' 0.9500 . ? C27' C28' 1.32(2) . ? C27' H27' 0.9500 . ? C28' C29' 1.400(17) . ? C28' H28' 0.9500 . ? C29' H29' 0.9500 . ? P2'B C12B 1.824(13) . ? P2'B C18B 1.838(13) . ? P2'B C61' 1.849(15) . ? P3'B C60' 1.824(19) . ? P3'B C30' 1.833(13) . ? P3'B C24B 1.846(15) . ? C12B C13B 1.383(15) . ? C12B C17B 1.395(14) . ? C13B C14B 1.386(14) . ? C13B H13B 0.9500 . ? C14B C15B 1.372(15) . ? C14B H14B 0.9500 . ? C15B C16B 1.384(16) . ? C15B H15B 0.9500 . ? C16B C17B 1.398(16) . ? C16B H16B 0.9500 . ? C17B H17B 0.9500 . ? C18B C19B 1.403(15) . ? C18B C23B 1.407(14) . ? C19B C20B 1.370(14) . ? C19B H19B 0.9500 . ? C20B C21B 1.373(14) . ? C20B H20B 0.9500 . ? C21B C22B 1.361(17) . ? C21B H21B 0.9500 . ? C22B C23B 1.380(16) . ? C22B H22B 0.9500 . ? C23B H23B 0.9500 . ? C24B C25B 1.365(14) . ? C24B C29B 1.432(13) . ? C25B C26B 1.402(16) . ? C25B H25B 0.9500 . ? C26B C27B 1.427(17) . ? C26B H26B 0.9500 . ? C27B C28B 1.341(17) . ? C27B H27B 0.9500 . ? C28B C29B 1.405(12) . ? C28B H28B 0.9500 . ? C29B H29B 0.9500 . ? C30' C31' 1.3938 . ? C31' H31' 0.9500 . ? C32' C33' 1.390(12) . ? C32' H32' 0.9500 . ? C33' C34' 1.403(12) . ? C33' H33' 0.9500 . ? C34' C35' 1.391(10) . ? C34' H34' 0.9500 . ? C35' H35' 0.9500 . ? C36' C41' 1.354(12) . ? C36' C37' 1.406(12) . ? C37' C38' 1.363(13) . ? C37' H37' 0.9500 . ? C38' C39' 1.377(15) . ? C38' H38' 0.9500 . ? C39' C40' 1.357(14) . ? C39' H39' 0.9500 . ? C40' C41' 1.414(13) . ? C40' H40' 0.9500 . ? C41' H41' 0.9500 . ? C42' C43' 1.390(10) . ? C42' C47' 1.402(10) . ? C43' C44' 1.376(11) . ? C43' H43' 0.9500 . ? C44' C45' 1.366(12) . ? C44' H44' 0.9500 . ? C45' C46' 1.375(12) . ? C45' H45' 0.9500 . ? C46' C47' 1.407(11) . ? C46' H46' 0.9500 . ? C47' H47' 0.9500 . ? C48' C49' 1.382(12) . ? C48' C53' 1.403(12) . ? C49' C50' 1.424(12) . ? C49' H49' 0.9500 . ? C50' C51' 1.356(14) . ? C50' H50' 0.9500 . ? C51' C52' 1.347(15) . ? C51' H51' 0.9500 . ? C52' C53' 1.414(13) . ? C52' H52' 0.9500 . ? C53' H53' 0.9500 . ? C54' O57' 1.158(9) . ? C55' O58' 1.141(9) . ? C56' O59' 1.147(9) . ? C60' C61' 1.53(2) . ? C60' H60C 0.9900 . ? C60' H60D 0.9900 . ? C61' H61E 0.9900 . ? C61' H61F 0.9900 . ? C60B C61B 1.48(3) . ? C60B H60E 0.9900 . ? C60B H60F 0.9900 . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? 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 F6W P1W F2W 97.2(4) . . ? F6W P1W F4W 92.4(4) . . ? F2W P1W F4W 170.2(4) . . ? F6W P1W F1W 88.7(3) . . ? F2W P1W F1W 89.6(3) . . ? F4W P1W F1W 88.5(3) . . ? F6W P1W F3W 91.0(3) . . ? F2W P1W F3W 89.6(3) . . ? F4W P1W F3W 92.4(3) . . ? F1W P1W F3W 179.1(4) . . ? F6W P1W F5W 175.4(4) . . ? F2W P1W F5W 87.3(3) . . ? F4W P1W F5W 83.1(3) . . ? F1W P1W F5W 90.3(3) . . ? F3W P1W F5W 90.1(3) . . ? F4WB P2W F1WA 113.7(9) . . ? F4WB P2W F4WA 152.2(9) . . ? F1WA P2W F4WA 92.9(5) . . ? F4WB P2W F1WB 111.0(10) . . ? F1WA P2W F1WB 135.3(8) . . ? F4WB P2W F8W 96.7(9) . . ? F1WA P2W F8W 91.2(5) . . ? F4WA P2W F8W 90.7(4) . . ? F1WB P2W F8W 86.3(7) . . ? F4WB P2W F7W 84.4(9) . . ? F1WA P2W F7W 89.2(5) . . ? F4WA P2W F7W 87.9(4) . . ? F1WB P2W F7W 92.5(7) . . ? F8W P2W F7W 178.6(4) . . ? F4WB P2W F2WA 61.6(8) . . ? F1WA P2W F2WA 175.0(5) . . ? F4WA P2W F2WA 91.5(4) . . ? F1WB P2W F2WA 49.3(7) . . ? F8W P2W F2WA 91.1(4) . . ? F7W P2W F2WA 88.7(4) . . ? F1WA P2W F3WA 87.6(4) . . ? F4WA P2W F3WA 178.8(5) . . ? F1WB P2W F3WA 136.9(8) . . ? F8W P2W F3WA 90.4(4) . . ? F7W P2W F3WA 91.0(4) . . ? F2WA P2W F3WA 87.9(4) . . ? F4WB P2W F2WB 98.1(10) . . ? F4WA P2W F2WB 108.5(8) . . ? F1WB P2W F2WB 150.9(11) . . ? F8W P2W F2WB 91.7(9) . . ? F7W P2W F2WB 88.9(9) . . ? F2WA P2W F2WB 159.8(8) . . ? F3WA P2W F2WB 72.1(8) . . ? F4WB P2W F3WB 173.4(10) . . ? F1WA P2W F3WB 59.7(7) . . ? F1WB P2W F3WB 75.6(8) . . ? F8W P2W F3WB 84.2(6) . . ? F7W P2W F3WB 94.8(6) . . ? F2WA P2W F3WB 125.0(6) . . ? F3WA P2W F3WB 146.7(6) . . ? F2WB P2W F3WB 75.3(9) . . ? Cl5W C4W Cl6W 116.2(12) . . ? Cl5W C4W H4W1 108.2 . . ? Cl6W C4W H4W1 108.2 . . ? Cl5W C4W H4W2 108.2 . . ? Cl6W C4W H4W2 108.2 . . ? H4W1 C4W H4W2 107.4 . . ? Cl8W C7W Cl9W 109.6(5) . . ? Cl8W C7W H7W1 109.8 . . ? Cl9W C7W H7W1 109.8 . . ? Cl8W C7W H7W2 109.8 . . ? Cl9W C7W H7W2 109.8 . . ? H7W1 C7W H7W2 