# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_contact_author_name 'Veronica Gomez' _publ_contact_author_address ;Department de Quimica Inorganica, Facultat de Quimica Universitat de Barcelona C/ Marti i Franques 1-11 08028 Barcelona, Spain ; _publ_contact_author_email veronica.gomez@qi.ub.es loop_ _publ_author_name _publ_author_address 'Gomez, Veronica' ;Department de Quimica Inorganica, Facultat de Quimica Universitat de Barcelona C/ Marti i Franques 1-11 08028 Barcelona, Spain ; 'Corbella, Montserrat' ;Department de Quimica Inorganica, Facultat de Quimica Universitat de Barcelona C/ Marti i Franques 1-11 08028 Barcelona, Spain ; 'Roubeau, Olivier' ;Instituto de Ciencia de Materiales de Aragon CSIC and Universidad de Zaragoza Plaza San Francisco s/n, 50009, Zaragoza, Spain ; 'Teat, Simon J.' ;Advanced Light Source, Berkeley Laboratory 1 Cyclotron Road, Berkeley, CA 94720, USA ; _publ_section_title ; 'Magneto-structural correlations in dinuclear Mn(III) compounds with general formula [{Mn(L)(NN)}(m-O)(m-RC6H4COO)2{Mn(L')(NN)}]n+ ; _publ_requested_category FM # Attachment '- compounds1-3.cif' #TrackingRef '- compounds1-3.cif' #-------------------------------------- # Compound 1 #-------------------------------------- data_compound1 _database_code_depnum_ccdc_archive 'CCDC 832169' #TrackingRef '- compounds1-3.cif' _audit_creation_date 2008-11-21T10:52:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H26 Cl2 Mn2 N5 O9, 2(C2 H3 N), N O3 ' _chemical_formula_sum 'C38 H32 Cl2 Mn2 N8 O12' _chemical_formula_weight 973.50 _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_ _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 17.6780(15) _cell_length_b 24.196(2) _cell_length_c 10.2260(9) _cell_angle_alpha 90 _cell_angle_beta 104.927(3) _cell_angle_gamma 90 _cell_volume 4226.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1979 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 23.09 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.998 #----------------------------------------------------------------------------# # 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_monochromator 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 0.0727 _diffrn_reflns_av_unetI/netI 0.1021 _diffrn_reflns_number 27989 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 8617 _reflns_number_gt 5206 _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^)+(0.0332P)^2^+9.0428P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8617 _refine_ls_number_parameters 561 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.366 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.104 #----------------------------------------------------------------------------# # 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' 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' 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 0.84661(4) 0.04976(2) 0.19598(6) 0.01302(15) Uani 1 1 d . . . Mn2 Mn 0.69052(4) 0.10871(3) 0.04408(7) 0.01389(16) Uani 1 1 d . . . N1 N 0.95893(19) 0.01879(13) 0.2300(3) 0.0129(8) Uani 1 1 d . . . C2 C 0.9815(2) -0.01815(16) 0.1497(4) 0.0156(9) Uani 1 1 d . . . H2 H 0.9438 -0.0322 0.0733 0.019 Uiso 1 1 calc R . . C3 C 1.0577(3) -0.03632(17) 0.1748(5) 0.0209(10) Uani 1 1 d . . . H3 H 1.0724 -0.0625 0.1167 0.025 Uiso 1 1 calc R . . C4 C 1.1123(3) -0.01578(17) 0.2859(4) 0.0192(10) Uani 1 1 d . . . H4 H 1.1652 -0.0279 0.3051 0.023 Uiso 1 1 calc R . . C5 C 1.0899(2) 0.02260(17) 0.3692(4) 0.0172(10) Uani 1 1 d . . . H5 H 1.1270 0.0372 0.4457 0.021 Uiso 1 1 calc R . . C6 C 1.0128(2) 0.03918(16) 0.3390(4) 0.0144(9) Uani 1 1 d . . . C7 C 0.9806(2) 0.07771(16) 0.4236(4) 0.0143(9) Uani 1 1 d . . . C8 C 1.0246(3) 0.10390(17) 0.5381(4) 0.0200(10) Uani 1 1 d . . . H8 H 1.0798 0.0988 0.5657 0.024 Uiso 1 1 calc R . . C9 C 0.9879(3) 0.13748(18) 0.6119(4) 0.0225(11) Uani 1 1 d . . . H9 H 1.0175 0.1559 0.6905 0.027 Uiso 1 1 calc R . . C10 C 0.9077(3) 0.14393(18) 0.5703(4) 0.0211(10) Uani 1 1 d . . . H10 H 0.8814 0.1664 0.6208 0.025 Uiso 1 1 calc R . . C11 C 0.8660(3) 0.11737(17) 0.4544(4) 0.0177(10) Uani 1 1 d . . . H11 H 0.8108 0.1217 0.4258 0.021 Uiso 1 1 calc R . . N12 N 0.9023(2) 0.08540(13) 0.3815(3) 0.0155(8) Uani 1 1 d . . . N13 N 0.5959(2) 0.07627(13) 0.1035(4) 0.0151(8) Uani 1 1 d . . . C14 C 0.6029(2) 0.05100(17) 0.2220(4) 0.0168(9) Uani 1 1 d . . . H14 H 0.6531 0.0478 0.2835 0.020 Uiso 1 1 calc R . . C15 C 0.5380(3) 0.02925(17) 0.2571(5) 0.0205(10) Uani 1 1 d . . . H15 H 0.5435 0.0115 0.3419 0.025 Uiso 1 1 calc R . . C16 C 0.4653(3) 0.03390(17) 0.1662(5) 0.0217(11) Uani 1 1 d . . . H16 H 0.4203 0.0187 0.1870 0.026 Uiso 1 1 calc R . . C17 C 0.4589(3) 0.06103(17) 0.0443(5) 0.0197(10) Uani 1 1 d . . . H17 H 0.4092 0.0651 -0.0184 0.024 Uiso 1 1 calc R . . C18 C 0.5249(2) 0.08210(16) 0.0148(4) 0.0143(9) Uani 1 1 d . . . C19 C 0.5261(2) 0.11116(17) -0.1122(4) 0.0161(9) Uani 1 1 d . . . C20 C 0.4599(3) 0.12054(17) -0.2160(5) 0.0206(10) Uani 1 1 d . . . H20 H 0.4098 0.1086 -0.2096 0.025 Uiso 1 1 calc R . . C21 C 0.4689(3) 0.14791(18) -0.3296(5) 0.0229(11) Uani 1 1 d . . . H21 H 0.4244 0.1553 -0.4023 0.028 Uiso 1 1 calc R . . C22 C 0.5419(3) 0.16452(18) -0.3383(5) 0.0215(10) Uani 1 1 d . . . H22 H 0.5483 0.1832 -0.4165 0.026 Uiso 1 1 calc R . . C23 C 0.6056(3) 0.15351(17) -0.2315(4) 0.0179(10) Uani 1 1 d . . . H23 H 0.6562 0.1645 -0.2376 0.022 Uiso 1 1 calc R . . N24 N 0.59837(19) 0.12780(13) -0.1194(3) 0.0147(8) Uani 1 1 d . . . O25 O 0.69370(16) 0.03543(11) -0.0746(3) 0.0168(7) Uani 1 1 d . . . O26 O 0.81677(16) 0.00826(11) 0.0232(3) 0.0180(7) Uani 1 1 d . . . C27 C 0.7509(2) 0.00395(17) -0.0625(4) 0.0160(9) Uani 1 1 d . . . C28 C 0.7419(2) -0.04515(17) -0.1554(5) 0.0177(10) Uani 1 1 d . . . C29 C 0.7723(3) -0.09559(18) -0.0999(5) 0.0267(11) Uani 1 1 d . . . H29 H 0.7993 -0.0976 -0.0068 0.032 Uiso 1 1 calc R . . C30 C 0.7634(3) -0.1429(2) -0.1788(6) 0.0395(14) Uani 1 1 d . . . H30 H 0.7839 -0.1772 -0.1396 0.047 Uiso 1 1 calc R . . C31 C 0.7249(3) -0.1401(2) -0.3142(6) 0.0435(15) Uani 1 1 d . . . H31 H 0.7185 -0.1726 -0.3683 0.052 Uiso 1 1 calc R . . C32 C 0.6955(3) -0.0902(2) -0.3717(5) 0.0355(13) Uani 1 1 d . . . H32 H 0.6695 -0.0883 -0.4653 0.043 Uiso 1 1 calc R . . C33 C 0.7038(3) -0.04334(19) -0.2932(5) 0.0227(11) Uani 1 1 d . . . Cl34 Cl 0.66909(7) 0.01880(5) -0.37396(12) 0.0297(3) Uani 1 1 d . . . O35 O 0.76837(16) 0.14590(11) -0.0338(3) 0.0173(7) Uani 1 1 d . . . O36 O 0.88480(15) 0.11636(11) 0.0900(3) 0.0149(6) Uani 1 1 d . . . C37 C 0.8427(2) 0.14727(16) 0.0031(4) 0.0134(9) Uani 1 1 d . . . C38 C 0.8814(2) 0.19056(16) -0.0637(4) 0.0116(9) Uani 1 1 d . . . C39 C 0.8321(2) 0.22876(16) -0.1472(4) 0.0155(9) Uani 1 1 d . . . H39 H 0.7771 0.2264 -0.1585 0.019 Uiso 1 1 calc R . . C40 C 0.8621(3) 0.27015(17) -0.2139(4) 0.0184(10) Uani 1 1 d . . . H40 H 0.8278 0.2959 -0.2696 0.022 Uiso 1 1 calc R . . C41 C 0.9418(3) 0.27375(17) -0.1992(4) 0.0199(10) Uani 1 1 d . . . H41 H 0.9621 0.3020 -0.2451 0.024 Uiso 1 1 calc R . . C42 C 0.9923(3) 0.23648(17) -0.1178(4) 0.0177(10) Uani 1 1 d . . . H42 H 1.0471 0.2391 -0.1073 0.021 Uiso 1 1 calc R . . C43 C 0.9616(2) 0.19501(16) -0.0515(4) 0.0146(9) Uani 1 1 d . . . Cl44 Cl 1.03155(6) 0.15015(4) 0.04621(12) 0.0219(3) Uani 1 1 d . . . N1W N 0.1811(4) 0.2124(3) -0.1501(8) 0.100(3) Uani 1 1 d . . . C2W C 0.2185(4) 0.2097(3) -0.2242(8) 0.062(2) Uani 1 1 d . . . C3W C 0.2707(4) 0.2077(2) -0.3133(7) 0.062(2) Uani 1 1 d . . . H3W1 H 0.3210 0.2246 -0.2679 0.093 Uiso 1 1 calc R . . H3W2 H 0.2472 0.2280 -0.3968 0.093 Uiso 1 1 calc R . . H3W3 H 0.2792 0.1692 -0.3353 0.093 Uiso 1 1 calc R . . N5W N 0.4090(3) 0.2271(2) -0.0072(6) 0.0571(15) Uani 1 1 d . . . C6W C 0.4350(3) 0.2109(2) 0.0983(7) 0.0369(14) Uani 1 1 d . . . C7W C 0.4680(3) 0.1908(2) 0.2357(6) 0.0463(15) Uani 1 1 d . . . H7W1 H 0.4612 0.2188 0.3008 0.069 Uiso 1 1 calc R . . H7W2 H 0.5240 0.1832 0.2489 0.069 Uiso 1 1 calc R . . H7W3 H 0.4411 0.1567 0.2498 0.069 Uiso 1 1 calc R . . O7W O 0.6489(2) 0.22979(16) 0.3953(6) 0.0793(17) Uani 1 1 d . . . O8W O 0.6756(2) 0.14616(17) 0.4131(5) 0.0737(16) Uani 1 1 d . . . O9W O 0.7117(3) 0.1979(2) 0.5852(4) 0.0694(15) Uani 1 1 d . . . N10W N 0.6790(2) 0.19057(16) 0.4655(4) 0.0229(9) Uani 1 1 d . . . N11W N 0.7624(2) -0.05160(14) 0.2825(4) 0.0213(9) Uani 1 1 d . . . O12W O 0.7123(2) -0.04958(16) 0.1758(4) 0.0486(8) Uani 1 1 d . . . O13W O 0.7538(2) -0.08031(16) 0.3770(4) 0.0486(8) Uani 1 1 d . . . O14W O 0.82629(16) -0.02441(12) 0.3039(3) 0.0229(7) Uani 1 1 d . . . O15W O 0.75683(15) 0.08354(11) 0.1951(3) 0.0157(6) Uani 1 1 d . . . O16W O 0.66245(18) 0.18672(11) 0.1250(3) 0.0221(7) Uani 1 1 d D . . H16A H 0.659(3) 0.1897(18) 0.2060(15) 0.026 Uiso 1 1 d D . . H16B H 0.673(3) 0.2159(10) 0.087(4) 0.026 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0108(3) 0.0138(3) 0.0122(3) 0.0014(3) -0.0012(3) 0.0000(3) Mn2 0.0102(3) 0.0161(3) 0.0137(4) 0.0023(3) 0.0000(3) -0.0005(3) N1 0.0143(18) 0.0091(17) 0.0148(19) 0.0038(15) 0.0026(15) 0.0037(14) C2 0.019(2) 0.013(2) 0.013(2) 0.0011(18) 0.0011(19) -0.0021(18) C3 0.021(2) 0.021(2) 0.023(3) -0.001(2) 0.008(2) 0.0006(19) C4 0.015(2) 0.021(2) 0.022(3) 0.005(2) 0.005(2) 0.0040(19) C5 0.016(2) 0.018(2) 0.015(2) 0.0042(19) -0.0008(19) -0.0010(18) C6 0.016(2) 0.016(2) 0.011(2) 0.0062(18) 0.0017(18) -0.0024(17) C7 0.015(2) 0.012(2) 0.015(2) 0.0045(18) 0.0032(19) 0.0008(17) C8 0.015(2) 0.023(2) 0.020(3) 0.000(2) 0.0002(19) 0.0001(19) C9 0.032(3) 0.020(2) 0.011(2) -0.0022(19) -0.003(2) 0.001(2) C10 0.030(3) 0.021(2) 0.013(2) -0.0006(19) 0.006(2) 0.004(2) C11 0.018(2) 0.020(2) 0.016(2) 0.0055(19) 0.0044(19) 0.0040(19) N12 0.020(2) 0.0116(17) 0.014(2) 0.0022(15) 0.0026(16) -0.0014(15) N13 0.0156(19) 0.0112(17) 0.018(2) -0.0016(15) 0.0027(16) -0.0014(14) C14 0.017(2) 0.018(2) 0.015(2) -0.0005(19) 0.0039(19) 0.0006(19) C15 0.022(3) 0.019(2) 0.021(3) -0.004(2) 0.007(2) -0.0030(19) C16 0.017(2) 0.021(2) 0.031(3) -0.003(2) 0.012(2) -0.0033(19) C17 0.015(2) 0.019(2) 0.025(3) -0.001(2) 0.004(2) 0.0034(18) C18 0.008(2) 0.014(2) 0.019(2) 0.0004(18) -0.0008(18) 0.0020(17) C19 0.010(2) 0.013(2) 0.022(2) -0.0033(19) -0.0024(18) 0.0010(17) C20 0.016(2) 0.018(2) 0.024(3) -0.001(2) 0.000(2) -0.0008(18) C21 0.016(2) 0.024(2) 0.022(3) 0.003(2) -0.007(2) 0.0006(19) C22 0.023(3) 0.024(2) 0.016(2) 0.001(2) 0.002(2) 0.003(2) C23 0.018(2) 0.019(2) 0.015(2) -0.0005(19) 0.0009(19) 0.0025(19) N24 0.0141(19) 0.0138(18) 0.014(2) 0.0017(15) 0.0004(16) 0.0028(15) O25 0.0122(15) 0.0188(16) 0.0172(17) -0.0001(13) -0.0004(13) 0.0012(12) O26 0.0148(16) 0.0173(15) 0.0178(17) -0.0039(13) -0.0036(13) -0.0009(12) C27 0.015(2) 0.019(2) 0.013(2) 0.0004(19) 0.0022(19) -0.0036(19) C28 0.012(2) 0.016(2) 0.025(3) -0.003(2) 0.0033(19) -0.0018(18) C29 0.020(3) 0.023(3) 0.030(3) -0.007(2) -0.005(2) 0.001(2) C30 0.035(3) 0.024(3) 0.051(4) -0.011(3) -0.005(3) 0.003(2) C31 0.045(4) 0.032(3) 0.051(4) -0.023(3) 0.007(3) 0.001(3) C32 0.028(3) 0.047(3) 0.028(3) -0.020(3) 0.000(2) -0.003(2) C33 0.016(2) 0.026(2) 0.021(3) -0.006(2) -0.004(2) -0.003(2) Cl34 0.0265(7) 0.0395(7) 0.0187(6) 0.0033(5) -0.0018(5) 0.0006(5) O35 0.0127(16) 0.0200(15) 0.0169(17) 0.0043(13) -0.0002(13) -0.0011(12) O36 0.0130(15) 0.0123(14) 0.0196(17) 0.0037(12) 0.0041(13) 0.0022(12) C37 0.016(2) 0.011(2) 0.013(2) -0.0056(17) 0.0028(19) -0.0007(17) C38 0.017(2) 0.011(2) 0.007(2) -0.0016(17) 0.0024(18) -0.0024(17) C39 0.016(2) 0.016(2) 0.014(2) -0.0016(18) 0.0028(19) -0.0001(18) C40 0.024(2) 0.016(2) 0.014(2) 0.0010(19) 0.002(2) 0.0024(19) C41 0.029(3) 0.016(2) 0.018(3) -0.0015(19) 0.010(2) -0.006(2) C42 0.018(2) 0.023(2) 0.014(2) -0.0067(19) 0.007(2) -0.0046(19) C43 0.016(2) 0.013(2) 0.015(2) -0.0013(18) 0.0052(19) 0.0029(18) Cl44 0.0141(5) 0.0219(6) 0.0290(7) 0.0050(5) 0.0044(5) 0.0036(4) N1W 0.072(5) 0.133(6) 0.115(6) 0.052(5) 0.058(5) 0.033(4) C2W 0.049(4) 0.058(4) 0.091(6) 0.027(4) 0.036(4) 0.016(3) C3W 0.071(5) 0.049(4) 0.082(5) 0.010(4) 0.047(4) 0.015(3) N5W 0.075(4) 0.047(3) 0.048(4) -0.006(3) 0.014(3) -0.012(3) C6W 0.037(3) 0.029(3) 0.048(4) -0.020(3) 0.017(3) -0.008(3) C7W 0.040(3) 0.044(3) 0.055(4) -0.010(3) 0.012(3) 0.001(3) O7W 0.044(3) 0.032(2) 0.132(5) 0.030(3) -0.030(3) -0.004(2) O8W 0.056(3) 0.044(3) 0.101(4) -0.048(3) -0.016(3) 0.016(2) O9W 0.072(3) 0.117(4) 0.017(2) -0.013(2) 0.007(2) -0.052(3) N10W 0.023(2) 0.026(2) 0.021(2) 0.0019(19) 0.0080(18) -0.0059(18) N11W 0.030(2) 0.0144(18) 0.021(2) 0.0039(17) 0.0082(18) -0.0023(17) O12W 0.0428(17) 0.0649(19) 0.0299(16) 0.0150(14) -0.0056(13) -0.0276(15) O13W 0.0428(17) 0.0649(19) 0.0299(16) 0.0150(14) -0.0056(13) -0.0276(15) O14W 0.0110(16) 0.0250(17) 0.0281(19) 0.0101(15) -0.0036(14) -0.0052(13) O15W 0.0098(15) 0.0229(16) 0.0130(16) 0.0018(13) 0.0003(12) 0.0012(12) O16W 0.0334(19) 0.0203(17) 0.0136(17) 0.0006(14) 0.0081(15) 0.0008(14) _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 O15W 1.783(3) . ? Mn1 O26 1.982(3) . ? Mn1 N1 2.066(3) . ? Mn1 N12 2.086(3) . ? Mn1 O36 2.145(3) . ? Mn1 O14W 2.184(3) . ? Mn1 Mn2 3.1390(9) . ? Mn2 O15W 1.788(3) . ? Mn2 O35 1.976(3) . ? Mn2 N24 2.063(3) . ? Mn2 N13 2.075(3) . ? Mn2 O25 2.158(3) . ? Mn2 O16W 2.169(3) . ? N1 C2 1.342(5) . ? N1 C6 1.359(5) . ? C2 C3 1.376(6) . ? C2 H2 0.9500 . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 C7 1.482(6) . ? C7 N12 1.352(5) . ? C7 C8 1.381(6) . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 C10 1.380(6) . ? C9 H9 0.9500 . ? C10 C11 1.382(6) . ? C10 H10 0.9500 . ? C11 N12 1.347(5) . ? C11 H11 0.9500 . ? N13 C14 1.334(5) . ? N13 C18 1.353(5) . ? C14 C15 1.390(6) . ? C14 H14 0.9500 . ? C15 C16 1.384(6) . ? C15 H15 0.9500 . ? C16 C17 1.387(6) . ? C16 H16 0.9500 . ? C17 C18 1.376(6) . ? C17 H17 0.9500 . ? C18 C19 1.482(6) . ? C19 N24 1.359(5) . ? C19 C20 1.382(6) . ? C20 C21 1.381(6) . ? C20 H20 0.9500 . ? C21 C22 1.377(6) . ? C21 H21 0.9500 . ? C22 C23 1.378(6) . ? C22 H22 0.9500 . ? C23 N24 1.340(5) . ? C23 H23 0.9500 . ? O25 C27 1.246(5) . ? O26 C27 1.269(5) . ? C27 C28 1.504(6) . ? C28 C29 1.393(6) . ? C28 C33 1.397(6) . ? C29 C30 1.386(6) . ? C29 H29 0.9500 . ? C30 C31 1.379(7) . ? C30 H30 0.9500 . ? C31 C32 1.385(7) . ? C31 H31 0.9500 . ? C32 C33 1.374(6) . ? C32 H32 0.9500 . ? C33 Cl34 1.749(5) . ? O35 C37 1.270(5) . ? O36 C37 1.250(5) . ? C37 C38 1.507(5) . ? C38 C43 1.395(5) . ? C38 C39 1.400(5) . ? C39 C40 1.392(6) . ? C39 H39 0.9500 . ? C40 C41 1.380(6) . ? C40 H40 0.9500 . ? C41 C42 1.385(6) . ? C41 H41 0.9500 . ? C42 C43 1.397(6) . ? C42 H42 0.9500 . ? C43 Cl44 1.752(4) . ? N1W C2W 1.128(8) . ? C2W C3W 1.456(8) . ? C3W H3W1 0.9800 . ? C3W H3W2 0.9800 . ? C3W H3W3 0.9800 . ? N5W C6W 1.129(7) . ? C6W C7W 1.459(8) . ? C7W H7W1 0.9800 . ? C7W H7W2 0.9800 . ? C7W H7W3 0.9800 . ? O7W N10W 1.225(5) . ? O8W N10W 1.195(5) . ? O9W N10W 1.225(5) . ? N11W O12W 1.217(5) . ? N11W O13W 1.230(5) . ? N11W O14W 1.277(4) . ? O16W H16A 0.85(2) . ? O16W H16B 0.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O15W Mn1 O26 101.28(12) . . ? O15W Mn1 N1 169.28(14) . . ? O26 Mn1 N1 89.43(13) . . ? O15W Mn1 N12 91.50(13) . . ? O26 Mn1 N12 167.22(13) . . ? N1 Mn1 N12 77.80(13) . . ? O15W Mn1 O36 92.78(11) . . ? O26 Mn1 O36 88.65(11) . . ? N1 Mn1 O36 86.78(11) . . ? N12 Mn1 O36 90.72(12) . . ? O15W Mn1 O14W 96.73(12) . . ? O26 Mn1 O14W 89.63(12) . . ? N1 Mn1 O14W 83.85(12) . . ? N12 Mn1 O14W 88.89(12) . . ? O36 Mn1 O14W 170.49(11) . . ? O15W Mn1 Mn2 28.53(9) . . ? O26 Mn1 Mn2 77.93(8) . . ? N1 Mn1 Mn2 158.80(10) . . ? N12 Mn1 Mn2 114.28(10) . . ? O36 Mn1 Mn2 76.09(7) . . ? O14W Mn1 Mn2 112.66(8) . . ? O15W Mn2 O35 97.67(12) . . ? O15W Mn2 N24 168.80(13) . . ? O35 Mn2 N24 93.33(13) . . ? O15W Mn2 N13 90.97(13) . . ? O35 Mn2 N13 171.13(13) . . ? N24 Mn2 N13 78.12(14) . . ? O15W Mn2 O25 95.72(12) . . ? O35 Mn2 O25 91.48(11) . . ? N24 Mn2 O25 81.83(12) . . ? N13 Mn2 O25 89.64(12) . . ? O15W Mn2 O16W 97.50(12) . . ? O35 Mn2 O16W 90.50(11) . . ? N24 Mn2 O16W 84.47(12) . . ? N13 Mn2 O16W 86.37(12) . . ? O25 Mn2 O16W 166.25(11) . . ? O15W Mn2 Mn1 28.44(9) . . ? O35 Mn2 Mn1 77.97(8) . . ? N24 Mn2 Mn1 155.85(10) . . ? N13 Mn2 Mn1 110.82(10) . . ? O25 Mn2 Mn1 75.99(8) . . ? O16W Mn2 Mn1 117.71(9) . . ? C2 N1 C6 119.2(3) . . ? C2 N1 Mn1 124.2(3) . . ? C6 N1 Mn1 116.5(3) . . ? N1 C2 C3 122.0(4) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C2 C3 C4 118.8(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 118.8(4) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N1 C6 C5 121.5(4) . . ? N1 C6 C7 114.4(4) . . ? C5 C6 C7 124.0(4) . . ? N12 C7 C8 121.0(4) . . ? N12 C7 C6 114.6(4) . . ? C8 C7 C6 124.4(4) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 119.4(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N12 C11 C10 121.1(4) . . ? N12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 N12 C7 119.8(4) . . ? C11 N12 Mn1 124.1(3) . . ? C7 N12 Mn1 116.0(3) . . ? C14 N13 C18 120.6(4) . . ? C14 N13 Mn2 123.1(3) . . ? C18 N13 Mn2 116.3(3) . . ? N13 C14 C15 121.2(4) . . ? N13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 118.8(4) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.3(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? N13 C18 C17 120.4(4) . . ? N13 C18 C19 114.6(3) . . ? C17 C18 C19 124.9(4) . . ? N24 C19 C20 122.2(4) . . ? N24 C19 C18 114.4(4) . . ? C20 C19 C18 123.4(4) . . ? C21 C20 C19 117.8(4) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 118.7(4) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? N24 C23 C22 122.0(4) . . ? N24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 N24 C19 118.8(4) . . ? C23 N24 Mn2 124.6(3) . . ? C19 N24 Mn2 116.5(3) . . ? C27 O25 Mn2 125.8(3) . . ? C27 O26 Mn1 130.1(3) . . ? O25 C27 O26 126.5(4) . . ? O25 C27 C28 118.0(4) . . ? O26 C27 C28 115.5(4) . . ? C29 C28 C33 118.2(4) . . ? C29 C28 C27 117.9(4) . . ? C33 C28 C27 123.9(4) . . ? C30 C29 C28 120.9(5) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 119.7(5) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.2(5) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 120.0(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 121.0(4) . . ? C32 C33 Cl34 117.5(4) . . ? C28 C33 Cl34 121.5(3) . . ? C37 O35 Mn2 131.8(3) . . ? C37 O36 Mn1 127.0(3) . . ? O36 C37 O35 125.2(4) . . ? O36 C37 C38 118.7(4) . . ? O35 C37 C38 116.1(4) . . ? C43 C38 C39 117.6(4) . . ? C43 C38 C37 125.7(4) . . ? C39 C38 C37 116.8(4) . . ? C40 C39 C38 121.2(4) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C41 C40 C39 120.0(4) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.4(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C43 119.2(4) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C38 C43 C42 121.7(4) . . ? C38 C43 Cl44 123.7(3) . . ? C42 C43 Cl44 114.6(3) . . ? N1W C2W C3W 176.4(9) . . ? C2W C3W H3W1 109.5 . . ? C2W C3W H3W2 109.5 . . ? H3W1 C3W H3W2 109.5 . . ? C2W C3W H3W3 109.5 . . ? H3W1 C3W H3W3 109.5 . . ? H3W2 C3W H3W3 109.5 . . ? N5W C6W C7W 179.0(7) . . ? C6W C7W H7W1 109.5 . . ? C6W C7W H7W2 109.5 . . ? H7W1 C7W H7W2 109.5 . . ? C6W C7W H7W3 109.5 . . ? H7W1 C7W H7W3 109.5 . . ? H7W2 C7W H7W3 109.5 . . ? O8W N10W O9W 122.3(5) . . ? O8W N10W O7W 118.0(5) . . ? O9W N10W O7W 119.7(5) . . ? O12W N11W O13W 121.2(4) . . ? O12W N11W O14W 122.7(4) . . ? O13W N11W O14W 116.0(4) . . ? N11W O14W Mn1 126.2(3) . . ? Mn1 O15W Mn2 123.03(16) . . ? Mn2 O16W H16A 122(3) . . ? Mn2 O16W H16B 117(3) . . ? H16A O16W H16B 117(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 O26 Mn1 Mn2 O15W 144.3(2) . . . . ? N1 Mn1 Mn2 O15W -161.1(3) . . . . ? N12 Mn1 Mn2 O15W -39.7(2) . . . . ? O36 Mn1 Mn2 O15W -124.1(2) . . . . ? O14W Mn1 Mn2 O15W 59.8(2) . . . . ? O15W Mn1 Mn2 O35 132.8(2) . . . . ? O26 Mn1 Mn2 O35 -82.85(12) . . . . ? N1 Mn1 Mn2 O35 -28.3(3) . . . . ? N12 Mn1 Mn2 O35 93.17(13) . . . . ? O36 Mn1 Mn2 O35 8.77(12) . . . . ? O14W Mn1 Mn2 O35 -167.31(13) . . . . ? O15W Mn1 Mn2 N24 -156.4(3) . . . . ? O26 Mn1 Mn2 N24 -12.1(3) . . . . ? N1 Mn1 Mn2 N24 42.5(4) . . . . ? N12 Mn1 Mn2 N24 163.9(3) . . . . ? O36 Mn1 Mn2 N24 79.5(2) . . . . ? O14W Mn1 Mn2 N24 -96.6(3) . . . . ? O15W Mn1 Mn2 N13 -48.4(2) . . . . ? O26 Mn1 Mn2 N13 95.92(13) . . . . ? N1 Mn1 Mn2 N13 150.5(3) . . . . ? N12 Mn1 Mn2 N13 -88.06(14) . . . . ? O36 Mn1 Mn2 N13 -172.47(13) . . . . ? O14W Mn1 Mn2 N13 11.45(14) . . . . ? O15W Mn1 Mn2 O25 -132.5(2) . . . . ? O26 Mn1 Mn2 O25 11.76(11) . . . . ? N1 Mn1 Mn2 O25 66.4(3) . . . . ? N12 Mn1 Mn2 O25 -172.22(13) . . . . ? O36 Mn1 Mn2 O25 103.38(11) . . . . ? O14W Mn1 Mn2 O25 -72.70(12) . . . . ? O15W Mn1 Mn2 O16W 48.7(2) . . . . ? O26 Mn1 Mn2 O16W -167.00(12) . . . . ? N1 Mn1 Mn2 O16W -112.4(3) . . . . ? N12 Mn1 Mn2 O16W 9.02(14) . . . . ? O36 Mn1 Mn2 O16W -75.39(12) . . . . ? O14W Mn1 Mn2 O16W 108.53(13) . . . . ? O15W Mn1 N1 C2 179.2(6) . . . . ? O26 Mn1 N1 C2 -4.2(3) . . . . ? N12 Mn1 N1 C2 175.7(3) . . . . ? O36 Mn1 N1 C2 -92.9(3) . . . . ? O14W Mn1 N1 C2 85.5(3) . . . . ? Mn2 Mn1 N1 C2 -57.0(4) . . . . ? O15W Mn1 N1 C6 -3.0(9) . . . . ? O26 Mn1 N1 C6 173.6(3) . . . . ? N12 Mn1 N1 C6 -6.5(3) . . . . ? O36 Mn1 N1 C6 85.0(3) . . . . ? O14W Mn1 N1 C6 -96.7(3) . . . . ? Mn2 Mn1 N1 C6 120.8(3) . . . . ? C6 N1 C2 C3 0.4(6) . . . . ? Mn1 N1 C2 C3 178.1(3) . . . . ? N1 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? C2 N1 C6 C5 -0.3(6) . . . . ? Mn1 N1 C6 C5 -178.2(3) . . . . ? C2 N1 C6 C7 -177.4(3) . . . . ? Mn1 N1 C6 C7 4.6(4) . . . . ? C4 C5 C6 N1 -0.1(6) . . . . ? C4 C5 C6 C7 176.8(4) . . . . ? N1 C6 C7 N12 1.8(5) . . . . ? C5 C6 C7 N12 -175.3(4) . . . . ? N1 C6 C7 C8 -179.1(4) . . . . ? C5 C6 C7 C8 3.8(6) . . . . ? N12 C7 C8 C9 1.4(6) . . . . ? C6 C7 C8 C9 -177.7(4) . . . . ? C7 C8 C9 C10 0.4(6) . . . . ? C8 C9 C10 C11 -1.0(7) . . . . ? C9 C10 C11 N12 -0.1(6) . . . . ? C10 C11 N12 C7 1.8(6) . . . . ? C10 C11 N12 Mn1 -173.9(3) . . . . ? C8 C7 N12 C11 -2.5(6) . . . . ? C6 C7 N12 C11 176.7(3) . . . . ? C8 C7 N12 Mn1 173.6(3) . . . . ? C6 C7 N12 Mn1 -7.3(4) . . . . ? O15W Mn1 N12 C11 4.0(3) . . . . ? O26 Mn1 N12 C11 -176.1(5) . . . . ? N1 Mn1 N12 C11 -176.7(3) . . . . ? O36 Mn1 N12 C11 96.8(3) . . . . ? O14W Mn1 N12 C11 -92.7(3) . . . . ? Mn2 Mn1 N12 C11 21.7(3) . . . . ? O15W Mn1 N12 C7 -171.9(3) . . . . ? O26 Mn1 N12 C7 8.0(7) . . . . ? N1 Mn1 N12 C7 7.5(3) . . . . ? O36 Mn1 N12 C7 -79.1(3) . . . . ? O14W Mn1 N12 C7 91.4(3) . . . . ? Mn2 Mn1 N12 C7 -154.1(2) . . . . ? O15W Mn2 N13 C14 3.1(3) . . . . ? N24 Mn2 N13 C14 -179.5(3) . . . . ? O25 Mn2 N13 C14 98.8(3) . . . . ? O16W Mn2 N13 C14 -94.4(3) . . . . ? Mn1 Mn2 N13 C14 23.9(3) . . . . ? O15W Mn2 N13 C18 -177.1(3) . . . . ? N24 Mn2 N13 C18 0.4(3) . . . . ? O25 Mn2 N13 C18 -81.4(3) . . . . ? O16W Mn2 N13 C18 85.5(3) . . . . ? Mn1 Mn2 N13 C18 -156.2(3) . . . . ? C18 N13 C14 C15 1.0(6) . . . . ? Mn2 N13 C14 C15 -179.2(3) . . . . ? N13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C17 -1.4(6) . . . . ? C15 C16 C17 C18 1.0(6) . . . . ? C14 N13 C18 C17 -1.3(6) . . . . ? Mn2 N13 C18 C17 178.8(3) . . . . ? C14 N13 C18 C19 179.8(4) . . . . ? Mn2 N13 C18 C19 -0.1(4) . . . . ? C16 C17 C18 N13 0.3(6) . . . . ? C16 C17 C18 C19 179.1(4) . . . . ? N13 C18 C19 N24 -0.4(5) . . . . ? C17 C18 C19 N24 -179.3(4) . . . . ? N13 C18 C19 C20 179.1(4) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? N24 C19 C20 C21 -0.2(6) . . . . ? C18 C19 C20 C21 -179.7(4) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? C20 C21 C22 C23 -0.3(7) . . . . ? C21 C22 C23 N24 -0.8(7) . . . . ? C22 C23 N24 C19 1.3(6) . . . . ? C22 C23 N24 Mn2 179.1(3) . . . . ? C20 C19 N24 C23 -0.8(6) . . . . ? C18 C19 N24 C23 178.7(3) . . . . ? C20 C19 N24 Mn2 -178.8(3) . . . . ? C18 C19 N24 Mn2 0.7(4) . . . . ? O15W Mn2 N24 C23 -165.2(6) . . . . ? O35 Mn2 N24 C23 3.9(3) . . . . ? N13 Mn2 N24 C23 -178.5(3) . . . . ? O25 Mn2 N24 C23 -87.1(3) . . . . ? O16W