108.2 . . ? C56 Mn1 C55 86.5(3) . . ? C56 Mn1 C54 86.0(4) . . ? C55 Mn1 C54 96.5(3) . . ? C56 Mn1 N3 174.3(3) . . ? C55 Mn1 N3 91.9(3) . . ? C54 Mn1 N3 88.8(3) . . ? C56 Mn1 P2 93.6(3) . . ? C55 Mn1 P2 87.0(2) . . ? C54 Mn1 P2 176.5(3) . . ? N3 Mn1 P2 91.78(18) . . ? C56 Mn1 P3 88.0(3) . . ? C55 Mn1 P3 169.2(2) . . ? C54 Mn1 P3 92.4(3) . . ? N3 Mn1 P3 94.42(18) . . ? P2 Mn1 P3 84.17(8) . . ? C2 Au1 P1 174.9(2) . . ? C42A P1 C51 104.2(12) . . ? C42A P1 C36B 100.6(12) . . ? C51 P1 C36B 106.5(6) . . ? C42A P1 C36A 105.0(10) . . ? C51 P1 C36A 106.7(6) . . ? C51 P1 C42B 103.7(11) . . ? C36B P1 C42B 107.7(10) . . ? C36A P1 C42B 112.1(12) . . ? C42A P1 Au1 116.1(8) . . ? C51 P1 Au1 111.7(3) . . ? C36B P1 Au1 116.3(7) . . ? C36A P1 Au1 112.3(7) . . ? C42B P1 Au1 110.0(7) . . ? C12 P2 C18 105.5(4) . . ? C12 P2 C60 108.8(4) . . ? C18 P2 C60 101.7(4) . . ? C12 P2 Mn1 113.9(2) . . ? C18 P2 Mn1 117.5(3) . . ? C60 P2 Mn1 108.5(3) . . ? C24 P3 C30 101.0(4) . . ? C24 P3 C61 107.3(4) . . ? C30 P3 C61 103.1(4) . . ? C24 P3 Mn1 110.7(3) . . ? C30 P3 Mn1 123.5(3) . . ? C61 P3 Mn1 110.0(3) . . ? C2 N1 C5 108.6(6) . . ? C2 N1 C6 125.7(6) . . ? C5 N1 C6 125.7(6) . . ? N3 C2 N1 107.8(6) . . ? N3 C2 Au1 129.9(6) . . ? N1 C2 Au1 121.9(5) . . ? C2 N3 C4 106.9(6) . . ? C2 N3 Mn1 125.1(5) . . ? C4 N3 Mn1 127.8(5) . . ? C5 C4 N3 110.4(7) . . ? C5 C4 H4 124.8 . . ? N3 C4 H4 124.8 . . ? C4 C5 N1 106.2(7) . . ? C4 C5 H5 126.9 . . ? N1 C5 H5 126.9 . . ? C11 C6 C7 121.1(8) . . ? C11 C6 N1 119.9(7) . . ? C7 C6 N1 119.0(7) . . ? C8 C7 C6 117.5(8) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C9 C8 C7 122.1(8) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C10 C9 C8 118.0(8) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 122.0(8) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C6 C11 C10 119.2(8) . . ? C6 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C17 117.3(8) . . ? C13 C12 P2 123.2(6) . . ? C17 C12 P2 119.3(6) . . ? C14 C13 C12 120.5(8) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.5(8) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 120.0(8) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 119.9(8) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 121.8(7) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? C23 C18 C19 118.1(7) . . ? C23 C18 P2 123.5(6) . . ? C19 C18 P2 118.4(6) . . ? C20 C19 C18 120.4(9) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.4(9) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 118.8(9) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C23 122.4(8) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C22 C23 C18 119.8(8) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C25 C24 C29 119.3(8) . . ? C25 C24 P3 123.1(7) . . ? C29 C24 P3 117.3(6) . . ? C26 C25 C24 121.0(8) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C27 C26 C25 118.9(8) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 123.0(9) . . ? C26 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C29 C28 C27 117.9(9) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? C28 C29 C24 120.0(8) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? C35 C30 C31 119.0(8) . . ? C35 C30 P3 121.8(6) . . ? C31 C30 P3 118.9(6) . . ? C32 C31 C30 121.4(8) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 118.6(9) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 120.6(8) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 121.1(8) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C30 119.2(8) . . ? C34 C35 H35 120.4 . . ? C30 C35 H35 120.4 . . ? C37A C36A C41A 119.0(15) . . ? C37A C36A P1 122.4(13) . . ? C41A C36A P1 117.2(12) . . ? C36A C37A C38A 121.1(14) . . ? C36A C37A H37A 119.5 . . ? C38A C37A H37A 119.5 . . ? C39A C38A C37A 122.4(14) . . ? C39A C38A H38A 118.8 . . ? C37A C38A H38A 118.8 . . ? C38A C39A C40A 114.8(14) . . ? C38A C39A H39A 122.6 . . ? C40A C39A H39A 122.6 . . ? C41A C40A C39A 121.6(14) . . ? C41A C40A H40A 119.2 . . ? C39A C40A H40A 119.2 . . ? C40A C41A C36A 116.4(13) . . ? C40A C41A H41A 121.8 . . ? C36A C41A H41A 121.8 . . ? C47A C42A C43A 121.0(14) . . ? C47A C42A P1 118.4(12) . . ? C43A C42A P1 120.5(13) . . ? C44A C43A C42A 117.6(15) . . ? C44A C43A H43A 121.2 . . ? C42A C43A H43A 121.2 . . ? C45A C44A C43A 121.6(14) . . ? C45A C44A H44A 119.2 . . ? C43A C44A H44A 119.2 . . ? C44A C45A C46A 120.1(15) . . ? C44A C45A H45A 119.9 . . ? C46A C45A H45A 119.9 . . ? C47A C46A C45A 119.5(16) . . ? C47A C46A H46A 120.3 . . ? C45A C46A H46A 120.3 . . ? C42A C47A C46A 120.1(14) . . ? C42A C47A H47A 119.9 . . ? C46A C47A H47A 119.9 . . ? C49A C48A C53 120.6(15) . . ? C49A C48A H48A 119.7 . . ? C53 C48A H48A 119.7 . . ? C48A C49A C50A 120.7(16) . . ? C48A C49A H49A 119.7 . . ? C50A C49A H49A 119.7 . . ? C49A C50A C51 120.6(15) . . ? C49A C50A H50A 119.7 . . ? C51 C50A H50A 119.7 . . ? C37B C36B C41B 119.0(14) . . ? C37B C36B P1 119.4(12) . . ? C41B C36B P1 120.2(13) . . ? C36B C37B C38B 124.0(14) . . ? C36B C37B H37B 118.0 . . ? C38B C37B H37B 118.0 . . ? C39B C38B C37B 117.3(14) . . ? C39B C38B H38B 121.4 . . ? C37B C38B H38B 121.4 . . ? C38B C39B C40B 121.8(14) . . ? C38B C39B H39B 119.1 . . ? C40B C39B H39B 119.1 . . ? C41B C40B C39B 118.5(14) . . ? C41B C40B H40B 120.7 . . ? C39B C40B H40B 120.7 . . ? C40B C41B C36B 116.4(13) . . ? C40B C41B H41B 121.8 . . ? C36B C41B H41B 121.8 . . ? C47B C42B C43B 118.4(14) . . ? C47B C42B P1 118.6(12) . . ? C43B C42B P1 122.8(12) . . ? C44B C43B C42B 121.0(15) . . ? C44B C43B H43B 119.5 . . ? C42B C43B H43B 119.5 . . ? C45B C44B C43B 119.9(14) . . ? C45B C44B H44B 120.1 . . ? C43B C44B H44B 120.1 . . ? C44B C45B C46B 120.4(15) . . ? C44B C45B H45B 119.8 . . ? C46B C45B H45B 119.8 . . ? C47B C46B C45B 120.6(15) . . ? C47B C46B H46B 119.7 . . ? C45B C46B H46B 119.7 . . ? C42B C47B C46B 119.7(14) . . ? C42B C47B H47B 120.1 . . ? C46B C47B H47B 120.1 . . ? C49B C48B C53 121.2(16) . . ? C49B C48B H48B 119.4 . . ? C53 C48B H48B 119.4 . . ? C48B C49B C50B 119.9(16) . . ? C48B C49B H49B 120.0 . . ? C50B C49B H49B 120.0 . . ? C51 C50B C49B 120.3(16) . . ? C51 C50B H50B 119.8 . . ? C49B C50B H50B 119.8 . . ? C50B C51 C52 118.3(10) . . ? C52 C51 C50A 118.4(9) . . ? C50B C51 P1 118.2(9) . . ? C52 C51 P1 121.9(6) . . ? C50A C51 P1 119.1(8) . . ? C51 C52 C53 121.6(8) . . ? C51 C52 H52 119.2 . . ? C53 C52 H52 119.2 . . ? C48B C53 C52 117.0(10) . . ? C52 C53 C48A 117.0(10) . . ? C48B C53 H53 116.8 . . ? C52 C53 H53 121.5 . . ? C48A C53 H53 121.5 . . ? O57 C54 Mn1 174.2(8) . . ? O58 C55 Mn1 172.3(7) . . ? O59 C56 Mn1 175.1(8) . . ? C61 C60 P2 112.3(5) . . ? C61 C60 H60A 109.2 . . ? P2 C60 H60A 109.2 . . ? C61 C60 H60B 109.2 . . ? P2 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C60 C61 P3 109.5(6) . . ? C60 C61 H61A 109.8 . . ? P3 C61 H61A 109.8 . . ? C60 C61 H61B 109.8 . . ? P3 C61 H61B 109.8 . . ? H61A C61 H61B 108.2 . . ? C2' Au1' P1' 177.5(2) . . ? C56' Mn1' C54' 89.6(3) . . ? C56' Mn1' C55' 88.0(4) . . ? C54' Mn1' C55' 91.9(3) . . ? C56' Mn1' N3' 178.4(3) . . ? C54' Mn1' N3' 92.0(3) . . ? C55' Mn1' N3' 91.9(3) . . ? C56' Mn1' P2'B 93.2(3) . . ? C54' Mn1' P2'B 172.9(3) . . ? C55' Mn1' P2'B 94.7(3) . . ? N3' Mn1' P2'B 85.2(2) . . ? C56' Mn1' P3'A 88.2(5) . . ? C54' Mn1' P3'A 92.5(4) . . ? C55' Mn1' P3'A 174.1(5) . . ? N3' Mn1' P3'A 91.8(5) . . ? P2'B Mn1' P3'A 81.0(3) . . ? C56' Mn1' P3'B 86.2(4) . . ? C54' Mn1' P3'B 88.3(3) . . ? C55' Mn1' P3'B 174.1(4) . . ? N3' Mn1' P3'B 94.0(3) . . ? P2'B Mn1' P3'B 85.3(2) . . ? P3'A Mn1' P3'B 4.7(4) . . ? C56' Mn1' P2'A 82.1(3) . . ? C54' Mn1' P2'A 171.0(3) . . ? C55' Mn1' P2'A 91.2(3) . . ? N3' Mn1' P2'A 96.3(2) . . ? P2'B Mn1' P2'A 11.56(16) . . ? P3'A Mn1' P2'A 83.8(3) . . ? P3'B Mn1' P2'A 87.7(3) . . ? C36' P1' C42' 105.4(4) . . ? C36' P1' C48' 104.0(4) . . ? C42' P1' C48' 107.8(4) . . ? C36' P1' Au1' 113.8(3) . . ? C42' P1' Au1' 112.4(3) . . ? C48' P1' Au1' 112.8(3) . . ? C2' N1' C5' 109.7(6) . . ? C2' N1' C6' 125.0(6) . . ? C5' N1' C6' 125.0(6) . . ? N3' C2' N1' 108.5(6) . . ? N3' C2' Au1' 129.8(6) . . ? N1' C2' Au1' 121.6(5) . . ? C2' N3' C4' 106.1(6) . . ? C2' N3' Mn1' 127.4(5) . . ? C4' N3' Mn1' 126.5(5) . . ? C5' C4' N3' 110.5(7) . . ? C5' C4' H4' 124.8 . . ? N3' C4' H4' 124.8 . . ? C4' C5' N1' 105.2(7) . . ? C4' C5' H5' 127.4 . . ? N1' C5' H5' 127.4 . . ? C7' C6' C11' 120.9(9) . . ? C7' C6' N1' 121.5(8) . . ? C11' C6' N1' 