Mn2 N24 C23 94.1(3) . . . . ? Mn1 Mn2 N24 C23 -63.7(4) . . . . ? O15W Mn2 N24 C19 12.7(9) . . . . ? O35 Mn2 N24 C19 -178.2(3) . . . . ? N13 Mn2 N24 C19 -0.6(3) . . . . ? O25 Mn2 N24 C19 90.8(3) . . . . ? O16W Mn2 N24 C19 -88.0(3) . . . . ? Mn1 Mn2 N24 C19 114.1(3) . . . . ? O15W Mn2 O25 C27 -31.7(3) . . . . ? O35 Mn2 O25 C27 66.1(3) . . . . ? N24 Mn2 O25 C27 159.3(3) . . . . ? N13 Mn2 O25 C27 -122.7(3) . . . . ? O16W Mn2 O25 C27 164.3(4) . . . . ? Mn1 Mn2 O25 C27 -11.1(3) . . . . ? O15W Mn1 O26 C27 -3.5(4) . . . . ? N1 Mn1 O26 C27 177.2(4) . . . . ? N12 Mn1 O26 C27 176.7(5) . . . . ? O36 Mn1 O26 C27 -96.0(4) . . . . ? O14W Mn1 O26 C27 93.3(4) . . . . ? Mn2 Mn1 O26 C27 -20.0(3) . . . . ? Mn2 O25 C27 O26 1.8(6) . . . . ? Mn2 O25 C27 C28 -179.7(3) . . . . ? Mn1 O26 C27 O25 19.0(6) . . . . ? Mn1 O26 C27 C28 -159.5(3) . . . . ? O25 C27 C28 C29 -137.3(4) . . . . ? O26 C27 C28 C29 41.4(6) . . . . ? O25 C27 C28 C33 41.6(6) . . . . ? O26 C27 C28 C33 -139.8(4) . . . . ? C33 C28 C29 C30 -1.3(7) . . . . ? C27 C28 C29 C30 177.6(4) . . . . ? C28 C29 C30 C31 0.7(8) . . . . ? C29 C30 C31 C32 0.4(8) . . . . ? C30 C31 C32 C33 -0.8(8) . . . . ? C31 C32 C33 C28 0.1(7) . . . . ? C31 C32 C33 Cl34 177.2(4) . . . . ? C29 C28 C33 C32 0.9(7) . . . . ? C27 C28 C33 C32 -177.9(4) . . . . ? C29 C28 C33 Cl34 -176.1(3) . . . . ? C27 C28 C33 Cl34 5.1(6) . . . . ? O15W Mn2 O35 C37 6.2(4) . . . . ? N24 Mn2 O35 C37 -171.6(4) . . . . ? O25 Mn2 O35 C37 -89.7(4) . . . . ? O16W Mn2 O35 C37 103.9(4) . . . . ? Mn1 Mn2 O35 C37 -14.4(3) . . . . ? O15W Mn1 O36 C37 -32.5(3) . . . . ? O26 Mn1 O36 C37 68.7(3) . . . . ? N1 Mn1 O36 C37 158.2(3) . . . . ? N12 Mn1 O36 C37 -124.0(3) . . . . ? Mn2 Mn1 O36 C37 -9.2(3) . . . . ? Mn1 O36 C37 O35 3.2(6) . . . . ? Mn1 O36 C37 C38 -177.7(2) . . . . ? Mn2 O35 C37 O36 12.6(6) . . . . ? Mn2 O35 C37 C38 -166.5(3) . . . . ? O36 C37 C38 C43 9.4(6) . . . . ? O35 C37 C38 C43 -171.5(4) . . . . ? O36 C37 C38 C39 -172.0(4) . . . . ? O35 C37 C38 C39 7.1(5) . . . . ? C43 C38 C39 C40 -0.9(6) . . . . ? C37 C38 C39 C40 -179.6(4) . . . . ? C38 C39 C40 C41 0.5(6) . . . . ? C39 C40 C41 C42 -0.2(6) . . . . ? C40 C41 C42 C43 0.3(6) . . . . ? C39 C38 C43 C42 1.1(6) . . . . ? C37 C38 C43 C42 179.7(4) . . . . ? C39 C38 C43 Cl44 -178.9(3) . . . . ? C37 C38 C43 Cl44 -0.3(6) . . . . ? C41 C42 C43 C38 -0.8(6) . . . . ? C41 C42 C43 Cl44 179.2(3) . . . . ? O12W N11W O14W Mn1 22.2(6) . . . . ? O13W N11W O14W Mn1 -157.7(3) . . . . ? O15W Mn1 O14W N11W 43.5(3) . . . . ? O26 Mn1 O14W N11W -57.8(3) . . . . ? N1 Mn1 O14W N11W -147.2(3) . . . . ? N12 Mn1 O14W N11W 134.9(3) . . . . ? Mn2 Mn1 O14W N11W 19.0(3) . . . . ? O26 Mn1 O15W Mn2 -35.6(2) . . . . ? N1 Mn1 O15W Mn2 141.0(6) . . . . ? N12 Mn1 O15W Mn2 144.40(18) . . . . ? O36 Mn1 O15W Mn2 53.61(18) . . . . ? O14W Mn1 O15W Mn2 -126.54(18) . . . . ? O35 Mn2 O15W Mn1 -46.35(19) . . . . ? N24 Mn2 O15W Mn1 122.6(6) . . . . ? N13 Mn2 O15W Mn1 135.66(19) . . . . ? O25 Mn2 O15W Mn1 45.92(19) . . . . ? O16W Mn2 O15W Mn1 -137.88(17) . . . . ? # 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 #-------------------------------------- # Compound 2 #-------------------------------------- data_compound2 _database_code_depnum_ccdc_archive 'CCDC 832170' #TrackingRef '- compounds1-3.cif' _audit_creation_date 2008-04-15T17:10:48-00:00 _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 ; ? ; loop_ _chemical_formula_moiety 'C68 H48 Cl8 Mn4 N8 O27, C68 H52 Cl6 Mn4 N8 O21, 2(Cl O4),O' _chemical_formula_sum 'C136 H100 Cl16 Mn8 N16 O57' _chemical_formula_weight 3877.04 _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 13.8331(9) _cell_length_b 14.3137(8) _cell_length_c 19.8067(14) _cell_angle_alpha 85.011(4) _cell_angle_beta 80.989(4) _cell_angle_gamma 87.146(4) _cell_volume 3856.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1838 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.11 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.67 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.7915 _exptl_absorpt_correction_T_max 0.9431 #----------------------------------------------------------------------------# # 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_monochromator 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 0.0374 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_number 63281 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.69 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 14536 _reflns_number_gt 11253 _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 'SIR97 (Giacovazzo et al, 1997)' _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^)+(0.0472P)^2^+26.7644P] 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 14536 _refine_ls_number_parameters 1177 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1628 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.836 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # 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' 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' 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 0.22371(6) 0.14885(6) 0.98163(4) 0.0215(2) Uani 1 1 d . B . O1 O 0.3271(3) 0.2079(3) 0.93226(19) 0.0237(9) Uani 1 1 d . B . O2 O 0.2668(4) 0.0122(3) 0.9414(2) 0.0399(11) Uani 1 1 d D . . H2A H 0.278(6) 0.005(5) 0.8997(13) 0.048 Uiso 1 1 d D . . H2B H 0.270(6) -0.043(2) 0.956(4) 0.048 Uiso 1 1 d D . . O3 O 0.1361(3) 0.1662(3) 0.91204(19) 0.0245(9) Uani 1 1 d . B . O4 O 0.1858(3) 0.3035(3) 0.8561(2) 0.0245(9) Uani 1 1 d . B . Mn2 Mn 0.31941(6) 0.32631(6) 0.89672(4) 0.01947(19) Uani 1 1 d . . . C1 C 0.1360(4) 0.2312(4) 0.8641(3) 0.0229(12) Uani 1 1 d . . . C2 C 0.0698(4) 0.2193(4) 0.8123(3) 0.0237(12) Uani 1 1 d . A . C3 C 0.1043(5) 0.2209(4) 0.7423(3) 0.0314(14) Uani 1 1 d . . . Cl1 Cl 0.22416(15) 0.22203(16) 0.70900(10) 0.0353(7) Uani 0.765(6) 1 d P A 1 H3 H 0.171 0.2273 0.7266 0.042 Uiso 0.235(6) 1 d P A 2 C4 C 0.0403(7) 0.2128(5) 0.6952(4) 0.046(2) Uani 1 1 d . A . H4 H 0.065 0.2123 0.6477 0.055 Uiso 1 1 calc R . . C5 C -0.0574(7) 0.2058(5) 0.7173(4) 0.052(2) Uani 1 1 d . . . H5 H -0.1009 0.202 0.6851 0.062 Uiso 1 1 calc R A . C6 C -0.0936(6) 0.2040(5) 0.7865(4) 0.049(2) Uani 1 1 d . A . H6 H -0.1619 0.1988 0.8018 0.058 Uiso 1 1 calc R . . C7 C -0.0301(5) 0.2096(5) 0.8332(4) 0.0348(15) Uani 1 1 d . . . H7 H -0.049(8) 0.213(7) 0.877(6) 0.042 Uiso 0.765(6) 1 d P A 1 Cl1B Cl -0.0909(5) 0.1884(5) 0.9079(3) 0.030(2) Uani 0.235(6) 1 d P A 2 O5 O 0.1561(3) 0.2711(3) 1.02880(19) 0.0242(9) Uani 1 1 d . . . O6 O 0.2519(3) 0.3859(3) 0.97563(19) 0.0251(9) Uani 1 1 d . B . C8 C 0.1794(4) 0.3535(4) 1.0192(3) 0.0224(12) Uani 1 1 d . B . C9 C 0.1234(4) 0.4255(4) 1.0618(3) 0.0217(12) Uani 1 1 d . . . C10 C 0.0215(4) 0.4288(4) 1.0771(3) 0.0254(13) Uani 1 1 d . B . Cl2 Cl -0.05008(11) 0.35501(11) 1.04225(8) 0.0307(3) Uani 1 1 d . . . C11 C -0.0267(5) 0.4948(4) 1.1198(3) 0.0302(14) Uani 1 1 d . . . H11 H -0.0962 0.4972 1.1297 0.036 Uiso 1 1 calc R B . C12 C 0.0268(5) 0.5563(4) 1.1475(3) 0.0341(15) Uani 1 1 d . B . H12 H -0.0062 0.5997 1.1777 0.041 Uiso 1 1 calc R . . C13 C 0.1278(5) 0.5557(5) 1.1319(3) 0.0320(14) Uani 1 1 d . . . H13 H 0.1642 0.5991 1.1505 0.038 Uiso 1 1 calc R B . C14 C 0.1755(4) 0.4911(4) 1.0886(3) 0.0246(13) Uani 1 1 d . B . H14 H 0.2447 0.4914 1.0769 0.03 Uiso 1 1 calc R . . N1 N 0.1168(4) 0.0857(4) 1.0542(2) 0.0268(11) Uani 1 1 d . . . C15 C 0.0228(5) 0.0891(5) 1.0483(3) 0.0342(15) Uani 1 1 d . B . H15 H 0.0033 0.1124 1.0059 0.041 Uiso 1 1 calc R . . C16 C -0.0486(5) 0.0595(5) 1.1027(3) 0.0369(16) Uani 1 1 d . . . H16 H -0.1157 0.0613 1.0973 0.044 Uiso 1 1 calc R B . C17 C -0.0200(5) 0.0276(5) 1.1646(3) 0.0372(16) Uani 1 1 d . B . H17 H -0.0674 0.0072 1.2023 0.045 Uiso 1 1 calc R . . C18 C 0.0782(5) 0.0255(4) 1.1712(3) 0.0323(14) Uani 1 1 d . . . H18 H 0.099 0.0046 1.2137 0.039 Uiso 1 1 calc R B . C19 C 0.1459(5) 0.0544(4) 1.1146(3) 0.0266(13) Uani 1 1 d . B . C20 C 0.2521(5) 0.0570(4) 1.1151(3) 0.0274(13) Uani 1 1 d . . . C21 C 0.2999(5) 0.0159(5) 1.1671(3) 0.0326(14) Uani 1 1 d . B . H21 H 0.264 -0.0153 1.2068 0.039 Uiso 1 1 calc R . . C22 C 0.4005(5) 0.0206(5) 1.1606(3) 0.0358(15) Uani 1 1 d . . . H22 H 0.4341 -0.0063 1.1963 0.043 Uiso 1 1 calc R B . C23 C 0.4521(5) 0.0644(5) 1.1024(3) 0.0343(15) Uani 1 1 d . B . H23 H 0.5214 0.0664 1.0969 0.041 Uiso 1 1 calc R . . C24 C 0.4005(4) 0.1057(4) 1.0517(3) 0.0274(13) Uani 1 1 d . . . H24 H 0.4353 0.1374 1.0118 0.033 Uiso 1 1 calc R B . N2 N 0.3030(3) 0.1013(3) 1.0583(2) 0.0240(10) Uani 1 1 d . B . N3 N 0.3932(3) 0.2950(3) 0.8029(2) 0.0212(10) Uani 1 1 d . B . C25 C 0.4232(4) 0.2083(4) 0.7875(3) 0.0283(14) Uani 1 1 d . . . H25 H 0.4164 0.1587 0.8228 0.034 Uiso 1 1 calc R B . C26 C 0.4641(5) 0.1881(4) 0.7217(3) 0.0302(14) Uani 1 1 d . B . H26 H 0.4851 0.1259 0.7118 0.036 Uiso 1 1 calc R . . C27 C 0.4735(5) 0.2610(5) 0.6707(3) 0.0324(15) Uani 1 1 d . . . H27 H 0.5019 0.2493 0.6253 0.039 Uiso 1 1 calc R B . C28 C 0.4415(4) 0.3514(4) 0.6859(3) 0.0272(13) Uani 1 1 d . B . H28 H 0.4469 0.4017 0.6511 0.033 Uiso 1 1 calc R . . C29 C 0.4015(4) 0.3670(4) 0.7529(3) 0.0222(12) Uani 1 1 d . . . C30 C 0.3653(4) 0.4583(4) 0.7761(3) 0.0196(11) Uani 1 1 d . B . C31 C 0.3709(4) 0.5418(4) 0.7346(3) 0.0261(13) Uani 1 1 d . . . H31 H 0.3981 0.5418 0.6875 0.031 Uiso 1 1 calc R B . C32 C 0.3367(4) 0.6247(4) 0.7622(3) 0.0296(14) Uani 1 1 d . B . H32 H 0.34 0.6821 0.7341 0.035 Uiso 1 1 calc R . . C33 C 0.2973(4) 0.6237(4) 0.8316(3) 0.0286(13) Uani 1 1 d . . . H33 H 0.2734 0.68 0.8515 0.034 Uiso 1 1 calc R B . C34 C 0.2939(4) 0.5390(4) 0.8703(3) 0.0246(12) Uani 1 1 d . B . H34 H 0.2675 0.538 0.9176 0.029 Uiso 1 1 calc R . . N4 N 0.3264(3) 0.4573(3) 0.8439(2) 0.0189(10) Uani 1 1 d . B . O7 O 0.4680(3) 0.3635(4) 0.9257(2) 0.0413(12) Uani 0.5 1 d P B 1 Cl3A Cl 0.6899(2) 0.2382(2) 0.96616(15) 0.0322(7) Uani 0.5 1 d P C 1 O7A O 0.7115(10) 0.3132(9) 1.0068(6) 0.065(3) Uani 0.5 1 d P C 1 O8A O 0.7006(8) 0.2714(8) 0.8958(5) 0.055(3) Uani 0.5 1 d P C 1 O9A O 0.7514(10) 0.1600(8) 0.9789(5) 0.067(4) Uani 0.5 1 d P C 1 O10A O 0.5963(9) 0.2090(11) 0.9879(6) 0.072(4) Uani 0.5 1 d P C 1 Cl3B Cl 0.5529(3) 0.3137(3) 0.94532(18) 0.0465(9) Uani 0.5 1 d P B 2 O7B O 0.4680(3) 0.3635(4) 0.9257(2) 0.0413(12) Uani 0.5 1 d P B 2 O8B O 0.6362(8) 0.3707(10) 0.9337(7) 0.074(4) Uani 0.5 1 d P B 2 O9B O 0.5711(10) 0.2374(8) 0.9006(6) 0.065(3) Uani 0.5 1 d P B 2 O10B O 0.5389(10) 0.2783(7) 1.0132(5) 0.055(3) Uani 0.5 1 d P B 2 Mn3 Mn 0.32403(6) 0.37898(6) 0.38925(4) 0.01980(19) Uani 1 1 d . . . Mn4 Mn 0.25785(6) 0.18193(6) 0.45805(4) 0.01670(19) Uani 1 1 d . E . O11 O 0.3485(3) 0.2566(3) 0.41151(19) 0.0208(8) Uani 1 1 d . E . O12 O 0.1902(3) 0.3531(3) 0.3501(2) 0.0237(9) Uani 1 1 d . E . O13 O 0.1547(3) 0.2101(3) 0.40267(18) 0.0210(8) Uani 1 1 d . . . C35 C 0.1445(4) 0.2793(4) 0.3577(3) 0.0193(12) Uani 1 1 d . E . C36 C 0.0686(4) 0.2663(4) 0.3140(3) 0.0194(11) Uani 1 1 d . . . C37 C 0.0930(4) 0.2631(4) 0.2429(3) 0.0224(12) Uani 1 1 d . D . Cl4 Cl 0.21393(12) 0.26883(13) 0.20384(8) 0.0302(5) Uani 0.907(5) 1 d P D 1 H37 H 0.1582 0.2679 0.2227 0.036 Uiso 0.093(5) 1 d P D 2 C38 C 0.0230(5) 0.2534(4) 0.2023(3) 0.0284(13) Uani 1 1 d . . . H38 H 0.0411 0.2522 0.1541 0.034 Uiso 1 1 calc R E . C39 C -0.0743(5) 0.2455(4) 0.2317(3) 0.0316(14) Uani 1 1 d . E . H39 H -0.123 0.2389 0.2037 0.038 Uiso 1 1 calc R . . C40 C -0.1001(4) 0.2472(4) 0.3023(3) 0.0289(14) Uani 1 1 d . . . H40 H -0.1668 0.2421 0.3225 0.035 Uiso 1 1 calc R E . C41 C -0.0296(4) 0.2564(4) 0.3434(3) 0.0255(13) Uani 1 1 d . D . H41 H -0.043(6) 0.264(5) 0.397(5) 0.031 Uiso 0.907(5) 1 d P D 1 Cl4B Cl -0.0825(12) 0.2476(13) 0.4220(8) 0.029(5) Uani 0.093(5) 1 d P D 2 O14 O 0.2523(3) 0.4146(3) 0.47594(19) 0.0224(8) Uani 1 1 d . E . O15 O 0.1956(3) 0.2799(3) 0.52908(19) 0.0262(9) Uani 1 1 d . . . C42 C 0.1988(4) 0.3665(4) 0.5240(3) 0.0208(12) Uani 1 1 d . E . C43 