117.6(8) . . ? C6' C7' C8' 118.7(10) . . ? C6' C7' H7' 120.7 . . ? C8' C7' H7' 120.7 . . ? C9' C8' C7' 117.5(10) . . ? C9' C8' H8' 121.2 . . ? C7' C8' H8' 121.2 . . ? C8' C9' C10' 125.9(11) . . ? C8' C9' H9' 117.0 . . ? C10' C9' H9' 117.0 . . ? C9' C10' C11' 116.3(11) . . ? C9' C10' H10' 121.9 . . ? C11' C10' H10' 121.9 . . ? C6' C11' C10' 120.7(10) . . ? C6' C11' H11' 119.7 . . ? C10' C11' H11' 119.7 . . ? C18' P2'A C12' 103.3(10) . . ? C18' P2'A C61B 98.6(9) . . ? C12' P2'A C61B 108.9(9) . . ? C18' P2'A Mn1' 120.3(7) . . ? C12' P2'A Mn1' 115.8(6) . . ? C61B P2'A Mn1' 108.3(7) . . ? C24' P3'A C30' 101.7(9) . . ? C24' P3'A C60B 102.3(13) . . ? C30' P3'A C60B 103.5(11) . . ? C24' P3'A Mn1' 116.7(9) . . ? C30' P3'A Mn1' 120.3(8) . . ? C60B P3'A Mn1' 110.1(11) . . ? C13' C12' C17' 123.6(15) . . ? C13' C12' P2'A 115.5(12) . . ? C17' C12' P2'A 120.9(12) . . ? C12' C13' C14' 117.8(15) . . ? C12' C13' H13' 121.1 . . ? C14' C13' H13' 121.1 . . ? C15' C14' C13' 120.4(16) . . ? C15' C14' H14' 119.8 . . ? C13' C14' H14' 119.8 . . ? C16' C15' C14' 119.7(15) . . ? C16' C15' H15' 120.2 . . ? C14' C15' H15' 120.2 . . ? C15' C16' C17' 121.2(15) . . ? C15' C16' H16' 119.4 . . ? C17' C16' H16' 119.4 . . ? C16' C17' C12' 116.9(15) . . ? C16' C17' H17' 121.5 . . ? C12' C17' H17' 121.5 . . ? C19' C18' C23' 117.7(15) . . ? C19' C18' P2'A 120.5(12) . . ? C23' C18' P2'A 121.8(12) . . ? C20' C19' C18' 120.7(14) . . ? C20' C19' H19' 119.7 . . ? C18' C19' H19' 119.7 . . ? C19' C20' C21' 123.0(16) . . ? C19' C20' H20' 118.5 . . ? C21' C20' H20' 118.5 . . ? C22' C21' C20' 115.8(16) . . ? C22' C21' H21' 122.1 . . ? C20' C21' H21' 122.1 . . ? C21' C22' C23' 125.0(15) . . ? C21' C22' H22' 117.5 . . ? C23' C22' H22' 117.5 . . ? C22' C23' C18' 117.8(16) . . ? C22' C23' H23' 121.1 . . ? C18' C23' H23' 121.1 . . ? C25' C24' C29' 118.3(15) . . ? C25' C24' P3'A 124.3(14) . . ? C29' C24' P3'A 117.3(12) . . ? C24' C25' C26' 121.5(17) . . ? C24' C25' H25' 119.2 . . ? C26' C25' H25' 119.2 . . ? C25' C26' C27' 118.0(16) . . ? C25' C26' H26' 121.0 . . ? C27' C26' H26' 121.0 . . ? C28' C27' C26' 120.3(16) . . ? C28' C27' H27' 119.8 . . ? C26' C27' H27' 119.8 . . ? C27' C28' C29' 120.4(17) . . ? C27' C28' H28' 119.8 . . ? C29' C28' H28' 119.8 . . ? C28' C29' C24' 120.5(15) . . ? C28' C29' H29' 119.7 . . ? C24' C29' H29' 119.7 . . ? C12B P2'B C18B 102.3(7) . . ? C12B P2'B C61' 106.0(7) . . ? C18B P2'B C61' 106.1(7) . . ? C12B P2'B Mn1' 120.4(4) . . ? C18B P2'B Mn1' 112.5(5) . . ? C61' P2'B Mn1' 108.5(5) . . ? C60' P3'B C30' 109.7(8) . . ? C60' P3'B C24B 103.3(9) . . ? C30' P3'B C24B 100.9(6) . . ? C60' P3'B Mn1' 106.3(8) . . ? C30' P3'B Mn1' 119.6(6) . . ? C24B P3'B Mn1' 116.0(6) . . ? C13B C12B C17B 121.1(12) . . ? C13B C12B P2'B 119.8(9) . . ? C17B C12B P2'B 119.1(9) . . ? C12B C13B C14B 119.6(11) . . ? C12B C13B H13B 120.2 . . ? C14B C13B H13B 120.2 . . ? C15B C14B C13B 120.5(13) . . ? C15B C14B H14B 119.8 . . ? C13B C14B H14B 119.8 . . ? C14B C15B C16B 119.8(12) . . ? C14B C15B H15B 120.1 . . ? C16B C15B H15B 120.1 . . ? C15B C16B C17B 121.1(12) . . ? C15B C16B H16B 119.5 . . ? C17B C16B H16B 119.5 . . ? C12B C17B C16B 117.9(12) . . ? C12B C17B H17B 121.1 . . ? C16B C17B H17B 121.1 . . ? C19B C18B C23B 118.2(11) . . ? C19B C18B P2'B 120.2(9) . . ? C23B C18B P2'B 121.4(10) . . ? C20B C19B C18B 120.9(11) . . ? C20B C19B H19B 119.5 . . ? C18B C19B H19B 119.5 . . ? C19B C20B C21B 120.7(13) . . ? C19B C20B H20B 119.7 . . ? C21B C20B H20B 119.7 . . ? C22B C21B C20B 118.6(13) . . ? C22B C21B H21B 120.7 . . ? C20B C21B H21B 120.7 . . ? C21B C22B C23B 123.2(12) . . ? C21B C22B H22B 118.4 . . ? C23B C22B H22B 118.4 . . ? C22B C23B C18B 118.2(12) . . ? C22B C23B H23B 120.9 . . ? C18B C23B H23B 120.9 . . ? C25B C24B C29B 118.7(11) . . ? C25B C24B P3'B 123.6(11) . . ? C29B C24B P3'B 117.7(8) . . ? C24B C25B C26B 123.8(13) . . ? C24B C25B H25B 118.1 . . ? C26B C25B H25B 118.1 . . ? C25B C26B C27B 114.6(13) . . ? C25B C26B H26B 122.7 . . ? C27B C26B H26B 122.7 . . ? C28B C27B C26B 124.2(13) . . ? C28B C27B H27B 117.9 . . ? C26B C27B H27B 117.9 . . ? C27B C28B C29B 119.5(11) . . ? C27B C28B H28B 120.2 . . ? C29B C28B H28B 120.2 . . ? C28B C29B C24B 119.0(8) . . ? C28B C29B H29B 120.5 . . ? C24B C29B H29B 120.5 . . ? C31' C30' P3'A 119.6(5) . . ? C35' C30' P3'A 120.2(7) . . ? C31' C30' P3'B 122.1(4) . . ? C35' C30' P3'B 117.6(6) . . ? C32' C31' H31' 120.1 . . ? C30' C31' H31' 120.3 . . ? C31' C32' H32' 119.5 . . ? C33' C32' H32' 119.5 . . ? C32' C33' C34' 119.8(8) . . ? C32' C33' H33' 120.1 . . ? C34' C33' H33' 120.1 . . ? C35' C34' C33' 119.2(8) . . ? C35' C34' H34' 120.4 . . ? C33' C34' H34' 120.4 . . ? C34' C35' H35' 119.8 . . ? C30' C35' H35' 119.8 . . ? C41' C36' C37' 117.9(9) . . ? C41' C36' P1' 123.8(7) . . ? C37' C36' P1' 118.2(7) . . ? C38' C37' C36' 120.6(10) . . ? C38' C37' H37' 119.7 . . ? C36' C37' H37' 119.7 . . ? C37' C38' C39' 120.2(10) . . ? C37' C38' H38' 119.9 . . ? C39' C38' H38' 119.9 . . ? C40' C39' C38' 121.2(10) . . ? C40' C39' H39' 119.4 . . ? C38' C39' H39' 119.4 . . ? C39' C40' C41' 117.9(10) . . ? C39' C40' H40' 121.0 . . ? C41' C40' H40' 121.0 . . ? C36' C41' C40' 122.2(9) . . ? C36' C41' H41' 118.9 . . ? C40' C41' H41' 118.9 . . ? C43' C42' C47' 119.0(7) . . ? C43' C42' P1' 119.7(6) . . ? C47' C42' P1' 121.3(6) . . ? C44' C43' C42' 120.5(8) . . ? C44' C43' H43' 119.7 . . ? C42' C43' H43' 119.7 . . ? C45' C44' C43' 120.6(8) . . ? C45' C44' H44' 119.7 . . ? C43' C44' H44' 119.7 . . ? C44' C45' C46' 120.7(8) . . ? C44' C45' H45' 119.7 . . ? C46' C45' H45' 119.7 . . ? C45' C46' C47' 119.7(8) . . ? C45' C46' H46' 120.1 . . ? C47' C46' H46' 120.1 . . ? C42' C47' C46' 119.5(8) . . ? C42' C47' H47' 120.3 . . ? C46' C47' H47' 120.3 . . ? C49' C48' C53' 119.7(8) . . ? C49' C48' P1' 117.8(7) . . ? C53' C48' P1' 122.4(7) . . ? C48' C49' C50' 119.7(9) . . ? C48' C49' H49' 120.1 . . ? C50' C49' H49' 120.1 . . ? C51' C50' C49' 119.9(10) . . ? C51' C50' H50' 120.1 . . ? C49' C50' H50' 120.1 . . ? C52' C51' C50' 120.7(10) . . ? C52' C51' H51' 119.6 . . ? C50' C51' H51' 119.6 . . ? C51' C52' C53' 121.8(10) . . ? C51' C52' H52' 119.1 . . ? C53' C52' H52' 119.1 . . ? C48' C53' C52' 118.1(10) . . ? C48' C53' H53' 120.9 . . ? C52' C53' H53' 120.9 . . ? O57' C54' Mn1' 172.5(7) . . ? O58' C55' Mn1' 174.8(7) . . ? O59' C56' Mn1' 178.4(7) . . ? C61' C60' P3'B 109.1(12) . . ? C61' C60' H60C 109.9 . . ? P3'B C60' H60C 109.9 . . ? C61' C60' H60D 109.9 . . ? P3'B C60' H60D 109.9 . . ? H60C C60' H60D 108.3 . . ? C60' C61' P2'B 110.9(11) . . ? C60' C61' H61E 109.5 . . ? P2'B C61' H61E 109.5 . . ? C60' C61' H61F 109.5 . . ? P2'B C61' H61F 109.5 . . ? H61E C61' H61F 108.0 . . ? C61B C60B P3'A 110.7(17) . . ? C61B C60B H60E 109.5 . . ? P3'A C60B H60E 109.5 . . ? C61B C60B H60F 109.5 . . ? P3'A C60B H60F 109.5 . . ? H60E C60B H60F 108.1 . . ? C60B C61B P2'A 111.3(16) . . ? C60B C61B H61C 109.4 . . ? P2'A C61B H61C 109.4 . . ? C60B C61B H61D 109.4 . . ? P2'A C61B H61D 109.4 . . ? H61C C61B H61D 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C56 Mn1 P2 C12 -164.4(4) . . . . ? C55 Mn1 P2 C12 -78.1(4) . . . . ? C12' P2'A C61B C60B 88.1(18) . . . . ? Mn1' P2'A C61B C60B -38.6(18) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-05-04 at 11:35:29 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.dat # CIF files read : jv07bk1n struct data_18 _database_code_depnum_ccdc_archive 'CCDC 725958' _audit_creation_date 2007-05-04T11:35:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C23 H18 Mn N4 O3, Cl O4' _chemical_formula_sum 'C23 H18 Cl Mn N4 O7' _chemical_formula_weight 552.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9537(2) _cell_length_b 10.4298(2) _cell_length_c 13.1270(3) _cell_angle_alpha 79.323(2) _cell_angle_beta 80.7630(10) _cell_angle_gamma 73.7540(10) _cell_volume 1148.84(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1933 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 28.26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Yello _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.94 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0242 _diffrn_reflns_number 35256 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.1 _diffrn_reflns_theta_full 27.1 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5040 _reflns_number_gt 4476 