C 0.1385(4) 0.4195(4) 0.5779(3) 0.0213(12) Uani 1 1 d . . . C44 C 0.0376(4) 0.4182(4) 0.5883(3) 0.0264(13) Uani 1 1 d . E . Cl5 Cl -0.02330(12) 0.36158(14) 0.53367(10) 0.0462(5) Uani 1 1 d . . . C45 C -0.0182(5) 0.4649(4) 0.6404(3) 0.0320(15) Uani 1 1 d . . . H45 H -0.0876 0.4661 0.6456 0.038 Uiso 1 1 calc R E . C46 C 0.0285(5) 0.5095(5) 0.6845(3) 0.0388(17) Uani 1 1 d . E . H46 H -0.0092 0.5393 0.7214 0.047 Uiso 1 1 calc R . . C47 C 0.1291(5) 0.5113(5) 0.6754(4) 0.0401(17) Uani 1 1 d . . . H47 H 0.1607 0.5417 0.7062 0.048 Uiso 1 1 calc R E . N5 N 0.3125(3) 0.5183(3) 0.3504(2) 0.0244(11) Uani 1 1 d . E . C48 C 0.1842(5) 0.4685(4) 0.6211(4) 0.0348(15) Uani 1 1 d . E . H48 H 0.2534 0.4726 0.6133 0.042 Uiso 1 1 calc R . . C49 C 0.2809(4) 0.5898(4) 0.3875(3) 0.0285(13) Uani 1 1 d . . . H49 H 0.2602 0.5777 0.4353 0.034 Uiso 1 1 calc R E . C50 C 0.2771(5) 0.6817(5) 0.3588(4) 0.0357(15) Uani 1 1 d . E . H50 H 0.2549 0.7319 0.3863 0.043 Uiso 1 1 calc R . . C51 C 0.3067(5) 0.6981(5) 0.2889(4) 0.0412(17) Uani 1 1 d . . . H51 H 0.3047 0.7602 0.2678 0.049 Uiso 1 1 calc R E . C52 C 0.3388(5) 0.6246(5) 0.2499(3) 0.0341(15) Uani 1 1 d . E . H52 H 0.3579 0.6355 0.2017 0.041 Uiso 1 1 calc R . . C53 C 0.3431(4) 0.5336(5) 0.2816(3) 0.0286(14) Uani 1 1 d . . . C54 C 0.3816(4) 0.4509(4) 0.2479(3) 0.0282(13) Uani 1 1 d . E . C55 C 0.4115(5) 0.4498(5) 0.1764(3) 0.0382(17) Uani 1 1 d . . . H55 H 0.4052 0.5049 0.1468 0.046 Uiso 1 1 calc R E . C56 C 0.4500(5) 0.3675(6) 0.1506(3) 0.0455(19) Uani 1 1 d . E . H56 H 0.471 0.3661 0.1026 0.055 Uiso 1 1 calc R . . C57 C 0.4587(5) 0.2867(5) 0.1931(3) 0.0389(16) Uani 1 1 d . . . H57 H 0.4856 0.2299 0.1753 0.047 Uiso 1 1 calc R E . C58 C 0.4263(4) 0.2916(5) 0.2635(3) 0.0326(15) Uani 1 1 d . E . H58 H 0.4306 0.2366 0.2935 0.039 Uiso 1 1 calc R . . N6 N 0.3897(3) 0.3706(4) 0.2895(2) 0.0250(11) Uani 1 1 d . E . N7 N 0.1679(3) 0.0927(3) 0.5232(2) 0.0184(9) Uani 1 1 d . . . C59 C 0.0717(4) 0.0937(4) 0.5257(3) 0.0199(11) Uani 1 1 d . E . H59 H 0.0428 0.1315 0.4918 0.024 Uiso 1 1 calc R . . C60 C 0.0116(4) 0.0414(4) 0.5764(3) 0.0237(12) Uani 1 1 d . . . H60 H -0.0574 0.0433 0.5777 0.028 Uiso 1 1 calc R E . C61 C 0.0556(4) -0.0135(4) 0.6250(3) 0.0247(13) Uani 1 1 d . E . H61 H 0.0164 -0.0501 0.6603 0.03 Uiso 1 1 calc R . . C62 C 0.1553(4) -0.0155(4) 0.6228(3) 0.0249(13) Uani 1 1 d . . . H62 H 0.1856 -0.054 0.6556 0.03 Uiso 1 1 calc R E . C63 C 0.2113(4) 0.0405(4) 0.5711(3) 0.0192(11) Uani 1 1 d . E . C64 C 0.3172(4) 0.0506(4) 0.5658(3) 0.0204(12) Uani 1 1 d . . . C65 C 0.3765(4) 0.0006(4) 0.6070(3) 0.0235(12) Uani 1 1 d . E . H65 H 0.35 -0.0468 0.6404 0.028 Uiso 1 1 calc R . . C66 C 0.4747(4) 0.0199(4) 0.5995(3) 0.0233(12) Uani 1 1 d . . . H66 H 0.5161 -0.0141 0.6278 0.028 Uiso 1 1 calc R E . C67 C 0.5121(4) 0.0888(4) 0.5507(3) 0.0217(12) Uani 1 1 d . E . H67 H 0.5791 0.1037 0.5453 0.026 Uiso 1 1 calc R . . C68 C 0.4497(4) 0.1360(4) 0.5095(3) 0.0203(11) Uani 1 1 d . . . H68 H 0.4753 0.1825 0.4751 0.024 Uiso 1 1 calc R E . N8 N 0.3545(3) 0.1176(3) 0.5170(2) 0.0182(9) Uani 1 1 d . E . Cl6 Cl 0.26409(10) -0.01896(10) 0.36319(7) 0.0236(3) Uani 1 1 d . E . O16 O 0.3086(3) 0.0623(3) 0.3825(2) 0.0322(10) Uani 1 1 d . . . O17 O 0.2277(3) -0.0766(3) 0.4252(2) 0.0370(11) Uani 1 1 d . . . O18 O 0.3365(3) -0.0717(3) 0.3204(2) 0.0329(10) Uani 1 1 d . . . O19 O 0.1844(3) 0.0107(3) 0.3270(2) 0.0299(10) Uani 1 1 d . . . O20 O 0.4643(3) 0.4298(3) 0.4169(2) 0.0321(10) Uani 0.5 1 d P E 1 Cl7A Cl 0.6809(2) 0.2837(2) 0.45432(14) 0.0266(6) Uani 0.5 1 d P F 1 O20A O 0.6544(9) 0.3432(8) 0.3975(5) 0.056(3) Uani 0.5 1 d P F 1 O21A O 0.7728(6) 0.3083(8) 0.4686(5) 0.044(2) Uani 0.5 1 d P F 1 O22A O 0.6053(7) 0.2959(7) 0.5122(5) 0.039(2) Uani 0.5 1 d P F 1 O23A O 0.6859(8) 0.1893(7) 0.4386(6) 0.049(3) Uani 0.5 1 d P F 1 Cl7B Cl 0.5309(2) 0.3915(2) 0.45783(14) 0.0253(6) Uani 0.5 1 d P E 2 O20B O 0.4643(3) 0.4298(3) 0.4169(2) 0.0321(10) Uani 0.5 1 d P E 2 O21B O 0.5966(6) 0.4631(6) 0.4655(4) 0.033(2) Uani 0.5 1 d P E 2 O22B O 0.5848(7) 0.3136(7) 0.4246(6) 0.046(3) Uani 0.5 1 d P E 2 O23B O 0.4768(7) 0.3592(7) 0.5221(4) 0.040(2) Uani 0.5 1 d P E 2 Cl8 Cl 0.33408(11) 0.90460(10) 0.78916(7) 0.0279(3) Uani 1 1 d D . . O24 O 0.3324(4) 0.8467(3) 0.8530(2) 0.0384(11) Uani 1 1 d . G . O25 O 0.4315(6) 0.9229(7) 0.7566(5) 0.047(2) Uani 0.725(9) 1 d P G 1 O26 O 0.2827(6) 0.8582(6) 0.7438(4) 0.0368(18) Uani 0.725(9) 1 d P G 1 O27 O 0.2810(7) 0.9944(5) 0.8033(4) 0.049(2) Uani 0.725(9) 1 d P G 1 O25B O 0.4274(15) 0.8790(17) 0.7484(14) 0.047(2) Uani 0.275(9) 1 d PD G 2 O26B O 0.2530(13) 0.8954(16) 0.7593(11) 0.0368(18) Uani 0.275(9) 1 d PD G 2 O27B O 0.3515(19) 0.9993(13) 0.8056(10) 0.049(2) Uani 0.275(9) 1 d P G 2 O28B O 0.4340(7) 0.5380(7) 1.0091(5) 0.044(2) Uani 0.5 1 d P H 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 Mn1 0.0226(4) 0.0282(5) 0.0128(4) -0.0021(3) 0.0014(3) -0.0043(4) O1 0.021(2) 0.032(2) 0.0153(19) -0.0028(16) 0.0057(16) -0.0029(17) O2 0.063(3) 0.029(2) 0.027(2) -0.007(2) -0.001(2) -0.006(2) O3 0.025(2) 0.034(2) 0.015(2) -0.0035(17) -0.0018(16) -0.0050(17) O4 0.022(2) 0.028(2) 0.023(2) -0.0057(17) -0.0035(17) 0.0040(17) Mn2 0.0209(4) 0.0244(4) 0.0109(4) -0.0034(3) 0.0056(3) -0.0006(3) C1 0.020(3) 0.023(3) 0.025(3) -0.013(2) 0.004(2) 0.000(2) C2 0.028(3) 0.020(3) 0.023(3) -0.001(2) -0.005(2) 0.000(2) C3 0.044(4) 0.026(3) 0.022(3) -0.003(2) -0.002(3) 0.005(3) Cl1 0.0365(12) 0.0510(14) 0.0190(10) -0.0109(9) -0.0012(8) -0.0021(9) C4 0.086(6) 0.029(4) 0.027(4) -0.006(3) -0.023(4) 0.014(4) C5 0.074(6) 0.034(4) 0.060(5) -0.007(4) -0.045(5) -0.003(4) C6 0.047(4) 0.035(4) 0.070(6) 0.010(4) -0.032(4) -0.008(3) C7 0.029(4) 0.039(4) 0.037(4) 0.001(3) -0.004(3) -0.007(3) Cl1B 0.023(3) 0.046(4) 0.018(3) -0.001(3) 0.003(2) -0.003(3) O5 0.025(2) 0.028(2) 0.018(2) -0.0032(16) 0.0052(16) -0.0044(17) O6 0.025(2) 0.031(2) 0.016(2) -0.0073(17) 0.0105(16) -0.0084(17) C8 0.017(3) 0.038(4) 0.012(3) -0.003(2) 0.000(2) -0.007(2) C9 0.026(3) 0.027(3) 0.010(3) 0.001(2) 0.003(2) -0.001(2) C10 0.026(3) 0.033(3) 0.016(3) 0.002(2) 0.000(2) -0.003(2) Cl2 0.0245(7) 0.0433(9) 0.0238(7) 0.0004(6) -0.0023(6) -0.0060(6) C11 0.027(3) 0.034(3) 0.023(3) 0.003(3) 0.009(3) 0.003(3) C12 0.042(4) 0.030(3) 0.024(3) 0.000(3) 0.011(3) 0.005(3) C13 0.042(4) 0.031(3) 0.022(3) -0.006(3) -0.001(3) 0.001(3) C14 0.027(3) 0.026(3) 0.018(3) -0.003(2) 0.004(2) -0.001(2) N1 0.026(3) 0.037(3) 0.017(2) -0.005(2) 0.005(2) -0.013(2) C15 0.036(4) 0.044(4) 0.025(3) -0.008(3) -0.007(3) -0.010(3) C16 0.032(4) 0.045(4) 0.033(4) -0.010(3) 0.005(3) -0.019(3) C17 0.037(4) 0.040(4) 0.032(4) -0.004(3) 0.009(3) -0.017(3) C18 0.039(4) 0.030(3) 0.025(3) 0.002(3) 0.006(3) -0.008(3) C19 0.034(3) 0.026(3) 0.020(3) -0.005(2) 0.000(2) -0.009(3) C20 0.036(3) 0.027(3) 0.017(3) -0.002(2) 0.002(2) -0.005(3) C21 0.039(4) 0.037(4) 0.020(3) 0.004(3) -0.002(3) -0.009(3) C22 0.038(4) 0.040(4) 0.028(3) 0.010(3) -0.006(3) -0.007(3) C23 0.031(3) 0.044(4) 0.029(3) 0.001(3) -0.005(3) -0.011(3) C24 0.027(3) 0.034(3) 0.020(3) 0.001(2) 0.000(2) -0.005(3) N2 0.026(3) 0.028(3) 0.019(2) -0.003(2) -0.002(2) -0.005(2) N3 0.022(2) 0.025(3) 0.014(2) 0.0009(19) 0.0046(19) 0.0022(19) C25 0.031(3) 0.034(3) 0.017(3) 0.000(2) 0.001(2) 0.009(3) C26 0.035(3) 0.026(3) 0.025(3) -0.004(2) 0.007(3) 0.008(3) C27 0.040(4) 0.038(4) 0.017(3) -0.004(3) 0.003(3) 0.003(3) C28 0.030(3) 0.037(3) 0.014(3) -0.001(2) 0.000(2) -0.002(3) C29 0.021(3) 0.030(3) 0.015(3) -0.004(2) -0.001(2) -0.002(2) C30 0.016(3) 0.025(3) 0.017(3) 0.001(2) 0.000(2) -0.004(2) C31 0.026(3) 0.033(3) 0.018(3) 0.003(2) -0.001(2) -0.005(3) C32 0.028(3) 0.027(3) 0.032(3) 0.008(3) -0.003(3) -0.008(3) C33 0.023(3) 0.025(3) 0.036(4) -0.005(3) 0.002(3) -0.003(2) C34 0.023(3) 0.029(3) 0.020(3) -0.003(2) 0.002(2) -0.005(2) N4 0.020(2) 0.022(2) 0.013(2) -0.0021(18) 0.0035(18) -0.0033(19) O7 0.027(2) 0.065(3) 0.031(3) 0.003(2) -0.004(2) -0.004(2) Cl3A 0.0387(17) 0.0329(16) 0.0194(14) 0.0076(12) 0.0061(12) 0.0036(13) O7A 0.086(9) 0.069(8) 0.045(7) -0.004(6) -0.015(6) -0.018(7) O8A 0.065(7) 0.075(8) 0.017(5) 0.019(5) 0.005(5) 0.013(6) O9A 0.120(11) 0.045(6) 0.029(5) 0.002(5) -0.017(6) 0.054(7) O10A 0.047(7) 0.116(12) 0.050(7) 0.021(7) -0.009(6) -0.028(7) Cl3B 0.043(2) 0.061(2) 0.0311(18) 0.0119(16) 0.0014(15) -0.0069(17) O7B 0.027(2) 0.065(3) 0.031(3) 0.003(2) -0.004(2) -0.004(2) O8B 0.045(7) 0.107(11) 0.066(8) 0.032(7) -0.012(6) -0.037(7) O9B 0.096(10) 0.055(7) 0.041(6) -0.009(5) -0.001(6) 0.006(7) O10B 0.109(10) 0.036(6) 0.017(5) -0.005(4) -0.006(5) 0.008(6) Mn3 0.0207(4) 0.0254(5) 0.0115(4) 0.0014(3) 0.0031(3) -0.0055(3) Mn4 0.0178(4) 0.0195(4) 0.0118(4) 0.0006(3) -0.0003(3) -0.0006(3) O11 0.0169(19) 0.028(2) 0.0170(19) -0.0022(16) 0.0001(15) 0.0013(16) O12 0.022(2) 0.027(2) 0.022(2) 0.0021(16) -0.0023(16) -0.0043(17) O13 0.0189(19) 0.027(2) 0.0156(19) 0.0056(16) -0.0026(15) -0.0012(16) C35 0.023(3) 0.021(3) 0.012(3) 0.002(2) -0.001(2) 0.008(2) C36 0.021(3) 0.020(3) 0.017(3) 0.005(2) -0.002(2) -0.004(2) C37 0.021(3) 0.028(3) 0.017(3) 0.000(2) -0.001(2) -0.002(2) Cl4 0.0246(9) 0.0486(11) 0.0170(8) -0.0053(7) 0.0010(6) -0.0061(7) C38 0.039(4) 0.026(3) 0.020(3) 0.003(2) -0.007(3) -0.003(3) C39 0.033(3) 0.027(3) 0.037(4) 0.006(3) -0.016(3) -0.007(3) C40 0.022(3) 0.029(3) 0.035(4) 0.008(3) -0.004(3) -0.005(2) C41 0.024(3) 0.028(3) 0.021(3) 0.010(2) 0.002(2) -0.006(2) Cl4B 0.016(8) 0.054(11) 0.016(8) 0.002(7) 0.003(6) -0.005(7) O14 0.021(2) 0.025(2) 0.019(2) 0.0010(16) 0.0058(16) -0.0066(16) O15 0.037(2) 0.022(2) 0.015(2) 0.0001(16) 0.0103(17) -0.0036(18) C42 0.024(3) 0.023(3) 0.014(3) 0.001(2) 0.000(2) -0.002(2) C43 0.026(3) 0.017(3) 0.018(3) 0.001(2) 0.005(2) -0.002(2) C44 0.028(3) 0.027(3) 0.022(3) 0.000(2) 0.001(2) -0.003(2) Cl5 0.0307(9) 0.0626(12) 0.0489(11) -0.0251(9) -0.0067(8) 0.0007(8) C45 0.028(3) 0.033(3) 0.029(3) 0.001(3) 0.012(3) 0.001(3) C46 0.052(4) 0.033(4) 0.025(3) -0.004(3) 0.009(3) 0.011(3) C47 0.043(4) 0.038(4) 0.042(4) -0.021(3) -0.007(3) 0.001(3) N5 0.024(3) 0.030(3) 0.020(2) 0.010(2) -0.007(2) -0.011(2) C48 0.031(3) 0.031(3) 0.043(4) -0.016(3) 0.000(3) 0.000(3) C49 0.026(3) 0.031(3) 0.027(3) 0.005(3) -0.001(3) -0.003(3) C50 0.032(4) 0.031(3) 0.041(4) 0.011(3) -0.003(3) -0.002(3) C51 0.036(4) 0.040(4) 0.045(4) 0.020(3) -0.012(3) -0.007(3) C52 0.034(4) 0.041(4) 0.027(3) 0.017(3) -0.010(3) -0.013(3) C53 0.022(3) 0.044(4) 0.021(3) 0.007(3) -0.007(2) -0.016(3) C54 0.027(3) 0.039(4) 0.018(3) 0.006(3) -0.002(2) -0.013(3) C55 0.040(4) 0.056(5) 0.017(3) 0.008(3) 0.001(3) -0.019(3) C56 0.038(4) 0.079(6) 0.019(3) -0.007(3) 0.007(3) -0.021(4) C57 0.034(4) 0.056(5) 0.027(3) -0.013(3) 0.002(3) -0.010(3) C58 0.024(3) 0.044(4) 0.031(4) -0.007(3) -0.003(3) -0.010(3) N6 0.021(2) 0.033(3) 0.021(3) -0.003(2) -0.001(2) -0.007(2) N7 0.019(2) 0.024(2) 0.012(2) -0.0024(18) 0.0001(18) -0.0069(19) C59 0.025(3) 0.019(3) 0.015(3) -0.003(2) 0.000(2) -0.003(2) C60 0.024(3) 0.024(3) 0.022(3) -0.002(2) -0.001(2) -0.005(2) C61 0.029(3) 0.021(3) 0.021(3) 0.003(2) 0.005(2) -0.008(2) C62 0.026(3) 0.027(3) 0.020(3) 0.005(2) 0.000(2) -0.003(2) C63 0.026(3) 0.014(3) 0.016(3) -0.003(2) 0.001(2) -0.002(2) C64 0.024(3) 0.021(3) 0.016(3) -0.003(2) -0.001(2) -0.003(2) C65 0.028(3) 0.021(3) 0.020(3) 0.003(2) -0.002(2) -0.001(2) C66 0.024(3) 0.023(3) 0.022(3) 0.001(2) -0.003(2) 0.003(2) C67 0.020(3) 0.021(3) 0.024(3) -0.006(2) -0.002(2) -0.001(2) C68 0.020(3) 0.020(3) 0.021(3) -0.007(2) 0.000(2) -0.003(2) N8 0.024(2) 0.015(2) 0.015(2) -0.0040(17) -0.0016(19) -0.0014(18) Cl6 0.0206(7) 0.0267(7) 0.0225(7) -0.0036(5) 0.0004(5) -0.0007(5) O16 0.023(2) 0.041(3) 0.034(2) -0.017(2) -0.0019(18) -0.0010(19) O17 0.038(3) 0.041(3) 0.026(2) 0.012(2) 0.006(2) -0.005(2) O18 0.030(2) 0.031(2) 0.035(3) -0.0118(19) 0.0051(19) 0.0072(19) O19 0.024(2) 0.041(3) 0.025(2) -0.0025(19) -0.0012(17) -0.0029(18) O20 0.029(2) 0.040(3) 0.028(2) 0.0008(19) -0.0036(18) -0.0131(19) Cl7A 0.0254(14) 0.0353(16) 0.0169(13) 0.0009(11) 0.0034(11) -0.0059(12) O20A 0.073(8) 0.059(7) 0.035(6) 0.014(5) -0.015(6) 0.004(6) O21A 0.025(5) 0.072(7) 0.038(6) -0.022(5) -0.004(4) -0.010(5) O22A 0.034(5) 0.042(5) 0.034(5) -0.009(4) 0.021(4) -0.011(4) O23A 0.052(6) 0.035(6) 0.056(7) -0.007(5) 0.008(5) -0.010(5) Cl7B 0.0281(15) 0.0278(15) 0.0191(13) 0.0037(11) -0.0018(11) -0.0091(12) O20B 0.029(2) 0.040(3) 0.028(2) 0.0008(19) -0.0036(18) -0.0131(19) O21B 0.032(5) 0.048(5) 0.021(4) 0.004(4) -0.007(4) -0.025(4) O22B 0.031(5) 0.035(5) 0.065(7) -0.001(5) 0.010(5) -0.006(4) O23B 0.056(6) 0.049(6) 0.013(4) 0.007(4) 0.001(4) -0.028(5) Cl8 0.0392(8) 0.0235(7) 0.0187(7) -0.0011(5) 0.0045(6) -0.0068(6) O24 0.064(3) 0.026(2) 0.021(2) 0.0063(18) 0.003(2) -0.006(2) O25 0.031(3) 0.069(7) 0.037(4) 0.017(5) -0.002(3) -0.027(4) O26 0.039(4) 0.036(5) 0.037(4) 0.002(3) -0.009(3) -0.014(3) O27 0.076(6) 0.028(3) 0.037(3) -0.003(3) 0.010(4) 0.014(4) O25B 0.031(3) 0.069(7) 0.037(4) 0.017(5) -0.002(3) -0.027(4) O26B 0.039(4) 0.036(5) 0.037(4) 0.002(3) -0.009(3) -0.014(3) O27B 0.076(6) 0.028(3) 0.037(3) -0.003(3) 0.010(4) 0.014(4) O28B 0.052(6) 0.051(6) 0.028(5) 0.000(4) -0.006(4) -0.009(5) #----------------------------------------------------------------------------# # 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 O1 1.804(4) . ? Mn1 O3 1.965(4) . ? Mn1 N2 2.059(5) . ? Mn1 N1 2.076(5) . ? Mn1 O5 2.159(4) . ? Mn1 O2 2.196(5) . ? Mn1 Mn2 3.1507(12) . ? O1 Mn2 1.783(4) . ? O2 H2A 0.83(2) . ? O2 H2B 0.82(2) . ? O3 C1 1.270(7) . ? O4 C1 1.257(7) . ? O4 Mn2 2.178(4) . ? Mn2 O6 1.933(4) . ? Mn2 N3 2.049(4) . ? Mn2 N4 2.065(5) . ? Mn2 O7 2.317(5) . ? C1 C2 1.503(8) . ? C2 C7 1.390(9) . ? C2 C3 1.393(8) . ? C3 C4 1.398(10) . ? C3 Cl1 1.686(7) . ? C3 H3 0.933(7) . ? Cl1 H3 0.766(2) . ? C4 C5 1.359(12) . ? C4 H4 0.95 . ? C5 C6 1.381(12) . ? C5 H5 0.95 . ? C6 C7 1.382(10) . ? C6 H6 0.95 . ? C7 Cl1B 1.594(9) . ? C7 H7 0.87(12) . ? Cl1B H7 0.84(13) . ? O5 C8 1.228(7) . ? O6 C8 1.293(6) . ? C8 C9 1.498(8) . ? C9 C10 1.394(8) . ? C9 C14 1.398(8) . ? C10 C11 1.396(8) . ? C10 Cl2 1.738(6) . ? C11 C12 1.379(10) . ? C11 H11 0.95 . ? C12 C13 1.384(9) . ? C12 H12 0.95 . ? C13 C14 1.388(8) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? N1 C15 1.321(8) . ? N1 C19 1.356(8) . ? C15 C16 1.395(9) . ? C15 H15 0.95 . ? C16 C17 1.379(10) . ? C16 H16 0.95 . ? C17 C18 1.384(10) . ? C17 H17 0.95 . ? C18 C19 1.391(8) . ? C18 H18 0.95 . ? C19 C20 1.473(9) . ? C20 N2 1.356(7) . ? C20 C21 1.382(9) . ? C21 C22 1.383(9) . ? C21 H21 0.95 . ? C22 C23 1.374(9) . ? C22 H22 0.95 . ? C23 C24 1.395(9) . ? C23 H23 0.95 . ? C24 N2 1.339(8) . ? C24 H24 0.95 . ? N3 C25 1.334(8) . ? N3 C29 1.362(7) . ? C25 C26 1.386(8) . ? C25 H25 0.95 . ? C26 C27 1.383(9) . ? C26 H26 0.95 . ? C27 C28 1.389(9) . ? C27 H27 0.95 . ? C28 C29 1.388(8) . ? C28 H28 0.95 . ? C29 C30 1.462(8) . ? C30 N4 1.365(7) . ? C30 C31 1.388(8) . ? C31 C32 1.381(9) . ? C31 H31 0.95 . ? C32 C33 1.396(9) . ? C32 H32 0.95 . ? C33 C34 1.375(8) . ? C33 H33 0.95 . ? C34 N4 1.351(7) . ? C34 H34 0.95 . ? Cl3A O10A 1.373(12) . ? Cl3A O9A 1.401(10) . ? Cl3A O8A 1.420(9) . ? Cl3A O7A 1.465(12) . ? Cl3B O10B 1.383(10) . ? Cl3B O8B 1.423(12) . ? Cl3B O9B 1.454(12) . ? Mn3 O11 1.798(4) . ? Mn3 O14 1.939(4) . ? Mn3 N6 2.053(5) . ? Mn3 N5 2.081(5) . ? Mn3 O12 2.176(4) . ? Mn3 O20 2.267(4) . ? Mn3 Mn4 3.1382(12) . ? Mn4 O11 1.778(4) . ? Mn4 O13 1.938(4) . ? Mn4 N8 2.044(5) . ? Mn4 N7 2.052(4) . ? Mn4 O15 2.128(4) . ? Mn4 O16 2.379(4) . ? O12 C35 1.244(7) . ? O13 C35 1.291(6) . ? C35 C36 1.490(8) . ? C36 C37 1.400(8) . ? C36 C41 1.400(8) . ? C37 C38 1.370(8) . ? C37 Cl4 1.732(6) . ? C37 H37 0.931(6) . ? Cl4 H37 0.8027(16) . ? C38 C39 1.386(9) . ? C38 H38 0.95 . ? C39 C40 1.390(9) . ? C39 H39 0.95 . ? C40 C41 1.384(9) . ? C40 H40 0.95 . ? C41 Cl4B 1.610(16) . ? C41 H41 1.05(9) . ? Cl4B H41 0.72(9) . ? O14 C42 1.281(6) . ? O15 C42 1.238(7) . ? C42 C43 1.487(7) . ? C43 C44 1.380(8) . ? C43 C48 1.392(9) . ? C44 C45 1.388(8) . ? C44 Cl5 1.744(6) . ? C45 C46 1.379(10) . ? C45 H45 0.95 . ? C46 C47 1.377(10) . ? C46 H46 0.95 . ? C47 C48 1.386(9) . ? C47 H47 0.95 . ? N5 C49 1.328(8) . ? N5 C53 1.365(7) . ? C48 H48 0.95 . ? C49 C50 1.388(9) . ? C49 H49 0.95 . ? C50 C51 1.383(10) . ? C50 H50 0.95 . ? C51 C52 1.374(10) . ? C51 H51 0.95 . ? C52 C53 1.399(9) . ? C52 H52 0.95 . ? C53 C54 1.446(9) . ? C54 N6 1.366(8) . ? C54 C55 1.413(8) . ? C55 C56 1.375(11) . ? C55 H55 0.95 . ? C56 C57 1.382(11) . ? C56 H56 0.95 . ? C57 C58 1.402(9) . ? C57 H57 0.95 . ? C58 N6 1.327(8) . ? C58 H58 0.95 . ? N7 C59 1.323(7) . ? N7 C63 1.353(7) . ? C59 C60 1.388(8) . ? C59 H59 0.95 . ? C60 C61 1.386(8) . ? C60 H60 0.95 . ? C61 C62 1.371(8) . ? C61 H61 0.95 . ? C62 C63 1.401(8) . ? C62 H62 0.95 . ? C63 C64 1.466(8) . ? C64 N8 1.359(7) . ? C64 C65 1.379(8) . ? C65 C66 1.382(8) . ? C65 H65 0.95 . ? C66 C67 1.380(8) . ? C66 H66 0.95 . ? C67 C68 1.390(8) . ? C67 H67 0.95 . ? C68 N8 1.339(7) . ? C68 H68 0.95 . ? Cl6 O19 1.434(4) . ? Cl6 O18 1.436(4) . ? Cl6 O16 1.449(4) . ? Cl6 O17 1.453(4) . ? Cl7A O23A 1.408(10) . ? Cl7A O21A 1.411(9) . ? Cl7A O20A 1.435(10) . ? Cl7A O22A 1.443(8) . ? Cl7B O23B 1.424(8) . ? Cl7B O21B 1.435(8) . ? Cl7B O22B 1.458(10) . ? Cl8 O26B 1.365(15) . ? Cl8 O25 1.426(7) . ? Cl8 O24 1.448(4) . ? Cl8 O26 1.451(7) . ? Cl8 O25B 1.459(17) . ? Cl8 O27B 1.46(2) . ? Cl8 O27 1.474(7) . ? 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 O1 Mn1 O3 97.36(17) . . ? O1 Mn1 N2 92.34(19) . . ? O3 Mn1 N2 167.21(19) . . ? O1 Mn1 N1 169.29(19) . . ? O3 Mn1 N1 92.66(18) . . ? N2 Mn1 N1 78.3(2) . . ? O1 Mn1 O5 96.10(16) . . ? O3 Mn1 O5 90.04(16) . . ? N2 Mn1 O5 97.21(17) . . ? N1 Mn1 O5 80.04(18) . . ? O1 Mn1 O2 94.29(19) . . ? O3 Mn1 O2 86.58(19) . . ? N2 Mn1 O2 84.40(19) . . ? N1 Mn1 O2 90.1(2) . . ? O5 Mn1 O2 169.40(18) . . ? O1 Mn1 Mn2 28.35(13) . . ? O3 Mn1 Mn2 81.65(12) . . ? N2 Mn1 Mn2 110.53(14) . . ? N1 Mn1 Mn2 152.07(15) . . ? O5 Mn1 Mn2 72.68(10) . . ? O2 Mn1 Mn2 116.64(13) . . ? Mn2 O1 Mn1 122.9(2) . . ? Mn1 O2 H2A 123(6) . . ? Mn1 O2 H2B 139(6) . . ? H2A O2 H2B 98(7) . . ? C1 O3 Mn1 127.9(4) . . ? C1 O4 Mn2 128.3(4) . . ? O1 Mn2 O6 100.29(17) . . ? O1 Mn2 N3 93.14(18) . . ? O6 Mn2 N3 166.50(18) . . ? O1 Mn2 N4 171.44(17) . . ? O6 Mn2 N4 87.94(17) . . ? N3 Mn2 N4 78.59(18) . . ? O1 Mn2 O4 92.57(17) . . ? O6 Mn2 O4 94.27(16) . . ? N3 Mn2 O4 86.50(17) . . ? N4 Mn2 O4 89.15(17) . . ? O1 Mn2 O7 93.71(18) . . ? O6 Mn2 O7 89.63(17) . . ? N3 Mn2 O7 88.06(18) . . ? N4 Mn2 O7 83.90(18) . . ? O4 Mn2 O7 171.91(16) . . ? O1 Mn2 Mn1 28.72(12) . . ? O6 Mn2 Mn1 80.83(12) . . ? N3 Mn2 Mn1 112.18(14) . . ? N4 Mn2 Mn1 158.13(13) . . ? O4 Mn2 Mn1 73.17(11) . . ? O7 Mn2 Mn1 114.52(12) . . ? O4 C1 O3 126.3(5) . . ? O4 C1 C2 117.6(5) . . ? O3 C1 C2 116.2(5) . . ? C7 C2 C3 117.5(6) . . ? C7 C2 C1 120.2(6) . . ? C3 C2 C1 122.3(5) . . ? C2 C3 C4 120.9(7) . . ? C2 C3 Cl1 123.4(5) . . ? C4 C3 Cl1 115.4(5) . . ? C2 C3 H3 119.4(6) . . ? C4 C3 H3 119.7(7) . . ? C5 C4 C3 120.1(7) . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 120.3(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 119.7(8) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 121.6(7) . . ? C6 C7 Cl1B 107.3(6) . . ? C2 C7 Cl1B 130.5(6) . . ? C6 C7 H7 124(7) . . ? C2 C7 H7 114(7) . . ? C8 O5 Mn1 129.8(4) . . ? C8 O6 Mn2 126.8(4) . . ? O5 C8 O6 125.9(5) . . ? O5 C8 C9 119.7(5) . . ? O6 C8 C9 114.4(5) . . ? C10 C9 C14 118.5(5) . . ? C10 C9 C8 122.8(5) . . ? C14 C9 C8 118.7(5) . . ? C9 C10 C11 120.3(6) . . ? C9 C10 Cl2 122.0(5) . . ? C11 C10 Cl2 117.6(5) . . ? C12 C11 C10 119.9(6) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.8(6) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 119.2(6) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C9 121.2(6) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? C15 N1 C19 120.1(5) . . ? C15 N1 Mn1 123.6(4) . . ? C19 N1 Mn1 115.4(4) . . ? N1 C15 C16 121.8(6) . . ? N1 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C17 C16 C15 118.8(6) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 119.6(6) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 118.8(6) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? N1 C19 C18 121.0(6) . . ? N1 C19 C20 114.7(5) . . ? C18 C19 C20 124.2(6) . . ? N2 C20 C21 120.7(6) . . ? N2 C20 C19 114.6(5) . . ? C21 C20 C19 124.7(5) . . ? C20 C21 C22 119.2(6) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 120.0(6) . . ? C23 C22 H22 120 . . ? C21 C22 H22 120 . . ? C22 C23 C24 118.7(6) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? N2 C24 C23 121.2(5) . . ? N2 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 N2 C20 120.2(5) . . ? C24 N2 Mn1 123.3(4) . . ? C20 N2 Mn1 116.2(4) . . ? C25 N3 C29 119.8(5) . . ? C25 N3 Mn2 123.7(4) . . ? C29 N3 Mn2 116.0(4) . . ? N3 C25 C26 122.3(6) . . ? N3 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C27 C26 C25 118.2(6) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C26 C27 C28 120.1(6) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 118.8(6) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? N3 C29 C28 120.7(5) . . ? N3 C29 C30 114.7(5) . . ? C28 C29 C30 124.6(5) . . ? N4 C30 C31 120.7(5) . . ? N4 C30 C29 114.9(5) . . ? C31 C30 C29 124.3(5) . . ? C32 C31 C30 119.6(5) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.6(5) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 118.3(6) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? N4 C34 C33 122.8(5) . . ? N4 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 N4 C30 119.0(5) . . ? C34 N4 Mn2 125.7(4) . . ? C30 N4 Mn2 115.3(4) . . ? O10A Cl3A O9A 105.6(9) . . ? O10A Cl3A O8A 109.8(7) . . ? O9A Cl3A O8A 113.1(6) . . ? O10A Cl3A O7A 110.2(8) . . ? O9A Cl3A O7A 108.5(8) . . ? O8A Cl3A O7A 109.6(7) . . ? O10B Cl3B O8B 108.6(8) . . ? O10B Cl3B O9B 110.1(7) . . ? O8B Cl3B O9B 108.6(9) . . ? O11 Mn3 O14 99.83(16) . . ? O11 Mn3 N6 92.79(19) . . ? O14 Mn3 N6 167.18(19) . . ? O11 Mn3 N5 171.12(19) . . ? O14 Mn3 N5 88.71(18) . . ? N6 Mn3 N5 78.8(2) . . ? O11 Mn3 O12 93.33(16) . . ? O14 Mn3 O12 92.44(16) . . ? N6 Mn3 O12 84.54(17) . . ? N5 Mn3 O12 88.70(17) . . ? O11 Mn3 O20 96.01(17) . . ? O14 Mn3 O20 90.39(16) . . ? N6 Mn3 O20 90.51(17) . . ? N5 Mn3 O20 81.39(17) . . ? O12 Mn3 O20 169.63(15) . . ? O11 Mn3 Mn4 28.48(12) . . ? O14 Mn3 Mn4 79.50(11) . . ? N6 Mn3 Mn4 111.48(14) . . ? N5 Mn3 Mn4 158.88(14) . . ? O12 Mn3 Mn4 74.51(10) . . ? O20 Mn3 Mn4 115.83(11) . . ? O11 Mn4 O13 99.02(16) . . ? O11 Mn4 N8 92.42(17) . . ? O13 Mn4 N8 165.10(17) . . ? O11 Mn4 N7 170.92(18) . . ? O13 Mn4 N7 89.94(17) . . ? N8 Mn4 N7 79.00(18) . . ? O11 Mn4 O15 96.34(16) . . ? O13 Mn4 O15 91.62(17) . . ? N8 Mn4 O15 96.60(17) . . ? N7 Mn4 O15 81.88(16) . . ? O11 Mn4 O16 90.52(16) . . ? O13 Mn4 O16 84.91(16) . . ? N8 Mn4 O16 85.48(16) . . ? N7 Mn4 O16 91.71(17) . . ? O15 Mn4 O16 172.73(15) . . ? O11 Mn4 Mn3 28.82(12) . . ? O13 Mn4 Mn3 80.78(11) . . ? N8 Mn4 Mn3 113.35(13) . . ? N7 Mn4 Mn3 154.50(13) . . ? O15 Mn4 Mn3 74.75(10) . . ? O16 Mn4 Mn3 110.86(11) . . ? Mn4 O11 Mn3 122.7(2) . . ? C35 O12 Mn3 127.7(4) . . ? C35 O13 Mn4 129.9(4) . . ? O12 C35 O13 125.6(5) . . ? O12 C35 C36 120.1(5) . . ? O13 C35 C36 114.3(5) . . ? C37 C36 C41 118.3(5) . . ? C37 C36 C35 121.3(5) . . ? C41 C36 C35 120.4(5) . . ? C38 C37 C36 121.5(5) . . ? C38 C37 Cl4 118.0(4) . . ? C36 C37 Cl4 120.5(4) . . ? C38 C37 H37 119.3(6) . . ? C36 C37 H37 119.2(6) . . ? C37 C38 C39 119.9(6) . . ? C37 C38 H38 120 . . ? C39 C38 H38 120 . . ? C38 C39 C40 119.6(6) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 120.6(6) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C36 120.1(6) . . ? C40 C41 Cl4B 107.8(7) . . ? C36 C41 Cl4B 132.1(8) . . ? C40 C41 H41 126(5) . . ? C36 C41 H41 114(5) . . ? C42 O14 Mn3 130.9(4) . . ? C42 O15 Mn4 129.4(3) . . ? O15 C42 O14 124.6(5) . . ? O15 C42 C43 