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'DIRDIF96 (Beurskens, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0326P)^2^+0.8297P] 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_number_reflns 5040 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.035 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.607 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.76282(3) 0.36305(2) 0.269563(19) 0.01235(7) Uani 1 1 d . . . N3 N 0.95332(16) 0.22755(14) 0.20432(11) 0.0138(3) Uani 1 1 d . . . C2 C 0.96687(19) 0.10031(17) 0.19711(13) 0.0139(3) Uani 1 1 d . . . N1 N 1.10823(16) 0.04480(14) 0.14630(11) 0.0134(3) Uani 1 1 d . . . C5 C 1.18956(19) 0.14422(17) 0.11821(13) 0.0146(3) Uani 1 1 d . . . C6 C 1.3458(2) 0.12690(18) 0.05515(14) 0.0187(4) Uani 1 1 d . . . H6A H 1.3643 0.2139 0.0285 0.028 Uiso 1 1 calc R . . H6B H 1.3483 0.0803 -0.0019 0.028 Uiso 1 1 calc R . . H6C H 1.4255 0.0753 0.0983 0.028 Uiso 1 1 calc R . . C4 C 1.0922(2) 0.25510(17) 0.15492(13) 0.0153(3) Uani 1 1 d . . . N6 N 0.77314(16) 0.22187(14) 0.40104(11) 0.0133(3) Uani 1 1 d . . . C7 C 0.68641(19) 0.13164(17) 0.42919(13) 0.0166(3) Uani 1 1 d . . . H7 H 0.6162 0.1294 0.3849 0.02 Uiso 1 1 calc R . . C8 C 0.6976(2) 0.04242(18) 0.52111(14) 0.0181(4) Uani 1 1 d . . . H8 H 0.6373 -0.0197 0.5376 0.022 Uiso 1 1 calc R . . C9 C 0.7994(2) 0.04638(18) 0.58845(14) 0.0194(4) Uani 1 1 d . . . H9 H 0.806 -0.0109 0.6519 0.023 Uiso 1 1 calc R . . C10 C 0.8916(2) 0.13722(17) 0.55996(13) 0.0168(3) Uani 1 1 d . . . H10 H 0.9617 0.1413 0.6037 0.02 Uiso 1 1 calc R . . C11 C 0.87762(19) 0.22194(16) 0.46511(13) 0.0143(3) Uani 1 1 d . . . C12 C 0.97234(19) 0.31984(16) 0.42574(13) 0.0142(3) Uani 1 1 d . . . C13 C 1.1026(2) 0.32094(17) 0.47047(13) 0.0169(3) Uani 1 1 d . . . H13 H 1.1354 0.2572 0.5275 0.02 Uiso 1 1 calc R . . C14 C 1.1829(2) 0.41797(18) 0.42909(14) 0.0190(4) Uani 1 1 d . . . H14 H 1.2719 0.419 0.4566 0.023 Uiso 1 1 calc R . . C15 C 1.1282(2) 0.51369(18) 0.34598(14) 0.0186(4) Uani 1 1 d . . . H15 H 1.178 0.5819 0.3185 0.022 Uiso 1 1 calc R . . C16 C 0.9988(2) 0.50649(17) 0.30440(13) 0.0163(3) Uani 1 1 d . . . H16 H 0.9622 0.5714 0.249 0.02 Uiso 1 1 calc R . . N17 N 0.92385(16) 0.40908(14) 0.34119(11) 0.0135(3) Uani 1 1 d . . . C18 C 0.77843(19) 0.48293(17) 0.15244(13) 0.0151(3) Uani 1 1 d . . . O19 O 0.79154(15) 0.55304(12) 0.07473(9) 0.0209(3) Uani 1 1 d . . . C20 C 0.6219(2) 0.31195(17) 0.21118(14) 0.0183(4) Uani 1 1 d . . . O21 O 0.52677(16) 0.29024(14) 0.17316(12) 0.0299(3) Uani 1 1 d . . . C22 C 0.5981(2) 0.47987(17) 0.33277(13) 0.0163(3) Uani 1 1 d . . . O23 O 0.49053(15) 0.54917(13) 0.37192(10) 0.0238(3) Uani 1 1 d . . . C31 C 1.16164(19) -0.09269(16) 0.12626(13) 0.0141(3) Uani 1 1 d . . . C32 C 1.0633(2) -0.14857(17) 0.08703(13) 0.0166(3) Uani 1 1 d . . . H32 H 0.9629 -0.0979 0.0744 0.02 Uiso 1 1 calc R . . C33 C 1.1163(2) -0.28081(18) 0.06684(13) 0.0188(4) Uani 1 1 d . . . H33 H 1.0508 -0.3193 0.041 0.023 Uiso 1 1 calc R . . C34 C 1.2669(2) -0.35597(18) 0.08507(14) 0.0201(4) Uani 1 1 d . . . H34 H 1.3028 -0.444 0.0704 0.024 Uiso 1 1 calc R . . C35 C 1.3634(2) -0.29916(17) 0.12529(14) 0.0193(4) Uani 1 1 d . . . H35 H 1.464 -0.3497 0.1377 0.023 Uiso 1 1 calc R . . C36 C 1.3113(2) -0.16769(17) 0.14707(13) 0.0172(3) Uani 1 1 d . . . H36 H 1.3754 -0.1303 0.1752 0.021 Uiso 1 1 calc R . . Cl24 Cl 0.32643(5) 0.15641(4) 0.70917(3) 0.01828(10) Uani 1 1 d . . . O25 O 0.17065(16) 0.14561(15) 0.70391(11) 0.0280(3) Uani 1 1 d . . . O26 O 0.4285(2) 0.02469(14) 0.73640(13) 0.0402(4) Uani 1 1 d . . . O27 O 0.32033(17) 0.23957(14) 0.78600(11) 0.0298(3) Uani 1 1 d . . . O28 O 0.38436(16) 0.21630(15) 0.60827(11) 0.0307(3) Uani 1 1 d . . . H4 H 1.110(2) 0.3399(19) 0.1504(14) 0.011(4) Uiso 1 1 d . . . H2 H 0.896(2) 0.052(2) 0.2241(16) 0.017(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01166(12) 0.01313(13) 0.01245(13) -0.00200(9) -0.00338(9) -0.00232(9) N3 0.0138(7) 0.0156(7) 0.0122(7) -0.0022(5) -0.0034(5) -0.0032(5) C2 0.0143(8) 0.0153(8) 0.0121(8) -0.0007(6) -0.0029(6) -0.0040(6) N1 0.0136(6) 0.0141(7) 0.0126(7) -0.0014(5) -0.0032(5) -0.0030(5) C5 0.0141(8) 0.0172(8) 0.0123(8) 0.0003(6) -0.0041(6) -0.0040(6) C6 0.0151(8) 0.0184(8) 