118.4(5) . . ? O14 C42 C43 117.0(5) . . ? C44 C43 C48 118.8(5) . . ? C44 C43 C42 121.4(5) . . ? C48 C43 C42 119.8(5) . . ? C43 C44 C45 121.1(6) . . ? C43 C44 Cl5 120.6(5) . . ? C45 C44 Cl5 118.2(5) . . ? C46 C45 C44 119.2(6) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C47 C46 C45 120.6(6) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 119.8(6) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C49 N5 C53 120.1(5) . . ? C49 N5 Mn3 125.1(4) . . ? C53 N5 Mn3 114.8(4) . . ? C47 C48 C43 120.4(6) . . ? C47 C48 H48 119.8 . . ? C43 C48 H48 119.8 . . ? N5 C49 C50 122.4(6) . . ? N5 C49 H49 118.8 . . ? C50 C49 H49 118.8 . . ? C51 C50 C49 118.1(7) . . ? C51 C50 H50 121 . . ? C49 C50 H50 121 . . ? C52 C51 C50 120.1(6) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 119.5(6) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? N5 C53 C52 119.8(6) . . ? N5 C53 C54 114.8(5) . . ? C52 C53 C54 125.4(6) . . ? N6 C54 C55 119.7(6) . . ? N6 C54 C53 116.3(5) . . ? C55 C54 C53 124.0(6) . . ? C56 C55 C54 118.7(6) . . ? C56 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? C55 C56 C57 121.1(6) . . ? C55 C56 H56 119.4 . . ? C57 C56 H56 119.4 . . ? C56 C57 C58 117.6(7) . . ? C56 C57 H57 121.2 . . ? C58 C57 H57 121.2 . . ? N6 C58 C57 122.2(7) . . ? N6 C58 H58 118.9 . . ? C57 C58 H58 118.9 . . ? C58 N6 C54 120.7(5) . . ? C58 N6 Mn3 124.2(4) . . ? C54 N6 Mn3 114.6(4) . . ? C59 N7 C63 120.5(5) . . ? C59 N7 Mn4 123.6(4) . . ? C63 N7 Mn4 115.3(4) . . ? N7 C59 C60 122.1(5) . . ? N7 C59 H59 118.9 . . ? C60 C59 H59 118.9 . . ? C61 C60 C59 117.8(5) . . ? C61 C60 H60 121.1 . . ? C59 C60 H60 121.1 . . ? C62 C61 C60 120.7(5) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C61 C62 C63 118.5(5) . . ? C61 C62 H62 120.7 . . ? C63 C62 H62 120.7 . . ? N7 C63 C62 120.4(5) . . ? N7 C63 C64 115.3(5) . . ? C62 C63 C64 124.3(5) . . ? N8 C64 C65 120.8(5) . . ? N8 C64 C63 114.2(5) . . ? C65 C64 C63 124.9(5) . . ? C64 C65 C66 119.6(5) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C67 C66 C65 119.4(5) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? C66 C67 C68 118.7(5) . . ? C66 C67 H67 120.6 . . ? C68 C67 H67 120.6 . . ? N8 C68 C67 121.8(5) . . ? N8 C68 H68 119.1 . . ? C67 C68 H68 119.1 . . ? C68 N8 C64 119.6(5) . . ? C68 N8 Mn4 124.5(4) . . ? C64 N8 Mn4 115.9(4) . . ? O19 Cl6 O18 110.0(3) . . ? O19 Cl6 O16 109.8(3) . . ? O18 Cl6 O16 109.2(3) . . ? O19 Cl6 O17 109.6(3) . . ? O18 Cl6 O17 109.7(3) . . ? O16 Cl6 O17 108.5(3) . . ? Cl6 O16 Mn4 135.4(2) . . ? O23A Cl7A O21A 109.4(6) . . ? O23A Cl7A O20A 109.8(7) . . ? O21A Cl7A O20A 109.9(7) . . ? O23A Cl7A O22A 109.2(6) . . ? O21A Cl7A O22A 111.0(6) . . ? O20A Cl7A O22A 107.4(7) . . ? O23B Cl7B O21B 111.5(5) . . ? O23B Cl7B O22B 110.4(6) . . ? O21B Cl7B O22B 110.3(6) . . ? O26B Cl8 O25 128.3(10) . . ? O26B Cl8 O24 112.6(10) . . ? O25 Cl8 O24 112.1(4) . . ? O25 Cl8 O26 110.0(5) . . ? O24 Cl8 O26 109.0(4) . . ? O26B Cl8 O25B 115.6(14) . . ? O24 Cl8 O25B 104.4(12) . . ? O26 Cl8 O25B 89.9(11) . . ? O26B Cl8 O27B 115.9(13) . . ? O25 Cl8 O27B 75.0(9) . . ? O24 Cl8 O27B 105.3(8) . . ? O26 Cl8 O27B 139.6(9) . . ? O25B Cl8 O27B 101.8(12) . . ? O26B Cl8 O27 79.4(10) . . ? O25 Cl8 O27 109.1(5) . . ? O24 Cl8 O27 108.9(3) . . ? O26 Cl8 O27 107.7(5) . . ? O25B Cl8 O27 134.1(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn1 O1 Mn2 56.8(3) . . . . ? N2 Mn1 O1 Mn2 -131.6(3) . . . . ? N1 Mn1 O1 Mn2 -102.3(11) . . . . ? O5 Mn1 O1 Mn2 -34.0(3) . . . . ? O2 Mn1 O1 Mn2 143.9(3) . . . . ? O1 Mn1 O3 C1 -27.0(5) . . . . ? N2 Mn1 O3 C1 -166.1(7) . . . . ? N1 Mn1 O3 C1 149.2(5) . . . . ? O5 Mn1 O3 C1 69.2(4) . . . . ? O2 Mn1 O3 C1 -120.9(5) . . . . ? Mn2 Mn1 O3 C1 -3.3(4) . . . . ? Mn1 O1 Mn2 O6 48.1(3) . . . . ? Mn1 O1 Mn2 N3 -133.4(3) . . . . ? Mn1 O1 Mn2 O4 -46.8(3) . . . . ? Mn1 O1 Mn2 O7 138.4(3) . . . . ? C1 O4 Mn2 O1 5.1(5) . . . . ? C1 O4 Mn2 O6 -95.5(4) . . . . ? C1 O4 Mn2 N3 98.0(5) . . . . ? C1 O4 Mn2 N4 176.7(4) . . . . ? C1 O4 Mn2 Mn1 -16.4(4) . . . . ? O3 Mn1 Mn2 O1 -123.0(3) . . . . ? N2 Mn1 Mn2 O1 53.0(3) . . . . ? N1 Mn1 Mn2 O1 157.2(4) . . . . ? O5 Mn1 Mn2 O1 144.3(3) . . . . ? O2 Mn1 Mn2 O1 -41.1(3) . . . . ? O1 Mn1 Mn2 O6 -132.2(3) . . . . ? O3 Mn1 Mn2 O6 104.84(17) . . . . ? N2 Mn1 Mn2 O6 -79.18(19) . . . . ? N1 Mn1 Mn2 O6 25.0(3) . . . . ? O5 Mn1 Mn2 O6 12.18(17) . . . . ? O2 Mn1 Mn2 O6 -173.3(2) . . . . ? O1 Mn1 Mn2 N3 51.6(3) . . . . ? O3 Mn1 Mn2 N3 -71.41(19) . . . . ? N2 Mn1 Mn2 N3 104.6(2) . . . . ? N1 Mn1 Mn2 N3 -151.2(3) . . . . ? O5 Mn1 Mn2 N3 -164.08(18) . . . . ? O2 Mn1 Mn2 N3 10.5(2) . . . . ? O1 Mn1 Mn2 N4 167.8(4) . . . . ? O3 Mn1 Mn2 N4 44.8(4) . . . . ? N2 Mn1 Mn2 N4 -139.2(4) . . . . ? N1 Mn1 Mn2 N4 -35.0(5) . . . . ? O5 Mn1 Mn2 N4 -47.8(4) . . . . ? O2 Mn1 Mn2 N4 126.7(4) . . . . ? O1 Mn1 Mn2 O4 130.5(3) . . . . ? O3 Mn1 Mn2 O4 7.51(16) . . . . ? N2 Mn1 Mn2 O4 -176.52(18) . . . . ? N1 Mn1 Mn2 O4 -72.3(3) . . . . ? O5 Mn1 Mn2 O4 -85.16(15) . . . . ? O2 Mn1 Mn2 O4 89.40(19) . . . . ? O1 Mn1 Mn2 O7 -46.8(3) . . . . ? O3 Mn1 Mn2 O7 -169.79(18) . . . . ? N2 Mn1 Mn2 O7 6.2(2) . . . . ? N1 Mn1 Mn2 O7 110.4(3) . . . . ? O5 Mn1 Mn2 O7 97.54(18) . . . . ? O2 Mn1 Mn2 O7 -87.9(2) . . . . ? Mn2 O4 C1 O3 21.3(8) . . . . ? Mn2 O4 C1 C2 -158.5(4) . . . . ? Mn1 O3 C1 O4 -8.2(8) . . . . ? Mn1 O3 C1 C2 171.6(4) . . . . ? O4 C1 C2 C7 -122.1(6) . . . . ? O3 C1 C2 C7 58.0(7) . . . . ? O4 C1 C2 C3 55.4(7) . . . . ? O3 C1 C2 C3 -124.4(6) . . . . ? C7 C2 C3 C4 -0.2(9) . . . . ? C1 C2 C3 C4 -177.8(6) . . . . ? C7 C2 C3 Cl1 -174.1(5) . . . . ? C1 C2 C3 Cl1 8.3(8) . . . . ? C2 C3 C4 C5 1.8(10) . . . . ? Cl1 C3 C4 C5 176.1(6) . . . . ? C3 C4 C5 C6 -1.7(11) . . . . ? C4 C5 C6 C7 0.2(11) . . . . ? C5 C6 C7 C2 1.5(11) . . . . ? C5 C6 C7 Cl1B -170.6(6) . . . . ? C3 C2 C7 C6 -1.4(10) . . . . ? C1 C2 C7 C6 176.3(6) . . . . ? C3 C2 C7 Cl1B 168.6(7) . . . . ? C1 C2 C7 Cl1B -13.7(10) . . . . ? O1 Mn1 O5 C8 4.9(5) . . . . ? O3 Mn1 O5 C8 -92.5(5) . . . . ? N2 Mn1 O5 C8 98.0(5) . . . . ? N1 Mn1 O5 C8 174.8(5) . . . . ? O2 Mn1 O5 C8 -163.8(9) . . . . ? Mn2 Mn1 O5 C8 -11.3(5) . . . . ? O1 Mn2 O6 C8 -41.3(5) . . . . ? N3 Mn2 O6 C8 145.0(7) . . . . ? N4 Mn2 O6 C8 141.1(5) . . . . ? O4 Mn2 O6 C8 52.1(5) . . . . ? O7 Mn2 O6 C8 -135.0(5) . . . . ? Mn1 Mn2 O6 C8 -20.0(4) . . . . ? Mn1 O5 C8 O6 1.5(9) . . . . ? Mn1 O5 C8 C9 -176.4(4) . . . . ? Mn2 O6 C8 O5 19.4(8) . . . . ? Mn2 O6 C8 C9 -162.6(4) . . . . ? O5 C8 C9 C10 -43.4(8) . . . . ? O6 C8 C9 C10 138.5(6) . . . . ? O5 C8 C9 C14 135.4(6) . . . . ? O6 C8 C9 C14 -42.8(7) . . . . ? C14 C9 C10 C11 -1.8(8) . . . . ? C8 C9 C10 C11 176.9(5) . . . . ? C14 C9 C10 Cl2 176.1(4) . . . . ? C8 C9 C10 Cl2 -5.2(8) . . . . ? C9 C10 C11 C12 -0.6(9) . . . . ? Cl2 C10 C11 C12 -178.6(5) . . . . ? C10 C11 C12 C13 2.0(9) . . . . ? C11 C12 C13 C14 -1.1(9) . . . . ? C12 C13 C14 C9 -1.4(9) . . . . ? C10 C9 C14 C13 2.8(8) . . . . ? C8 C9 C14 C13 -176.0(5) . . . . ? O1 Mn1 N1 C15 144.4(10) . . . . ? O3 Mn1 N1 C15 -14.9(5) . . . . ? N2 Mn1 N1 C15 174.3(5) . . . . ? O5 Mn1 N1 C15 74.7(5) . . . . ? O2 Mn1 N1 C15 -101.5(5) . . . . ? Mn2 Mn1 N1 C15 62.3(6) . . . . ? O1 Mn1 N1 C19 -24.2(13) . . . . ? O3 Mn1 N1 C19 176.6(4) . . . . ? N2 Mn1 N1 C19 5.8(4) . . . . ? O5 Mn1 N1 C19 -93.8(4) . . . . ? O2 Mn1 N1 C19 90.0(4) . . . . ? Mn2 Mn1 N1 C19 -106.3(5) . . . . ? C19 N1 C15 C16 -1.3(10) . . . . ? Mn1 N1 C15 C16 -169.3(5) . . . . ? N1 C15 C16 C17 1.3(10) . . . . ? C15 C16 C17 C18 -0.1(10) . . . . ? C16 C17 C18 C19 -1.0(10) . . . . ? C15 N1 C19 C18 0.1(9) . . . . ? Mn1 N1 C19 C18 169.0(5) . . . . ? C15 N1 C19 C20 -178.1(5) . . . . ? Mn1 N1 C19 C20 -9.2(7) . . . . ? C17 C18 C19 N1 1.1(9) . . . . ? C17 C18 C19 C20 179.1(6) . . . . ? N1 C19 C20 N2 8.2(8) . . . . ? C18 C19 C20 N2 -169.9(6) . . . . ? N1 C19 C20 C21 -169.8(6) . . . . ? C18 C19 C20 C21 12.1(10) . . . . ? N2 C20 C21 C22 0.2(10) . . . . ? C19 C20 C21 C22 178.0(6) . . . . ? C20 C21 C22 C23 -1.2(10) . . . . ? C21 C22 C23 C24 1.8(10) . . . . ? C22 C23 C24 N2 -1.6(10) . . . . ? C23 C24 N2 C20 0.6(9) . . . . ? C23 C24 N2 Mn1 -173.7(5) . . . . ? C21 C20 N2 C24 0.1(9) . . . . ? C19 C20 N2 C24 -177.9(5) . . . . ? C21 C20 N2 Mn1 174.8(5) . . . . ? C19 C20 N2 Mn1 -3.3(7) . . . . ? O1 Mn1 N2 C24 -12.0(5) . . . . ? O3 Mn1 N2 C24 127.4(8) . . . . ? N1 Mn1 N2 C24 173.3(5) . . . . ? O5 Mn1 N2 C24 -108.4(5) . . . . ? O2 Mn1 N2 C24 82.1(5) . . . . ? Mn2 Mn1 N2 C24 -34.3(5) . . . . ? O1 Mn1 N2 C20 173.5(4) . . . . ? O3 Mn1 N2 C20 -47.1(10) . . . . ? N1 Mn1 N2 C20 -1.2(4) . . . . ? O5 Mn1 N2 C20 77.1(4) . . . . ? O2 Mn1 N2 C20 -92.4(4) . . . . ? Mn2 Mn1 N2 C20 151.2(4) . . . . ? O1 Mn2 N3 C25 3.0(5) . . . . ? O6 Mn2 N3 C25 176.8(7) . . . . ? N4 Mn2 N3 C25 -179.3(5) . . . . ? O4 Mn2 N3 C25 -89.4(5) . . . . ? O7 Mn2 N3 C25 96.6(5) . . . . ? Mn1 Mn2 N3 C25 -19.2(5) . . . . ? O1 Mn2 N3 C29 175.9(4) . . . . ? O6 Mn2 N3 C29 -10.2(10) . . . . ? N4 Mn2 N3 C29 -6.3(4) . . . . ? O4 Mn2 N3 C29 83.5(4) . . . . ? O7 Mn2 N3 C29 -90.5(4) . . . . ? Mn1 Mn2 N3 C29 153.7(4) . . . . ? C29 N3 C25 C26 0.6(9) . . . . ? Mn2 N3 C25 C26 173.3(5) . . . . ? N3 C25 C26 C27 -0.1(10) . . . . ? C25 C26 C27 C28 -0.6(10) . . . . ? C26 C27 C28 C29 0.9(10) . . . . ? C25 N3 C29 C28 -0.4(8) . . . . ? Mn2 N3 C29 C28 -173.6(4) . . . . ? C25 N3 C29 C30 179.5(5) . . . . ? Mn2 N3 C29 C30 6.3(6) . . . . ? C27 C28 C29 N3 -0.3(9) . . . . ? C27 C28 C29 C30 179.8(6) . . . . ? N3 C29 C30 N4 -1.6(7) . . . . ? C28 C29 C30 N4 178.2(5) . . . . ? N3 C29 C30 C31 176.8(5) . . . . ? C28 C29 C30 C31 -3.3(9) . . . . ? N4 C30 C31 C32 0.0(9) . . . . ? C29 C30 C31 C32 -178.3(5) . . . . ? C30 C31 C32 C33 0.3(9) . . . . ? C31 C32 C33 C34 -0.1(9) . . . . ? C32 C33 C34 N4 -0.4(9) . . . . ? C33 C34 N4 C30 0.7(8) . . . . ? C33 C34 N4 Mn2 -177.4(4) . . . . ? C31 C30 N4 C34 -0.5(8) . . . . ? C29 C30 N4 C34 178.0(5) . . . . ? C31 C30 N4 Mn2 177.8(4) . . . . ? C29 C30 N4 Mn2 -3.7(6) . . . . ? O6 Mn2 N4 C34 2.6(5) . . . . ? N3 Mn2 N4 C34 -176.5(5) . . . . ? O4 Mn2 N4 C34 96.9(5) . . . . ? O7 Mn2 N4 C34 -87.2(5) . . . . ? Mn1 Mn2 N4 C34 61.4(6) . . . . ? O6 Mn2 N4 C30 -175.5(4) . . . . ? N3 Mn2 N4 C30 5.4(4) . . . . ? O4 Mn2 N4 C30 -81.2(4) . . . . ? O7 Mn2 N4 C30 94.6(4) . . . . ? Mn1 Mn2 N4 C30 -116.7(4) . . . . ? O14 Mn3 Mn4 O11 -134.9(3) . . . . ? N6 Mn3 Mn4 O11 52.0(3) . . . . ? N5 Mn3 Mn4 O11 168.0(5) . . . . ? O12 Mn3 Mn4 O11 129.6(3) . . . . ? O20 Mn3 Mn4 O11 -49.6(3) . . . . ? O11 Mn3 Mn4 O13 -128.7(3) . . . . ? O14 Mn3 Mn4 O13 96.46(17) . . . . ? N6 Mn3 Mn4 O13 -76.64(19) . . . . ? N5 Mn3 Mn4 O13 39.4(4) . . . . ? O12 Mn3 Mn4 O13 0.94(16) . . . . ? O20 Mn3 Mn4 O13 -178.24(17) . . . . ? O11 Mn3 Mn4 N8 46.4(3) . . . . ? O14 Mn3 Mn4 N8 -88.46(18) . . . . ? N6 Mn3 Mn4 N8 98.4(2) . . . . ? N5 Mn3 Mn4 N8 -145.5(4) . . . . ? O12 Mn3 Mn4 N8 176.01(17) . . . . ? O20 Mn3 Mn4 N8 -3.17(19) . . . . ? O11 Mn3 Mn4 N7 161.4(4) . . . . ? O14 Mn3 Mn4 N7 26.5(3) . . . . ? N6 Mn3 Mn4 N7 -146.6(3) . . . . ? N5 Mn3 Mn4 N7 -30.6(5) . . . . ? O12 Mn3 Mn4 N7 -69.0(3) . . . . ? O20 Mn3 Mn4 N7 111.8(3) . . . . ? O11 Mn3 Mn4 O15 137.1(3) . . . . ? O14 Mn3 Mn4 O15 2.23(17) . . . . ? N6 Mn3 Mn4 O15 -170.88(19) . . . . ? N5 Mn3 Mn4 O15 -54.8(4) . . . . ? O12 Mn3 Mn4 O15 -93.30(16) . . . . ? O20 Mn3 Mn4 O15 87.53(18) . . . . ? O11 Mn3 Mn4 O16 -47.7(3) . . . . ? O14 Mn3 Mn4 O16 177.37(16) . . . . ? N6 Mn3 Mn4 O16 4.27(19) . . . . ? N5 Mn3 Mn4 O16 120.3(4) . . . . ? O12 Mn3 Mn4 O16 81.85(16) . . . . ? O20 Mn3 Mn4 O16 -97.33(17) . . . . ? O13 Mn4 O11 Mn3 51.3(3) . . . . ? N8 Mn4 O11 Mn3 -138.3(2) . . . . ? O15 Mn4 O11 Mn3 -41.4(3) . . . . ? O16 Mn4 O11 Mn3 136.2(2) . . . . ? O14 Mn3 O11 Mn4 45.0(3) . . . . ? N6 Mn3 O11 Mn4 -132.8(3) . . . . ? O12 Mn3 O11 Mn4 -48.1(2) . . . . ? O20 Mn3 O11 Mn4 136.4(2) . . . . ? O11 Mn3 O12 C35 13.1(5) . . . . ? O14 Mn3 O12 C35 -86.9(4) . . . . ? N6 Mn3 O12 C35 105.6(5) . . . . ? N5 Mn3 O12 C35 -175.6(5) . . . . ? O20 Mn3 O12 C35 167.3(8) . . . . ? Mn4 Mn3 O12 C35 -8.5(4) . . . . ? O11 Mn4 O13 C35 -16.4(5) . . . . ? N8 Mn4 O13 C35 -156.1(6) . . . . ? N7 Mn4 O13 C35 162.2(5) . . . . ? O15 Mn4 O13 C35 80.3(4) . . . . ? O16 Mn4 O13 C35 -106.1(5) . . . . ? Mn3 Mn4 O13 C35 6.0(4) . . . . ? Mn3 O12 C35 O13 16.4(8) . . . . ? Mn3 O12 C35 C36 -165.3(4) . . . . ? Mn4 O13 C35 O12 -15.1(8) . . . . ? Mn4 O13 C35 C36 166.5(3) . . . . ? O12 C35 C36 C37 63.6(7) . . . . ? O13 C35 C36 C37 -117.9(6) . . . . ? O12 C35 C36 C41 -116.7(6) . . . . ? O13 C35 C36 C41 61.8(7) . . . . ? C41 C36 C37 C38 2.0(8) . . . . ? C35 C36 C37 C38 -178.4(5) . . . . ? C41 C36 C37 Cl4 -176.7(4) . . . . ? C35 C36 C37 Cl4 3.0(8) . . . . ? C36 C37 C38 C39 -0.8(9) . . . . ? Cl4 C37 C38 C39 177.9(5) . . . . ? C37 C38 C39 C40 -0.1(9) . . . . ? C38 C39 C40 C41 -0.3(9) . . . . ? C39 C40 C41 C36 1.5(9) . . . . ? C39 C40 C41 Cl4B -175.6(8) . . . . ? C37 C36 C41 C40 -2.3(8) . . . . ? C35 C36 C41 C40 178.0(5) . . . . ? C37 C36 C41 Cl4B 174.0(10) . . . . ? C35 C36 C41 Cl4B -5.7(13) . . . . ? O11 Mn3 O14 C42 -28.2(5) . . . . ? N6 Mn3 O14 C42 141.6(8) . . . . ? N5 Mn3 O14 C42 154.2(5) . . . . ? O12 Mn3 O14 C42 65.6(5) . . . . ? O20 Mn3 O14 C42 -124.4(5) . . . . ? Mn4 Mn3 O14 C42 -8.2(5) . . . . ? O11 Mn4 O15 C42 21.6(5) . . . . ? O13 Mn4 O15 C42 -77.7(5) . . . . ? N8 Mn4 O15 C42 114.8(5) . . . . ? N7 Mn4 O15 C42 -167.4(5) . . . . ? Mn3 Mn4 O15 C42 2.3(5) . . . . ? Mn4 O15 C42 O14 -8.8(9) . . . . ? Mn4 O15 C42 C43 172.7(4) . . . . ? Mn3 O14 C42 O15 13.0(9) . . . . ? Mn3 O14 C42 C43 -168.5(4) . . . . ? O15 C42 C43 C44 -63.6(8) . . . . ? O14 C42 C43 C44 117.8(6) . . . . ? O15 C42 C43 C48 113.6(7) . . . . ? O14 C42 C43 C48 -65.0(7) . . . . ? C48 C43 C44 C45 0.3(9) . . . . ? C42 C43 C44 C45 177.5(5) . . . . ? C48 C43 C44 Cl5 177.6(5) . . . . ? C42 C43 C44 Cl5 -5.2(8) . . . . ? C43 C44 C45 C46 -3.1(9) . . . . ? Cl5 C44 C45 C46 179.5(5) . . . . ? C44 C45 C46 C47 2.7(10) . . . . ? C45 C46 C47 C48 0.5(11) . . . . ? O14 Mn3 N5 C49 10.1(5) . . . . ? N6 Mn3 N5 C49 -172.7(5) . . . . ? O12 Mn3 N5 C49 102.6(5) . . . . ? O20 Mn3 N5 C49 -80.5(5) . . . . ? Mn4 Mn3 N5 C49 65.8(7) . . . . ? O14 Mn3 N5 C53 -171.6(4) . . . . ? N6 Mn3 N5 C53 5.6(4) . . . . ? O12 Mn3 N5 C53 -79.1(4) . . . . ? O20 Mn3 N5 C53 97.8(4) . . . . ? Mn4 Mn3 N5 C53 -115.9(4) . . . . ? C46 C47 C48 C43 -3.4(11) . . . . ? C44 C43 C48 C47 3.0(10) . . . . ? C42 C43 C48 C47 -174.3(6) . . . . ? C53 N5 C49 C50 0.2(9) . . . . ? Mn3 N5 C49 C50 178.4(5) . . . . ? N5 C49 C50 C51 0.6(10) . . . . ? C49 C50 C51 C52 -0.1(10) . . . . ? C50 C51 C52 C53 -1.2(10) . . . . ? C49 N5 C53 C52 -1.6(8) . . . . ? Mn3 N5 C53 C52 -179.9(4) . . . . ? C49 N5 C53 C54 176.2(5) . . . . ? Mn3 N5 C53 C54 -2.2(6) . . . . ? C51 C52 C53 N5 2.0(9) . . . . ? C51 C52 C53 C54 -175.5(6) . . . . ? N5 C53 C54 N6 -5.0(8) . . . . ? C52 C53 C54 N6 172.6(6) . . . . ? N5 C53 C54 C55 175.9(6) . . . . ? C52 C53 C54 C55 -6.5(10) . . . . ? N6 C54 C55 C56 -1.2(9) . . . . ? C53 C54 C55 C56 177.9(6) . . . . ? C54 C55 C56 C57 0.7(10) . . . . ? C55 C56 C57 C58 0.4(10) . . . . ? C56 C57 C58 N6 -1.0(10) . . . . ? C57 C58 N6 C54 0.5(9) . . . . ? C57 C58 N6 Mn3 171.4(5) . . . . ? C55 C54 N6 C58 0.7(9) . . . . ? C53 C54 N6 C58 -178.5(5) . . . . ? C55 C54 N6 Mn3 -171.1(5) . . . . ? C53 C54 N6 Mn3 9.8(7) . . . . ? O11 Mn3 N6 C58 3.2(5) . . . . ? O14 Mn3 N6 C58 -166.8(7) . . . . ? N5 Mn3 N6 C58 -179.7(5) . . . . ? O12 Mn3 N6 C58 -89.9(5) . . . . ? O20 Mn3 N6 C58 99.2(5) . . . . ? Mn4 Mn3 N6 C58 -18.9(5) . . . . ? O11 Mn3 N6 C54 174.6(4) . . . . ? O14 Mn3 N6 C54 4.6(11) . . . . ? N5 Mn3 N6 C54 -8.3(4) . . . . ? O12 Mn3 N6 C54 81.5(4) . . . . ? O20 Mn3 N6 C54 -89.4(4) . . . . ? Mn4 Mn3 N6 C54 152.5(4) . . . . ? O13 Mn4 N7 C59 -17.5(4) . . . . ? N8 Mn4 N7 C59 172.6(4) . . . . ? O15 Mn4 N7 C59 74.2(4) . . . . ? O16 Mn4 N7 C59 -102.4(4) . . . . ? Mn3 Mn4 N7 C59 50.6(6) . . . . ? O13 Mn4 N7 C63 171.6(4) . . . . ? N8 Mn4 N7 C63 1.7(4) . . . . ? O15 Mn4 N7 C63 -96.7(4) . . . . ? O16 Mn4 N7 C63 86.7(4) . . . . ? Mn3 Mn4 N7 C63 -120.4(4) . . . . ? C63 N7 C59 C60 -0.7(8) . . . . ? Mn4 N7 C59 C60 -171.1(4) . . . . ? N7 C59 C60 C61 -0.4(8) . . . . ? C59 C60 C61 C62 0.1(9) . . . . ? C60 C61 C62 C63 1.1(9) . . . . ? C59 N7 C63 C62 2.0(8) . . . . ? Mn4 N7 C63 C62 173.2(4) . . . . ? C59 N7 C63 C64 -175.6(5) . . . . ? Mn4 N7 C63 C64 -4.3(6) . . . . ? C61 C62 C63 N7 -2.2(8) . . . . ? C61 C62 C63 C64 175.1(5) . . . . ? N7 C63 C64 N8 5.5(7) . . . . ? C62 C63 C64 N8 -171.9(5) . . . . ? N7 C63 C64 C65 -176.6(5) . . . . ? C62 C63 C64 C65 6.0(9) . . . . ? N8 C64 C65 C66 1.2(8) . . . . ? C63 C64 C65 C66 -176.6(5) . . . . ? C64 C65 C66 C67 -0.2(9) . . . . ? C65 C66 C67 C68 -1.1(8) . . . . ? C66 C67 C68 N8 1.4(8) . . . . ? C67 C68 N8 C64 -0.5(8) . . . . ? C67 C68 N8 Mn4 -179.1(4) . . . . ? C65 C64 N8 C68 -0.8(8) . . . . ? C63 C64 N8 C68 177.1(5) . . . . ? C65 C64 N8 Mn4 177.9(4) . . . . ? C63 C64 N8 Mn4 -4.1(6) . . . . ? O11 Mn4 N8 C68 -2.8(4) . . . . ? O13 Mn4 N8 C68 137.5(6) . . . . ? N7 Mn4 N8 C68 -179.9(4) . . . . ? O15 Mn4 N8 C68 -99.5(4) . . . . ? O16 Mn4 N8 C68 87.5(4) . . . . ? Mn3 Mn4 N8 C68 -23.3(4) . . . . ? O11 Mn4 N8 C64 178.5(4) . . . . ? O13 Mn4 N8 C64 -41.2(9) . . . . ? N7 Mn4 N8 C64 1.5(4) . . . . ? O15 Mn4 N8 C64 81.9(4) . . . . ? O16 Mn4 N8 C64 -91.1(4) . . . . ? Mn3 Mn4 N8 C64 158.1(3) . . . . ? O19 Cl6 O16 Mn4 66.2(4) . . . . ? O18 Cl6 O16 Mn4 -173.2(3) . . . . ? O17 Cl6 O16 Mn4 -53.6(4) . . . . ? O11 Mn4 O16 Cl6 -158.0(4) . . . . ? O13 Mn4 O16 Cl6 -59.0(4) . . . . ? N8 Mn4 O16 Cl6 109.6(4) . . . . ? N7 Mn4 O16 Cl6 30.8(4) . . . . ? Mn3 Mn4 O16 Cl6 -137.1(4) . . . . ? # END of CIF #-------------------------------------- # Compound 3 #-------------------------------------- data_compound3 _database_code_depnum_ccdc_archive 'CCDC 832171' #TrackingRef '- compounds1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H24 Cl2 Mn2 N6 O11' _chemical_formula_weight 921.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2237 0.8587 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.849(7) _cell_length_b 25.673(6) _cell_length_c 12.600(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.432(3) _cell_angle_gamma 90.00 _cell_volume 10388(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1878 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 21.12 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 17089 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 22.92 _reflns_number_total 5510 _reflns_number_gt 3389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. The data were cut at 1 angstrom as above I/sigma(I) was < 2. All non-hydrogens were refined anisotropically. One of the nitrate ions was disordered over two positions of one of its O atom. Both nitrates were refined with displacement parameter restrains. Hydrogens were placed geometrically on their riding atoms. Only residual electron peaks at most corresponding to 1/4 of an O atom were found in the voids between the manganese complexes. These could not be modeled satisfactorily and the corresponding volume was taken into account with PLATON/SQUEEZE, that recovered a total of 536 electrons per cell, in two voids of 1730 cubic angstrom each. These figures would agree with about 30 diffuse water molecules per cell, e.g. 4 per formula unit. The treatment resulted in an improvement in R1 of ca. 5% and in wR2 of ca. 15%. ; _vrf_THETM01_compound3 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Crystals were poorly diffracting at high angles, and the data were cut at 1 angstrom as above the average I/sigma(I) was much below 2. This poor diffraction is likely related to large areas of the unit cell occupied by diffuse solvent molecules, as analyzed with PLATON/SQUEEZE. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.022 1730 263 ' ' 2 0.500 0.500 0.088 1730 263 ' ' _platon_squeeze_details ; ; _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^)+(0.0869P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5510 _refine_ls_number_parameters 541 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.31404(3) 0.21423(3) 0.37986(7) 0.0533(3) Uani 1 1 d . . . Mn2 Mn 0.38168(3) 0.12562(3) 0.46479(7) 0.0551(3) Uani 1 1 d . . . Cl1 Cl 0.21330(6) 0.09168(7) 0.21996(16) 0.0898(6) Uani 1 1 d . . . Cl2 Cl 0.35287(6) 0.09245(6) 0.78367(13) 0.0769(6) Uani 1 1 d . . . O1 O 0.29324(12) 0.14783(15) 0.2710(3) 0.0551(11) Uani 1 1 d . . . O2 O 0.34525(14) 0.08964(14) 0.3309(3) 0.0575(11) Uani 1 1 d . . . O3 O 0.29217(13) 0.18162(14) 0.4926(3) 0.0553(11) Uani 1 1 d . . . O4 O 0.33425(14) 0.11235(15) 0.5423(3) 0.0541(11) Uani 1 1 d . . . O5 O 0.36661(13) 0.19173(13) 0.4272(3) 0.0573(11) Uani 1 1 d . . . O6 O 0.32758(15) 0.28196(16) 0.4941(3) 0.0719(12) Uani 1 1 d U A . O7 O 0.37974(19) 0.3172(2) 0.4575(5) 0.1165(19) Uani 1 1 d U A . O8 O 0.3841(4) 0.3116(5) 0.6187(11) 0.108(4) Uani 0.50 1 d PU A 1 O8B O 0.3615(4) 0.3363(5) 0.6073(10) 0.107(4) Uani 0.50 1 d PU A 2 O9 O 0.43132(18) 0.1131(2) 0.3942(5) 0.1005(16) Uani 1 1 d U . . O10 O 0.48912(18) 0.1262(2) 0.3601(5) 0.1048(16) Uani 1 1 d U . . O11 O 0.45692(19) 0.1891(2) 0.4153(5) 0.1204(19) Uani 1 1 d U . . N1 N 0.3236(2) 0.25606(18) 0.2505(4) 0.0585(14) Uani 1 1 d . . . N2 N 0.25503(19) 0.24311(16) 0.3002(4) 0.0533(14) Uani 1 1 d . . . N3 N 0.41977(15) 0.14850(19) 0.6224(4) 0.0585(14) Uani 1 1 d . . . N4 N 0.40342(15) 0.05397(17) 0.5387(4) 0.0533(13) Uani 1 1 d . . . N5 N 0.3606(3) 0.3085(2) 0.5215(6) 0.0831(17) Uani 1 1 d U . . N6 N 0.4565(2) 0.1421(3) 0.3906(5) 0.0860(17) Uani 1 1 d U . . C1 C 0.3598(3) 0.2619(2) 0.2301(5) 0.073(2) Uani 1 1 d . . . H1A H 0.3841 0.2462 0.2793 0.087 Uiso 1 1 calc R . . C2 C 0.3629(3) 0.2911(3) 0.1363(6) 0.082(2) Uani 1 1 d . . . H2A H 0.3890 0.2956 0.1239 0.098 Uiso 1 1 calc R . . C3 C 0.3273(3) 0.3124(2) 0.0647(6) 0.079(2) Uani 1 1 d . . . H3A H 0.3288 0.3321 0.0023 0.095 Uiso 1 1 calc R . . C4 C 0.2887(3) 0.3056(2) 0.0814(5) 0.064(2) Uani 1 1 d . . . C5 C 0.2502(3) 0.3244(2) 0.0092(6) 0.076(2) Uani 1 1 d U . . H5A H 0.2497 0.3434 -0.0558 0.091 Uiso 1 1 calc R . . C6 C 0.2147(3) 0.3159(2) 0.0304(5) 0.072(2) Uani 1 1 d U . . H6A H 0.1892 0.3278 -0.0210 0.087 Uiso 1 1 calc R . . C7 C 0.2145(3) 0.2889(2) 0.1311(5) 0.0638(18) Uani 1 1 d . . . C8 C 0.1782(3) 0.2788(2) 0.1590(5) 0.071(2) Uani 1 1 d . . . H8A H 0.1519 0.2904 0.1116 0.085 Uiso 1 1 calc R . . C9 C 0.1813(2) 0.2516(2) 0.2571(5) 0.0643(18) Uani 1 1 d . . . H9A H 0.1572 0.2442 0.2776 0.077 Uiso 1 1 calc R . . C10 C 0.2204(2) 0.2356(2) 0.3242(5) 0.0563(17) Uani 1 1 d . . . H10A H 0.2222 0.2180 0.3920 0.068 Uiso 1 1 calc R . . C11 C 0.2526(2) 0.2707(2) 0.2029(5) 0.0549(17) Uani 1 1 d . . . C12 C 0.2896(3) 0.2776(2) 0.1781(5) 0.0517(16) Uani 1 1 d . . . C13 C 0.4264(2) 0.1964(3) 0.6612(6) 0.078(2) Uani 1 1 d . . . H13A H 0.4157 0.2248 0.6124 0.094 Uiso 1 1 calc R . . C14 C 0.4489(3) 0.2060(3) 0.7738(7) 0.102(3) Uani 1 1 d . . . H14A H 0.4537 0.2409 0.7992 0.122 Uiso 1 1 calc R . . C15 C 0.4640(2) 0.1667(3) 0.8469(6) 0.085(2) Uani 1 1 d . . . H15A H 0.4787 0.1738 0.9232 0.102 Uiso 1 1 calc R . . C16 C 0.4575(2) 0.1149(2) 0.8069(5) 0.0652(18) Uani 1 1 d . . . C17 C 0.4717(2) 0.0692(3) 0.8747(5) 0.0680(18) Uani 1 1 d . . . H17A H 0.4871 0.0733 0.9517 0.082 Uiso 1 1 calc R . . C18 C 0.4639(2) 0.0215(3) 0.8321(5) 0.0708(19) Uani 1 1 d . . . H18A H 0.4736 -0.0077 0.8794 0.085 Uiso 1 1 calc R . . C19 C 0.44066(19) 0.0132(2) 0.7143(5) 0.0595(17) Uani 1 1 d . . . C20 C 0.4316(2) -0.0360(2) 0.6636(5) 0.0661(19) Uani 1 1 d . . . H20A H 0.4412 -0.0669 0.7054 0.079 Uiso 1 1 calc R . . C21 C 0.4087(2) -0.0385(2) 0.5534(5) 0.0678(19) Uani 1 1 d . . . H21A H 0.4018 -0.0714 0.5180 0.081 Uiso 1 1 calc R . . C22 C 0.3954(2) 0.0064(2) 0.4932(5) 0.0589(17) Uani 1 1 d . . . H22A H 0.3799 0.0036 0.4161 0.071 Uiso 1 1 calc R . . C23 C 0.42629(18) 0.0572(2) 0.6478(5) 0.0517(16) Uani 1 1 d . . . C24 C 0.43519(19) 