0.0211(9) -0.0025(7) 0.0005(7) -0.0036(7) C4 0.0158(8) 0.0151(8) 0.0160(8) -0.0010(6) -0.0030(6) -0.0059(6) N6 0.0119(6) 0.0155(7) 0.0124(7) -0.0035(5) -0.0007(5) -0.0029(5) C7 0.0134(8) 0.0210(8) 0.0170(8) -0.0041(7) -0.0021(6) -0.0062(7) C8 0.0169(8) 0.0196(8) 0.0190(9) -0.0024(7) 0.0004(7) -0.0083(7) C9 0.0217(9) 0.0202(9) 0.0148(8) 0.0006(7) -0.0012(7) -0.0056(7) C10 0.0167(8) 0.0201(8) 0.0146(8) -0.0027(7) -0.0040(7) -0.0051(7) C11 0.0120(7) 0.0150(8) 0.0158(8) -0.0047(6) -0.0022(6) -0.0015(6) C12 0.0158(8) 0.0145(8) 0.0127(8) -0.0038(6) -0.0010(6) -0.0038(6) C13 0.0170(8) 0.0188(8) 0.0156(8) -0.0030(7) -0.0033(7) -0.0047(7) C14 0.0169(8) 0.0237(9) 0.0195(9) -0.0059(7) -0.0028(7) -0.0083(7) C15 0.0217(9) 0.0200(8) 0.0173(8) -0.0042(7) -0.0008(7) -0.0104(7) C16 0.0201(8) 0.0153(8) 0.0142(8) -0.0025(6) -0.0015(7) -0.0059(7) N17 0.0143(7) 0.0138(6) 0.0121(7) -0.0033(5) -0.0011(5) -0.0027(5) C18 0.0135(8) 0.0149(8) 0.0181(9) -0.0069(7) -0.0051(6) -0.0008(6) O19 0.0266(7) 0.0191(6) 0.0155(6) -0.0002(5) -0.0039(5) -0.0043(5) C20 0.0206(9) 0.0153(8) 0.0177(9) -0.0006(7) -0.0038(7) -0.0026(7) O21 0.0292(7) 0.0318(8) 0.0352(8) -0.0032(6) -0.0176(6) -0.0118(6) C22 0.0175(8) 0.0171(8) 0.0163(8) 0.0000(7) -0.0041(7) -0.0085(7) O23 0.0186(6) 0.0224(7) 0.0284(7) -0.0065(6) 0.0022(6) -0.0030(5) C31 0.0165(8) 0.0137(8) 0.0112(8) -0.0011(6) -0.0010(6) -0.0029(6) C32 0.0162(8) 0.0194(8) 0.0138(8) -0.0006(6) -0.0037(6) -0.0041(7) C33 0.0242(9) 0.0192(8) 0.0157(8) -0.0029(7) -0.0043(7) -0.0086(7) C34 0.0268(9) 0.0149(8) 0.0161(8) -0.0029(7) -0.0010(7) -0.0019(7) C35 0.0168(8) 0.0178(8) 0.0192(9) 0.0003(7) -0.0028(7) 0.0006(7) C36 0.0160(8) 0.0199(8) 0.0160(8) -0.0023(7) -0.0033(7) -0.0046(7) Cl24 0.0205(2) 0.0159(2) 0.0202(2) -0.00327(16) -0.00860(16) -0.00376(16) O25 0.0281(7) 0.0388(8) 0.0234(7) 0.0037(6) -0.0079(6) -0.0216(6) O26 0.0540(10) 0.0194(7) 0.0468(10) -0.0048(7) -0.0304(8) 0.0048(7) O27 0.0343(8) 0.0295(7) 0.0307(8) -0.0150(6) -0.0123(6) -0.0047(6) O28 0.0212(7) 0.0441(9) 0.0267(7) 0.0007(6) -0.0027(6) -0.0120(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C18 1.8064(18) . ? Mn1 C20 1.8169(18) . ? Mn1 C22 1.8234(17) . ? Mn1 N17 2.0453(14) . ? Mn1 N6 2.0466(14) . ? Mn1 N3 2.0665(14) . ? N3 C2 1.318(2) . ? N3 C4 1.386(2) . ? C2 N1 1.358(2) . ? C2 H2 0.90(2) . ? N1 C5 1.391(2) . ? N1 C31 1.439(2) . ? C5 C4 1.356(2) . ? C5 C6 1.489(2) . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C4 H4 0.933(19) . ? N6 C7 1.347(2) . ? N6 C11 1.355(2) . ? C7 C8 1.379(2) . ? C7 H7 0.93 . ? C8 C9 1.381(3) . ? C8 H8 0.93 . ? C9 C10 1.388(2) . ? C9 H9 0.93 . ? C10 C11 1.388(2) . ? C10 H10 0.93 . ? C11 C12 1.476(2) . ? C12 N17 1.354(2) . ? C12 C13 1.391(2) . ? C13 C14 1.383(2) . ? C13 H13 0.93 . ? C14 C15 1.386(3) . ? C14 H14 0.93 . ? C15 C16 1.384(2) . ? C15 H15 0.93 . ? C16 N17 1.346(2) . ? C16 H16 0.93 . ? C18 O19 1.150(2) . ? C20 O21 1.146(2) . ? C22 O23 1.142(2) . ? C31 C32 1.387(2) . ? C31 C36 1.390(2) . ? C32 C33 1.388(2) . ? C32 H32 0.93 . ? C33 C34 1.390(3) . ? C33 H33 0.93 . ? C34 C35 1.388(3) . ? C34 H34 0.93 . ? C35 C36 1.387(2) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? Cl24 O27 1.4326(13) . ? Cl24 O28 1.4379(15) . ? Cl24 O26 1.4389(14) . ? Cl24 O25 1.4439(14) . ? 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 C18 Mn1 C20 87.52(8) . . ? C18 Mn1 C22 93.46(7) . . ? C20 Mn1 C22 87.85(8) . . ? C18 Mn1 N17 95.82(7) . . ? C20 Mn1 N17 176.40(7) . . ? C22 Mn1 N17 93.27(7) . . ? C18 Mn1 N6 173.29(6) . . ? C20 Mn1 N6 97.27(7) . . ? C22 Mn1 N6 91.42(7) . . ? N17 Mn1 N6 79.29(6) . . ? C18 Mn1 N3 88.57(6) . . ? C20 Mn1 N3 93.81(7) . . ? C22 Mn1 N3 177.44(7) . . ? N17 Mn1 N3 84.96(5) . . ? N6 Mn1 N3 86.44(5) . . ? C2 N3 C4 105.82(14) . . ? C2 N3 Mn1 127.94(12) . . ? C4 N3 Mn1 126.19(11) . . ? N3 C2 N1 110.86(15) . . ? N3 C2 H2 126.6(13) . . ? N1 C2 H2 122.5(13) . . ? C2 N1 C5 107.72(13) . . ? C2 N1 C31 125.21(14) . . ? C5 N1 C31 127.07(14) . . ? C4 C5 N1 105.07(14) . . ? C4 C5 C6 130.13(16) . . ? N1 C5 C6 124.69(15) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C4 N3 110.53(15) . . ? C5 C4 H4 127.8(11) . . ? N3 C4 H4 121.6(11) . . ? C7 N6 C11 118.08(15) . . ? C7 N6 Mn1 126.42(12) . . ? C11 N6 Mn1 115.51(11) . . ? N6 C7 C8 122.61(16) . . ? N6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C7 C8 C9 119.27(16) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 118.92(16) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 118.96(16) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? N6 C11 C10 122.08(15) . . ? N6 C11 C12 114.30(15) . . ? C10 C11 C12 123.62(15) . . ? N17 C12 C13 121.89(16) . . ? N17 C12 C11 114.82(14) . . ? C13 C12 C11 123.29(15) . . ? C14 C13 C12 119.18(16) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 118.88(16) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.15(16) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? N17 C16 C15 122.44(16) . . ? N17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 N17 C12 118.30(15) . . ? C16 N17 Mn1 126.16(12) . . ? C12 N17 Mn1 114.88(11) . . ? O19 C18 Mn1 176.04(14) . . ? O21 C20 Mn1 174.61(15) . . ? O23 C22 Mn1 176.73(15) . . ? C32 C31 C36 121.03(15) . . ? C32 C31 N1 119.69(15) . . ? C36 C31 N1 119.28(15) . . ? C31 C32 C33 119.35(16) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C32 C33 C34 120.22(16) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.78(16) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C34 120.58(16) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 119.00(16) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.5 . . ? O27 Cl24 O28 110.06(9) . . ? O27 Cl24 O26 109.64(9) . . ? O28 Cl24 O26 109.29(10) . . ? O27 Cl24 O25 109.34(9) . . ? O28 Cl24 O25 108.30(8) . . ? O26 Cl24 O25 110.19(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 Mn1 N3 C2 -130.49(15) . . . . ? C20 Mn1 N3 C2 -43.07(15) . . . . ? N17 Mn1 N3 C2 133.54(15) . . . . ? N6 Mn1 N3 C2 54.00(14) . . . . ? C18 Mn1 N3 C4 46.68(14) . . . . ? C20 Mn1 N3 C4 134.10(14) . . . . ? N17 Mn1 N3 C4 -49.29(14) . . . . ? N6 Mn1 N3 C4 -128.83(14) . . . . ? C4 N3 C2 N1 0.54(18) . . . . ? Mn1 N3 C2 N1 178.17(10) . . . . ? N3 C2 N1 C5 -0.71(19) . . . . ? N3 C2 N1 C31 179.19(14) . . . . ? C2 N1 C5 C4 0.56(18) . . . . ? C31 N1 C5 C4 -179.34(15) . . . . ? C2 N1 C5 C6 -175.95(16) . . . . ? C31 N1 C5 C6 4.2(3) . . . . ? N1 C5 C4 N3 -0.24(19) . . . . ? C6 C5 C4 N3 176.00(16) . . . . ? C2 N3 C4 C5 -0.18(19) . . . . ? Mn1 N3 C4 C5 -177.86(11) . . . . ? C20 Mn1 N6 C7 -4.20(14) . . . . ? C22 Mn1 N6 C7 83.81(14) . . . . ? N17 Mn1 N6 C7 176.87(14) . . . . ? N3 Mn1 N6 C7 -97.59(13) . . . . ? C20 Mn1 N6 C11 176.30(12) . . . . ? C22 Mn1 N6 C11 -95.68(12) . . . . ? N17 Mn1 N6 C11 -2.63(11) . . . . ? N3 Mn1 N6 C11 82.91(11) . . . . ? C11 N6 C7 C8 1.5(2) . . . . ? Mn1 N6 C7 C8 -177.98(12) . . . . ? N6 C7 C8 C9 1.2(3) . . . . ? C7 C8 C9 C10 -2.2(3) . . . . ? C8 C9 C10 C11 0.5(2) . . . . ? C7 N6 C11 C10 -3.2(2) . . . . ? Mn1 N6 C11 C10 176.32(12) . . . . ? C7 N6 C11 C12 177.37(14) . . . . ? Mn1 N6 C11 C12 -3.09(17) . . . . ? C9 C10 C11 N6 2.2(2) . . . . ? C9 C10 C11 C12 -178.42(15) . . . . ? N6 C11 C12 N17 10.3(2) . . . . ? C10 C11 C12 N17 -169.10(15) . . . . ? N6 C11 C12 C13 -169.09(15) . . . . ? C10 C11 C12 C13 11.5(2) . . . . ? N17 C12 C13 C14 1.6(2) . . . . ? C11 C12 C13 C14 -179.03(15) . . . . ? C12 C13 C14 C15 1.8(2) . . . . ? C13 C14 C15 C16 -2.4(3) . . . . ? C14 C15 C16 N17 -0.5(3) . . . . ? C15 C16 N17 C12 3.8(2) . . . . ? C15 C16 N17 Mn1 -166.36(13) . . . . ? C13 C12 N17 C16 -4.4(2) . . . . ? C11 C12 N17 C16 176.22(14) . . . . ? C13 C12 N17 Mn1 166.88(12) . . . . ? C11 C12 N17 Mn1 -12.52(17) . . . . ? C18 Mn1 N17 C16 3.54(14) . . . . ? C22 Mn1 N17 C16 -90.27(14) . . . . ? N6 Mn1 N17 C16 178.90(14) . . . . ? N3 Mn1 N17 C16 91.58(13) . . . . ? C18 Mn1 N17 C12 -166.92(12) . . . . ? C22 Mn1 N17 C12 99.26(12) . . . . ? N6 Mn1 N17 C12 8.43(11) . . . . ? N3 Mn1 N17 C12 -78.89(11) . . . . ? C2 N1 C31 C32 46.6(2) . . . . ? C5 N1 C31 C32 -133.49(17) . . . . ? C2 N1 C31 C36 -133.10(17) . . . . ? C5 N1 C31 C36 46.8(2) . . . . ? C36 C31 C32 C33 -1.0(3) . . . . ? N1 C31 C32 C33 179.31(15) . . . . ? C31 C32 C33 C34 -0.5(3) . . . . ? C32 C33 C34 C35 1.1(3) . . . . ? C33 C34 C35 C36 -0.3(3) . . . . ? C34 C35 C36 C31 -1.1(3) . . . . ? C32 C31 C36 C35 1.8(3) . . . . ? N1 C31 C36 C35 -178.50(15) . . . . ?