0.1084(2) 0.6934(5) 0.0547(16) Uani 1 1 d . . . C25 C 0.3092(2) 0.1041(2) 0.2677(5) 0.0529(16) Uani 1 1 d . . . C26 C 0.2867(2) 0.0658(2) 0.1807(5) 0.0535(16) Uani 1 1 d . . . C27 C 0.2444(3) 0.0598(2) 0.1505(5) 0.0636(18) Uani 1 1 d . . . C28 C 0.2232(3) 0.0265(3) 0.0633(6) 0.086(2) Uani 1 1 d . . . H28A H 0.1938 0.0227 0.0423 0.103 Uiso 1 1 calc R . . C29 C 0.2461(3) -0.0005(3) 0.0089(6) 0.081(2) Uani 1 1 d . . . H29A H 0.2322 -0.0229 -0.0513 0.098 Uiso 1 1 calc R . . C30 C 0.2879(3) 0.0041(2) 0.0392(5) 0.071(2) Uani 1 1 d . . . H30A H 0.3033 -0.0150 0.0009 0.085 Uiso 1 1 calc R . . C31 C 0.3080(2) 0.0367(2) 0.1263(5) 0.0610(18) Uani 1 1 d . . . H31A H 0.3375 0.0390 0.1492 0.073 Uiso 1 1 calc R . . C32 C 0.3049(2) 0.1401(2) 0.5491(4) 0.0507(16) Uani 1 1 d . . . C33 C 0.2813(2) 0.1231(2) 0.6227(5) 0.0529(17) Uani 1 1 d . . . C34 C 0.2996(2) 0.0978(2) 0.7270(5) 0.0603(18) Uani 1 1 d . . . C35 C 0.2752(3) 0.0791(2) 0.7891(6) 0.071(2) Uani 1 1 d . . . H35A H 0.2882 0.0626 0.8589 0.085 Uiso 1 1 calc R . . C36 C 0.2324(3) 0.0841(2) 0.7512(6) 0.075(2) Uani 1 1 d . . . H36A H 0.2162 0.0704 0.7940 0.090 Uiso 1 1 calc R . . C37 C 0.2131(2) 0.1091(2) 0.6505(6) 0.072(2) Uani 1 1 d . . . H37A H 0.1837 0.1131 0.6241 0.087 Uiso 1 1 calc R . . C38 C 0.2383(3) 0.1288(2) 0.5874(5) 0.0633(19) Uani 1 1 d . . . H38A H 0.2251 0.1463 0.5189 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0810(8) 0.0473(5) 0.0342(5) 0.0081(4) 0.0218(5) 0.0048(5) Mn2 0.0741(8) 0.0518(5) 0.0375(6) 0.0064(4) 0.0151(5) 0.0045(5) Cl1 0.0919(15) 0.0990(14) 0.0859(14) 0.0075(11) 0.0384(11) -0.0027(11) Cl2 0.1013(16) 0.0832(12) 0.0417(10) 0.0154(8) 0.0163(9) 0.0015(10) O1 0.077(3) 0.051(2) 0.037(2) 0.0011(18) 0.018(2) 0.006(2) O2 0.085(3) 0.054(2) 0.031(2) 0.0023(18) 0.014(2) 0.010(2) O3 0.082(3) 0.051(2) 0.036(2) 0.0122(19) 0.024(2) 0.003(2) O4 0.077(3) 0.047(2) 0.042(2) 0.0043(18) 0.024(2) 0.003(2) O5 0.082(3) 0.046(2) 0.046(2) 0.0108(18) 0.024(2) 0.009(2) O6 0.093(3) 0.061(3) 0.061(3) -0.005(2) 0.022(2) 0.006(2) O7 0.126(5) 0.129(4) 0.107(4) -0.032(4) 0.056(4) -0.032(3) O8 0.128(9) 0.092(8) 0.081(4) -0.003(7) 0.001(5) -0.017(6) O8B 0.155(11) 0.099(9) 0.060(6) -0.017(5) 0.026(6) -0.030(6) O9 0.112(4) 0.100(3) 0.095(4) 0.004(3) 0.041(3) -0.018(3) O10 0.109(4) 0.105(4) 0.103(4) 0.002(3) 0.038(3) -0.001(3) O11 0.149(5) 0.079(3) 0.131(5) -0.007(3) 0.041(4) 0.000(3) N1 0.080(5) 0.054(3) 0.047(3) 0.005(3) 0.028(3) 0.001(3) N2 0.090(5) 0.044(3) 0.030(3) -0.001(2) 0.023(3) 0.004(3) N3 0.071(4) 0.053(3) 0.045(3) 0.002(3) 0.009(3) -0.003(3) N4 0.068(4) 0.053(3) 0.040(3) 0.006(2) 0.018(3) 0.007(2) N5 0.120(5) 0.062(3) 0.063(3) -0.002(3) 0.022(3) -0.014(3) N6 0.110(5) 0.070(3) 0.076(4) 0.004(3) 0.027(4) -0.004(3) C1 0.102(7) 0.071(4) 0.047(4) 0.012(3) 0.026(4) 0.004(4) C2 0.118(7) 0.066(4) 0.073(5) 0.014(4) 0.046(5) -0.001(4) C3 0.141(8) 0.056(4) 0.046(5) 0.007(3) 0.038(5) -0.004(5) C4 0.117(7) 0.036(3) 0.045(5) -0.003(3) 0.037(5) -0.001(4) C5 0.138(7) 0.051(4) 0.040(4) 0.013(3) 0.029(5) 0.006(4) C6 0.125(7) 0.051(4) 0.034(4) 0.012(3) 0.014(4) 0.010(4) C7 0.088(6) 0.053(4) 0.046(4) -0.007(3) 0.016(4) 0.000(4) C8 0.102(7) 0.050(4) 0.049(5) -0.005(3) 0.007(4) 0.013(4) C9 0.079(6) 0.062(4) 0.049(4) -0.001(3) 0.016(4) 0.003(4) C10 0.076(6) 0.050(4) 0.040(4) 0.006(3) 0.015(4) 0.003(4) C11 0.083(6) 0.042(3) 0.036(4) -0.007(3) 0.015(4) 0.006(4) C12 0.085(6) 0.041(3) 0.031(4) -0.003(3) 0.021(4) 0.003(4) C13 0.089(6) 0.060(5) 0.068(5) 0.005(4) 0.000(4) -0.005(4) C14 0.117(7) 0.069(5) 0.092(7) -0.012(5) -0.006(5) -0.009(5) C15 0.088(6) 0.083(5) 0.061(5) 0.000(4) -0.009(4) 0.003(4) C16 0.075(5) 0.069(5) 0.045(4) 0.001(3) 0.010(4) -0.004(3) C17 0.074(5) 0.081(5) 0.042(4) -0.001(4) 0.009(3) 0.001(4) C18 0.082(5) 0.081(5) 0.049(5) 0.015(4) 0.021(4) 0.013(4) C19 0.067(5) 0.079(5) 0.032(4) 0.010(3) 0.014(3) 0.016(4) C20 0.096(6) 0.049(4) 0.054(5) 0.004(3) 0.025(4) 0.009(3) C21 0.100(6) 0.052(4) 0.050(5) -0.002(3) 0.022(4) 0.003(4) C22 0.085(5) 0.059(4) 0.033(4) 0.000(3) 0.018(3) 0.009(3) C23 0.057(4) 0.063(4) 0.031(4) 0.006(3) 0.007(3) 0.007(3) C24 0.061(4) 0.057(4) 0.041(4) 0.006(3) 0.009(3) -0.002(3) C25 0.078(5) 0.051(4) 0.028(4) 0.012(3) 0.016(4) 0.011(4) C26 0.078(6) 0.047(4) 0.036(4) 0.010(3) 0.018(4) 0.002(4) C27 0.095(6) 0.050(4) 0.046(4) 0.006(3) 0.023(4) 0.002(4) C28 0.114(7) 0.062(5) 0.071(5) 0.021(4) 0.012(5) -0.009(5) C29 0.132(9) 0.048(4) 0.049(5) 0.000(3) 0.008(5) -0.008(5) C30 0.118(7) 0.049(4) 0.043(5) 0.011(3) 0.022(5) 0.007(4) C31 0.097(6) 0.046(3) 0.033(4) 0.005(3) 0.012(4) 0.014(4) C32 0.082(5) 0.040(4) 0.028(3) -0.004(3) 0.014(3) -0.006(3) C33 0.084(6) 0.038(3) 0.043(4) 0.004(3) 0.029(4) 0.008(3) C34 0.094(6) 0.045(3) 0.048(4) -0.001(3) 0.030(4) -0.005(3) C35 0.122(7) 0.048(4) 0.053(4) 0.004(3) 0.043(5) -0.003(4) C36 0.116(7) 0.048(4) 0.082(6) 0.000(4) 0.065(5) -0.006(4) C37 0.094(6) 0.054(4) 0.082(5) 0.003(4) 0.046(5) 0.002(4) C38 0.102(7) 0.040(3) 0.061(4) 0.004(3) 0.045(5) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 1.785(4) . ? Mn1 O3 1.983(4) . ? Mn1 N1 2.061(5) . ? Mn1 N2 2.069(6) . ? Mn1 O1 2.161(4) . ? Mn1 O6 2.211(4) . ? Mn1 Mn2 3.1645(13) . ? Mn2 O5 1.792(3) . ? Mn2 O2 1.976(4) . ? Mn2 N3 2.081(5) . ? Mn2 N4 2.088(4) . ? Mn2 O4 2.154(4) . ? Mn2 O9 2.159(6) . ? Cl1 C27 1.770(7) . ? Cl2 C34 1.721(7) . ? O1 C25 1.252(6) . ? O2 C25 1.283(7) . ? O3 C32 1.279(6) . ? O4 C32 1.247(7) . ? O6 N5 1.260(7) . ? O7 N5 1.204(7) . ? O8 N5 1.234(13) . ? O8B N5 1.289(13) . ? O9 N6 1.145(7) . ? O10 N6 1.342(8) . ? O11 N6 1.243(7) . ? N1 C1 1.338(8) . ? N1 C12 1.340(7) . ? N2 C10 1.316(7) . ? N2 C11 1.396(7) . ? N3 C13 1.315(7) . ? N3 C24 1.355(7) . ? N4 C22 1.339(7) . ? N4 C23 1.350(7) . ? C1 C2 1.432(9) . ? C1 H1A 0.9500 . ? C2 C3 1.371(10) . ? C2 H2A 0.9500 . ? C3 C4 1.397(9) . ? C3 H3A 0.9500 . ? C4 C12 1.406(8) . ? C4 C5 1.418(9) . ? C5 C6 1.329(9) . ? C5 H5A 0.9500 . ? C6 C7 1.448(9) . ? C6 H6A 0.9500 . ? C7 C8 1.401(9) . ? C7 C11 1.402(9) . ? C8 C9 1.395(9) . ? C8 H8A 0.9500 . ? C9 C10 1.387(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.395(8) . ? C13 C14 1.404(9) . ? C13 H13A 0.9500 . ? C14 C15 1.352(9) . ? C14 H14A 0.9500 . ? C15 C16 1.415(9) . ? C15 H15A 0.9500 . ? C16 C24 1.400(8) . ? C16 C17 1.441(8) . ? C17 C18 1.329(8) . ? C17 H17A 0.9500 . ? C18 C19 1.460(8) . ? C18 H18A 0.9500 . ? C19 C23 1.400(8) . ? C19 C20 1.404(8) . ? C20 C21 1.361(8) . ? C20 H20A 0.9500 . ? C21 C22 1.376(8) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.428(8) . ? C25 C26 1.491(8) . ? C26 C31 1.363(8) . ? C26 C27 1.368(8) . ? C27 C28 1.398(9) . ? C28 C29 1.376(10) . ? C28 H28A 0.9500 . ? C29 C30 1.348(10) . ? C29 H29A 0.9500 . ? C30 C31 1.377(9) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.469(8) . ? C33 C38 1.389(8) . ? C33 C34 1.420(8) . ? C34 C35 1.393(9) . ? C35 C36 1.379(9) . ? C35 H35A 0.9500 . ? C36 C37 1.387(9) . ? C36 H36A 0.9500 . ? C37 C38 1.429(9) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? 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 O5 Mn1 O3 100.52(16) . . ? O5 Mn1 N1 92.5(2) . . ? O3 Mn1 N1 166.9(2) . . ? O5 Mn1 N2 170.39(19) . . ? O3 Mn1 N2 88.70(19) . . ? N1 Mn1 N2 78.3(2) . . ? O5 Mn1 O1 92.70(16) . . ? O3 Mn1 O1 90.07(15) . . ? N1 Mn1 O1 90.58(16) . . ? N2 Mn1 O1 84.49(16) . . ? O5 Mn1 O6 93.29(17) . . ? O3 Mn1 O6 85.01(16) . . ? N1 Mn1 O6 93.04(17) . . ? N2 Mn1 O6 90.22(17) . . ? O1 Mn1 O6 172.86(17) . . ? O5 Mn1 Mn2 27.86(11) . . ? O3 Mn1 Mn2 81.27(12) . . ? N1 Mn1 Mn2 111.38(17) . . ? N2 Mn1 Mn2 154.98(13) . . ? O1 Mn1 Mn2 72.74(11) . . ? O6 Mn1 Mn2 111.49(12) . . ? O5 Mn2 O2 99.70(17) . . ? O5 Mn2 N3 91.35(18) . . ? O2 Mn2 N3 167.87(17) . . ? O5 Mn2 N4 169.40(18) . . ? O2 Mn2 N4 90.32(18) . . ? N3 Mn2 N4 78.38(19) . . ? O5 Mn2 O4 94.53(17) . . ? O2 Mn2 O4 87.71(16) . . ? N3 Mn2 O4 86.42(17) . . ? N4 Mn2 O4 82.34(17) . . ? O5 Mn2 O9 103.0(2) . . ? O2 Mn2 O9 86.3(2) . . ? N3 Mn2 O9 96.2(2) . . ? N4 Mn2 O9 80.9(2) . . ? O4 Mn2 O9 162.16(18) . . ? O5 Mn2 Mn1 27.73(13) . . ? O2 Mn2 Mn1 81.83(12) . . ? N3 Mn2 Mn1 106.46(14) . . ? N4 Mn2 Mn1 154.10(14) . . ? O4 Mn2 Mn1 72.76(11) . . ? O9 Mn2 Mn1 122.81(15) . . ? C25 O1 Mn1 132.1(4) . . ? C25 O2 Mn2 127.5(4) . . ? C32 O3 Mn1 127.9(4) . . ? C32 O4 Mn2 131.7(4) . . ? Mn1 O5 Mn2 124.4(2) . . ? N5 O6 Mn1 125.9(5) . . ? N6 O9 Mn2 127.3(6) . . ? C1 N1 C12 117.6(6) . . ? C1 N1 Mn1 126.3(5) . . ? C12 N1 Mn1 116.0(5) . . ? C10 N2 C11 117.9(6) . . ? C10 N2 Mn1 129.0(4) . . ? C11 N2 Mn1 112.8(5) . . ? C13 N3 C24 118.6(5) . . ? C13 N3 Mn2 126.8(4) . . ? C24 N3 Mn2 114.1(4) . . ? C22 N4 C23 117.8(5) . . ? C22 N4 Mn2 128.1(4) . . ? C23 N4 Mn2 114.0(4) . . ? O7 N5 O8 109.7(11) . . ? O7 N5 O6 122.4(7) . . ? O8 N5 O6 123.0(9) . . ? O7 N5 O8B 125.8(9) . . ? O8 N5 O8B 45.2(7) . . ? O6 N5 O8B 108.2(9) . . ? O9 N6 O11 124.7(9) . . ? O9 N6 O10 120.2(7) . . ? O11 N6 O10 115.0(7) . . ? N1 C1 C2 121.9(7) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 118.2(8) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 121.4(7) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C3 C4 C12 115.3(7) . . ? C3 C4 C5 125.1(7) . . ? C12 C4 C5 119.5(8) . . ? C6 C5 C4 121.5(7) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C7 120.6(7) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C8 C7 C11 118.5(6) . . ? C8 C7 C6 123.7(7) . . ? C11 C7 C6 117.8(7) . . ? C9 C8 C7 119.2(7) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C10 C9 C8 118.6(7) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? N2 C10 C9 124.2(6) . . ? N2 C10 H10A 117.9 . . ? C9 C10 H10A 117.9 . . ? C12 C11 N2 117.0(6) . . ? C12 C11 C7 121.5(6) . . ? N2 C11 C7 121.5(7) . . ? N1 C12 C11 115.6(6) . . ? N1 C12 C4 125.5(7) . . ? C11 C12 C4 118.9(7) . . ? N3 C13 C14 120.9(6) . . ? N3 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C15 C14 C13 121.7(7) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C14 C15 C16 118.4(6) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? C24 C16 C15 116.6(6) . . ? C24 C16 C17 118.7(6) . . ? C15 C16 C17 124.7(6) . . ? C18 C17 C16 121.5(6) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 121.4(6) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C23 C19 C20 118.0(5) . . ? C23 C19 C18 117.6(6) . . ? C20 C19 C18 124.4(6) . . ? C21 C20 C19 118.6(6) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C20 C21 C22 120.3(6) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? N4 C22 C21 122.8(5) . . ? N4 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? N4 C23 C19 122.5(5) . . ? N4 C23 C24 116.6(5) . . ? C19 C23 C24 120.9(5) . . ? N3 C24 C16 123.8(5) . . ? N3 C24 C23 116.4(5) . . ? C16 C24 C23 119.8(5) . . ? O1 C25 O2 125.1(6) . . ? O1 C25 C26 119.4(6) . . ? O2 C25 C26 115.4(6) . . ? C31 C26 C27 118.0(6) . . ? C31 C26 C25 120.2(7) . . ? C27 C26 C25 121.7(6) . . ? C26 C27 C28 121.4(7) . . ? C26 C27 Cl1 123.0(5) . . ? C28 C27 Cl1 115.6(7) . . ? C29 C28 C27 117.9(8) . . ? C29 C28 H28A 121.0 . . ? C27 C28 H28A 121.0 . . ? C30 C29 C28 121.5(7) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 119.2(7) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C26 C31 C30 121.9(7) . . ? C26 C31 H31A 119.0 . . ? C30 C31 H31A 119.0 . . ? O4 C32 O3 125.0(6) . . ? O4 C32 C33 118.6(5) . . ? O3 C32 C33 116.3(6) . . ? C38 C33 C34 116.9(6) . . ? C38 C33 C32 119.4(6) . . ? C34 C33 C32 123.5(7) . . ? C35 C34 C33 120.9(7) . . ? C35 C34 Cl2 118.0(6) . . ? C33 C34 Cl2 121.0(5) . . ? C36 C35 C34 121.2(7) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C35 C36 C37 120.0(7) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 118.7(7) . . ? C36 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? C33 C38 C37 122.3(6) . . ? C33 C38 H38A 118.9 . . ? C37 C38 H38A 118.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.92 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.242 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.059